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Report 149 ISSN: 0889-3144

Analysis of Plastics

Martin J. Forrest

Volume 13, Number 5, 2002

Rapra Review Reports


Expert overviews covering the science and
technology of rubber and plastics
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Item 1
Source of
Macromolecules
original article
33, No.6, 21st March 2000, p.2171-83
Title EFFECT OF THERMAL HISTORY ON THE RHEOLOGICAL
BEHAVIOR OF THERMOPLASTIC POLYURETHANES
Authors and
Pil Joong Yoon; Chang Dae Han affiliation
Akron,University
The effect of thermal history on the rheological behaviour of ester- and
ether-based commercial thermoplastic PUs (Estane 5701, 5707 and 5714
from B.F.Goodrich) was investigated. It was found that the injection
moulding temp. used for specimen preparation had a marked effect on the
variations of dynamic storage and loss moduli of specimens with time
observed during isothermal annealing. Analysis of FTIR spectra indicated
that variations in hydrogen bonding with time during isothermal annealing Abstract
very much resembled variations of dynamic storage modulus with time
during isothermal annealing. Isochronal dynamic temp. sweep experiments
indicated that the thermoplastic PUs exhibited a hysteresis effect in the
heating and cooling processes. It was concluded that the microphase
separation transition or order-disorder transition in thermoplastic PUs could
not be determined from the isochronal dynamic temp. sweep experiment.
The plots of log dynamic storage modulus versus log loss modulus varied
with temp. over the entire range of temps. (110-190C) investigated. 57 refs. Companies or
GOODRICH B.F. organisations
Location USA mentioned
Accession no.771897

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Report 5 CAD/CAM in the Polymer Industry, N.W. Sandland Report 39 Polymers in Chemically Resistant Applications,
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Report 19 Recycling and Disposal of Plastics Packaging,
R.C. Fox, Plas/Tech Ltd. Report 51 Biomedical Applications of Polymers, C.G. Gebelein,
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H. Hardy, Chronos Richardson Ltd.
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Plessey Research (Caswell) Ltd.
Report 23 Offshore Applications of Polymers, J.W.Brockbank, Report 54 Health and Safety in the Rubber Industry, A.R. Nutt,
Avon Industrial Polymers Ltd. Arnold Nutt & Co. and J. Wade.
Report 24 Recent Developments in Materials for Food Report 55 Computer Modelling of Polymer Processing,
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Industriforskning, Norway.
Volume 3 Report 56 Plastics in High Temperature Applications,
J. Maxwell, Consultant.
Report 25 Foams and Blowing Agents, J.M. Methven, Cellcom Report 57 Joining of Plastics, K.W. Allen, City University.
Technology Associates.
Report 58 Physical Testing of Rubber, R.P. Brown, Rapra
Report 26 Polymers and Structural Composites in Civil
Technology Ltd.
Engineering, L. Hollaway, University of Surrey.
Report 59 Polyimides - Materials, Processing and Applications,
Report 27 Injection Moulding of Rubber, M.A. Wheelans,
A.J. Kirby, Du Pont (U.K.) Ltd.
Consultant.
Report 28 Adhesives for Structural and Engineering Report 60 Physical Testing of Thermoplastics, S.W. Hawley,
Applications, C. O’Reilly, Loctite (Ireland) Ltd. Rapra Technology Ltd.
Report 29 Polymers in Marine Applications, C.F.Britton,
Corrosion Monitoring Consultancy. Volume 6
Report 30 Non-destructive Testing of Polymers, W.N. Reynolds, Report 61 Food Contact Polymeric Materials, J.A. Sidwell,
National NDT Centre, Harwell. Rapra Technology Ltd.
Report 31 Silicone Rubbers, B.R. Trego and H.W.Winnan, Report 62 Coextrusion, D. Djordjevic, Klöckner ER-WE-PA GmbH.
Dow Corning Ltd.
Report 63 Conductive Polymers II, R.H. Friend, University of
Report 32 Fluoroelastomers - Properties and Applications, Cambridge, Cavendish Laboratory.
D. Cook and M. Lynn, 3M United Kingdom Plc and
3M Belgium SA. Report 64 Designing with Plastics, P.R. Lewis, The Open University.
Report 33 Polyamides, R.S. Williams and T. Daniels, Report 65 Decorating and Coating of Plastics, P.J. Robinson,
T & N Technology Ltd. and BIP Chemicals Ltd. International Automotive Design.
Report 34 Extrusion of Rubber, J.G.A. Lovegrove, Nova Report 66 Reinforced Thermoplastics - Composition, Processing
Petrochemicals Inc. and Applications, P.G. Kelleher, New Jersey Polymer
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Report 35 Polymers in Household Electrical Goods, D.Alvey,
Hotpoint Ltd. Report 67 Plastics in Thermal and Acoustic Building Insulation,
Report 36 Developments in Additives to Meet Health and V.L. Kefford, MRM Engineering Consultancy.
Environmental Concerns, M.J. Forrest, Rapra Report 68 Cure Assessment by Physical and Chemical
Technology Ltd. Techniques, B.G. Willoughby, Rapra Technology Ltd.
Report 69 Toxicity of Plastics and Rubber in Fire, P.J. Fardell, Report 94 Compressive Behaviour of Composites,
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and Medicine.
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M.E. Adams, D.J. Buckley, R.E. Colborn, W.P. England Report 95 Thermal Analysis of Polymers, M. P. Sepe, Dickten &
and D.N. Schissel, General Electric Corporate Research Masch Manufacturing Co.
and Development Center. Report 96 Polymeric Seals and Sealing Technology, J.A. Hickman,
Report 71 Rotational Moulding, R.J. Crawford, The Queen’s St Clair (Polymers) Ltd.
University of Belfast.
Report 72 Advances in Injection Moulding, C.A. Maier,
Econology Ltd.
Volume 9
Report 97 Rubber Compounding Ingredients - Need, Theory
and Innovation, Part II: Processing, Bonding, Fire
Volume 7 Retardants, C. Hepburn, University of Ulster.
Report 98 Advances in Biodegradable Polymers, G.F. Moore &
Report 73 Reactive Processing of Polymers, M.W.R. Brown,
S.M. Saunders, Rapra Technology Ltd.
P.D. Coates and A.F. Johnson, IRC in Polymer Science
and Technology, University of Bradford. Report 99 Recycling of Rubber, H.J. Manuel and W. Dierkes,
Vredestein Rubber Recycling B.V.
Report 74 Speciality Rubbers, J.A. Brydson.
Report 100 Photoinitiated Polymerisation - Theory and
Report 75 Plastics and the Environment, I. Boustead, Boustead Applications, J.P. Fouassier, Ecole Nationale Supérieure
Consulting Ltd. de Chimie, Mulhouse.
Report 76 Polymeric Precursors for Ceramic Materials, Report 101 Solvent-Free Adhesives, T.E. Rolando, H.B. Fuller
R.C.P. Cubbon. Company.
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Goodyear Technical Center. Technology Ltd.
Report 78 PVC - Compounds, Processing and Applications, Report 103 Gas Assisted Moulding, T.C. Pearson, Gas Injection Ltd.
J.Leadbitter, J.A. Day, J.L. Ryan, Hydro Polymers Ltd. Report 104 Plastics Profile Extrusion, R.J. Kent, Tangram
Report 79 Rubber Compounding Ingredients - Need, Theory Technology Ltd.
and Innovation, Part I: Vulcanising Systems, Report 105 Rubber Extrusion Theory and Development,
Antidegradants and Particulate Fillers for General B.G. Crowther.
Purpose Rubbers, C. Hepburn, University of Ulster.
Report 106 Properties and Applications of Elastomeric
Report 80 Anti-Corrosion Polymers: PEEK, PEKK and Other Polysulfides, T.C.P. Lee, Oxford Brookes University.
Polyaryls, G. Pritchard, Kingston University.
Report 107 High Performance Polymer Fibres, P.R. Lewis,
Report 81 Thermoplastic Elastomers - Properties and Applications, The Open University.
J.A. Brydson. Report 108 Chemical Characterisation of Polyurethanes,
Report 82 Advances in Blow Moulding Process Optimization, M.J. Forrest, Rapra Technology Ltd.
Andres Garcia-Rejon,Industrial Materials Institute,
National Research Council Canada.
Report 83 Molecular Weight Characterisation of Synthetic
Volume 10
Polymers, S.R. Holding and E. Meehan, Rapra Report 109 Rubber Injection Moulding - A Practical Guide,
Technology Ltd. and Polymer Laboratories Ltd. J.A. Lindsay.
Report 84 Rheology and its Role in Plastics Processing, Report 110 Long-Term and Accelerated Ageing Tests on Rubbers,
P. Prentice, The Nottingham Trent University. R.P. Brown, M.J. Forrest and G. Soulagnet,
Rapra Technology Ltd.
Report 111 Polymer Product Failure, P.R. Lewis,
Volume 8 The Open University.
Report 85 Ring Opening Polymerisation, N. Spassky, Université Report 112 Polystyrene - Synthesis, Production and Applications,
Pierre et Marie Curie. J.R. Wünsch, BASF AG.
Report 86 High Performance Engineering Plastics, Report 113 Rubber-Modified Thermoplastics, H. Keskkula,
D.J. Kemmish, Victrex Ltd. University of Texas at Austin.

Report 87 Rubber to Metal Bonding, B.G. Crowther, Rapra Report 114 Developments in Polyacetylene - Nanopolyacetylene,
Technology Ltd. V.M. Kobryanskii, Russian Academy of Sciences.

Report 88 Plasticisers - Selection, Applications and Implications, Report 115 Metallocene-Catalysed Polymerisation, W. Kaminsky,
A.S. Wilson. University of Hamburg.
Report 116 Compounding in Co-rotating Twin-Screw Extruders,
Report 89 Polymer Membranes - Materials, Structures and
Y. Wang, Tunghai University.
Separation Performance, T. deV. Naylor, The Smart
Chemical Company. Report 117 Rapid Prototyping, Tooling and Manufacturing,
R.J.M. Hague and P.E. Reeves, Edward Mackenzie
Report 90 Rubber Mixing, P.R. Wood. Consulting.
Report 91 Recent Developments in Epoxy Resins, I. Hamerton, Report 118 Liquid Crystal Polymers - Synthesis, Properties and
University of Surrey. Applications, D. Coates, CRL Ltd.
Report 92 Continuous Vulcanisation of Elastomer Profiles, Report 119 Rubbers in Contact with Food, M.J. Forrest and
A. Hill, Meteor Gummiwerke. J.A. Sidwell, Rapra Technology Ltd.
Report 93 Advances in Thermoforming, J.L. Throne, Sherwood Report 120 Electronics Applications of Polymers II, M.T. Goosey,
Technologies Inc. Shipley Ronal.
Volume 11
Report 121 Polyamides as Engineering Thermoplastic Materials,
I.B. Page, BIP Ltd.

Report 122 Flexible Packaging - Adhesives, Coatings and


Processes, T.E. Rolando, H.B. Fuller Company.

Report 123 Polymer Blends, L.A. Utracki, National Research


Council Canada.

Report 124 Sorting of Waste Plastics for Recycling, R.D. Pascoe,


University of Exeter.

Report 125 Structural Studies of Polymers by Solution NMR,


H.N. Cheng, Hercules Incorporated.
Report 126 Composites for Automotive Applications, C.D. Rudd,
University of Nottingham.
Report 127 Polymers in Medical Applications, B.J. Lambert and
F.-W. Tang, Guidant Corp., and W.J. Rogers, Consultant.
Report 128 Solid State NMR of Polymers, P.A. Mirau,
Lucent Technologies.
Report 129 Failure of Polymer Products Due to Photo-oxidation,
D.C. Wright.
Report 130 Failure of Polymer Products Due to Chemical Attack,
D.C. Wright.
Report 131 Failure of Polymer Products Due to Thermo-oxidation,
D.C. Wright.
Report 132 Stabilisers for Polyolefins, C. Kröhnke and F. Werner,
Clariant Huningue SA.

Volume 12
Report 133 Advances in Automation for Plastics Injection
Moulding, J. Mallon, Yushin Inc.
Report 134 Infrared and Raman Spectroscopy of Polymers,
J.L. Koenig, Case Western Reserve University.
Report 135 Polymers in Sport and Leisure, R.P. Brown.
Report 136 Radiation Curing, R.S. Davidson, DavRad Services.
Report 137 Silicone Elastomers, P. Jerschow, Wacker-Chemie GmbH.
Report 138 Health and Safety in the Rubber Industry, N. Chaiear,
Khon Kaen University.
Report 139 Rubber Analysis - Polymers, Compounds and
Products, M.J. Forrest, Rapra Technology Ltd.
Report 140 Tyre Compounding for Improved Performance,
M.S. Evans, Kumho European Technical Centre.
Report 141 Particulate Fillers for Polymers, Professor R.N.
Rothon, Rothon Consultants and Manchester
Metropolitan University.
Report 142 Blowing Agents for Polyurethane Foams, S.N. Singh,
Huntsman Polyurethanes.
Report 143 Adhesion and Bonding to Polyolefins, D.M. Brewis
and I. Mathieson, Institute of Surface Science &
Technology, Loughborough University.
Report 144 Rubber Curing Systems, R.N. Datta, Flexsys BV.

Volume 13
Report 145 Multi-Material Injection Moulding, V. Goodship and
J.C. Love, The University of Warwick.
Report 146 In-Mould Decoration of Plastics, J.C. Love and
V. Goodship, The University of Warwick
Report 147 Rubber Product Failure, Roger P. Brown
Report 148 Plastics Waste – Feedstock Recycling, Chemical
Recycling and Incineration, A. Tukker, TNO
Analysis of Plastics

Martin J. Forrest
(Rapra Technology Limited)

ISBN 1-85957-333-9
Analysis of Plastics

Contents
1. Introduction .............................................................................................................................................. 3
2. Analytical Techniques ............................................................................................................................. 3
2.1 Wet Chemistry Techniques ............................................................................................................. 3
2.2 Spectroscopic Techniques ............................................................................................................... 4
2.2.1 Infrared Spectroscopy (IR) ................................................................................................. 4
2.2.2 Ultraviolet Light Spectroscopy (UV) ................................................................................. 4
2.2.3 Nuclear Magnetic Resonance Spectroscopy (NMR) ......................................................... 4
2.2.4 Atomic Absorption Spectroscopy (AAS) ........................................................................... 4
2.2.5 X-Ray Fluorescence Spectroscopy (XRF) ......................................................................... 5
2.2.6 Raman Spectroscopy .......................................................................................................... 5
2.3 Chromatographic Techniques ......................................................................................................... 5
2.3.1 Gas Chromatography-Mass Spectrometry (GC-MS) ......................................................... 5
2.3.2 Gas Chromatography (GC) ................................................................................................ 6
2.3.3 High Performance Liquid Chromatography (HPLC) ......................................................... 6
2.3.4 Liquid Chromatography-Mass Spectroscopy (LC-MS) ..................................................... 6
2.3.5 Gel Permeation Chromatography (GPC) ........................................................................... 6
2.3.6 Thin Layer Chromatography (TLC) ................................................................................... 7
2.4 Thermal Techniques ........................................................................................................................ 7
2.4.1 Differential Scanning Calorimetry (DSC) ......................................................................... 7
2.4.2 Dynamic Mechnanical Thermal Analysis (DMTA) ........................................................... 8
2.4.3 Thermogravimetric Analysis (TGA) .................................................................................. 9
2.5 Elemental Techniques ................................................................................................................... 12
2.6 Microscopy Techniques ................................................................................................................ 12
2.7 Miscellaneous Techniques ............................................................................................................ 12
3. Determination of Molecular Weight and Microstructure of Plastic Polymers ................................ 12
3.1 Determination of Molecular Weight ............................................................................................. 12
3.1.1 Gel Permeation Chromatography (GPC) ......................................................................... 13
3.1.2 Viscosity ........................................................................................................................... 14
3.1.3 Osmometry ....................................................................................................................... 14
3.1.4 Light Scattering ................................................................................................................ 14
3.1.5 Other Methods .................................................................................................................. 15
3.2 Monomer Types and Microstructure ............................................................................................ 15
4. Determination of Polymer Type ........................................................................................................... 15
5. Determination of the Plasticiser and Filler in a Plastic Compound ................................................. 19
5.1 Determination of Plasticiser ......................................................................................................... 19
5.2 Determination of Fillers ................................................................................................................ 19
5.2.1 Particulate Fillers .............................................................................................................. 19
5.2.2 Fibrous Fillers ................................................................................................................... 20
6. Determination of Stabilisers in a Plastics Compound ....................................................................... 21
6.1 UV Stabilisers ............................................................................................................................... 21
6.2 Antioxidants .................................................................................................................................. 22

1
Analysis of Plastics

7. Determination of Functional Additives ............................................................................................... 24


7.1 Process Aids and Lubricants ......................................................................................................... 24
7.2 Slip Additives ................................................................................................................................ 25
7.3 Pigments ........................................................................................................................................ 25
7.4 Antistatic Agents ........................................................................................................................... 25
7.5 Crosslinking Agents and Co-Agents............................................................................................. 26
7.6 Blowing Agents............................................................................................................................. 27
7.7 Flame Retardants .......................................................................................................................... 28
7.8 Impact Modifiers........................................................................................................................... 28
8. Analysis of Plastics for Food Contact Use ........................................................................................... 28
8.1 Global Migration Tests ................................................................................................................. 29
8.2 Specific migration and residual monomer tests............................................................................ 30
9. Determination of Stabilisers in PVC ................................................................................................... 31
10. Analysis of Plastic Laminates and Fibres ............................................................................................ 32
11. Surface Analysis of Plastics ................................................................................................................... 34
11.1 X-Ray Photoelectron Spectroscopy (XPS) ................................................................................... 34
11.2 Laser Induced Mass Analysis (LIMA) ......................................................................................... 34
11.3 Secondary Ion Mass Spectroscopy (SIMS) .................................................................................. 36
12. Failure Diagnosis ................................................................................................................................... 36
12.1 Common Compositional Problems ............................................................................................... 36
12.2 Environmental Stress Cracking .................................................................................................... 37
12.3 Contamination Problems .............................................................................................................. 37
12.4 Odour and Emissions Problems .................................................................................................... 37
13. Conclusions ............................................................................................................................................. 38
Additional References ................................................................................................................................... 39
Appendix 1. Solubility Parameters of Plastics, Plasticisers and Typical Solvents .................................. 41
Appendix 2. Specific Gravities of Plastics and Compound Ingredients .................................................. 43
Abbreviations and Acronyms ....................................................................................................................... 45
Abstracts from the Polymer Library Database .......................................................................................... 47
Subject Index ............................................................................................................................................... 133

The views and opinions expressed by authors in Rapra Review Reports do not necessarily reflect those of
Rapra Technology Limited or the editor. The series is published on the basis that no responsibility or
liability of any nature shall attach to Rapra Technology Limited arising out of or in connection with any
utilisation in any form of any material contained therein.

2
Analysis of Plastics

1 Introduction efficiently and obtain better results. To assist in the


acquisition of this knowledge opportunities have been
Plastics present chemical analysts with one of their most taken within the text to not only detail the analytical
difficult, but satisfying, challenges. In order to obtain methods, but provide examples of the species that they
useful products that perform under a variety of may be used to detect and quantify. In other words, in
demanding conditions, the plastic matrix can be tailor order to have a full understanding of the principles
made by the bringing together of a wide range of behind and surrounding the analytical methods and
polymers and additives. There is a very wide range of approaches it is vital to have an understanding of plastic
polymer types available and in some cases they are technology itself.
blended together. The technology of plastics is therefore
a mature one, allowing fine tuning of a compound to fit Relevant books and academic papers are cited
a number of design criteria and product requirements. throughout the review, but there are also a number of
general texts which will provide useful further reading
The choice of materials available means that plastics (79, 199, 315, 377, 387, 398, a.1-a7).
can be used in many applications, ranging from
replacement windows to packaging materials, and The appendices provide useful additional information.
from mundane products such as disposable cutlery to Appendix 1 gives solubility parameters of a range of
highly specialised components in electrical and materials. Appendix 2 lists the specific gravities of a
aerospace products. range of plastics and compounding ingredients.

The plastics analyst has therefore to bear in mind the


possible complexity of the system that confronts him
and the potential interferences that may be brought
into play. When reverse engineering a plastic 2 Analytical Techniques
compound a considerable number of elemental,
spectroscopic, chromatographic and thermal 2.1 Wet Chemistry Techniques
techniques have to be used in an integrated and
structured approach in order to accumulate and cross Before the advent of modern instrumental techniques,
check the data necessary for an accurate result. With plastic analysis relied on a sequence of wet chemistry
sufficient experience and access to the necessary reactions to determine information such as the generic
instrumental techniques, it should be possible for the polymer type of a material.
analyst to successfully elucidate a formulation. The
determination of the particular ‘grade’ of plastic,
The amount of wet chemistry carried out in the modern
although a consistent request, is however rarely
polymer analysis laboratory in the 21st Century is
possible. This is mainly due to the fact that a number
minimal. There are some tests which can still be
of manufacturers produce very similar, if not identical,
grouped under this heading, although even some of
products or that the material has been specially
these can employ an instrumental technique to provide
compounded for a particular purpose. Commercial
the final answer.
confidentiality can also restrict the ability to use the
analytical data to identify a particular manufacturer’s
product as a significant amount of compositional One such method is the oxygen flask combustion
information may not be disclosed. method, which can be used on PVC products to
determine the amount of PVC in the formulation by
The objective of this review is to present, as fully as is quantifying the chlorine present.
possible within this format, an introduction to the
techniques and methods that are used to characterise The oxygen flask method (ISO 6528.1-1992 and BS
and carry out quality control work on plastics; to 7164 Section 23.1- 1993) uses an initial burn in oxygen
investigate the failure of plastic products; and to (although the sample is trapped between two platinum
deformulate plastic compounds. gauge ‘flags’) and trapping of the volatile products in
an absorbing solution comprising 1-5 ml of 0.05M
With respect to the last category, the analyst’s job when potassium hydroxide, 0.2 ml of 30% hydrogen peroxide
characterising ‘unknowns’ is always made much easier and 10 ml of distilled water. Once the volatiles have
if at least some information is available on the sample been trapped there is a choice of analytical method. A
and the types of species that may be present in it. Armed titration can be performed, or ion chromatography can
with this knowledge they can work much more be used to quantify the chloride ion.

3
Analysis of Plastics

2.2 Spectroscopic Techniques analysis of plastics. It is used in the qualitative and


quantitative analysis of additives, particularly
2.2.1 Infrared Spectroscopy (IR) antioxidants and UV stabilisers.

Infrared spectroscopy (IR) is used extensively in the


analysis of plastics. It is a very good, relatively quick 2.2.3 Nuclear Magnetic Resonance Spectroscopy
technique for the determination of the polymer present (NMR)
in a plastic product. Unlike rubbers, where the majority
of compounds contain additives such as carbon black NMR is a powerful tool for the determination of
and plasticisers that can interfere with the infrared data polymer structure. It is at its most sensitive when used
obtained, it is normally possible to record infrared spectra on analytes in solution. Table 1 gives examples of
directly from the plastic sample using either a surface solvents used for NMR. Amorphous plastics, such as
technique (e.g., attenuated total reflectance (ATR) polystyrene can be dissolved in deuterated chloroform,
spectroscopy) or in transmission through the sample whereas for the less soluble semi-crystalline plastics
from a film produced by pressing a specimen above its (e.g., PET) solvents such as trichloroacetic acid have
glass transition or melting point. to be used. Of the conventional instruments, both proton
and carbon 13 instruments have been used in plastics
Some plasticised plastics products (e.g., PVC or nylon analysis. Combinations of two solvents can be used to
11) will need to be extracted with a solvent (e.g., achieve a good degree of solubility and elevated
methanol) first to remove the plasticiser. Products that temperatures (e.g., 70 °C) are also common. The proton
are filled (e.g., polypropylene/talc kettle bodies) will NMR solvents can be used for carbon 13 experiments,
require a pyrolysis technique where a pyrolysis but the reverse is rarely the case.
condensates infrared library, such as the one published
by Rapra Technology, needs to be available. Techniques are available for work on a specific plastic
type, e.g., in the analysis of polyvinylidene fluoride,
It is also possible with amorphous plastics that are soluble fluorine 19 NMR can be used. In this case a solvent
in conventional solvents (e.g., chloroform) at room such as dimethylformamide is employed.
temperature to record infrared spectra from films cast
from solution. This approach has the drawback that all The 13 C NMR spectrum for a polypropylene-
the solvent needs to be removed from the film if polyethylene copolymer is shown in Figure 1. The
interference bands are to be avoided. spectrum was obtained at 90 °C in a solution of ortho-
dichlorobenzene. The major peaks at 21, 27 and 46
Analysis of the solvent extract obtained to prepare the ppm are due to the polypropylene, with the other, minor
plastic sample for an IR technique can be used to identify peaks being due to polyethylene.
the plasticiser present in a compound. IR analysis of an
ash of the compound obtained by heating at 550 °C can
help to identify inorganic fillers. IR can also be used to 2.2.4 Atomic Absorption Spectroscopy (AAS)
identify specialist additives such as fire retardants.
This technique, and the related inductively coupled
plasma (ICP), are used where it is necessary to quantify
2.2.2 Ultraviolet Light Spectroscopy (UV) metals in a plastic compound. Although not often
required it can be of use in the analysis of flame
Although not as universally used as IR, UV is another retardant systems, where additives such as antimony
spectroscopic technique which has a role to play in the trioxide and zinc borate have been used.

Table 1 Examples of solvents used in NMR work on plastics


Proton NMR Carbon 13 NMR
Deuterated chloroform Orthodichlorobenzene
Trifluoroacetic acid Trichlorobenzene
Deuterated benzene Aliphatic hydrocarbons, e.g., heptane
1,1,2,2-Tetrachloro-deuterated ethane

4
Analysis of Plastics

Figure 1
13C NMR spectrum of polypropylene-polyethylene copolymer

2.2.5 X-Ray Fluorescence Spectroscopy (XRF) have led to the development of the Raman microscope -
an instrument analogous to the IR microscope.
This technique is very useful for obtaining semi-
quantitative elemental data from plastic compounds and This has enabled Raman spectroscopy to be used
their ashes. Among other things, it helps to identify routinely for the identification of polymer types and
inorganic fillers and pigments in samples. The the analysis of contaminants within polymer samples.
technique is usually used in conjunction with IR.

When it comes to analysing small samples, sample


2.3 Chromatographic Techniques
surfaces or contaminants in samples, the scanning
electron microscope (SEM)/XRF combination
(sometimes referred to as energy dispersive analysis 2.3.1 Gas Chromatography-Mass Spectrometry
(Edax)) can be a very valuable tool. (GC-MS)

This powerful, versatile technique can be used to


2.2.6 Raman Spectroscopy obtain a significant amount of compositional
information on plastic samples. It is particularly useful
in identifying minor components of the sample such
Until 1986 Raman spectrometers were either dispersive
as the stabiliser, antistatic agent and, where
long focal length double monochromators or shorter
appropriate, the crosslinking system.
focal length triple monochromators and required highly
trained scientists to obtain good quality data. The advent
of the Fourier Transform (FT)-Raman technique in 1986 It can also be used to investigate the polymer fraction
significantly reduced data acquisition times and also within a sample when the instrument is fitted with a
brought the technical advantage of suppressing any laser pyrolysis unit set at around 600 °C.
induced fluorescence within the sample. Further
developments have enabled smaller, low cost, high The technique also plays a role in failure diagnosis by
performance, quality instruments to be produced and being able to provide information on odours, and

5
Analysis of Plastics

organic contaminants that may have degraded the the interface between the chromatograph and the
plastic matrix. detector. Today, the two most popular types of
interface for the benchtop single quadrupole LC-MS
There are a variety of ways that the sample or fractions are the particle beam interface and the atmospheric
of the sample (e.g., an extract) can be analysed by GC- pressure ionisation (API) interface. The particle
MS. These include static headspace, dynamic beam interface is used to generate electron ionisation
headspace, solution injection and pyrolysis. (EI) spectra and the API interface is used to generate
either electrospray (ESI) or atmospheric pressure
chemical ionisation (APCI) spectra. A further
2.3.2 Gas Chromatography (GC) complexity is that the API interface can generate
either positive (i.e., molecular ion plus one
hydrogen) spectra or negative (i.e., molecular ion
This technique can also be used to obtain polymer type
minus one hydrogen) spectra.
information by use of a pyrolysis approach, although
the technique is less powerful because of the absence
The particle beam interface is very good for
of a mass spectrometer, and a pyrogram ‘fingerprint’
qualitative work because the 70 eV spectra contain
has to be used and a comparison made against a library
a significant amount of structural information and
of known standards.
can be searched against conventional mass spectra
libraries. However, in the full scan mode the
This technique is also used for the identification and
sensitivity is restricted to the low nanogram levels.
quantification of additives such as antioxidants and,
where sufficient volatility exists, plasticisers and
In the case of the API interface, both the electrospray
organic flame retardants.
and APCI modes are soft ionisation techniques which
leave the molecular ion (or pseudomolecular ion)
intact without much fragmentation. The interface
2.3.3 High Performance Liquid Chromatography therefore offers more sensitivity and is ideal for
(HPLC) quantitative work at low levels (e.g., contamination
of drug and food matrices by polymer additives/
HPLC can be used to identify and quantify additives breakdown products).
that are either too involatile or insufficiently stable to
be determined by GC/GC-MS. This is particularly the
case with antioxidants such as Irganox 1010 and 1036. 2.3.5 Gel Permeation Chromatography (GPC)
HPLC also comes into its own in the quantification of For this technique to be successful the sample must
plasticisers such as dioctyl phthalate (DOP). be readily soluble in an organic solvent. It has a wide
application in the analysis of plastic samples. It is
possible to obtain molecular weight data on both
2.3.4 Liquid Chromatography-Mass Spectroscopy amorphous plastics and semi-crystalline plastics. In
(LC-MS) the amorphous case (e.g., polystyrene), the system
used is set around ambient temperature (30 °C) and
This instrument is essentially a coupling of an HPLC solvents such as THF, chloroform and toluene are
with a mass selective detector and as such offers a used. With semi-crystalline plastics (e.g.,
significant enhancement in performance to the polymer polyolefins), more aggressive solvents such as ortho-
chemist. Although such combinations have been around dichlorobenzene and meta-cresol are used at elevated
for many years, they were complex and expensive (i.e., (140 °C) temperatures.
effectively research tools only), and it is only within
the last five years or so that single quadrupole benchtop In the case of some complex plastic systems (e.g.,
LC-MS systems have become reasonably common blends), the development of interfaces such as the
place due to their relative ease of use and cost. Lab Connections LC Transform, have proved very
useful in increasing the amount of information that
A mass spectrometer can be the ideal detector for can be obtained in a GPC analysis by enabling IR
liquid chromatography because it offers both data to be recorded on the resultant chromatogram.
universality and the required selectivity for complex Hence, with the correct choice of separating column,
analytical problems. For many years development polymer blends can be separated and identified as
work has concentrated particular on the design of well as plasticisers.

6
Analysis of Plastics

2.3.6 Thin Layer Chromatography (TLC) differentiate between different polyethylenes (i.e.,
LDPE, LLDPE, HDPE, etc.) from their melting points
TLC is a relatively simple technique that can be used and the appearance of their melting endotherms as well
for both the separation and identification of additives as being able to detect and, with appropriate standard
such as antioxidants and UV stabilisers. A number of materials, quantify plastic blends, e.g., PP/PE and nylon
approaches are possible using different developing 6/nylon 6,6.
solvents and spraying agents.
The DSC trace for a quenched sample of PET is shown
It is also the case that TLC can be used in a preparative in Figure 2. This trace shows the Tg (around 75 °C) of
way for the isolation of sample fractions for subsequent the material, the exothermic formation of the crystalline
chromatographic or spectroscopic analysis. phase (at 156.9 °C) and the endotherm due to the
melting of this phase (at 255 °C).
TLC does have the image of being somewhat old
fashioned and it is to be expected that the market The DSC trace of a plastic blend is shown in Figure 3.
penetration of LC-MS systems will further erode the The data obtained has been compared to standards and
standing of this technique in the modern analytical the material has been shown to be a blend of ethylene-
laboratory. vinyl acetate copolymer (EVA) and LDPE. The
approximate proportions of each is EVA 15-20%/LDPE
20-25%. In addition the EVA copolymer is thought to
contain around 20-25% of vinyl acetate (VA).
2.4 Thermal Techniques
Although not as sensitive as dynamic mechanical
2.4.1 Differential Scanning Calorimetry (DSC) thermal analysis (DMTA) to glass transitions, DSC can
be used to identify a plastic from the glass transition in
DSC is used extensively in the analysis of plastics, its thermogram. The glass transition (Tg) and crystalline
particularly those that are semi-crystalline - polyolefins, melting temperatures (Tm) of a range of plastics are
nylons, polyesters, etc. It is sensitive enough to given in Table 2.

Figure 2
DSC trace for a quenched sample of PET

7
Analysis of Plastics

Figure 3
DSC trace of a blend of EVA and LDPE

It is also possible to use DSC to provide quality control of temperature on this important material property can
fingerprint thermograms from which deviations in the be obtained over a wide temperature range (typically
composition of a plastic compound can be detected. –150 °C to +200 °C), along with the glass transition
One reason for this is that although the technique is temperature and information on thermal stability.
not capable of determining the molecular weight of a
plastic, differences in molecular weight will be apparent The use of DMTA to differentiate between plastic
in the melting endotherm region. samples that have a similar chemical composition, but
very different physical properties is shown in
Using appropriate standard materials it is also Figure 4. Both of these samples are polymethyl-
possible to use DSC to quantify the level of certain methacrylate (PMMA), but the top one is crosslinked
additives, e.g., peroxides, in a sample. having been prepared with a small amount of
difunctional monomer and the bottom sample is the
DSC can also be used in thermal stability studies of standard thermoplastic material. It can be seen that
the plastic compound, and to investigate the the crosslinked sample does not melt and the modulus
effectiveness of antidegradants and fire retardants. does not fall away significantly until thermal
degradation occurs.

2.4.2 Dynamic Mechnanical Thermal Analysis The sensitivity of DMTA to glass transition
(DMTA) temperatures (approximately 1,000 times greater than
DSC which measures heat capacity changes rather than
DMTA is very useful for generating modulus versus modulus) is very useful in the analysis of plastics and
temperature data on plastic compounds. The effects their blends.

8
Analysis of Plastics

Table 2 Glass transition (Tg) and crystalline melting temperatures (Tm) of a range of plastics
Plastics Type Tg (°C) Tm (°C)
105 (LDPE)
Polyethylene –20 115 (MDPE)
135 (HDPE)
Polypropylene 5 160
Polybut-1-ene –20 12 0
Polypent-1-ene 24 70
PTFE 115 32 7
Polychlorotrifluoroethylene (PCTFE) 52 22 1
Polyvinyl alcohol 70 Decomposes below Tg
Polyvinyl chloride 80 -
Polyvinylidene chloride –18 19 0
Polyacrylonitrile 80 to 140 -
Atactic polystyrene 95 -
Isotactic polystyrene 100 23 0
PET 67 25 6
Methyl methacrylate 100 -
Polycarbonate of bisphenol A 150 22 5
Polysulfone of bisphenol A 195 -
Nylon 6 50 21 5
Nylon 6,6 60 26 6
Polyethylene oxide –55 66
Polypropylene oxide –62 65
Polyvinyl methyl ether –31 14 4
Polyvinyl ethyl ether - 86
Polyvinyl t-butyl ether - 250

2.4.3 Thermogravimetric Analysis (TGA) A typical TGA programme would be:

This technique is useful in the analysis of compounded Heat from ambient to 550 °C in a nitrogen atmosphere
plastic samples. It is possible to obtain accurate at 20 °C/min until no further weight loss occurs. Then,
quantifications of the principal compound constituents reduce the heat to 300 °C, change the atmosphere to
such as plasticiser, polymer and inorganic species. air and heat at 20 °C/min to 1,000 °C.
This data can be obtained on small (e.g., 10 mg)
samples in a relatively short time (around 45 minutes). It is common to plot the weight loss derivative in
By the use of the temperature maxima at which weight conjunction with the weight loss, and this can be used
events occur it is also possible to use the technique to to detect the presence of a polymer blend of two or more
obtain some qualitative assignments for the plasticiser components. Thermal decomposition temperatures of a
and polymer. range of plastics are shown in Table 3.

9
Analysis of Plastics

Figure 4
DMTA results for (a) crosslinked and (b) standard grades of PMMA

10
Analysis of Plastics

Table 3 Thermal decomposition temperatures of a range of plastics


Plastic Type Temperature to achieve 50% decomposition* (°C)
Polyvinyl chloride 260
Polymethyl methacrylate 327
Polypropylene 387
Polyethylene 414
Poly-p-xylene 432
PTFE 509
*The temperature at which the polymer loses half its weight in vacuo at 30 minutes preceded by 5 minutes preheating at that temperature

Other uses for the technique include the production of The introduction of high resolution TGA instruments
compositional fingerprints for quality control purposes has enabled more accurate quantifications of minor
and the investigation of thermal stability and the effects weight loss events to be made. For example, the use of
that additives such as flame retardants and antioxidants high resolution TGA to quantify the amount of residual
have on it. monomer in a sample of polymethylmethacrylate is
shown in Figure 5. The residual monomer weight loss
It is possible to interface modern TGA instruments directly event peaks at 297.5 °C.
to IR instruments or mass spectrometers, thus obtaining
both quantitative and qualitative data in one analytical step.

Figure 5
High resolution TGA of polymethylmethacrylate

11
Analysis of Plastics

2.5 Elemental Techniques of inorganic additives (e.g., rutile and anatase forms
of titanium dioxide) and direct probe mass
The determination of the concentration of certain spectroscopy (for the determination of high molecular
elements can be very useful in plastic analysis work. weight antioxidants).
In particular, it is often necessary to determine the
amount of nitrogen or a halogen such as chlorine or Surface analysis techniques such as secondary ion mass
fluorine in the calculation of polymer content or spectrometry (SIMS), laser induced mass analysis
polymer blend proportions. Also, the targeting of (LIMA) and X-ray photoelectron spectroscopy (XPS)
specific elements can enable the quantity of a are used for failure diagnosis work associated with such
particular additive (e.g., phosphate flame retardant or things as poor bonding to substrates and for surface
titanium dioxide pigment) to be calculated. characterisation work.

The determination of nitrogen is usually done using A chromatography technique that achieved prominence
carbon/hydrogen/nitrogen analysers and the technique in the research literature around ten to fifteen years
is relatively simple and uses small amounts (e.g., 20- ago for the determination of relative high molecular
50 mg) of sample. weight additives (e.g., antioxidants) and the study of
plastic oligomers is supercritical fluid chromatography
With the other elements, the technique will vary (SFC). This is essentially a liquid chromatography
according to the element being quantified. Sulfur and technique that uses similar analytical columns to HPLC
chlorine, for example, can be determined using but where the mobile phase is a substance (e.g., carbon
oxygen combustion followed by ion chromatography dioxide) that is kept in a supercritical state by a suitable
analysis of the products. combination of temperature and pressure. One of the
benefits of the technique is that the analytes can be
easily separated from the mobile phase once the
chromatography has taken place so, for example, they
2.6 Microscopy Techniques
can be deposited on infrared transparent substrates for
analysis using an infrared microscope. The relatively
High magnification (e.g., 150x) optical microscopy
expensive nature of the instrumentation and the
can be used to examine the dispersion of fillers within
development of other techniques (e.g., LC-MS) have
the plastic matrix. The success of this operation is
restricted its market penetration.
usually dependent on the generation of high quality
microtome sections of the sample.

The technique of scanning electron microscopy has


already been briefly mentioned in Section 2.2.5 in 3 Determination of Molecular Weight
relation to the elemental analysis of surfaces in and Microstructure of Plastic
conjunction with XRF. It can also be used in its own
right, where its high magnification powers can be Polymers
employed to determine the particle size of fillers and
in the detailed examination of fracture surfaces. This section covers analytical techniques that can be
applied both to uncompounded plastic resins and
Transmission electron microscopy (TEM) can be used compounded materials.
to investigate the phase morphology of polymer
blends and the dispersion of fillers.
3.1 Determination of Molecular Weight
For other spectroscopic techniques see Section 2.2.
In common with other polymers, plastics have a
distribution of molecular weights. This distribution will
2.7 Miscellaneous Techniques be widest for polymers produced by free radical
polymerisation (e.g., polystyrene) and narrowest for
There are a number of other analytical techniques that plastics produced using specialised catalyst systems
can be used to characterise plastic samples and many such as metallocenes.
of these feature in the abstracts at the back of this
Review Report. These include X-ray diffraction There are a number of ways in which the molecular
(XRD) to identify between different crystalline forms weight distribution of a plastic can be expressed:

12
Analysis of Plastics

Mn = Number average molecular weight = Sum nM 3.1.1 Gel Permeation Chromatography (GPC)
Sum n
This is the pre-eminent technique and has been refined
Mw = Weight average molecular weight = Sum nM2 and developed extensively over the past 30 years.
Sum nM
It is possible to use it on both uncompounded resins
Mz = Z average molecular weight = Sum nM3 and plastic compounds and Mn, Mw and Mz values
Sum nM2 can be obtained. GPC is essentially a liquid
chromatography technique where the sample is
where n = the number of molecules of molar mass M. dissolved in a suitable solvent (e.g., THF for
polystyrene) and injected into a system where the
molecules are separated according to their molecular
The Z average is very sensitive to high molecular
size by a column that contains a swollen, particulate,
weight molecules within the polymer. The weight
porous gel packing.
average is always of greater value than the number
average. A measure of the breadth of the molecular
Figure 6 shows the GPC chromatograms for two
distribution of the polymer can be obtained by dividing
polymers that have different molecular weight
the weight average by the number average:
distributions but similar calculated molecular weight
averages.
Polydispersity = Mw
Mn
The standard detector for GPC systems is the refractive
index (RI) detector, but a feature of developments over
As the polymer tends to monodispersity the the past 10 years is the development of double (RI and
polydispersity approaches unity. viscosity) or triple detector systems (RI, viscosity and
light scattering). These multiple detection systems
There are a wide variety of methods that can be used provide measures of ‘true’ molecular weight by
to obtain molecular weights. The principal ones are obtaining the actual Mark-Houwink parameters (in the
as follows. case of the viscosity detector) for the polymer being

Figure 6
GPC chromatograms for two polymers with different molecular weight distributions but similar
molecular weight averages

13
Analysis of Plastics

analysed, as opposed to the polystyrene equivalent 3.1.3 Osmometry


molecular weight from the use of monodisperse
polystyrene calibrants alone. An inherent property of There are two principal osmometry techniques: vapour
the light scattering detector is that it provides ‘true’ pressure osmometry and membrane osmometry.
molecular weight data.
Vapour pressure osmometry involves the indirect
It is also possible to use spectroscopic detectors such measuring of the lowering of the vapour pressure of a
as infrared and ultraviolet. One practical use of the solvent due to the presence of a solute. It is based on the
latter is to determine if chemical modifiers (e.g., silane measurement of the temperature difference between
coupling agents) are bound to polymer molecules. droplets of pure solvent and of polymer solution
This is done by measuring the molecular weight maintained in an isothermal atmosphere saturated with
distribution of the modified plastic at a UV the solvent vapour. Calibration is by the analysis of
wavelength where the polymer itself does not standards of known molecular weight and should be over
contribute to the absorbance and comparing this to the entire range of molecular weights of interest to ensure
the distribution of the unmodified plastic. the best results. The technique is useful for polymers
that have molecular weights in the 500-50,000 range.
The use of the LC transform module with GPC has
extended its capabilities by allowing IR data to be Membrane osmometry involves the use of a
generated on the species during the course of an analysis. membrane between the solvent and the polymer
This is done by impinging the species onto a germanium solution that is permeable to the solvent molecules
disc which is then placed into a module fitted into the but not to the solvated polymer molecules. This is
sample compartment of an IR bench. IR data is collected the major restriction on the technique and means that
on the entire chromatogram using continuous collection it cannot be used for low molecular weight polymers
software, which enables the IR spectrum of any particular (< approximately 50,000).
section to be viewed. This technique is very useful for
plastic blends and highly compounded plastics such at
PVC, as it allows the polymers in the blend to be 3.1.4 Light Scattering
identified, as well as relatively high molecular weight
additives such as plasticisers. Recent developments in instrumentation have led to a
resurgence of this technique where the weight average
molecular weight is obtained from the light scattering
3.1.2 Viscosity behaviour of polymer solutions. These developments
have centred around low angle laser light scattering
This is a standard procedure for molecular weight (LALLS), multi-angle laser light scattering (MALLS)
determinations and involves the use of specially and evaporative light scattering (ELS). As well as being
designed viscometers to accurately measure the stand alone instruments, light scattering detectors have
viscosity of a polymer solution. From this the intrinsic been developed for GPC systems. MALLS detectors
viscosity is determined and hence the molecular weight. can provide direct information on the branching ratio
The time taken for the polymer solution to pass between of a polymer (a.8).
two marks on the viscometer is compared to that of
pure solvent and the ratio is the viscosity of the solution. Care has to be taken to ensure that the polymer solution
Successive dilutions give a range of concentrations and is clear (to reduce variability) and low cell volumes
times from which the intrinsic viscosity can be (0.1 μl) and dilute solutions help this. Solvent choice
calculated. The value for this is then entered into the is also critical, with the best results being with solvents
Mark-Houwink equation: that have a very different refractive index to the
polymer, and that are low-scattering themselves.
Intrinsic viscosity = KMX
Evaporative light scattering involves the removal of
where K and X are constants for the particular solvent the solvent from the solvated polymer as it elutes down
being used and are referred to as the Mark-Houwink a drift tube and the isolated polymer particles then
parameters. scatter light from the light source.

Depending on the source of the Mark-Houwink Light scattering can produce precise data and has been
parameters the molecular weight can be expressed as used successfully on polymers with molecular weights
either the number or weight average. ranging from 10,000 to 10,000,000.

14
Analysis of Plastics

3.1.5 Other Methods compared to conventional transmission spectra


(historically used to compile databases) and there is a
Other methods include end group analysis (Mn), slight shifting in the absorption wavenumber value of
ultracentrifugation (Mw) and, indirectly by determining the bands.
glass transition temperatures, DSC/DTA.
If more traditional spectra are required, the usual
A review of the determination of the molecular weight approach is to press a thin film of the samples using a
of polymers has been produced by Holding and temperature which is above the Tg or Tm and to record
Meehan (396). a transmission spectrum. A transmission infrared
spectrum of polypropylene produced from a film
pressed at 170 °C is shown in Figure 7. Another
technique that can be used to obtain transmission
3.2 Monomer Types and Microstructure spectra is to dissolve the sample up using a suitable
solvent and to cast a film. Care has to be taken to
The use of transmission IR, pyrolysis IR and pyrolysis remove all of the solvent by drying in an oven otherwise
GC to determine the polymer type of a plastic is covered it can influence the data obtained. A transmission
in Section 2.1. Where appropriate standards are infrared spectrum of PVC produced from a film cast
available, it is also possible to use IR to quantify the from a solution in THF is shown in Figure 8.
amounts of monomers in copolymers and terpolymers.
For those plastic compounds that contain a plasticiser
Another technique that is very effective at identifying and/or organic flame retardant, a certain amount of
the monomers present in a plastic materials is NMR. preparation work is required to effectively remove the
The NMR technique will also provide information on interference of these constituents. After milling or
the proportions of the various monomers in copolymers comminuting the sample to increase surface area, a
and tripolymers. In contrast to IR this information can solvent extraction is performed to remove these organic
be obtained without having to analyse standards of species. It is then usually possible to record the infrared
known monomer composition; the areas under the spectrum using either an ATR technique or by
diagnostic chemical shifts being used. transmission through a hot pressed film.

NMR instruments can also be used to obtain One of the most comprehensive databases available
fundamental structural information on polymers such of plastic infrared spectra has been produced by
as end group chemistry, branch points and structural Hummel (a.9).
isomerism. It is also possible to use IR for the latter,
although some of the isomeric structures have relatively Where the plastic sample contains both a major organic
weak absorptions which makes detection difficult when additive and a filler, it is necessary to pyrolyse the
they are at a low concentration. extracted portion of the sample and then record an
infrared spectrum of the collected pyrolysis
condensates. Providing that an extensive database of
pyrolysate spectra is available (234), this method is
very successful in identifying generic polymer types
4 Determination of Polymer Type and polymer blends. In the case of blends, it is also
possible to express the results semi-quantitatively if
One of the most basic and useful tests to carry out on a the appropriate standards are available.
plastic sample is to determine its polymer type.
If the plastic only contains a filler, the pyrolysis
Due to their relative simplicity, it is usually possible to approach can be employed without using the initial
carry out an infrared analysis of the plastic material in solvent extraction step.
the as received state and identify the plastic by reference
to a standards database. The advent of the single bounce The pyrolysate infrared spectra of nylon 6 and low
attenuated total reflectance (ATR) accessories for density polyethylene are shown in Figures 9 and 10,
Fourier transform infrared spectroscopy (FTIR) respectively.
instruments enables this operation to be carried out in
a matter of minutes on a sample a few millimetres in Another method which enables the polymer type within
size. Some care should be taken as the relative a plastic sample to be identified is pyrolysis gas
intensities of the bands present in ATR spectra can vary chromatography. This method can be applied to either

15
Analysis of Plastics

Figure 7
Transmission infrared spectrum of polypropylene produced from a film pressed at 170 °C

Figure 8
Transmission infrared spectrum of unplasticised PVC produced from a film cast from a THF solution

16
Analysis of Plastics

Figure 9
Pyrolysate infrared spectrum of nylon 6

Figure 10
Pyrolysate infrared spectrum of low density polyethylene

17
Analysis of Plastics

the extracted portion of the sample or the sample as Adding a mass spectrometer into the system, so that
received. In the former case any relatively low molecular the technique becomes pyrolysis GC-MS, further
weight plasticiser elutes early on and does not have a increases the usefulness of the method and the
significant influence on the pyrogram as a whole. As information that can be obtained.
with pyrolysis IR, a database of standards needs to be
put together and then the pyrogram fingerprints of The principal diagnostic pyrolysis species which can
unknowns can be matched. The temperature that the be detected in pyrograms of plastics are shown in
pyrolysis unit is set at, and the design of the unit (e.g., Table 4.
Curie point or microfurnace), will affect the pyrograms
produced from a particular sample. Again, it is possible It can be seen from the above list that certain plastics
to identify and quantify blends and blend ratios. ‘unzip’ to regenerate their monomers whereas other
undergo decomposition reactions to generate
Typical experimental conditions for pyrolysis GC characteristic breakdown products. In reality, a
experiments are as follows: certain amount of both types of reaction take place
for the majority of polymers and it is the one that
Sample weights 0.1-5.0 mg
predominates that determines what the major
Pyrolysis temperatures 400-800 °C (microfurnace pyrolysis products will be.
and Curie point)
With respect to the quantification of the polymer
800-1200 °C (platinum component within a plastic compound, the easiest
filament) technique to use is TGA. It is also possible to detect a
blend of polymers with TGA and to often obtain a
Microfurnace type pyrolyser - specific example using semi-quantification of the blend ratio by reference to
an SGE Pyrojector the splitting of the weight loss derivative.
Unfortunately, some plastic types (e.g., PVC) undergo
Weight of sample 0.4 mg two stage weight loss processes when heated and the
Pyrolysis temperature 600 °C first stage (loss of hydrogen chloride) will overlap
with the volatilisation of organics (e.g., plasticiser)
Pyrolysis gas Helium at 0.10 MPa stage. It is therefore not possible to use TGA alone to
determine the polymer content of these samples.
GC column 5% Diphenyl siloxane 30
m x 0.25 mm, 1.0 μm film
Another complicating factor is that a number of plastics
GC column temperature 2 min at 50 °C followed (e.g., halogenated, polyamides, polyurethanes,
program by 10 °C/min to 280 °C polyesters, other heteroatom containing systems) do
and then 10 min at 280 °C not completely pyrolyse during the nitrogen
atmosphere region and leave a carbonaceous residue
GC carrier gas Helium at 0.06 MPa which essentially oxidises to carbon dioxide in the air
region. This carbonaceous residue, which may to an
GC injector temperature 320 °C
extent overlap with any weight loss due to a carbon
Detector Flame ionisation detector black pigment, has to be included in order to obtain an
(FID) at 350 °C accurate polymer content.

Table 4 Diagnostic pyrolysis species in pyrograms of plastics


Plastic type Species
Polystyrene benzene, toluene, ethylbenzene and styrene
Polymethylmethacrylate methylmethacrylate, methyl isobutyrate
Polyethylene n-hexane, n-pentane, other straight chain hydrocarbons
Polypropylene branched hydrocarbons such as 2,4-dimethyl heptane
PVC hydrogen chloride, benzene, chlorobenzenes

18
Analysis of Plastics

5 Determination of the Plasticiser and conventional carbon black; the former having a
maximum oxidation weight loss around 700 °C and
Filler in a Plastic Compound the latter around 550 °C.

5.1 Determination of Plasticiser The TGA trace for an EVA cable covering filled with
a conducting black is shown in Figure 11.
Mention has already been made in Section 4 of the
isolation of plasticisers from a plastic matrix by The fact that a number of rubbers (e.g., halogenated,
solvent extraction. Careful choice of solvent is nitrile and polyurethane) produce carbonaceous
required to ensure that the polymer itself doesn’t residues during the nitrogen atmosphere region has
undergo dissolution and that the plasticiser is already been mentioned in Section 4.1, and care must
selectively isolated. A solvent which has been found be taken to ensure that these do not affect the
to be useful for polymers such as PVC is methanol. quantification of the carbonaceous filler in the air
The extraction is carried out under Soxhlet atmosphere region. Use of a high resolution TGA
conditions with the weight of extract being obtained instrument will assist in this as it will improve the
from the weight gain of the conditioned solvent separation of the two weight loss events.
reservoir flask once the solvent has been dried off
at 105 °C. TGA is also convenient for the quantification of
inorganic fillers such as barytes, silica and silicates.
Having quantified the plasticiser present by The limitation of the technique is that the total
extraction it is then possible to obtain an inorganic content of the plastic is obtained, with no
identification by the use of transmission IR. There indication of the relative proportion if a blend of
is an excellent database available (399) which inorganic fillers is present. It is therefore common
enables an identification to be made. Where the practice to complement the TGA data with a least a
plasticisers have distinct IR spectra (e.g., phthalates semi-quantitative elemental technique such as XRF
and sulfonamides) it is possible to detect the in order to obtain qualitative as well as quantitative
presence of a blend of plasticisers. If a quantification data. A useful exception to this rule is where the
of the blend composition is required, though, this is compound contains calcium carbonate (a relatively
usually easier to achieve by HPLC then IR. common diluent filler), in which case the carbonate
will undergo quantitative degradation at around 680-
The TGA technique can usually provide a good 700 °C into carbon dioxide and calcium oxide (which
quantification of plasticiser content. Plasticisers that remains as a residue). It is therefore possible to
have higher molecular weights (e.g., so called quantity the amount of calcium carbonate in the
polymerised plasticisers) can give problems as the sample from the carbon dioxide weight loss (which
weight loss event due to their volatilisation can will represent 44% of the carbonate by mass) and
merge with the pyrolysis weight loss event of the the remaining quantity of residue will indicate if any
polymer. As mentioned in the above section, other inorganics are present.
polymers that lose small molecules by heat
degradation (e.g., HCl lost by PVC) give more The other technique commonly used for the
complicated TGA traces and will require a solvent quantification and isolation of inorganic materials
extraction step to determine their plasticiser level. (both fillers and additives such as glass fibres) is
furnace ashing. This method is described in ISO
345-1 (1997) and a temperature of 500-600 °C is
5.2 Determination of Fillers usually used.

5.2.1 Particulate Fillers Once the ash has been obtained, qualitative
information on the inorganic species present can be
On some occasions, carbonaceous fillers such as a obtained by IR (liquid paraffin mull technique), XRF
conducting black (acetylene black) or graphite are or, where the quantification of specific species is
added to a plastic to enable it to meet certain required, ICP.
conductivity requirements. It is possible to use TGA
to quantify these types of fillers. It is also a useful Some of the principal diagnostic IR absorption bands
way of differentiating between these materials and for inorganic fillers are given in Table 5.

19
Analysis of Plastics

Figure 11
TGA trace for an EVA cable cover compound showing weight loss and derivative weight loss curves

Table 5 Diagnostic IR absorption bands for inorganic fillers


Filler Band
Silica Broad band at 950-1330 cm which peaks at 1050-1100 cm
Silicates Broad band at 850-1300 cm which peaks at 950-1100 cm
Calcium carbonate 1420, 870 and 710 cm
Barium sulfate 1080 and 610 cm

5.2.2 Fibrous Fillers It is usually obvious whether a plastic contains a fibrous


filler from either a visual inspection or the use of a
In certain applications it is necessary to impart the relatively low powered optical microscope.
strength required to a plastic part by the use of a fibrous
fillers. The following types are among those used: Glass fibres can be isolated and gravimetrically
determined by ashing at 600 °C in a muffle furnace.
(1) Glass fibres Higher temperatures (above 700 °C) can cause problems
as the glass will eventually reach its melting point.
(2) Carbon fibres
Confirmation that the fibres are glass can be carried out
(3) Synthetic polymer fibres (e.g., nylon) using an infrared microscope. The IR microscope will
(4) Wood flour also give the cellulose spectrum which is expected for

20
Analysis of Plastics

the wood flour filler type, and be able to detect the type antidegradant identified by reference to its molecular
of synthetic fibre (e.g., nylon or polypropylene) used ion and a database. The direct probe mass spectroscopy
from its characteristic transmission spectrum. technique can be carried out on samples in the as
received state as well as sample extracts, whereas LC-
TGA will enable the amount of carbon fibres in a MS is only used for extracts.
composite to be quantified. The oxidation temperature
of around 700 °C (instead of the 500-600 °C
experienced with carbon blacks) will also provide a
6.1 UV Stabilisers
confirmation of their presence.
There is a large range of commercial UV stabilisers
As mentioned above, synthetic polymeric fibres can be
for plastic materials and a number of analytical
identified by the IR microscope once sufficiently isolated
approaches can be used for their detection and
or, by use of their melting point, by the hot stage
quantification.
microscope or DSC. In the case of DSC, some
quantification data can be obtained from the size of the
The UV stabilisers can be divided into five different
melting endotherm providing standards are available.
groups:

(a) Benzophenone derivatives


(b) Salicyclic acid esters
6 Determination of Stabilisers in a
(c) Resorcinol esters
Plastics Compound
(d) Benzotriazole compounds
In common with other polymer systems, to maintain (e) Coumarin drivatives
the physical properties of a plastic compound stabilisers
need to be added to stop, or at least retard, degradation In a number of cases specific methods have been
by a number of agencies (e.g., heat and UV light). developed to determine a particular stabiliser within a
particular polymer. Some representative methods are
The use of an initial solvent extraction/dissolution step outlined next.
is common in the analysis of a plastic matrix for
antidegradants, as these species may not be volatile In some cases (e.g., the determination of 2-hydroxy-4-
enough to be removed by heating the sample. In some n-octoxybenzophenone in polyethylene) the stabiliser
cases (e.g., butylated hydroxytoluene) heating a sample has distinctive diagnostic bands and the relative
liberates enough of the species to enable an identification simplicity of the infrared characteristics of the polymer
to be made using GC-MS; however quantification will matrix enables it to be quantified using transmission
usually require removal by a solvent (to as near 100% infrared spectroscopy. A thin film of the sample is
efficiency as possible). Analysis of the extract can then produced by hot pressing at 120 °C, along with films
be carried out by HPLC, UV spectroscopy, or GC if the of virgin polyethylene containing known amounts of
species is heat stable and sufficiently volatile. Relatively the stabiliser. The absorbance maxima of the diagnostic
non-specific solvents (i.e., having mid-range solubility band between 15.8 and 16.2 microns in the standard
parameters) such as chloroform are good extracting films is used to produce a calibration curve from which
solvents. Another common approach is to dissolve up the amount of stabiliser in the unknown is calculated.
the sample in a suitable solvent and then add a non- The method is capable of detecting the stabiliser down
solvent to precipitate the polymer. The stabiliser will to 0.02% w/w with an accuracy of +/- 5%.
remain in the solvent phase.
A number of methods use the UV absorbing properties
If the type of organic antidegradant in a compound is of the UV stabiliser. For example, Tinuvin 326 can be
completely unknown, analysis of the solvent extract detected in polypropylene down to 0.02% w/w by using
by GC-MS or LC-MS is an excellent method for an extraction with chloroform under reflux followed
identification. Once the identification has been by analysis of the extract using a UV/Vis spectrometer.
achieved, a quantification can be carried out using a The ultraviolet absorption peak at 355 nm is used and
preferred method and a validated procedure if available. a calibration curve produced by dissolving known
amounts of Tinuvin 326 in chloroform.
Where the antidegradant is not volatile enough to be
identified using a GC based technique, direct probe Another technique uses the fluorescence of these
mass spectrometry or LC-MS can be used and the compounds. Uvitex OB can be detected in a chloroform

21
Analysis of Plastics

solution (0.8% w/v of polymer) of polystyrene by The chromatogram obtained for the determination of
excitation at 370 nm and recording the fluorescence at Irganox 1076 in an HDPE compound is shown in
435 nm. Standard solutions at the 0.8 w/v level of virgin Figure 12. An extract of the polymer was analysed
polystyrene and known amounts of Uvitex OB are used using a C18 reverse phase column with UV detection at
as calibrants. 230 nm and a mobile phase of 70:30 methanol/water
changing to 100% methanol.
It is also possible to use gas chromatography (e.g.,
Tinuvin P, Tinuvin 326, Tinuvin 327 and Cyasorb There is a useful HPLC method which can be used on
UV531 in toluene extracts of polyethylenes), thin layer plastics for the detection and quantification of a wide
chromatography (e.g., benzophenone and salicylic acid range (20 species) of antidegradants. The sample is
types in polyethylenes) and HPLC. This latter method dissolved up using a suitable solvent at an elevated
has been used extensively for the determination of temperature if necessary. A non-solvent (e.g., methanol)
antioxidants but has not received as much attention in is then added and the extract analysed by HPLC using
the literature for UV stabilisers. the following conditions:

It is also the case that the white pigment titanium Injection volume 25 μl
dioxide provides protection against UV light and so
this can be added at reasonable high loadings (e.g., 10% HPLC column Aqua 5 C18 ODS reverse phase
or greater) to products such as window frames. The column 150 mm x 3.0 mm
amount of titanium dioxide in a plastic can be (or similar)
determined after acid digestion of the matrix by the
use of an elemental technique such as AAS/ICP. Mobile phase A= 75:25 Methanol/Water
B= 50:50 Ethyl Acetate/Acetonitrile

Gradient Time %A %B
6.2 Antioxidants
Initial 90 10
HPLC based techniques have been widely used by After 25 min 0 100
analysts for the determination of antioxidants in plastics
and a review has been provided by Sidwell (400). Flow rate 2.0 ml/min

Figure 12
HPLC chromatogram of HDPE for determining Irganox 1076

22
Analysis of Plastics

Detection UV detector set at 270 nm The chromatogram obtained using this method to
separate a complex cocktail of antidegradants is shown
Temperature 40 °C in Figure 13.

The following antioxidants are examples of those that The wide applicability of this method is due to the
can be determined using this technique: mobile phase mixture.

(1) Irganox 1010 The capability of HPLC has been greatly extended by
the commercialisation of affordable liquid
(2) Irganox 1098 chromatography-mass spectroscopy (LC-MS)
instruments. The mass selective detector enables
(3) Irganox 1076 unknown samples to be analysed and the antioxidants
present to be identified. The LC-MS technique
(4) Irganox 1330
therefore compliments GC-MS and, with it, enables
(5) Butylated hydroxytoluene the complete molecular weight/volatility/polarity range
to be covered.
(6) Irgafos 168
TLC is comparatively easy and cheap to use and it is
(7) Triclosan both quick and accurate for the identification of

Figure 13
HPLC chromatogram of a complex mixture of antidegradants

23
Analysis of Plastics

antioxidants in plastic extracts. Irrespective of the Injection volume: 5 μl


complexity of the extract composition and the amount
used, this method can be used to give a sharp separation MS conditions: Atmospheric Pressure Chemical
for identification purposes. Distinctive Rf values and Ionisation (APCI)
colours can be seen for each antioxidant depending on
the stationary phase, the developing solvent used and Ion mode: Positive or negative
the detection agent.
Vapouriser: 300 °C
TLC, in addition to being used for identification
purposes, can be used in a semi quantitative way; Scan range: 200-1600 amu
the logarithm of the spot area being proportional to
the quantity of the analyte in the spot, and this value Fragmentor: 70 or 120 volts (The fragmentor
being compared to spots containing standard voltage is chosen to modify the
amounts of the analyte. degree of fragmentation and
hence sensitivity)
Gas chromatography has been used for the analysis of
phenolic and amine type antioxidants. Antioxidants Antioxidants which have been identified in polyolefins
which have high boiling points cannot be directly by using the above conditions include:
GC but they can be analysed as derivatives such as
acetates, trifluoroacetates, trimethyl silyl-ethers, methyl • Irgafos 168
ethers, etc. Trimethyl silane based antioxidants, for
example, give good separations on standard silicone • Irganox 1076
based columns (a.10).
• Irganox B225 (50:50 mixture of Irganox 1010
Benchtop LC-MS instruments are proving to be and Irgafos 168)
excellent tools in the analysis of plastics of unknown
composition to identify and, once this is achieved,
quantify the antioxidant present. Prior to the advent
of LC-MS it was very difficult to use conventional
HPLC for this task because of the large range of
7 Determination of Functional
possible compounds. Additives

Using the general analysis conditions shown below a 7.1 Process Aids and Lubricants
number of antioxidants can be detected in toluene or
chloroform extracts of plastics: In PVC technology certain polymeric additives can be
considered as process aids. These polymers have a
Sample preparation: Around 5 mg of extract is diluted similar composition to those used as impact modifiers
1/20 with 80% acetonitrile/water in PVC formulations but are more compatible and so
are primarily included to ensure more uniform flow
Instrument: Agilant 1100 series LC-MS and hence improve surface finish. Such process aids
include ABS, chlorinated polyethylene, MBS, EVA-
Column: Zorbac SB-C18, 5 um, PVC graft polymers and acrylate-methacrylate
2.1 mm x 150 mm copolymers. As these are usually found in unplasticised
PVC, direct analysis of the product by IR will usually
Mobile phase: A=water, B=acetonitrile indicate the presence of those that have a distinctive
spectrum as no masking by plasticiser will take place.
Gradient Time A B However, even rigid PVC can contain a small amount
of phthalate and so it is advisable to carry out a solvent
Initially 15% 85%
extraction to clean up the matrix first. Where the
after 10 min 1% 99% process aid (e.g., chlorinated polyethylene) has a
relatively bland spectrum, a technique such as NMR
or Initially 35% 65% will be required to both detect and quantify it. NMR
after 10 min 10% 90% will usually be required to quantify the other types as
well, unless the spectrum is very distinctive and
Flow rate: 0.7 ml/min standards of known composition are available.

24
Analysis of Plastics

In the case where a relatively large quantity of filler available, they have relatively high molecular weights
(talc) has to be incorporated into a polymer (e.g., and so cannot be easily removed from the matrix by
polypropylene) it is often necessary to use a process solvent extraction and can be thermally labile.
aid/lubricant such as a zinc or calcium stearate. A
quantification of the process aid can be achieved by One technique which has been used to identify both these
the analysis of the sample for the metal by acid types of pigment and inorganic ones is vapour phase
digestion-AAS. The stearate can be qualitatively ultraviolet absorption spectrometry at 200 nm (a.11). In
detected by solvent extraction GC-MS. this method the samples are powdered and then directly
vapourised in the heated graphite atomiser. Thermal
ultraviolet profiles of organic pigments show absorption
7.2 Slip Additives bands between 300 °C and 900 °C, while profiles of
inorganic pigments are characterised by absorption bands
at temperatures above 900 °C. Specific assignments are
It is common for aliphatic amides to be incorporated
made with respect to temperature, relative intensity and
into plastics, particularly polyethylenes, to act as slip
additives. width of the absorption bands.

It is possible to use LC-MS to detect these types of A relatively unknown technique (laser desorption fourier
slip additives in plastic samples. Using the LC-MS transform ion cyclotron resonance mass spectroscopy)
conditions described in Section 6.2, it is possible to has been used (397) to identify dyes in plastics such as
detect Behenamide (mixture of two aliphatic amides polymethylmethacrylate. A detection limit of 0.1% was
of molecular weight 331 and 339) and erucamide obtained, which compared with a limit of 1-2% using
(molecular weight 337) in solvent extracts of an ATR infrared spectroscopy technique.
polyethylene and polypropylene.
Infrared spectroscopy techniques can be useful,
It is also possible to use GC and GC-MS to analyse particularly if the plastic matrix itself (e.g., polyethylene)
these and another common slip additive oleamide in has a relatively simple infrared spectrum and if standard
extracts from plastics as they have sufficient volatility infrared spectra of a wide range of pigments is available.
to elute from the GC column.
Carbon black is used extensively as a black pigment in
products such as cable sheaths. The amount present is
usually less than 2% and so its quantification by TGA
7.3 Pigments can be difficult due to the small sample size (10 mg)
used. The standard method to quantify the amount of
Pigments are used extensively in plastic compounds carbon black in such a product is therefore the tube
and can be of one of four main types: furnace as much larger sample sizes can be used (e.g.,
2 g) and hence more accurate quantifications obtained.
(1) Inorganic compounds

(2) Organo-metallic compounds


7.4 Antistatic Agents
(3) Organic compounds
Antistatic agents are usually hygroscopic compounds
(4) Carbon black which readily attract moisture and so inhibit the build
up of a static charge on the surface of a plastic product.
Pigments such as titanium dioxide and iron oxide They are used in many applications from the body of
belong to the first group and the analysis of these is the humble plastic pen to numerous packaging
relatively easy as they are thermally stable (so can be applications.
determined in both the sample ash or in the sample in
the as received state) and have a diagnostic metal atom The selection of an antistatic agent depends greatly on
together with a simple chemical structure. Analysis the polymer matrix since a degree of incompatibility
techniques used are therefore elemental methods such is vital to ensure that migration to the surface of the
as AAS and ICP. product occurs at a fast rate after manufacture. Exact
chemical composition information can be difficult to
Groups 2 and 3 present the analyst with a greater obtain from suppliers and so analysis for these additives
challenge as there is a very wide number commercially can be difficult.

25
Analysis of Plastics

In the case of polystyrene, quaternary ammonium Column type: RTX5-MS 30 m x 0.25 mm,
compounds are widely used and for polyethylene, 0.25 μm film thickness
polyethylene glycol alkyl esters can be used.
Column temperature: 40 °C for 5 min, 20 °C/min
In the case of the glycol esters, these can of sufficiently up to 300 °C held for 12 min
low molecular weight to be extractable by solvents such
as diethyl ether and then identified by a chromatographic MS settings: 20 to 620 Daltons scanned
technique such as GC-MS. As in a number of cases it is every 0.33 s
to be expected that LC-MS will play a role in the analysis
of these additives in the future. In the case of the dynamic headspace approach a
relatively small amount of sample (e.g., 3 mg) is heated
in the oven of a dynamic desorption unit and the
volatiles produced collected in a cryogenically cooled
7.5 Crosslinking Agents and Co-Agents
Tenax filled trap. The experimental conditions are as
follows:
For some plastic products (e.g., cable sheathing) it
can be necessary to impart a degree of crosslinking
into the product to achieve the requisite physical Dynamic Headspace
properties. This can be achieved by irradiation using Instrument: Perkin Elmer ATD 400
gamma rays. However, some polymers degrade when
subjected to high energy radiation as illustrated in Desorption temperature: 150 °C for 10 min
Table 6. Chemical agents such as peroxides are also
used. These species produce diagnostic breakdown Desorption flow: Helium @ 20 ml/min
products the identification of which will reveal the Trap collection temperature: –30 °C
type of peroxide used.
Trap injection temperature: 250 °C
The most useful technique for this type of work is GC-
MS. There are two possible modes of sample Trap outlet split flow: 9 ml/min
introduction: solution injection and dynamic Trap inlet split flow: off
headspace. In the case of the former a useful method
of sample preparation involves cryogenic grinding of Split: 10:1
0.3 g of the sample, followed by extraction using 2 ml
of diethyl ether in an ultrasonic bath for 30 minutes. GC-MS
The resulting extract is then analysed under the
following conditions: The conditions used are the same as for the diethyl
ether method with the exception of the following:
Instrument: Hewlett Packard 6890/5973 GC-MSD
GC Column temperature: –30 °C to 50 °C at 5 °C/min,
Carrier: Helium @ 2.0 ml/min constant flow following by 20 °C/min to
300 °C and then held at
Injection mode: 1 μl splitless (0.75 min; 50 ml/min) 300 °C for 12 min

Injection temperature: 320 °C Carrier Helium @ 0.07 MPa

Table 6 Behaviour of polymers subjected to high energy radiation


Polymers that crosslink Polymers that degrade
Polyethylene Poly(α-methylstyrene)
Polyacrylic acid Polymethyl methacrylate
Polymethyl acrylate Polymethacylic acid
Polyacrylamide Polyvinylidene chloride
Styrene-acrylonitrile copolymers PCTFE
PTFE
Polypropylene

26
Analysis of Plastics

Table 7 Diagnostic species associated with different cure systems


Peroxide curative Diagnostic species
Perkadox 14/40 Tertiary butanol
1,3 Di-(1,1-Dimethylmethanol) benzene methanol)
Tert-butyl cumyl peroxide 1,1-Dimethyl benzene methanol
Acetophenone
Tertiary butanol
Dicumyl peroxide 1,1-Dimethyl benzene methanol
Acetophenone

For either analytical approach, identification of the (2) Physical Low boiling point organic compounds
diagnostic cure system breakdown species is by (e.g., dichloromethane or pentane)
reference to mass spectral libraries such as those which volatilise at the processing
produced by the National Institute of Standards and temperature to create a cellular
Technology (USA) (NIST), the Royal Society of structure.
Chemistry, Wiley/NBS (a.12) and the US
Environmental Protection Agency (EPA)/National With plastics, the most widely used type are the
Institute of Health (NIH). The mass spectra of the physical blowing agents.
majority of species of interest are in these libraries and
so, providing the knowledge to reconstruct cure systems Where it is suspected that a physical type blowing
is available, successful attempts can be made. agent has been used to produce a foam, is it possible
to use headspace GC-MS to identify it. Even in the
One problem associated with this task is that a number blown state, the high sensitivity of the technique
of peroxide curing agents breakdown to give more that enables an assignment to be made from the small
one product and a number of these are common to more amount of residual blowing agent that will be present.
than one peroxide species. This is demonstrated in It is usual to use this type of blowing agent in
Table 7. amorphous plastics that have glass transition
temperatures around 100 °C, e.g., styrenics. This
In addition to identifying the type of peroxide used, enable the expansion of the plastic to be well
these GC-MS techniques will also identify the type of controlled.
co-agent (e.g., triallyl cyanurate (TAC) or triallyl
isocyanurate (TAIC)) used. The reactivity of the chemical blowing agent type can
make analysis difficult (e.g., they will decompose in
the injection port of a GC-MS instrument), and the
7.6 Blowing Agents approach that is used is to indirectly identify them by
the determination of breakdown fragments. The GC-
There are two main types of blowing agent used with MS instrument is the best choice for this and a library
polymer systems in general: of typical breakdown fragments is required.

(1) Chemical Chemical compounds (principally Quantification of the chemical blowing agent in an
organic) that undergo chemical unblown product is very difficult as the polarity and
decomposition at the processing reactivity (e.g., hydrogen bonding reactions and
temperature to form a gaseous species thermal instability) can cause problems during isolation
(e.g., nitrogen) which will create the from the compound and subsequent analysis. In terms
cellular structure. of reverse engineering, this is unlikely to be required
since the product will invariably be already blown. For
Examples include azo compounds, laboratories that are carrying out quality control work,
nitroso compounds, sulfonyl hydrazide other properties such density and expansion ration can
compounds and sodium bicarbonate. be used to determine compound loadings.

27
Analysis of Plastics

7.7 Flame Retardants distribution within the matrix of the domains that
contain it. Actual impact performance is determined
As with blowing agents, there are two main categories by physical tests such as the Charpy and Izod impact
of flame retardant: organic and inorganic. tests, and the size and distribution of domains is
investigated by transmission electron microscopy
The amount and type of organic flame retardant present (TEM), but there are a number of chemical tests that
in a plastic compound can be determined in an can be carried out to determine the level of modifier.
analogous way to the plasticiser, since this type of flame
retardant is usually similar in molecular weight and (1) IR analysis - this is performed on a pressed film
polarity and, hence, extractability. Once the type of and the relative size of the absorption bands due to
organic flame retardant has been determined by IR, an styrene (700 cm) and butadiene (966 cm) are taken
accurate quantification can be obtained by carrying out and compared to standards of known styrene-
an elemental analysis for the halogen (or other relevant butadiene levels.
element, e.g., phosphorus) on the unextracted sample.
The extract value itself will rarely provide a meaningful (2) NMR - the plastic is dissolved and the level of the
quantification as other species, particularly any process two polymers determined by specific shift areas.
aid/plasticiser, will contribute to it as well. In some
instances (e.g., organophosphates) it may be possible (3) Classical wet chemistry - the butadiene level is
to use an HPLC analysis of the extract to quantify the determined in solution by reaction of a reagent with
flame retardant. GC based techniques can also be used the double bonds.
in some cases, but bromide types present problems for
these techniques because of their relatively high There are some instances (e.g., rubber impact
molecular weights (> 900). modification of nylon) where the chemical properties
of the two polymers are so dissimilar that solubility
Care must be taken over the quantification of inorganic differences can be used to isolate and, in this case,
flame retardants, since some of them (e.g., antimony quantify the rubber modifier. The test is carried out by
trioxide) can react with the organic flame retardant taking an accurately weighed sample and refluxing it
present, or break down to produce volatile products, in formic acid until the plastic is digested and only the
under quantitative ashing conditions, and during rubber phase remains. The rubber is then washed, dried
analysis by thermal techniques such as TGA. A good and weighed.
initial approach is a semi-quantitative elemental
analysis by XRF, to see which types are present. Other plastics which can contain rubber modifiers (or
Accurate quantifications can then be obtained by at least modifiers that have lower glass transition
precise elemental determinations. temperatures than the plastic phase) include PET and
PVC. In the case of PVC, acrylates and methacrylates
If it is known that hydrated alumina is present in the are common and the normal approach is to use IR to
sample, it is possible to quantify this reasonably well detect the modifier and then NMR to quantify it.
using TGA, by making use of the water loss data.
Hydrated alumina loses close to 35% of its weight when
it is heated to 550 °C in a TGA experiment.
8 Analysis of Plastics for Food
Contact Use
7.8 Impact Modifiers
For more than 30 years work has been going on
The most commonly encountered impact modified involving food contact plastics and the effect that
plastic is high impact polystyrene (HIPS). The impact migrants from plastics products have on food. The first
modification is achieved by incorporating discreet European Directive (78/142/EEC), which was on the
domains of a rubber (butadiene) within the polystyrene vinyl chloride monomer content of food contact PVC,
matrix. The level of butadiene can be varied according was published in the late 1970s and this was followed
to the requirements of the end use. A high level can ultimately by the more comprehensive Plastics
convert a glassy brittle material into a ductile, tough Directive (90/128/EEC) in 1990. Since 1990, there has
product. The efficiency of the butadiene to improve been a gradual harmonisation of European testing
impact resistance alone is not solely related to requirements through amendments to 90/128/EEC. The
concentration, but is also dependent on the size and seventh amendment (2002/17/EC) has recently been

28
Analysis of Plastics

published and the initial requirements for testing overall 8.1 Global Migration Tests
and specific monomer migration have now grown to
include additive (e.g., antioxidant) migration. The following food simulants are used for food contact
plastics:
In general, there are two types of analytical test that
are carried out on food contact plastics: Distilled water - Aqueous food use

(1) Global migration tests - In these, the plastic is put Distilled water 95%:Ethanol 5% - Alcoholic
into contact with an appropriate food simulant beverages such as beers and lagers
under representative end use conditions and the
total amount of material that has migrated into the Distilled water 85%:Ethanol 15% - Wines
simulant determined gravimetrically or, in the case
of involatile food simulants such as olive oil, by Distilled water 60%:Ethanol 40% - Spirits
gas chromatography.
A solution of 3% w/v acetic acid in distilled water -
(2) Specific migration tests - Again, the plastic is Acidic aqueous foods
contacted with a food simulant but any analytical
work in targeted on a specific additive and its Olive oil* - Fatty foods (also isopropanol or hexane)
concentration determined using an appropriate (*Isopropanol and Hexane have been introduced
chromatographic technique. as fatty food simulants to circumvent the analytical
problems that can occur with olive oil due to its
In the case of certain plastics materials, e.g., ABS, potential variability as a natural product and
grades that are intended for food use have to meet involatility.)
certain residual monomer targets. Direct analysis of
these polymers is undertaken to determine the As mentioned, the global migration figure for a particular
concentration of these monomers. plastics material is determined gravimetrically. One

Table 8 Contact time and temperature for food contact testing


(EC Directive 82/711/EC)
Conditions of contact in actual use Test conditions
1. Contact time > 24 hours
T < 5 °C 10 days at 5 °C
5 °C < T < 40 °C 10 days at 40 °C
2. Contact time between 2 hours and 24 hours
T < 5 °C 24 hours at 5 °C
5 °C < T < 40 °C 24 hours at 40 °C
T > 40 °C In accordance with National Laws
3. Contact time less than 2 hours
T<5 2 hours at 5 °C
5 °C < T < 40 °C 2 hours at 40 °C
40 °C < T < 70 °C 2 hours at 70 °C
70 °C < T < 100 °C 1 hour at 100 °C
100 °C < T < 121 °C 30 min at 121 °C
T >121 °C In accordance with National Laws

29
Analysis of Plastics

approach is to use conditioned glass crucibles and to 8.2 Specific migration and residual monomer tests
dry off the simulant on a hot plate after the contact
experiment has been performed under the appropriate In addition to the global migration limit 90/128/EEC
conditions (time and temperature). also provides a number of specific migration limits
(SMLs) for plastic monomers (Table 9).
Once the appropriate simulant has been chosen the
contact time and temperature to use are given in EC There are also SMLs for plastic additives, some
Directive 82/711/EEC (Table 8). examples are shown in Table 10.

In addition, for plastics in contact with food for which In the case of some monomers, 90/128/EEC gives limits
a preservation temperature of less than 20 °C is required (called quantification limit-monomer (Qm)) relating to
the test condition will be 10 days at 20 °C. the plastic material itself. For example, vinylidene
chloride has a QM of 5 mg/kg of plastic.
The overall global migration limit for plastics is stated
in the EC Directive 90/128/EEC as being 10 mg/dm2 Over the years, the detection of species migrating from
(surface area of plastic). This limit can be expressed as food contact materials has advanced hand in hand with
60 mg/kg of foodstuff in certain situations. To be used the gradual lowering of analytical detection limits
for food contact a plastics product must meet this brought about by the refinement of the techniques. For
requirement. example, the SML for acrylonitrile is set at not
detectable above 0.02 mg/kg (i.e., 20 parts per billion)
In a number of packaging types, only one side of a and this would not be obtainable on a routine basis
plastic film or laminate may contact the food. Specific without the benefits of modern instrumentation.
single side migration cells have been developed (e.g.,
by PIRA) to enable the migration from a material under The development of suitable methods for the detection
these conditions to be investigated. of the wide range of monomers and additives used in

Table 9 SMLs for plastic monomers (90/128/EEC)


Monomer SM L
Vinyl acetate 12 mg/kg foodstuff
Acrylonitrile Not detectable above 0.02 mg/kg foodstuff
Caprolactam 15 mg/kg foodstuff
Formaldehyde 15 mg/kg foodstuff
Terephthalic acid 7.5 mg/kg foodstuff
Vinylidene chloride Not detectable above 0.05 mg/kg foodstuff

Table 10 SMLs for some plastic additives (90/128/EEC)


Additive SM L
Adipate and phthalate esters 1.5 mg/kg foodstuff
Antimony trioxide 0.01 mg/kg foodstuff
BHT 3.0 mg/kg foodstuff
Hydrogenated hydrocarbons 3.0 mg/kg foodstuff
Conventional hydrocarbons 0.3 mg/kg foodstuff
Oleamide/stearamide Cannot be used for fatty food use

30
Analysis of Plastics

food contact materials requires the application of state 9 Determination of Stabilisers in PVC
of the art analytical techniques. Normally, headspace
methods are preferred for volatile monomers as such
Although it is one of the bulk thermoplastics, PVC
methods overcome a lot of the problems of sample matrix
suffers from relatively poor stability to ageing agencies
clean-up. In principle the food contact simulant, foodstuff
such as heat and UV light. In order to achieve its status
or plastic material is heated in a sealed vial fitted with
as an important plastic it was therefore necessary to
an inert septum (usually PTFE coated rubber). The vial
develop a specific additive group: PVC stabilisers.
is heated to an accurate set temperature normally in the
range 80-100 °C, for an equilibrium time of at least one
These technological developments have resulted in a
hour. The headspace above the sample is then analysed
range of stabilisers being available that are appropriate
for the presence of the analyte. The quantity of analyte
for different grades of PVC, products and end uses.
in the headspace will always be in equilibrium with the
Some of the main types are:
amount present in the sample. Standard addition methods
are used to obtain calibration curves, with the calibrant
vials being analysed under the same conditions (i.e., time, (a) Lead stabilisers (e.g., lead carbonate, lead stearate,
temperature and ratio of headspace to bulk material lead phthalate)
(polymer if necessary)) as the samples. To acquire
sufficiently low detection limits it is sometimes (b) Metallic soaps (e.g., stearates, palmitates,
necessary to use specific detectors (e.g., a nitrogen/ ricinoleates and octoates of cadmium, barium,
phosphorus detector (NPD)) or, in the case of mass calcium and zinc)
selective detectors, a single ion monitoring approach.
For species that are too involatile for headspace based (c) Organo-tin compounds (e.g., dibutyltin di-iso-
methods, other chromatographic and spectroscopic octylthioglycollate)
methods are employed.
(d) Epoxide stabilisers (e.g., epoxidised oils and
A summary of the analytical techniques used in food bisphenol A epoxide resins).
migration work is shown in Table 11.
The analyst has to bear in mind that it is common for a
In the cases where HPLC has been assigned, LC-MS number of different stabilisers to be used in a PVC
would also be applicable. compound in order achieve the optimum ageing resistance.

Table 11 Analytical techniques used in migration testing


Analyte Technique
Vinyl chloride Headspace GC
Styrene Headspace GC and HPLC
Terephthalic acid HPLC
Ethylene glycol Headspace GC
Acrylonitrile Headspace GC with NPD
Butadiene Headspace GC with mass selective detector (MSD)
Isocyanates Derivatisation HPLC
Formaldehyde Derivatisation colorimetry
Organic acids Ion pair HPLC or IC
Plasticisers HPLC
Antioxidants HPLC, GC or SFC
Inorganics AAS or ICP
Polar organics HPLC and capillary electrophoresis

31
Analysis of Plastics

It is obvious that a large number of these stabilisers Of the other types of organo-metallic stabilisers,
contain metal atoms and so a cost effective way of Mal’kova and co-workers (a.17) have described an
achieving an initial evaluation of the type of stabiliser alternating current polarographic method for the
present is to use a semi-quantitative XRF technique determination of cadmium, zinc and barium stearates
on the sample in the as received state. Care should be or laurates in PVC. Other techniques used on PVC
taken with this as some inorganic pigments/fillers extracts include, column chromatography for barium,
(e.g., titanium dioxide) can mask certain key elements cadmium and zinc salts of fatty acids, paper
(e.g., cadmium). chromatography for cadmium, lead and zinc salts of
fatty acids (a.18) and polarography for cadmium, lead
If it is a case of quantifying a known stabiliser, then and zinc salts (a.19).
AAS or ICP can be used to quantify the metal and, with
knowledge of the compound formula, the result obtained. The advent of bench top LC-MS instruments has
enabled the analysis of stabilisers such as the organo-
tin type to be re-examined and laboratories such as
The organo-tin compounds are widely used and for
the Analysis Division at Rapra Technology Limited
analytical considerations it is convenient to divide them
are investigating the capability of this technique in
into those that contain sulfur and those that do not. To
this area. This could be another area of plastics
the first group belong compounds like dialkyltin
analysis where LC-MS replaces the more traditional
mercaptides, mercaptoesters and mercapto
techniques.
carboxylates, to the second, dialkyltin carboxylates and
their esters. The identification of acids and alcohols
present in tin stabilisers containing no sulfur and the
identification of alcohols from stabilisers containing
10 Analysis of Plastic Laminates and
mercaptoesters presents little or no difficulty. However,
the identification of the thioacid and of the alkyl groups Fibres
attached directly to tin can prove more difficult,
especially if long chain acids form part of the compound Plastic laminates are used extensively from the ordinary
or if the stabiliser is not pure, e.g., if it contains crisp packet to high specification products for medical
plasticiser. The thioacid may also tend to decompose and pharmaceutical use. In all these cases, laminates
during hydrolysis procedures. The application of a are used since the application demands a number of
number of analytical methods (e.g., NMR, IR and GC) properties which no single polymer exhibits.
to determine these types of stabiliser in PVC extracts
have been described by Udris (a.13). Taking the example of the crisp packet, the innermost
layer must be inert to the product and provide a barrier
Some classic methods based on titration and TLC to to air, the outside layer has to be capable of being
printed onto and the middle layer (or tie layer) has to
determine organo-tin compounds in solvent extracts
be able to stick both of the other two together.
of PVC include:
One of the principle analytical techniques for the
• Potentiometric titration of organo-tin in the extract
analysis of laminates is the infrared microscope. This
with standard sodium methoxide in pyridine using
instrument is capable of recording transmission infrared
antimony and calomel electrodes (a.14).
spectra from sample down to 10 square microns in size.
The approach is usually to prepare a section of the
• Titration of dialkyltin thiol compounds in benzene/ laminate by microtoming a section and then recording
methanol extract with standard silver nitrate (in IPA a spectrum of each layer aided by the masking off of
medium) using sulfide coated wire electrode (a.13). the other layers. The sectioning is often undertaken
obliquely in order to maximise the apparent layer
• TLC of organo-tin thioacids and thiols using thickness. The microscope also allows the thickness
Kielselgel G plates with development with of each layer to be determined.
glacial acetic acid and detection with catechol
violet (a.15). It is also possible to use an ATR technique to record
infrared spectra of the outside layers and reserve the
• TLC of organo-tins using Kieselgel GF 254 with IR microscope for the central layers. This is possible
development using butanol/glacial acetic acid because the ATR technique only penetrates a few
and detection with catechol violet and UV microns into the surface of the layers. It is also possible
irradiation (a.16). by choosing the appropriate crystal (e.g., germanium,

32
Analysis of Plastics

zinc selenide, etc) to control the depth of penetration.


This can be useful if the layers are particularly thin.

Using the knowledge gained by infrared spectroscopy


of the generic polymer types present, the assignments
can be refined by the use of DSC. Due to the fact that
laminates by their nature are often constructed of
completely different plastic types, the complete
structure can be analysed in one operation and the
melting endotherm transitions obtained used to
differentiate between various grades. For example in
the case of a laminate which had been shown to be
comprised of a polyethylene and a nylon, it would be
possible to differentiate between LLDPE, LDPE and
HDPE, and nylon 6 from nylon 6,6.

It is also possible to use a Raman microscope to analyse


the different layers that are present within a laminate.
As with the IR microscope, it has the ability to isolate
individual layers and, given a satisfactory database, the
spectra obtained can be used for identification purposes.

The Raman spectra for four common polymer types


are shown in Figure 14.

Examination of the cross section of laminate samples


under an optical microscope enables the individual
layers to be viewed. Phase contrast microscopes can
aid the differentiation of layers of similar refractive
index. The use of a polarising microscope can also assist
in characterising individual layers and is particularly
useful when heating laminates under a microscope on
a hot stage to recognize the characteristic melting
temperature of the individual layers.

There are a number of synthetic fibres that can be used


to produce both woven and non-woven fabrics. The
most popular include polyamide, polyester and acrylics
and they can be used in products as varied as clothing
and life rafts.

Once again, the infrared microscope is ideal at


recording generic polymer identification spectra from
individual fibres. Once the generic type has been
established, further refinement of the assignment can
be obtained by DSC (e.g., specific polyamide type)
and, where a number of fibres are available GPC
(molecular weight).

Other microscopic techniques, such as optical (aspect


ratio), SEM (surface morphology) and EDAX Figure 14
(elemental analysis), Raman microscopy and atomic
force microscopy can be used to further characterise Raman spectra of (a) polyethylene, (b) PVC, (c)
the product. polystyrene and (d) polyethylene terephthalate

33
Analysis of Plastics

11 Surface Analysis of Plastics Because of its ability to determine surface chemistry,


XPS can be particularly useful in the analysis of
polymer surfaces to see if oxidation has taken place
There are a number of analytical techniques that can
and, if so, what functional groups (e.g., ester, acid,
be used to obtain data on the surface of plastics
aldehyde) the oxygen is present in.
materials or products. Three of the techniques, IR and
Raman microscopy and Edax are covered in Sections
2.2.1, 2.2.6 and 2.6. It can be argued that these This ability of XPS to detect oxygen containing
techniques have come into being as the logical functional groups is shown in the narrow and broad
development of the original, general purpose scan spectra of PET presented in Figure 15.
techniques.
Another application is the analysis of polymers to
There are however a number of analytical instruments determine if certain surface treatments (e.g., corona
that have been developed with the specific intention of discharge) have been carried out satisfactorily.
analysing surfaces. Three of the principal ones will be
mentioned in this section. In common with the other surface analysis techniques,
it can also be used to investigate surface
contamination problems and to determine the
composition of the fracture surfaces in adhesion
11.1 X-Ray Photoelectron Spectroscopy (XPS) failures.

In this case the surface of the sample is irradiated with


soft X-rays. These X-rays are sufficiently energetic to
cause photoemission of electrons from the core levels 11.2 Laser Induced Mass Analysis (LIMA)
of atoms present on the sample surface. The
photoelectrons generated are collected and passed to In the LIMA technique, the surface of the sample is
an electron energy analyser and detector. The measured subjected to a pulsed UV laser which is sufficiently
kinetic energy (KE) of an electron is given by : energetic to volatilise a small volume (about 1 μm
cube) of material. The ionised fragments in this
volume are then separated and identified by means of
KE = hv - BE - sigma
a time of flight mass spectrometer. Both negative and
positive fragment data can be obtained.
where: hv = energy of the X-ray photon
BE = Binding energy The analysis area in a LIMA experiment is typically
sigma = work function of the spectrometer 1-2 μm, the analysis depth 0.25-0.5 μm and the
detection limit 10-100 ppm. The technique has the
The binding energy of a given core electron is ability to detect all of the elements in a qualitative way.
characteristic of the element and it is this which
enables the elements on the surface of a sample to be The technique is very useful for determining
identified. It is also possible to carry out quantitative compounds on the surface by means of these elements
work by measuring the relative intensities of the and molecule fragments, but it is very sensitive, and
photoemission from each of the elements present. The care must be taken to ensure that the surface is not
binding energy of a core level depends principally on contaminated (e.g., by handling without gloves) and
the charge on the nucleus of the atom concerned and that the representative control samples are available
smaller changes are induced as a result of chemical to assist in the interpretation of the data.
bonding. Although small, such charges are measurable
and provide a means of studying the chemistry of the Its sensitivity and surface specificity make it ideal in
sample surface (a.20, a.21). the detection of very low levels of contamination/
modification. For example, the detection of a
Because only electrons from the top few atomic layers monolayer of silicone contamination of a plastic part
will have sufficient energy to escape, the technique is that was hampering the wetting of a paint. It can also
very surface specific and results are normally obtained be used to analyse particulate impurities, fibres and
from between 5 and 10 nm depth at a detection limit of defects in surface coatings.
around 0.1 atom percent. The analysis area is typically
3-10 mm2 and all the elements with the only exception LIMA is also referred to as laser microprobe mass
of hydrogen can be detected. spectroscopy (LAMMS).

34
Analysis of Plastics

(a)

(b)

Figure 15
XPS spectra of PET (a) narrow spectrum (b) broad spectrum

35
Analysis of Plastics

11.3 Secondary Ion Mass Spectroscopy (SIMS) formulation of the product initially, which is a
technological failing, the other is where the formulation
In this technique the sample surface is bombarded by a is correct for the application, but where there has been
primary ion beam (positive ions of argon, caesium, a problem in the mixing/processing side, leading to a
oxygen or gallium). These primary ions impart energy product that does not meet the specification. Analysing
to the surface and, as a consequence of the collisions the plastic component can be useful in failure diagnosis.
produced, ions, atoms and molecular fragments (called
sputtered particles) are ejected. The primary ions may
penetrate several atom layers into the surface, but the 12.1 Common Compositional Problems
sputtered particles only come from the outer 2-3 atom
layers. In common with the other two techniques, If it is suspected that the composition of the product is
therefore, SIMS is very surface specific and it is possible not correct, for example that the antioxidant or correct
to restrict it to a single monolayer. The analysis area is cure system has not been incorporated into the
typically 150 μm, the detection limit is 1 ppm and all compound, then the appropriate species specific tests
the elements are detectable. that have been discussed earlier can be carried out. If
possible, it is advisable to conduct the analysis
Two types of SIMS experiment can be carried out: static
alongside that of a sample known to be of the correct
SIMS and dynamic SIMS. In the former case, the surface
composition. This ensures that no product specific
is bombarded with low energy ions and molecular and
matrix effects/interference reactions affect the data
atomic fragments are produced without the experiment
obtained and hence the conclusions reached.
changing the nature of the surface appreciably; the
surface chemistry can therefore be investigated.
A surprisingly large number of failure problems can be
Dynamic SIMS uses high energy ions to obtain highly
solved by carrying out a simple series of tests including a
sensitive elemental data down to ppb levels, but the
polymer identification check by IR, a bulk compositional
structural information is lost.
analysis by TGA and a molecular weight determination.
In the case of static SIMS, dedicated libraries are required
to enable the mass spectra of the fragments to be Molecular weight determination is very important in the
identified (a.22). case of plastics because of the wide use (sometimes
unauthorised) of regrind material. Unfortunately, the
Another application of SIMS is in the study of the quality of regrind plastic can vary greatly due to the
migration of additives (e.g., slip additives and antistats) degradation, and hence reduction in molecular weight
onto the surface of plastics. and associated physical properties, that a plastic
undergoes when it is reground. This depends greatly on
It is often the case that complementary surface analysis the conditions (e.g., heat and time of heating) that it is
techniques such as SIMS and XPS can be used together subjected to during the regrinding process. Also, if a
in order to successfully solve a failure or characterisation material already contains a proportion of reground
problem. In such cases, XPS would be used to generate material the onset of degradation can be accelerated by
quantitative information, whilst SIMS would provide structural anomalies already present in the polymer. The
qualitative clues with respect to the chemistry. An widespread applicability of GPC to determine the
example of this is where XPS has successfully detected molecular weight distribution of the majority of common
and quantified silicon on a surface which is not plastics makes it the perfect technique to investigate if
responding well to bonding with an adhesive, but the regrind is in a sample. Although small amounts (e.g.,
chemical form that the silicon is in is not readily apparent, 5%) of reasonably high quality regrind can be hard to
i.e., it could be silica, silicate or silicone. Analysis of the spot, any significant amount will reveal itself by a shift
same surface by static SIMS enables the mass spectrum in the distribution towards the low molecular weight end.
of the sputtered top layer fragments to be determined As usual with GPC, the availability of reference samples
and the presence of m/e ions at 43, 73 and 147 confirm is important as the technique is mainly comparative.
that a polydimethyl siloxane is present.
Most of the failures that are associated with the use of
either some or too much regrind are related to a reduction
in the strength properties of the plastic, but another
12 Failure Diagnosis reasonably common type of failure is odour, especially
in packaging applications. This odour is invariably due
It is an unfortunate fact that plastic products fail in to oxygenated degradation products of the plastic and
service. One of the major reasons for this is an incorrect can be detected and analysed by headspace GC-MS.

36
Analysis of Plastics

12.2 Environmental Stress Cracking manufacturing stage (e.g., mixing, extruding or


moulding).
Environmental stress cracking (ESC) is the premature
initiation of cracking and embrittlement of a plastic More often than not this contamination is in the form
due to the simultaneous action of stress and strain and of solid, discreet entities which makes their removal
contact with specific fluids. It is estimated that 15% of from the product relatively easy. Once removed the
all plastic component failures are due to ESC. The microscopic techniques IR and Edax are excellent at
source of stress is often that which is unavoidably obtaining assignment data in a cost effective way.
processed in during moulding and so an applied stress Where enough of the contaminant is obtainable (e.g.,
is not a pre-requisite. The fluid is sometimes that for 1 mg), and if a mixture of chemicals is suspected, a
which the component was designed to contain or bulk composition by TGA can be obtained. If
conduct, but it is often supplied by such agencies as identification problems are still occurring, more
adhesives, paints, cleaning agents and inks. sophisticated techniques such as GC-MS, SIMS and
LIMA can be employed. Where the contamination is
Because this type of failure is associated with relatively in a liquid form, a similar analytical regime can be used.
mobile (i.e., low molecular weight) liquids which are A number of plastic products can suffer from solid
normally present in small concentrations the technique inclusions, but it is probably most common in extruded
of GC-MS is very well suitable to its investigation. A products such as car door seals.
particularly effective approach is dynamic headspace
GC where any stress cracking fluid can be removed It is also possible to use a Raman microscope system
from the plastic matrix without the use of another for the analysis of contaminants in plastic materials
solvent and long heating times enable it to be (293). One situation where the technique is particularly
concentrated up to aid detection. An area of plastic that useful is in the identification of very small (e.g., a few
has not stress cracked can be used as a control. micrometers in diameter) polymer gel inclusions within
the same polymer matrix. Often these gels have a higher
There are cases where stress cracking can occur due to degree of crystallinity and Raman spectroscopy with
the migration of a less volatile liquid (e.g., a plasticiser). its high spatial resolution and ability to differentiate
An example of such a case is the stress cracking of between difference degrees of crystallinity is the ideal
ABS due to the migration of plasticiser from PVC, and technique to differentiate between these and
this can be approached by the detection of phthalate in contamination by a foreign material.
the ABS matrix by solvent extraction and then analysis
of the extract using HPLC. Contamination of plastics products by a species at a
low level (i.e., less than 1% or at ppm levels) can
Where the liquid is relatively non-volatile and complex sometimes be important, for example if a product is to
in composition (such as silicone oil which causes be used in the pharmaceutical industry. If it is suspected
cracking of polyethylene) again a solvent extraction that the contaminant is, or contains, a metal, then AAS
technique has to be performed with either infrared can be employed. If the presence of an organic molecule
microscopy analysis of a cast micro-film or a liquid is suspected, then headspace GC-MS can be used to
chromatography method (i.e., LC-MS or HPLC) as the identify and quantify the species. The high sensitivity
analysis technique. of this technique normally makes the use of a control
sample extremely important for a quick interpretation
A review of the environmental stress cracking of of the output, which is often complex.
plastics has been produced by Wright (315).

12.4 Odour and Emissions Problems


12.3 Contamination Problems
The continuing drive to improve customer care and the
Plastic products can fail, both aesthetically and high profile of health and safety issues, has led to
physically, because of contaminants. Chemical pressure on the suppliers of plastics components to
resistance and electrical failure are less likely causes certain industries to minimise odours, and volatiles in
of failure as this type of contaminant is not usually general, from their products. This is particular true of
present at a high enough concentration. the automotive industry.

Contamination can enter the product stream either in There are a number of specific tests that automotive
the ingredients used in the production, or during the companies insist that plastics components manufactured

37
Analysis of Plastics

by suppliers have to pass. An example of such a test is 13 Conclusion


the VW emissions test which involves placing the
component in a cell of given dimensions and heating
the cell for a given time and a specified temperature. This review describes the analysis of plastics, plastic
Rather than carry out a detailed analysis of the compounds and plastic products in as comprehensive
components liberated from the component, the result is a way as is possible within the format of a Rapra
expressed in terms of ppm of total organic compounds Review Report. The abstracts from the Rapra
as determined by an organic vapour analyser (OVA). Polymer Library and the additional reading
Limits are given as to the permissible concentrations. references provided should greatly assist the analyst
who requires more information on recent
For quality control purposes it is the case at present developments.
that human smell panels will be used in preference to
instrumental analytical techniques which do not yet For the future, the reduction in cost of LC-MS
adequately mimic the human response. There are systems will increase their accessibility and, in
practical drawbacks to this approach, leading to a lot combination with GC-MS, will greatly improve the
of research going into ‘electronic noses’ utilising a efficiency and accuracy with which the analysis of
number (e.g., 32) of sensors based on organic antidegradants, cure systems, plasticisers and other
conducting polymers. These devices enable fingerprints additives can be carried out. The combination of
of satisfactory products to be recorded which are used these two instruments will enable the full spectrum
as references for quality checks. of polarity and molecular weight to be covered and
enable a quantum leap in capability to be achievable
Work has been carried out to determine the additives by all analytical laboratories. Experiments which for
which contribute the most to the overall odour of plastic years have had to be carried out by TLC because of
products. One of the most useful techniques is the limitations of conventional HPLC instruments
headspace GC-MS. It is advisable to use the dynamic will now be carried out by LC-MS.
form of headspace sampling as this enables the volatiles
from the sample to be concentrated. This benefit is
The specific analysis techniques SIMS, XPS and
important as some chemical species can cause an odour
LIMA are becoming increasing routine and, as a
problem at very low levels due to the specific sensitivity
result, cost effective for consultants to use in
of the human nose.
characterisation and failure diagnosis work and
therefore an expansion of their use is guaranteed.
For this type of work the dynamic headspace sampler
(e.g., the Perkin Elmer ATD 400) is operated in a
diffusion mode where the sample is heated at a In the thermal analysis field, a number of
relatively low temperature (e.g., 50 °C), which helps developments have occurred in recent years, with
to ensure that additional volatile species are not modulated temperature forms of TGA, DSC and
generated due to degradation of the sample, for a TMA being brought out by manufacturers.
relatively long period of time (e.g., in excess of 30 Modulating the temperature enables these techniques
minutes). The odour species collected in the trap of to deliver better, more informative data on samples.
the dynamic headspace sampler can then be analysed Another development within the thermal analysis
under the following conditions: group is the micro-thermal analysis (micro-TA)
instrument. This technique combines the
Headspace trap injection temperature: 200 °C topographical mapping capabilities of a scanning
probe microscope with the ability to perform
GC column type: SGE RTX5 MS 30 m x localised thermal analysis (DTA and TMA) on a
0.25 mm, 0.25 μm film micron scale. The instrument is also capable of being
connected to a GC-MS via a heated interface for the
GC column temperature –30 °C to 50 °C at 5 °C/ chemical identification of specific features.
min and then 20 °C/min
It is clear that, even with the development of new
(cryogenic cooling) to 320 °C. and more advanced techniques, the analysis of plastic
compounds and products will continue to present the
MS conditions 20 to 450 atomic mass units polymer analyst with complex and difficult
scanned every 0.33 s challenges.

38
Analysis of Plastics

Additional References a.12 F. Lafferty and D.B. Stauffer, Wiley/NBS


Registry of Mass Spectral Data, John Wiley &
a.1 Surface Characterisation of Advanced Sons, 1989.
Polymers, Eds., L. Sabbatini and P.G. a.13 J. Udris, Analyst, 1971, 96, 130.
Zambonin, Wiley-VCH, 1993.
a.14 A. Groagova and M.A. Pribyl, Analytical
a.2 G. Lawson and J. Sidwell, Plastics and Rubber Chemistry, 1968, 234, 423.
International, 1983, 8, 6, 15.
a.15 F. Belpaire, Revue Belge des Matieres
a.3 J.L. Koenig, Spectroscopy of Polymers, Plastiques, 1965, 6, 201.
Elsevier, 1999.
a.16 D. Simpson and B.R. Currell, Analyst, 1971,
a.4 T.R Crompton, Manual of Plastics Analysis, 96, 515.
Plenum, 1998.
a.17 L.N. Mal’kova, A.I. Kalanin and E.M.
a.5 T.R. Crompton, Practical Polymer Analysis, Derepletchikova, Zhurnal Analiticheskoi
Plenum Press, 1993.
Khimii, 1972, 27, 1924.
a.6 Polymer Spectroscopy, Ed., A.H. Fawcett,
a.18 E. Schroeder and K. Thinius, Deutsche Farben
Wiley, 1996.
Zeitschrift, 1960, 14, 146.
a.7 J. Haslam, H.A. Willis and D.C.M. Squirrell,
a.19 E. Schroeder and S. Malz, Deutsche Farben
Identification and Analysis of Plastics, 2nd
Zeitschrift, 1958, 5, 417.
Edition, Butterworth, 1972.
a.20 Practical Surface Analysis, Eds., D. Briggs and
a.8 P.J. Wyatt, Analytica Chimica Acta, 1992,
M.P. Seah, John Wiley and Sons, 1988.
272, 1.
a.21 Handbook of X-Ray Photoelectron
a.9 D.O. Hummel, Atlas of Polymer and Plastics
Spectroscopy, Ed., G.E. Muilenberg, Perkin
Analysis, Volume 2, Carl Hanser Verlag, 1984.
Elmer Corporation, Eden Prarie, MN, 1979
a.10 H.B.S Conacher and B.D. Page, Journal of (update 1992-95).
Chromatographic Science, 1979, 17, 188.
a.22 D. Brigg, A. Brown and J.C. Vickerman, A
a.11 P. Tittareli, T. Zerlia, A. Colli and G. Ferrari, Library of Standard Static SIMS Spectra,
Analytical Chemistry, 1983, 55, 220. Wiley, 1989.

39
Analysis of Plastics

40
Analysis of Plastics

Appendix 1
Solubility Parameters of Plastics, Plasticisers and Typical Solvents

Solubility parameters of plastics


Plastic Type Solubility Parameter
PTFE 6.2
PCTFE 7.2
Polyethylene 8.0
Polypropylene 8.0
Poly t-butyl methacrylate 8.3
Poly n-hexyl methacrylate 8.6
Poly n-butyl methacrylate 8.7
Poly butyl acrylate 8.8
Poly ethyl methacrylate 9.0
Polystyrene 9.2
Poly methyl methacrylate 9.2
PVC 9.5
Bisphenol A polycarbonate 9.5
Polyvinylidene chloride 9.8-12.2
Ethyl cellulose 8.5-10.3
Cellulose di-nitrate 10.55
PET 10.7
Acetal polymers 11.1
Cellulose di-acetate 11.35
Nylon 6,6 13.6
Polymethyl α-cyanoacrylate 14.1
Polyacrylonitrile 14.1

Solubility parameters of plasticisers


Plasticiser Solubility Parameter
Paraffinic oils 7.5
Aromatic oils 8.0
Dioctyl adipate 8.7
Dioctyl sebacate 8.7
Didecyl phthalate 8.8
Di butyl sebacate 8.9
Dioctyl phthalate 8.9
Di 2-butoxyethyl phthalate 9.3
Dibutyl phthalate 9.4
Triphenyl phosphate 9.8
Tritolyl phosphate 9.8
Trixylyl phosphate 9.9
Dibenzyl ether 10.0
Dimethyl phthalate 10.5

41
Analysis of Plastics

Solubility parameters of solvents


Solvent Solubility Parameter
Neo-pentane 6.3
n-Hexane 6.6
Diethyl ether 7.4
Di-isopropyl ketone 8.0
Cycohexane 8.2
sec-Amyl acetate 8.3
Carbon tetrachloride 8.6
Piperidine 8.7
Xylene 8.8
Dimethyl ether 8.8
Toluene 8.9
1,2-Dichloropropane 9.0
THF 9.1
Ethyl acetate 9.1
Benzene 9.2
Chloroform 9.3
Methyl ethyl ketone (MEK) 9.3
Trichloroethylene 9.3
Tetrachloroethylene 9.4
Trichloroethane 9.6
Dichloromethane (DCM) 9.7
Cyclohexanone 9.7
Ethylene dichloride 9.8
N,N-Diethyl acetamide 9.9
Acetone 9.9
o-Dichlorobenzene 10.0
Carbon disulfide 10.0
N,N-Diethyl formamide 10.6
n-Butanol 11.4
Cycohexanol 11.4
Acetonitrile 11.9
N,N-Dimethylformamide 12.1
Acetic acid 12.6
Ethanol 12.7
Dimethylsulfoxide 12.9
Formic acid 13.5
Methanol 14.5
Phenol 14.5
Ethylene glycol 14.6
Glycerol 16.5
Water 23.4

42
Analysis of Plastics

Appendix 2
Specific Gravities of Plastics and Compound Ingredients

Specific gravities of polymers


Polymer Specific Gravity
Low density polyethylene 0.92
High density polyethylene 0.96
Polypropylene 0.90
Polyvinyl chloride 1.41
PTFE 2.2
PCTFE 2.1
Polyvinylidene fluoride 1.5
Polyvinylidene chloride 1.7
Crystal polystyrene 1.05
Medium impact polystyrene 1.05
Very high impact polystyrene 1.02
SAN 1.06
Medium impact ABS 1.04-1.07
High impact ABS 1.01-1.04
MBS 1.07-1.10
Polybutylene terephthalate 1.31
Polyethylene terephthalate 1.37
General purpose phenolic resin 1.35
Melamine-phenolic resin 1.5-1.6
Urea-formaldehyde 1.5-1.6
Polysulfone 1.24
Polycarbonate 1.2
Polyphenylene oxide 1.06
Acetal homopolymer 1.43
Acetal copolymer 1.41
Polyimide 1.42
Nylon 4,6 1.18
Nylon 6,6 1.14
Nylon 6 1.13
Nylon 6,10 1.09
Nylon 6,12 1.07
Nylon 11 1.04
Nylon 12 1.02

43
Analysis of Plastics

Specific gravities of plastic compounding ingredients


Ingredient Specific Gravity
Aluminium silicate 2.10
Antimony trioxide 5.40
Bitumen 1.04
Barium sulfate 4.30
Calcium silicate 2.10
Carbon black 1.80
Carnauba wax 0.99
Calcined china clay 2.50
China clay (kaolin) 2.60
Cotton fibre 1.05
Diethylene glycol 1.12
Graphite 2.04
Iron oxide 4.5-5.1
Lanolin 1.08
Calcium oxide (lime) 2.19
Litharge 9.30
Magnesium oxide 3.60
Magnesium carbonate 2.21
Mica 2.80
Mineral oil 0.91
Oleic acid 0.90
Paraffin oil 0.80
Paraffin wax 0.90
Rosin 1.07
Silica 1.95
Stearic acid 0.85
Sulfur 2.05
Talc (magnesium silicate) 2.80
Titanium dioxide (anatase) 3.90
Titanium dioxide (rutile) 4.20
Calcium carbonate 2.65
Zinc oxide 5.55
Zinc stearate 1.10

44
Analysis of Plastics

Abbreviations and Acronyms

AAS atomic absorption spectroscopy


ABS acrylonitrile-butadiene-styrene
amu atomic mass units
APCI atmospheric pressure chemical ionisation
API atmospheric pressure ionisation
ATR attenuated total reflectance
BS British standard
DCM dichloromethane
DMTA dynamic mechanical thermal analysis
DOP dioctyl phthalate
DSC differential scanning calorimetry
Edax energy dispersive analysis
EI electron ionisation
ELS evaporative light scattering
EPA Environmental Protection Agency (US)
ESC environmental stress cracking
ESI electrospray ionisation
EVA ethylene-vinyl acetate copolymer
FID flame ionisation detector
FT Fourier transform
FTIR Fourier transform infrared spectroscopy
GC gas chromatography
GC-MS gas chromatography-mass spectrometry
GPC gel permeation chromatography
HDPE high density polyethylene
HIPS high impact polystyrene
HPLC high performance liquid chromatography
ICP inductively coupled plasma
IR infrared spectroscopy
ISO International Standards Organisation
KE kinetic energy
LALLS low angle laser light scattering
LAMMS laser microprobe mass spectroscopy
LC-MS liquid chromatography-mass spectroscopy
LDPE low density polyethylene
LIMA laser induced mass analysis
LLDPE linear low density polyethylene
MALLS multi-angle laser light scattering
MBS methylmethacrylate-butadiene-styrene

45
Analysis of Plastics

MEK methyl ethyl ketone


micro-TA micro-thermal analysis
Mn number average molecular weight
MSD mass selective detector
Mw weight average molecular weight
Mz Z average molecular weight
NIH National Institute of Health (US)
NIST National Institute of Standards and Technology (US)
NMR nuclear magnetic resonance
NPD nitrogen/phosphorus detector
OVA organic vapour analyser
PE polyethylene
PET polyethylene terephthalate
PMMA polymethylmethacrylate
PP polypropylene
PTFE polytetrafluoroethylene
PVC polyvinyl chloride
Rf Rf value is defined as ‘the distance from the start line on the plate to the analyte spot after
development, divided by the distance from the start line to the solvent front’ and is reasonably
constant for a given TLC plate type and developing solvent
RI refractive index
SAN styrene-acrylonitrile copolymer
SEM scanning electron microscope
SFC supercritical-fluid chromatography
SIMS secondary ion mass spectrometry
SML specific migration limits
TAC triallyl cyanurate
TAIC triallyl isocyanurate
TEM transmission electron microscopy
Tg glass transition temperature
TGA thermogravimetric analysis
THF tetrahydrofuran
TLC thin layer chromatography
Tm melting temperature
TMA thermomechanical analysis
UV ultraviolet
VA vinyl acetate
Vis visible light
XPS X-ray photoelectron spectroscopy
XRD X-ray diffraction
XRF X-ray fluorescence

46
References and Abstracts

Abstracts from the Polymer Library Database

Item 1 were determined by spectroscopic measurement of the


Polymer Testing absorption band area of the stabiliser around 308 nm in
21, No.5, 2002, p.591-5 the UV spectra and 1605 cm -1 in the FTIR spectra,
SPECTROSCOPIC BEHAVIOUR OF POLYVINYL corresponding to benzylidene malonate and benzylidene
ALCOHOL FILMS WITH DIFFERENT malonic groups respectively. Parallel measurements on
MOLECULAR WEIGHTS the free PBH-3 content after chloroform extraction of the
Abd El-Kader K M; Orabi A S photostabiliser from the polymer matrix by UV and gas
Suez Canal,University chromatography showed that in natural weathering
grafting took place in the LDPE film after very short
Details are given of the preparation of PVAL films by a
exposure times of 127 and 168 hours as indicated by UV
casting technique. Optical absorption and transmission
and FTIR respectively. The curves for the photografting
measurements were performed. The identification of
and the free HALS kinetics were similar. The
molecular structures and assignments of energy bands
photografting mechanism was thought to involve a quick
were also studied using FTIR and NMR. Correlations
photoreaction between the methylene double bond of the
between refractive index and molecular weight were
stabiliser and the polymer macroalkyl radicals, with
investigated. 17 refs.
consequent formation of polymer-bonded aminyl
EGYPT
stabiliser derivatives. 24 refs.
Accession no.856878 ALGERIA
Accession no.853710
Item 2
International Journal of Polymeric Materials
Item 4
51, No.4, 2002, p.315-23
Polymer Bulletin
EFFECTS OF CURING TEMPERATURE ON
48, No.1, March 2002, p.43-51
POLY(ETHYLENE TEREPHTHALATE)
PYROLYSIS OF GAMMA-IRRADIATED
Al-Raheil I A
BISPHENOL-A POLYCARBONATE
Mu’tah,University
Navarro-Gonzalez R; Coll P; Aliev R
The effect of cure temperature over the range from 280 CNRS; Mexico,Universidad Nacional Autonoma
to 350C on PETP was investigated and changes in polymer
This work shows the application of quantitative pyrolysis-
structure analysed by various techniques, including DSC,
gas chromatography coupled with infrared spectroscopy
TGA, scanning electron microscopy and hot-stage
and electron impact mass spectrometry in the study of
microscopy. Changes in the crystallisation behaviour of
radiation-induced scission of bisphenol-A polycarbonate
PETP at the different cure temperatures and the
(PC). PC under vacuum was gamma-irradiated using a
morphology of the PETP spherulites are discussed and
60Co source in the dose range from 0.125 to 1.0 MGy.
melting data of the melt crystallised PETP at 215C are
This was followed by flash pyrolysis under an inert
presented. 16 refs.
atmosphere observed by GC-FTIR-MS. Pyrolysis of the
JORDAN
irradiated PC gave different products depending on the
Accession no.856733 dose. Yields of carbon dioxide and methane decreased
with dose whereas those of phenol and 4-methylphenol
Item 3 increased. The yields of benzene and toluene were
Journal of Applied Polymer Science unaffected by irradiation. Analysis of the products in this
84, No.8, 23rd May 2002, p.1524-32 study helped to infer two main pathways for the radiation-
KINETIC STUDY OF HINDERED AMINE LIGHT induced scission of PC that involve carbonate bond
STABILIZER UNDER NATURAL WEATHERING rupture or aliphatic-aromatic bond rupture. 30 refs.
CONDITIONS EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
Kaci M; Hebal G; Benhamida A; Boukerrou A; MEXICO; WESTERN EUROPE
Djidjelli H; Sadoun T Accession no.853698
Bejaia,University
The photografting kinetics of a hindered amine light Item 5
stabiliser (HALS) containing a polymerisable double bond Journal of Polymers and the Environment
in low density polyethylene (LDPE) films was studied 8, No.4, Oct. 2000, p.167-74
under natural weathering conditions. The HALS (PBH- SENSITIVE ELECTROCHEMICAL IMPEDANCE
3, chemical structure shown) was added to the polymer SPECTROSCOPY METHOD FOR DETECTION
at a concentration of 0.3 wt.%. The photografting kinetics OF POLYIMIDE DEGRADATION BY

© Copyright 2002 Rapra Technology Limited 47


References and Abstracts

MICROORGANISMS and permitted the determination of gelation at every point


Gu J-G; Cheng S-P; Liu J; Gu J-D of the profile and weld without the need for calibration
Shenyang,Agricultural University; Nanjing,University; samples. 7 refs.
Beijing,University of Aeronautics & Astronautics; EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
Hong Kong,University UK; WESTERN EUROPE

An electrochemical impedance spectroscopy method was Accession no.852745


evaluated for monitoring the microbial degradation of
polyimides for electronic packaging. A mixed culture of Item 8
fungi isolated from degraded polyimides was used as the Polymer International
microbial inoculum and scanning electron microscopy 51, No.5, May 2002, p.379-85
was employed to examine fungi growing on the surface STUDIES OF CURE KINETICS OF
of the inoculated polyimides. The data from the POLYISOIMIDE BY DIFFERENTIAL SCANNING
microscopic analysis was utilised to further support the CALORIMETRY IN THE SOLID STATE
relationship between changes in the impedance spectra Kim Y J; Son G I; Kim J-H
and microbial degradation of the polyimide. 30 refs. Sung Kyun Kwan,University
CHINA; HONG KONG
Detailed kinetic studies of the thermal imidisation of
Accession no.853552 polyisoimide by DSC are described. Both isothermal and
dynamic methods were used to obtain kinetic parameters
Item 6 and a phenomenological rate equation for estimating the
PVC 2002: Towards a Sustainable Future. Proceedings degree of imidisation as a function of time. 15 refs.
of a conference held Brighton, 23rd-25th April 2002. KOREA
London, IOM Communications Ltd., 2002. Paper 14, Accession no.851649
p.157-65, 21cm, 012
PLATE-OUT IN PVC EXTRUSION
Gilbert M; Varshney N; Van Soom K; Schiller M Item 9
Loughborough,University; Honeywell; Chemson Journal of Adhesion
(Institute of Materials) 76, No.1, 2001, p.55-74
EVALUATING CURE OF A PMDI-WOOD
The results are reported of a study of plate-out in PVC BONDLINE USING SPECTROSCOPIC,
extrusion carried out using several analytical techniques, CALORIMETRIC AND MECHANICAL
including DSC, SEM-EDX, FTIR spectroscopy and laser METHODS
ionisation mass spectrometry. A special die and calibrator Harper D P; Wolcott M P; Rials T G
unit developed to investigate plate-out are illustrated and
Washington State,University; US,Dept.of
the reproducibility of the method evaluated. The effects
Agriculture,Forest Service
of water content and anti-plate-out additives, such as
alumina and silica, on plate-out are discussed and The cure of polymeric diphenylmethane diiso-
mechanisms explaining the formation of plate-out are cyanate(pMDI)/wood bondline in a controlled saturated
proposed. 11 refs. steam environment was monitored using micro-dielectric
AUSTRIA; BELGIUM; EUROPEAN COMMUNITY; EUROPEAN analysis(micro-DEA). Saturated steam environments were
UNION; UK; WESTERN EUROPE produced between 110 and 140C. The degree of cure
Accession no.852750 calculated from micro-DEA was a basis for further
spectroscopic, calorimetric and mechanical evaluation.
Item 7 Interpretation of calorimetric and spectroscopic analysis
PVC 2002: Towards a Sustainable Future. Proceedings revealed a high consumption of isocyanate early in cure.
of a conference held Brighton, 23rd-25th April 2002. Mechanical strength, however, as revealed by lap shear
London, IOM Communications Ltd., 2002. Paper 9, tests, did not develop until late in cure. Low lap shear
p.116-23, 21cm, 012 strengths and a plateau in conversion rates were detected
DETERMINING THE LEVEL OF GELATION BY for samples pressed at 110 and 120C. Several components
ODSC ON PVC WINDOW PROFILES of the analysis suggested that low temperature cure could
Klingenfuss H; Zahn A result in crystal formation, leading to diffusion controlled
Sueddeutsches Kunststoff-Zentrum cure. 24 refs.
(Institute of Materials) USA

The degree of gelation of PVC window profiles and of Accession no.851472


weld beads was investigated using oscillating differential
calorimetry (ODSC). Tests carried out on a PVC dry blend Item 10
revealed that this analytical technique was capable of Journal of Advanced Materials
determining the degree of gelation of very small samples 34, No.2, April 2002, p.33-7

48 © Copyright 2002 Rapra Technology Limited


References and Abstracts

DEGREE OF CURE, HEAT OF REACTION AND was measured from equilibrium melting point depression
VISCOSITY OF 8552 AND 977-3 HM EPOXY data. 50 refs.
RESINS INDIA
Ng S J; Boswell R; Claus S J; Arnold F; Vizzini A Accession no.850061
US,Naval Air Warfare Center; Maryland,University
The heat of cure, degree of cure and viscosity of two epoxy Item 13
resins (Hexcel 8552 and Cytec Fiberite 977-3 HM) were Chichester, John Wiley & Sons, 1999, pp.xiv,409.
investigated using a modulated differential scanning 23cm. 911
calorimeter and a rheometric digital analyser. MICROSTRUCTURAL CHARACTERISATION
Mathematical models were developed to correlate the rate OF MATERIALS
of the degree of cure and the viscosity with the degree of Brandon D; Kaplan W D
cure and used to predict the kinetic behaviour of the epoxy Haifa,Technion Institute
resins, which was then compared with that of Hercules This unreferenced book describes the technical and
3501-6. A comparison was also made of cure models theoretical aspects of a wide range of techniques for studying
developed based on neat and prepreg forms of the the microstructure of materials, including X-ray and electron
viscosity data. 6 refs. diffraction; optical microscopy, including polarised optical
USA microscopy and interference microscopy; transmission and
scanning electron microscopy; X-ray microanalysis; electron
Accession no.850900
energy loss spectroscopy; and surface analysis by
photoelectron spectroscopy, Auger electron spectroscopy,
Item 11 and secondary ion mass spectrometry. The techniques are
Polymers & Polymer Composites described from sample preparation through information
10, No.3, 2002, p.237-48 acquisition to interpretation of results. A final chapter
CURE BEHAVIOUR AND STRUCTURE OF describes the derivation of quantitative structural data from
DICYANATE-EPOXY NOVOLAC BLENDS the results of these techniques. Examples used in the
Guo B; Fu W; Jia D; Qiu Q; Wang L book mainly involve highly ordered materials such as
South China,University of Technology metals and inorganic crystalline materials, but many of
the techniques used are applicable to polymers. Problems
The objectives of this work are to investigate the cure
for the reader are included.
behaviour and structure of bisphenol A dicyanate-novolac
ISRAEL
epoxy blends. The cure characteristics were investigated
by gel time determination and dynamic DSC. To disclose Accession no.849739
the structural differences between cured cyanate-novolac
epoxy blends and more traditional cyanate-diglycidyl Item 14
ether systems, FTIR investigations were performed on Polimeros: Ciencia e Tecnologia
the two kinds of blends, and in situ FTIR was used to 11, No.4, Oct./Dec.2001, p.213-21
examine the Bauer mechanism. The effects of epoxy Portuguese
concentration in the blend on the cure kinetics was NEAR-INFRARED SPECTRA OF
investigated using two blends with different molar ratios, POLYSTYRENE, POLY(METHYL
and in situ FTIR. 33 refs. METHACRYLATE) AND POLYCARBONATE
CHINA
De Araujo S C; Kawano Y
Sao Paulo,Instituto de Quimica
Accession no.850546
The near-infrared (NIR) spectra of amorphous polymers
PS, PMMA and polycarbonate (PC) are studied. The
Item 12
tentative assignment of the overtone and combination
Macromolecular Chemistry & Physics
frequencies is made using the curve fitting calculations and
203, No.4, 15th March 2002, p.653-62
the local mode theory. Anharmonicity correction and
MISCIBILITY AND CRYSTALLIZATION
mechanical frequency are determined from a Birge-Sponer
BEHAVIOUR OF POLYETHYLENE
plot. A tentative assignment of stretch overtone frequency
TEREPHTHALATE/POLYVINYLIDENE
of CH2 and CH functional groups of PS; CH3 and CO
FLUORIDE BLENDS
functional groups of PMMA; and CH, CH3 and CO
Rahman M H; Nandi A K
functional groups of PC is made. An anharmonicity
Indian Association for the Cultivation of Science
correction of 57 and 58 cm-1 is obtained for CH2 and CH
The miscibility of PETP and PVDF was studied. The Tg, stretch modes of PS; 59 and 9 cm-1 for CH3 and CO stretch
melting point, the crystallisation temperature and the modes of PMMA; and 53, 59 and 10 cm-1 for CH, CH3
crystallinity values of the blends of different and CO stretch modes of PC, respectively. 21 refs.
compositions, prepared at different conditions were BRAZIL
measured. The polymer-polymer interaction parameter Accession no.849333

© Copyright 2002 Rapra Technology Limited 49


References and Abstracts

Item 15 Item 17
Macromolecules Injection Molding
35, No.7, 26th March 2002, p.2667-75 10, No.1, Jan. 2002, p.40-4
THERMAL PROPERTIES OF CROSS-LINKED THE MATERIALS ANALYST: PART 50. THE
POLYISOPROPYLACRYLAMIDE, CASE OF THE DISAPPEARING CONTAMINANT
POLYMETHACRYLIC ACID, THEIR RANDOM Sepe M
COPOLYMERS, AND SEQUENTIAL Dickten & Masch Mfg.
INTERPENETRATING POLYMER NETWORKS A report is presented on the diagnosis of the failure of a
Diez-Pena E; Quijada-Garrido I; Frutos P; Barrales- component made from a 33% glass-reinforced nylon 66
Rienda J M on the assembly line with the aid of DSC, thermal
CSIC gravimetric analysis, which was utilised to determine filler
The thermal properties of polyisopropyl acrylamide, content and type, X-ray fluorescence and IR spectroscopy.
polymethacrylic acid, isopropyl acrylamide-methacrylic The analytical procedures employed indicated that failure
acid copolymers and their blends were investigated by of the component could be attributed to the presence of
DSC and TGA. The state of the water was studied on the chlorine probably arising from contamination of the
basis of DSC traces of swollen samples. The Tg of the process by PVC.
same series of materials was also measured. 64 refs. USA
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; Accession no.848744
WESTERN EUROPE
Accession no.849122 Item 18
Journal of Polymer Science: Polymer Physics Edition
Item 16 40, No.5, 1st March 2002, p.434-53
Applied Spectroscopy FREE VOLUME, GLASS TRANSITION, AND
56, No.2, Feb.2002, p.187-91 DEGREE OF BRANCHING IN METALLOCENE-
RAMAN MICROSCOPY AND MAPPING AS A BASED PROPYLENE/ALPHA-OLEFIN
PROBE FOR PHOTODEGRADATION IN COPOLYMERS: POSITRON LIFETIME,
SURFACE RELIEF GRATINGS RECORDED ON DENSITY, AND DIFFERENTIAL SCANNING
LAYER-BY-LAYER FILMS OF CONGO RED/ CALORIMETRIC STUDIES
POLYELECTROLYTE Dlubek G; Bamford D; Rodriguez-Gonzalez A;
Constantino C J L; Aroco R F; He J A; Zucolotto Z; Li Bornemann S; Stejny J; Schade B; Alam M A; Arnold M
L; Olveira O N; Kumar J; Tripathy S K Bristol,University; ITA Institut fuer Innovative
Windsor,University; Lowell,Massachusetts University Technologien GmbH; Martin-Luther-Universitat Halle

Raman microscopy, mapping and surface-enhanced Results of the above studies are presented and are
Raman scattering techniques are applied to investigate discussed with particular reference to Tg and degree of
the degradation of Congo Red (CR) in a surface relief branching, local free volume and degree of branching,
grating (SRG) recorded on electrostatically assembled local free volume and Tg, specific volume and degree of
layer-by-layer film of CR alternated with polydimethyl branching, and number density of holes and degree of
diallylammonium chloride (PDAC). Photoinduced branching. 56 refs.
degradation is suggested by a decrease in the Raman bands EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
UK; WESTERN EUROPE
assigned to CR with a concomitant increase in the
background signal. More degradation is observed in the Accession no.848572
valleys of the SRG, which correspond to the most
illuminated areas. In a line mapping across the SRG, the Item 19
Raman intensity of CR bands follows the modulation of Polymer Preprints. Volume 42. Number 2. Fall 2001.
the grating, which indicates that photodegradation of CR Proceedings of a conference held Chicago, Il., 7th-11th
contributes at least partially to the SRG formation. April 2002.
Surface-enhanced resonance Raman scattering (SERRS) Washington, D.C., ACS,Div.of Polymer Chemistry,
indicates that the phenyl ring groups are located at the 2001, p.13-4
film surface. Mapping of the Raman signal over many POSITRON ANNIHILATION SPECTROSCOPY
periods of SRG shows that, within the limits of detection, AS A NOVEL SURFACE PROBE OF POLYMERS
the chromophores appear to be oriented in much the same Jean Y C; Zhang R; Mallon P; Chen H; Huang C-M; Li
way throughout the film. They have no preferred Y; Zhang J; Huang Y Y; Sandreczki T C; Wu Y
orientation in the peaks and valleys of the SRG after the Missouri-Kansas City,University
recording process is completed. 23 refs. (ACS,Div.of Polymer Chemistry)
CANADA; USA Positron annihilation spectroscopy (PAS) is a special non-
Accession no.848921 destructive evaluation (NDE) technique for materials

50 © Copyright 2002 Rapra Technology Limited


References and Abstracts

characterisation, which uses the positron (anti-electron). Item 21


Positron-electron annihilation gamma-rays reveal useful Macromolecules
information about the electronic and defect properties of 35, No.5, 26th Feb. 2002, p.1797-804
materials under study. The unique repulsive force between LIQUID CHROMATOGRAPHY OF SYNTHETIC
the positron and the ion cores of materials makes the POLYMERS UNDER CRITICAL CONDITIONS.
positron ideal for probing defects at the atomic and THE CASE OF SINGLE ELUENTS AND THE
molecular levels. In recent years, PAS was developed as a ROLE OF THETA CONDITIONS
useful tool to probe the microscopic properties of polymeric Macko T; Hunkeler D; Berek D
materials. One of the great successes in this line of research Swiss Federal Institute of Technology; Slovak
is the direct determination of polymer free volume and hole Academy of Sciences
properties at an atomic scale (0.2-2 nm). Most existing PAS
PMMA, polybutyl methacrylates and polystyrenes in
studies emphasise the bulk of polymers in measuring
various solvents were investigated with bare silica gel
positron annihilation lifetime. Recently, another method
and silica C18 bonded phases. The effect of variations in
of positron annihilation radiation, Doppler broadening of
eluent nature on polymer retention is discussed. Critical
energy spectra, coupled with a slow positron beam, has
conditions were identified in some single eluents which
been developed to examine the defect profile near the
are thermodynamically poor solvents for the polymers.
surface. The results of experiments on the photodegradation
37 refs.
of polymer-based coatings induced by 313 nm UV
SLOVAK REPUBLIC; SLOVAKIA; SWITZERLAND; WESTERN
irradiation as studied by slow positron annihilation EUROPE
spectroscopy are reported and correlated with gloss
Accession no.847047
measurements. The sub-nanometer defect S parameter is
found to decrease with exposure time. Current results
suggest that the slow positron technique is a sensitive tool Item 22
for detecting degradation of polymers in a time much earlier Macromolecules
than for any existing testing methods. It is particularly 35, No.5, 26th Feb. 2002, p.1677-84
sensitive to the surface defect properties. Applications of LOW-TEMPERATURE CRYSTALLIZATION OF
PAS to systems of polymers and fillers appear to be ETHYLENE-RAN-PROPYLENE COPOLYMERS.
interesting to investigate in the near future. 6 refs. CONFORMATIONAL REARRANGEMENT OF
USA SEQUENCES DURING THE FORMATION OF
Accession no.847946 THE AGGREGATES
Bracco S; Comotti A; Simionutti R; Camurati I;
Sozzani P
Item 20 Milan,University; Basell Spa
Adhesives & Sealants Industry
9, No.1, Feb. 2002, p.38-40 Low-temperature crystallisation of ethylene-propylene
ENHANCED DSC INSTRUMENTATION copolymers was followed by DSC and solid-state NMR.
IMPROVES DESIGN AND The trans conformation fraction identifying the aggregates
CHARACTERIZATION OF ADHESIVES was detected for all temperatures independent of thermal
Cassel R B history. 41 refs.
TA Instruments EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
WESTERN EUROPE
The use of differential scanning calorimetry (DSC) for the Accession no.847031
characterisation and development of adhesive products is
discussed. The Q Series DSC with Advanced Tzero
Technology from TA Instruments is described, with Item 23
reference to the advantages it affords as a new and enhanced Macromolecular Materials and Engineering
tool for improved design and characterisation of adhesives. 286, No.7, 27th July 2001, p421-8
The development incorporates a new measurement THERMOGRAVIMETRY OF THERMOPLASTIC
principle with an additional sensor that together provide POLYIMIDE POWDERS UNDER FOUR
compensation for intrinsic instrument distortion of the DSC DIFFERENT ATMOSPHERES
signal. With distortion virtually eliminated, it is possible Xin-Gui Li; Mei-Rong Huang; He Bai; Yu-Liang Yang
to measure specific-heat capacity directly in a single scan, Tongji,University; Tianjin Customs Central Laboratory;
and to achieve greater sensitivity and accuracy. Analysis Fudan,University
time is also reduced, especially for modulated temperature The high resolution thermogravimetry technique uses a
differential scanning calorimetry. It’s use in curing analysis variable heating rate response to changes in the weight
of a two-part epoxy, and of pressure-sensitive adhesives is loss rate to both reduce test times and improve definition.
demonstrated. 3 refs. The thermal degradation of a thermoplastic polyimide
USA polymer in nitrogen, helium, argon and air was analysed
Accession no.847415 using both conventional and high resolution

© Copyright 2002 Rapra Technology Limited 51


References and Abstracts

thermogravimetric analysis techniques. It was concluded state-of-the-art FTIR spectroscopy can be used. From the
that the thermal degradation results varied with both chromatographic and spectroscopic data, contour
atmosphere and test technique with the high resolution diagrams are generated that present the molecular
technique providing more precise data in the inert heterogeneity of the sample in the coordinates molar mass
atmosphere tests but less resolution in air. and chemical composition. 17 refs.
Thermogravimetric analysis data for a number of EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
polyimide polymers is tabulated. The thermoplastic WESTERN EUROPE
polyimide polymer evaluated was more thermally stable Accession no.846265
than many other polyimides. Complete details of the test
techniques are given with full discussion of the results.
Item 26
40 refs.
Polymer
CHINA
43,No.6,2002,p.1835-47
Accession no.846773 THERMAL DEGRADATION OF PET AND
ANALOGOUS POLYESTERS MEASURED BY
Item 24 THERMAL ANALYSIS-FOURIER TRANSFORM
Journal of Applied Polymer Science INFRARED SPECTROSCOPY
83, No.12, 2002, p.2522-7 Holland B J; Hay J N
CRYSTALLIZATION AND CROSSLINKING OF Birmingham,University
POLYAMIDE-1010 UNDER ELEVATED
The thermal degradation of two commercial PET samples
PRESSURE
and two laboratory prepared polyesters, poly(ethylene
Jun Yang; Wenfei Dong; Yucheng Luan; Jingjiang Liu;
isophthalate) and poly(diethylene glycol terephthalate),
Shue Liu; Xingguan Guo; Xudong Zhao; Wenhui Su
was studied using thermogravimetry and thermal analysis-
Changchun,Institute of Applied Chemistry;
FTIR. The commercial PET samples were copolymerised
Jilin,University
with diethylene glycol and isophthalic acid groups in
This study looked at the structural changes to polyamide- different proportions, and their thermal stabilities were
1010 (PA1010) when it was treated at 250 degC for 30 found to differ. Through a study of the thermal degradation
min at a pressure of 0.7-2.5 GPa. Crystals grew when the of poly(diethylene glycol terephthalate) and poly(ethylene
pressure was below 1.0 GPa or above 1.2 GPa. isophthalate), it was found that diethylene glycol and
Crosslinking occurred in the pressure range 1.0-1.2 GPa. isophthalate units promoted thermal degradation through
DSC and wide angle x-ray diffraction showed that PA1010 increased chain flexibility and more favourable bond
lost its crystallisation ability after treatment at pressures angles, respectively. The thermal degradation of all the
of 1.0-1.2 GPa. Crystallised PA1010 had a greater thermal polyesters tested led to the formation of non-volatile
stability than crosslinked PA1010 at 400 degC. 20 refs. residue. IR spectroscopic analysis indicated that the
CHINA residue consisted almost exclusively of interconnected
Accession no.846587 aromatic rings. 21 refs.
EU; EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE; WESTERN EUROPE-GENERAL
Item 25
Kautchuk und Gummi Kunststoffe Accession no.846155
55, No.1-2, 2002, p.9-14
German Item 27
ANALYSIS OF TECHNICAL POLYMER BLENDS Progress in Organic Coatings
WITH COUPLING OF LIQUID 43, No.4, Dec.2001, p.226-32
CHROMATOGRAPHY WITH FTIR SIMPLE RAMAN TECHNIQUE TO MEASURE
SPECTROSCOPY THE DEGREE OF CURE IN UV CURABLE
Pasch H; Rode K; Kloninger C; Esser E COATINGS
Deutsches Kunststoff-Institut Nichols M E; Seubert C M; Weber W H; Gerlock J L
Ford Research Laboratory
The coupling of liquid chromatography with FTIR
spectroscopy provides a new and interesting method for The curing of four UV-curable clearcoats was studied by
the detailed analysis of complex polymer systems. The confocal Raman microscopy. The disappearance of the
application of this hyphenated technique to the analysis C:C line near 1636/cm provided the signature for the
of polymer blends shows that it is possible to identify the curing of the samples, but quantification of the degree of
different blend components by their spectral cure by standard peak fitting and baseline subtraction
characteristics. Components of different chemical methods did not work well because of sample
compositions are determined selectively and their fluorescence, baseline shifts and overlapping peaks. A
chemical structure is analysed through well-resolved smoothed second-derivative processing approach
FTIR spectra. For structure elucidation, all facilities of overcame all of these difficulties and provided a simple,

52 © Copyright 2002 Rapra Technology Limited


References and Abstracts

rapid and objective quantification procedure. Steep cure average molec.wts. of the samples, as received and
gradients through the thickness of the clearcoat, due to purified, were determined by VPO in two different
screening of the bottom of the clearcoat by both the UVA solvents, trichloromethane and THF. Viscometric average
and photoinitiator, were observed. Cure gradients at the molec.wts. were obtained in trichloromethane at 25C. Five
top of the clearcoat due to oxygen inhibition were also different equations were used to calculate intrinsic
observed. The most complete cure throughout the film viscosities and viscometric constant values. Relative
thickness was obtained with a mixture of standard and molec.wts. and polydispersities were determined by SEC,
red-shifted photoinitiators. 9 refs. in THF at 35C and in trichlorobenzene at 135C. It was
USA confirmed that the results obtained in the latter solvent
Accession no.846135 were in better agreement with those obtained by the other
techniques. 25 refs.
Item 28 BRAZIL
Polymer Accession no.845967
43, No.5, 2002, p.1587-97
FULL COPOLYMER CHARACTERIZATION BY Item 30
SEC-NMR COMBINED WITH SEC-MALDI Plastics Engineering
Montaudo M S 58, No.2, Feb. 2002, p.40/55
CNR PLASTICS ANALYSIS - THE ENGINEERS
Random copolymers with units of methyl methacrylate, RESOURCE FOR TROUBLESHOOTING
butyl acrylate, styrene and maleic anhydride were studied PRODUCT AND PROCESS PROBLEMS AND
by fractionating the copolymer by size exclusion FOR COMPETITIVE ANALYSIS
chromatography(SEC), collecting 30 to 40 fractions and Ezrin M
then recording both the NMR and MALDI spectra of the Connecticut,University
fractions. In a successive step, bivariate distribution of Methods for competitive analysis, troubleshooting process
chain sizes and composition maps were derived from and product problems, plastics analysis, analysis of failed
knowledge of the molar mass, weight and composition products and analysis of polymeric formulations are
of the copolymer fractions. The compositional distribution discussed. Procedures covered include FTIR spectroscopy,
was obtained by summation of the sections of the bivariate Raman spectroscopy, NMR spectroscopy, surface analysis
distribution which belonged to a narrow compositional by spectroscopy, gas chromatography/mass spectrometry,
range. A model for SEC fractionation of copolymers was atomic force microscopy and techniques for analysing
developed which allowed prediction of the composition unidentified formulations. 47 refs.
and D(x) of the SEC fraction, D(x) being the ratio between
USA
the number-average and the weight-average molar mass,
with x being the fraction number. Off-line SEC-MALDI Accession no.845139
measurements were performed in order to measure D(x)
experimentally for the random copolymers. 31 refs. Item 31
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; Journal of Applied Medical Polymers
WESTERN EUROPE 5, No.2, Autumn 2001, p.77-9
Accession no.846119 NOVEL TECHNIQUE FOR THE DETECTION OF
A HINDERED AMINE LIGHT STABILIZER,
Item 29 BASED ON SILICON TECHNOLOGY
Polymer Testing Narayan S; Lee R E; Hallberg D; Malatesta V
21, No.2, 2002, p.155-61 Great Lakes Chemical Corp.; Great Lakes Chemical
BISPHENOL A-BASED POLYCARBONATES: Italia
CHARACTERIZATION OF COMMERCIAL Details are given of the development of a novel method
SAMPLES to detect the presence of a hindered amine light stabiliser
Delpech M C; Coutinho F M B; Habibe M E S in PP, based on silicon technology. The method consisted
Rio de Janeiro,Universidade Federal; Rio de of extracting the stabiliser from the PP matrix followed
Janeiro,Universidade Estadual; Polialden Petroquimica SA by detection and quantification using proton NMR. 3 refs.
Samples of bisphenol A polycarbonate were characterised EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; USA;
by DSC, TGA, FTIR spectroscopy, size exclusion WESTERN EUROPE
chromatography(SEC), vapour pressure osmometry Accession no.844622
(VPO) and viscometry. The samples exhibited the same
FTIR spectrum profile and almost the same values of Tg Item 32
and initial temp. of degradation. Slight differences were, Adhasion Kleben & Dichten
however, observed in differential TGA curves, which 45, No.12, 2001, p.34-8
could be due to the presence of additives. The number- German

© Copyright 2002 Rapra Technology Limited 53


References and Abstracts

NON-DESTRUCTIVE NUCLEAR MAGNETIC Item 34


RESONANCE CONTACT TECHNIQUE - Journal of Applied Polymer Science
EXAMPLES AND POSSIBILITIES 83, No.5, 31st Jan.2002, p.956-66
Hartwig A; Wolter B SAFETY ASSESSMENT OF POLYMERIC
Fraunhofer-Institut fuer Ang.Materialforschung; ADDITIVES FOR FOOD PACKAGING:
Bundesministerium fuer Wirtschaft; DECHEMA HYDROLYSIS OF POLYMERIC PLASTICISERS
BY DIGESTIVE FLUIDS
On page 25 of the November 2001 issue of Adhaesion, Hamdani M; Thil L; Gans G; Feigenbaum A E
Kleben & Dichten, the nuclear magnetic resonance Institut National de la Recherche Agronomique; BASF AG
contact technique was introduced as a new sort of method
for non-destructive characterisation of polymers. This The safety of polymeric plasticisers capable of migrating
article uses examples from the area of epoxy resins and into food was assessed by an in vitro study of the hydrolysis
thick-layer bondings to give an impression of typical, of poly(1,2-propylene adipate) (PPA) by digestive fluid
potential applications for this new non-destructive testing liquids. Freshly prepared simulated intestinal fluid solutions
method. 2 refs. produced a high degree of hydrolysis. As indicated by high
performance size exclusion chromatography, the bulk
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
WESTERN EUROPE plasticiser disappeared completely, and low molecular
weight oligomers were produced within 4 hours. Gas-phase
Accession no.844288
chromatography indicated no significant conversion to free
monomers after hydrolysis, and NMR tests showed that
Item 33 the cleavage selectivity occurred selectively at primary ester
Applied Spectroscopy linkages. Silica gel fractionation of the hydrolysate gave
55, No.12, Dec.2001, p.1729-32 six oligomeric fractions, which were recovered and
FORENSIC ANALYSIS OF SINGLE FIBRES BY analysed. Proton NMR was used to evaluate the absolute
RAMAN SPECTROSCOPY molecular weight of the plasticisers and the hydrolysis
Miller J V; Bartick E G products. Under simulated gastric and saliva conditions the
Washington G.,University; US,FBI degree of hydrolysis was less than 2%. 3 refs.
Microscopical analysis by FT-IR spectroscopy has been EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
GERMANY; WESTERN EUROPE
the preferred method for obtaining additional information
on the polymeric composition of a fibre. It allows Accession no.842741
unequivocal determination of the generic class and
frequently permits sub-classification. FT-IR analysis Item 35
cannot be conducted while the fibre is mounted due to Journal of Applied Polymer Science
the strong absorption of IR radiation by glass. The fibre 81, No.7, 15th Aug.2001, p.1588-94
must be removed from the slide and rinsed to clean off CHARACTERIZATION OF BRANCHED
the mounting medium before preparing the fibre. This POLYMERS BY SIZE EXCLUSION
increases sample preparation time and the chance for CHROMATOGRAPHY COUPLED WITH
sample loss. Glass produces little response to Raman MULTIANGLE LIGHT SCATTERING
spectroscopy. Therefore, Raman analysis of fibres can be DETECTOR. I. SIZE EXCLUSION
conducted while the fibre remains mounted on a glass CHROMATOGRAPHY ELUTION BEHAVIOR OF
slide under coverslips. The theoretical beam width of the BRANCHED POLYMERS
laser is 0.8 mu m; thus, Raman will potentially permit Podzimek S; Vlcek T; Johann C
measurement of microfibres used in some fabrics in the Wyatt Technology Corp.; Pardubice,University; Wyatt
current market. The samples do not need to be thinned or Technology Deutschland GmbH
flattened, as with IR, because the photons are scattered The elution behaviour of randomly branched PS and star-
from the surface and not transmitted through the sample. branched poly(benzyl methacrylate) with different levels
The current literature contains limited reports and citations of branching was studied by size exclusion
on the use of Raman microprobe spectroscopy for forensic chromatography (SEC) coupled with a multiangle light
analysis of fibres. It has previously been shown that it is scattering detector. The highly branched polymers showed
possible to scan fibres while they are taped onto a glass abnormal SEC elution behaviour. After normal elution at
slide. By the same sample preparation method, it has been small elution volumes, the molar mass and root mean
demonstrated that it is possible to differentiate between square radius of the eluting molecules increased with
several generic and sub-generic classes of fibres. It is increasing elution volume. Reasons for this were explored
illustrated that it is possible to scan through a glass and discussed. SEC separation was compared with
coverslip and mounting medium to obtain polymeric separation by thermal field flow fractionation. 8 refs.
identification of non-dyed fibres. 14 refs. CZECH REPUBLIC; EUROPEAN COMMUNITY; EUROPEAN
USA UNION; GERMANY; USA; WESTERN EUROPE
Accession no.843701 Accession no.842695

54 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Item 36 Item 38
Revista de Plasticos Modernos Synthetic Metals
81, No.538, April 2001, p.461-6 124, No.2-3, 22nd Oct.2001, p.407-14
Spanish STUDY OF THE SURFACE POTENTIAL AND
APPLICATION OF INFRARED SPECTROSCOPY PHOTOVOLTAGE OF CONDUCTING
AND THERMAL ANALYSIS IN MONITORING POLYMERS USING ELECTRIC FORCE
THE CURE OF THERMOSETTING RESINS MICROSCOPY
USED IN THE AIRCRAFT INDUSTRY Barisci J N; Stella R; Spinks G M; Wallace G G
Sanchez-Blazquez A Wollongong,University
CASA The effect of the polymer composition, preparation
The amine cure of Hexcel 8552 epoxy resin, for use as method and nature of the substrate on the surface potential
the matrix in carbon fibre-reinforced composites for (SP) of conducting polymer films is investigated. Both
application in aircraft construction, was monitored by the average value and the distribution of SP across the
near-infrared spectroscopy. This technique was validated polymer surface are influenced by these factors.
by comparison of the results with those obtained by Polythiophenes, potentially useful for solar energy
modulated DSC. 18 refs. conversion, are used to examine the generation of light-
induced changes in SP. Results suggest the possibility of
HEXCEL COMPOSITES determining the local variations of the surface
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
WESTERN EUROPE photovoltage and the photovoltaic properties of polymer
films intended for use in photovoltaic devices. 16 refs.
Accession no.842573
AUSTRALIA
Accession no.842093
Item 37
Progress in Colloid & Polymer Science
Vol.117, 2001, p.167-71 Item 39
SURFACE CHARACTERISATION OF Polymer Degradation and Stability
POLYLACTIDE/POLYGLYCOLIDE 75, No.1, 2002, p.185-91
COPOLYMERS STUDY ON METHANOLYTIC
Kiss E; Lam C N C; Due T M; Vargha-Butler E I DEPOLYMERIZATION OF PET WITH
Budapest,Eotvos Lorand University; SUPERCRITICAL METHANOL FOR
Toronto,University; Biophy Research CHEMICAL RECYCLING
Yong Yang; Yijun Lu; Hongwei Xiang; Yuanyuan Xu;
The wettability and the surface composition of Yongwang Li
biodegradable polymers used as drug delivery particles Chinese Academy of Sciences
are determined and compared. Films of polylactic acid,
polyglycolic acid and their copolymers with four different Polyethylene terephthalate (PET) was subjected to
lactide, glycolide ratios of 85/15, 75/25, 65/35 and 50; methanolytic depolymerisation with supercritical
50 are formed by solvent-casting on polar (silicone wafer methanol in a stirred stainless steel autoclave at
glass and silica) substrates. Advancing and receding water temperatures of 523-543 deg.C, pressure 8.5-14.0 MPa,
contact angles are measured goniometrically and also by and a 3-8 methanol to PET weight ratio. The solid products
using the automated axisymmetric drop shape analysis obtained, consisting mainly of dimethyl terephthalate and
method. Both the advancing and the receding water small amounts of methyl-(2-hydroxyethyl) terephthalate,
contact angles of the copolymers are higher than expected bis(hydroxyethyl) terephthalate, dimers, and oligomers,
from the values obtained for the two homopolymers were analysed by high performance liquid
considering the increasing glycolide content of the chromatography (HPLC), and the liquid products, mainly
copolymers. Surface analysis of the polyester films is ethylene glycol and methanol were analysed by gas
performed by X-ray photoelectron spectroscopy at various chromatography (GC). The temperature, weight ratio of
take-off angles to get information on the depth distribution methanol to PET, and the reaction time had a very marked
of the components. Surface enrichment of the nonpolar effect on dimethyl terephthalate yield and the degree of
(lactide) component in the outermost layer of the PET depolymerisation, but the effect of pressure was
copolymer films is detected. The wettability behaviour is insignificant above the methanol critical point. The
in accordance with the surface composition, results optimum PET depolymerisation conditions were:
suggesting a surface activity effect resulting in the temperature 533-543 K, pressure 9.0-11.0 MPa, and a
orientation of the nonpolar segments of the copolymer methanol to PET weight ratio of 6-8. The
chains towards the surface of the film and hence producing depolymerisation of several PET wastes from the Chinese
more hydrophobic character for the copolymer films than market was studied under the optimum conditions. 28 refs.
should be due to their bulk composition. 20 refs. CHINA
Accession no.842190 Accession no.841527

© Copyright 2002 Rapra Technology Limited 55


References and Abstracts

Item 40 EFFECTS OF THE STERILISATION METHOD


Polymer Degradation and Stability ON THE WEAR OF UHMWPE ACETABULAR
75, No.1, 2002, p.153-9 CUPS TESTED IN A HIP JOINT SIMULATOR
THE EFFECT OF ULTRAVIOLET STABILISERS Affatato S; Bordini B; Fagnano C; Taddei P; Tinti A;
ON THE PHOTODEGRADATION OF Toni A
POLY(ETHYLENE TEREPHTHALATE) Bologna,Istituti Ortopedici Rizzoli; Bologna,Universita
Fechine G J M; Rabello M S; Souto-Maior R M
Details are given of the effects of sterilisation methods
Pernambuco,Federal University; Paraiba,Universidad
on the wear and changes in physical properties of ultra-
Federal
high molecular weight PE acetabular cups. The
The weathering behaviour of polyethylene terephthalate crystallinity of the cups was evaluated by micro-Raman
(PET) samples obtained by bi-axial tension in the spectroscopy as a function of the inner surface position.
laboratory over a period of up to about 1100 hours was The partial least square calibration was used to correlate
studied. The mechanical properties of films obtained from the Raman spectra with the crystallinity of the polymer
the samples having different types of UV stabilisers, e.g. measured by DSC. 52 refs.
a triazine ultraviolet absorber (Tinivin 1577), carbon EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
black, or a TiO2/BaSO4 mixture, were tested, and the WESTERN EUROPE
films were examined by UV-VIS spectroscopy, titration, Accession no.840964
size exclusion chromatography, and FTIR. The results
showed that the unstabilised films were easily degraded,
Item 43
resulting in considerable deterioration in mechanical
Polymer Preprints. Volume 41. Number 2. Conference
properties and a molecular weight decrease. The triazine
proceedings.
was the most effective stabiliser. 38 refs.
Washington, D.C., 20th-24th Aug.2000, p.1792-3
BRAZIL
CHARACTERISATION OF PLANT FIBRES BY
Accession no.841524 INFRA-RED SPECTROSCOPY
Garside P; Wyeth P
Item 41 Southampton,University
Polymer Degradation and Stability (ACS,Div.of Polymer Chemistry)
75,No.1, 2002, p.123-9 The application of IR spectroscopy with respect to the
INITIAL STEPS AND EMBRITTLEMENT IN characterisation of cellulosic (plant) fibres is
THE THERMAL OXIDATION OF STABILISED demonstrated. The ability to characterise fibres is of
POLYPROPYLENE FILMS importance to textile conservators, as this information aids
Fayolle B; Audouin L; Verdu J in the determination of the age and origin of the artefact
Ecole Nationale Superieure des Arts et Metiers from which they are taken, and may influence the choice
Physicochemical and mechanical characterisation of treatment. The fibres under examination are taken
methods were used to study the oxidation of 100 micron largely from the bast group (flax, hemp, jute and ramie);
stabilised polypropylene films at 130 deg.C in air. in addition, sisal and cotton are compared. FT-IR
Stabiliser consumption (UV spectrophotometry) and microspectroscopy and ATR techniques are employed. To
molecular weight decrease (steric exclusion complement the conventional use of these methods, the
chromatography) could be observed during the induction inherent polarisation effects of the equipment are
period, when no carbonyl build-up could be detected by exploited to record polarised IR spectra. Jute, sisal and
IR spectroscopy. These structural modifications had an cotton are readily differentiated, but flax, hemp and ramie
effect on the fracture properties, as indicated by the prove more difficult to distinguish. Peak ratio techniques
essential work of fracture (EWF) method, whereas the are applied in the latter case. 2 refs.
ultimate tensile elongation showed no significant changes. EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
The results show that the EWF method is useful for WESTERN EUROPE
characterising the degradation induced embrittlement of Accession no.840045
initially ductile polymers. The experimental data reported
suggest that the problem of the spatial heterogeneity of
Item 44
the oxidation process requires further discussion. 21 refs.
Journal of Coatings Technology
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; 73, No.923, Dec. 2001, p.43-50
WESTERN EUROPE
ON THE USE OF THE ATOMIC FORCE
Accession no.841521 MICROSCOPE TO MONITOR PHYSICAL
DEGRADATION OF POLYMERIC COATING
Item 42 SURFACES
Biomaterials VanLandingham M R; Nguyen T; Byrd W E; Martin J W
23, No.6, March 2002, p.1439-46 US,National Inst.of Standards & Technology

56 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Changes in the surface properties of a model thermosetting RAMAN SPECTROSCOPY DETERMINATION


acrylic melamine polymeric coating system similar to OF THE THERMOPLASTIC CONTENT WITHIN
systems widely used as automotive clearcoats were EPOXY RESIN-COPOLYETHERSULFONE
followed using atomic force microscopy (AFM). The BLENDS
samples were exposed to a range of relative humidities, van Overbeke E; Devaux J; Legras R; Carter J T;
different temperatures and various UV wavelengths and McGrail P T; Carlier V
a full factorial experimental design was utilised. A Louvain,Universite Catholique; ICI
mechanism for the formation of pits in the surface of the Details are given of the possibility of using Raman
coatings, as observed by AFM, was developed and the spectroscopy to determine the local thermoplastic content
relationship between the chemical and physical within an epoxy resin/copolyethersulphone blend. The
degradation of the coatings discussed. 21 refs. required calibration of the Raman data is presented. The
USA applicability of the calibrations to blends containing
Accession no.839365 chlorine-ended copolyethersulphone is discussed. Results
obtained with small or large Raman confocal holes were
Item 45 also compared. 40 refs.
Polymer Plastics Technology and Engineering BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
UK; WESTERN EUROPE
40, No.5, 2001, p.767-81
STABILISATION OF FREE RADICALS IN Accession no.838755
FILLED OLIGOESTER ACRYLATES
Kadossov E B; Kovarski A L; Kasparov V V; Item 48
Zapadinski B I; Tikhonov A P Polymer Degradation and Stability
Russia,Academy of Science; Mendeleev University of 74, No.2, 2001, p.321-6
Chemical Technology XPS CHARACTERIZATION OF FRIEDEL-
CRAFTS CROSS-LINKED POLYSTYRENE
The results are reported of a study of the formation and
Jianqi Wang; Jianxin Du; Hongyang Yao; Wilkie C A
decay of free radicals during the photocrosslinking of an
Beijing,Institute of Technology; Marquette,University
oligocarbonate methacrylate filled with two types of silica
differing in particle size or hydroxyapatite using ESR The combination of a difunctional alkylating agent, either
spectroscopy. The data are correlated with those obtained hydroxymethylbenzyl chloride or alpha,alpha’-
for molecular mobility using a spin probe and the kinetics dichloroxylene, with PS or high-impact PS together with
of radical accumulation during photocrosslinking are a Friedel-Crafts catalyst, 2-ethylhexyldiphenylphosphate,
discussed along with the kinetics of termination of and an amine for reaction with hydrogen chloride was
radicals. 17 refs. studied by X-ray photoelectron spectroscopy. The results
RUSSIA confirmed the theories proposed from previous
investigations using TGA, i.e. crosslinking of the polymer
Accession no.839176
occurred as the temp. was raised and the alcohol-
containing alkylating agent gave a greater amount of
Item 46 crosslinking than did the dichloro compound. 13 refs.
Revista de Plasticos Modernos CHINA; USA
81, No.537, March 2001, p.345-52 Accession no.838285
Spanish
ANALYSIS OF SYNTHETIC POLYMERS BY
CAPILLARY ELECTROPHORESIS Item 49
Simo C; Barbas C; Cifuentes A Macromolecular Chemistry & Physics
Instituto de Fermentaciones Industriales; San Pablo- 202, No.16, 7th Nov. 2001, p.3228-33
CEU,Universidad CHARACTERIZATION OF THE
CROSSLINKING KINETICS OF A THIN
The principles of the various modes of capillary POLYMERIC LAYER BY REAL-TIME
electrophoresis are examined, and applications of these DIELECTRIC RELAXATION SPECTROSCOPY
techniques in the molecular weight characterisation of Schonhals A; Fritz A; Pfeiffer K
polymers are discussed. 40 refs. Berlin,University; Micro Resist Technology GmbH
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
WESTERN EUROPE The crosslinking kinetics of a thin polymeric layer on a
Accession no.839085 prepolymer of a phthalic acid diallyl ester was studied by
real-time dielectric spectroscopy. Activation energies were
estimated for the reaction using the temperature
Item 47 dependence of the time constant. The change of the
Applied Spectroscopy relaxation rate of the dynamic Tg with the reaction time
55, No.11, Nov. 2001, p.1514-22 was obtained from dielectric loss data. 20 refs.

© Copyright 2002 Rapra Technology Limited 57


References and Abstracts

EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; Item 52


WESTERN EUROPE Polymer
Accession no.838158 42, No.20, 2001, p.8425-34
PHYSICAL AND MECHANICAL PROPERTIES
Item 50 OF POLYETHYLENE FOR PIPES IN RELATION
LCGC Europe TO MOLECULAR ARCHITECTURE. PART I.
14, No.12, Suppl., Dec.2001, p.8/21 MICROSTRUCTURE AND CRYSTALLISATION
CONSIDERATIONS ON COLUMN SELECTION KINETICS
AND OPERATING CONDITIONS FOR LC-MS Hubert L; David L; Seguela R; Vigier G; Degoulet C;
Sandra P; Vanhoenacker G; Lynen F; Li L; Schelfaut M Germain Y
Kortrijk,Research Institute for Chromatography; Institute Nationale des Sciences Appliquees; Atofina
Ghent,University Five high density polyethylene bimodal copolymers with
Mass spectrometry is slowly, but surely becoming the varying molecular architectures designed for pipe
detection system of choice for liquid chromatography applications were tested to evaluate the relationships
analysis in many areas. An overview is presented of between structure properties contributing towards
column and mobile phase selection for LC-MS. Relatively improved end use properties. Crystallisation kinetics were
simple guidelines are advanced to successfully optimise studied in relation to molecular architecture using
LC-MS for several applications. This article discusses the chromatography, density columns, differential scanning
fundamentals of LC related to MS hyphenation, adapting calorimetry, X-ray scattering, rising temperature elution
LC to LC-MS methods, normal-phase liquid fractionation and infrared spectroscopy. From the test
chromatography, supercritical fluid chromatography, results, it was concluded that the normal correlation
reversed-phase liquid chromatography, size exclusion between kinetics, molecular structure and molecular
chromatography, ion-exchange chromatography, affinity topology found with unimodal copolymers does not apply
chromatography and capillary electrophoresis. 25 refs. with bimodal copolymers as the crystal surface free energy
BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION; was sensitive to topological changes resulting from
WESTERN EUROPE architectural molecular changes. Complete details of the
Accession no.837996 experimental procedures and test results are given with
extensive discussion of the background theory and results.
Item 51 60 refs.
Polymer BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
FRANCE; WESTERN EUROPE
42, No.20, 2001, p.8461-7
STATES OF WATER IN DIFFERENT Accession no.837023
HYDROPHILIC POLYMERS - DSC AND FTIR
STUDIES Item 53
Ping Z H; Nguyen Q T; Chen S M; Zhou J Q; Ding Y D LCGC Europe
Fudan,University; Rouen,University 14, No.9, Sept. 2001, p.564/9
Differential scanning calorimetry and Fourier transform INVESTIGATION OF A NOVEL SOL-GEL
infrared spectroscopy techniques were used to study the DERIVED STATIONARY PHASE FOR GAS
structure of water molecules in polyvinyl alcohol and CHROMATOGRAPHY
polyethylene grafted acrylate hydrophilic polymers. Cervini R; Day G; Hibberd A; Sharp G; Froud A
Varying amounts of water were added to test samples and SGE International Pty Ltd.; SGE Europe Ltd.
the samples conditioned to the sorption equilibrium state The effectiveness of using a novel, sol-gel material
in sealed containers for 24 hours prior to evaluation. It was incorporating PEG or wax as a capillary column stationary
concluded that below a threshold water content, depending phase is described. Chromatograms demonstrating
on the polymers physical and chemical structure, water inertness, partitioning capability and robustness for a
molecules absorbed in hydrophilic polymer cannot form range of applications are presented. 10 refs.
ice crystals in the polymer matrix. Above this threshold AUSTRALIA; EUROPEAN COMMUNITY; EUROPEAN UNION;
content, the water crystallises but below zero. It was also UK; WESTERN EUROPE
demonstrated that the absorbed water in hydrophilic Accession no.836916
polymers develops differing hydrogen bonds in the first
and second hydration layers. It was concluded that the
potential influence of these intermolecular interactions Item 54
should therefore be taken into account whenever a polymer Polymer Engineering and Science
is used with a solvent. 25 refs. 41, No.10, Oct.2001, p.1714-30
CHINA; EUROPEAN COMMUNITY; EUROPEAN UNION;
TEMPERATURE MODULATED DSC STUDIES
FRANCE; WESTERN EUROPE OF MELTING AND RECRYSTALLIZATION IN
Accession no.837027 POLY(OXY-1,4-PHENYLENEOXY-1,4-

58 © Copyright 2002 Rapra Technology Limited


References and Abstracts

PHENYLENECARBONYL-1,4- Item 56
PHENYLENE)(PEEK) Revista de Plasticos Modernos
Kampert W G; Sauer B B 81, No.536, Feb.2001, p.244-8
DuPont Central Research & Development Spanish
PERMEABILITY OF METHANOL, TOLUENE,
The thermal and crystal morphological properties of
FUELS AND OXYGENATED FUELS IN AN
amorphous and melt-crystallised PEEK were investigated.
ETHYLENE-VINYL ALCOHOL COPOLYMER
Two different molec.wts. were studied by temp.-
USED AS A BARRIER COMPONENT TO GASES,
modulated DSC(TMDSC) over a broad range of annealing
AROMAS AND HYDROCARBONS
times and temps. The lower molec.wt. PEEK under all
Lagaron J M; Powell A K
crystallisation conditions was found to exhibit secondary
Jaume I,Universitat; BP Chemicals Ltd.
crystal melting in the low endotherm region, followed by
melting of primary crystals superimposed with a large Measurements were made of the permeation rates of
recrystallisation contribution. Primary crystal melting methanol, toluene, a 50/50 toluene/isooctane fuel (fuel
broadly overlapped with melting of the recrystallised C) and fuel C with 10% ethanol or 15% methanol through
species and contributed to the broad highest endotherm. EVOH films. Large scale methanol and water induced
Recrystallisation contributions and the interpretation of plasticisation was suggested by large solvent uptakes and
TMDSC were partially confirmed by independent rapid confirmed by the observation of considerable decreases
heating rate m.p. determinations and variable heating rate in Tg. The permeability of fuel C increased significantly
DSC. The higher molec.wt. PEEK showed many when methanol was present, while the high barrier
similarities but generally had smaller levels of properties of EVOH to hydrocarbons was maintained for
reorganisation above the annealing temp. under most fuel C containing ethanol. 9 refs.
higher temp. crystallisation conditions. TMDSC provided EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK;
good resolution of recrystallisation and related events WESTERN EUROPE
compared with standard DSC. The broad and substantial Accession no.835449
exothermic recrystallisation in amorphous samples was
also examined, showing that recrystallisation continued
Item 57
through the final melting region. 42 refs.
Revista de Plasticos Modernos
USA
81, No.536, Feb.2001, p.236-43
Accession no.836355 Spanish
ETHYLENE-VINYL ALCOHOL COPOLYMERS
Item 55 AND THEIR APPLICATIONS IN FOOD
Macromolecular Symposia PACKAGING
Vol.174, Aug.2001, p.413-34 Cerrada M L
STRATEGIES IN TWO-DIMENSIONAL LIQUID Instituto de Ciencia y Tecnologia de Polimeros
CHROMATOGRAPHIC SEPARATION OF The gas barrier properties of ethylene-vinyl alcohol
COMPLEX POLYMER SYSTEMS copolymers are examined as a function of ethylene and
Berek D vinyl alcohol content, and their use in combination with
Slovak,Academy of Sciences other plastics in films, bottles and other containers for
The separation of complex polymer systems by two- food packaging is discussed. Results are presented of a
dimensional liquid chromatography is discussed. Methods study of the crystal structure of three copolymers having
are reviewed in which the effect of polymer molec.wt. on different compositions. 11 refs.
polymer retention is suppressed. The resulting ‘one EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
WESTERN EUROPE
parameter separation systems’ can be on-line or off-line
connected to another separation system such as size Accession no.835448
exclusion chromatography in order to provide more detailed
characterisation of complex polymers. Selected procedures Item 58
for the re-concentration of diluted polymer solutions are Polymer Preprints. Volume 41. Number 2. Conference
also considered. These could be used for increasing the proceedings.
concentration of sample(s) leaving the first dimension Washington, D.C., 20th-24th Aug.2000, p.1423-4
separation column. Some arrangements for controlled MAPPING CHEMICALLY HETEROGENEOUS
sample re-introduction into the second dimension POLYMER SYSTEM USING CHEMICAL
separation column are outlined. 48 refs. (World Polymer MODIFICATION AND ATOMIC FORCE
Congress, IUPAC MACRO 2000, 38th Macromolecular MICROSCOPY
IUPAC Symposium, Warsaw, Poland, July 2000) Raghavan D; Gu X; VanLandingham M; Nguyen T
SLOVAK REPUBLIC; SLOVAKIA Washington,Howard University; US,National Inst.of
Accession no.836231 Standards & Technology

© Copyright 2002 Rapra Technology Limited 59


References and Abstracts

(ACS,Div.of Polymer Chemistry) and crystalline structures deduced from transmission


electron microscopy (TEM) or X-ray studies. However,
Interactions between a film and its external environment
the resolution of the AFM can go beyond that easily
are strongly influenced by the surface chemistry and
achievable with TEM imaging of polymers. At higher
morphology of the film. Extensive research has been
resolution, AFM has, in some cases, revealed unpredicted
conducted to provide in-depth microstructural information
surface structures. 26 refs.
of thin polymer films using analytical techniques such as
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
small-angle X-ray scattering, X-ray photoelectron
WESTERN EUROPE
spectroscopy, neutron scattering and secondary ion-mass
spec trometry. However, these techniques lack the lateral Accession no.835289
resolution to detect and map the heterogeneity in polymer
films. With the advent of atomic force microscopy (AFM), Item 60
it is possible to provide direct spatial mapping of surface Polymer
topography and surface heterogeneity at nanometer 43, No.1, 2002, p.159-70
resolution. A combination of tapping mode and force QUANTIFYING SHORT CHAIN BRANCHING
mode AFM techniques has been effective in mapping MICROSTRUCTURES IN ETHYLENE 1-OLEFIN
mechanically heterogeneous regions in multi-component COPOLYMERS USING SIZE EXCLUSION
polymer systems. Recent developments in chemically CHROMATOGRAPHY AND FOURIER
functionalised AFM tips have allowed mapping of TRANSFORM INFRARED SPECTROSCOPY
chemically heterogeneous lithographically patterned (SEC-FTIR)
surfaces by AFM at the molecular scale. This technique Deslauriers P J; Rohlfing D C; Hsieh E T
is known as chemical force microscopy. However, Chevron Phillips Chemical Co.
mapping chemical heterogeneity in a polymer system by Ethylene-1-olefin copolymers are used to demonstrate an
chemical force microscopy pose difficulties because of SEC-FTIR method for the analysis of short chain
chain length variation and irregular packing of chains at branching distribution (SCBD) across the molecular
the probe surface. The objective is to chemically degrade weight distribution (MWD). The chromatograms were
one component of a model blend and then identify the obtained using the root mean square absorbance in the
degraded component by AFM. A model blend consisting 3000-2700 cm power -1 spectral range (with FTIR serving
of polyethylene acrylate (PEA) and PS is selected due to as a concentration detector). The spectra from individual
the difference in the hydrolysis characteristics of PEA time sections of the chromatogram were then analysed
and PS. Acid is selected as the aggressive chemical for comonomer branch levels using a chemometric
medium so as to accelerate the hydrolysis of one method, and the error in the reported SCB content of each
component in the model blend film. 9 refs. section was estimated. By using the appropriate training
USA sets, chemometric models for giving SCB versus
Accession no.835296 chemometric models were constructed for obtaining SCB
versus MWD profiles of enough accuracy for detecting
trends resulting from catalysis and process changes in low-
Item 59
and high-density polyethylene samples. The model was
Polymer Preprints. Volume 41. Number 2. Conference
used for accurate quantification of branching levels in
proceedings.
polyolefins within plus or minus 0.5/1000 total carbons
Washington, D.C., 20th-24th Aug.2000, p.1409-10
(i.e. about 0.1 mol percentage) in samples having
OVERVIEW OF STATE-OF-THE-ART SPM OF
relatively low SCB levels, i.e. less than 10 SCB/total
CRYSTALLINE POLYMERS
carbons and mixed branch types. 20 refs.
Miles M J; Hobbs J K; McMaster T J; Baker A A;
USA
James P J; Blakely S T; Aissaoui M-N
Bristol,University Accession no.835164
(ACS,Div.of Polymer Chemistry)
Item 61
Scanning probe microscopy is a family of a dozen or more Journal of Applied Polymer Science
microscopies essentially based on the concept and 82, No.7, 14th Nov.2001, p.1677-90
technology of the founding member, scanning tunnelling SURFACE MODIFICATION OF LOW DENSITY
microscopy. The most appropriate and widely-used of POLYETHYLENE (LDPE) FILM AND
these microscopies in the study of polymer systems is IMPROVEMENT OF ADHESION BETWEEN
atomic force microscopy (AFM), which in many of its EVAPORATED COPPER METAL FILM AND
modes of operation is suitable for imaging relatively soft LDPE
solids such as polymers and biological materials. In the Ju-Shik Kong; Dong-Jin Lee; Han-Do Kim
simplest AFM modes of operation (contact and ‘tapping’), Pusan,National University
topographic images representing the surface of the
polymer specimen can be obtained. At the lamellar crystal The effects of chromic acid treatment for periods of time
level, such images have generally confirmed morphology between 1 and 60 minutes and oxygen plasma treatment

60 © Copyright 2002 Rapra Technology Limited


References and Abstracts

for periods of time between 30 and 90 seconds on the drinks industry, were studied with and without a
surface of low density polyethylene films were examined compatibiliser. The compatibilising agent was a surlyn
by attenuated total reflectance fourier transform infrared copolymer of ethylene and methacrylic acid partially
spectroscopy, electron spectroscopy for chemical analysis neutralized with zinc, the olefinic segment of which is
(ESCA), scanning electron microscopy and water contact compatible with HDPE, whereas the carboxylic acid
angle. The effect of chromic acid treatment on the tensile groups form hydrogen bonds with the PET carbonyl
strength of the samples was evaluated and tensile strength groups. Infrared spectroscopy, differential scanning
reduced with increasing treatment time. Adhesion of calorimetry, scanning electron microscopy, and the
copper film to the treated surface was evaluated by a mechanical properties were used to assess the
scratch test. It was found that both surface roughness and effectiveness of the compatibiliser. 29 refs.
number of polar groups on the surface increased with MEXICO
increasing treatment times of both chromic acid and Accession no.832040
oxygen plasma, resulting in lowered water contact angle.
Blackening of a film sample occurred after 30 minutes
treatment in chromic acid. Adhesion of copper film Item 64
initially increased with increasing treatment times, but Polymer Degradation and Stability
optimum adhesion properties consistent with tensile 73, No.3, 2001, p.467-70
strength retention were established with 30 minutes CORRELATION BETWEEN THERMAL
chromic acid treatment followed by 30 seconds oxygen PROPERTIES AND CONFORMATIONAL
plasma treatment. 14 refs. CHANGES IN POLY(ETHYLENE
TEREPHTHALATE)/POLY(ETHER IMIDE)
KOREA
BLENDS
Accession no.834851 Ruvolo-Filho A; de Fatima Barros A
Sao Carlos,Universidade Federal
Item 62
Virgin and recycled polyethylene terephthalate (PET) was
Advanced Materials & Processes
blended with polyether-imide (PEI) in proportions
159, No.10, Oct.2001, p.66-7
between 0 and 50 percent PEI content and samples were
SURFACE ENGINEERING TECHNOLOGIES
examined by differential scanning calorimetry and Fourier
Sudarshan T S
transform infrared spectroscopy. All blends were
Materials Modification Inc.
completely miscible, as indicated by a single glass
The 15th International Conference on Surface transition temperature which is dependent on blend
Modification Technologies will be held in November in composition. Crystallisation rates of PET were retarded
Indianapolis. This article presents a few paper abstracts strongly at 20 percent PEI content and above, but degree
and lists the titles of the sessions. Papers include: structure of crystallinity was easily determined from a linear
and properties of HVOF sprayed amorphous polymer correlation between a structural parameter measured
matrix nanocomposite coatings; field experience with spectroscopically and enthalpy of fusion. Trans conformer
advanced soft-metal surfaces on carbon steel bolting activation energy measurement confirmed the effects of
materials used in gall-prone gasketed joints that operate PEI content on crystallisation of PET. 9 refs.
at elevated temperatures; characterisation of industrial BRAZIL
coatings with atomic force microscopy; characterising Accession no.831829
aluminium pretreatments for structural adhesive bonding;
the Air Force manufacturing technology laser peening
initiative; and iron aluminide based coating deposited by Item 65
high energy density processes. Polymer Degradation and Stability
USA
73, No.3, 2001, p.463-6
EFFECT OF INTERFACE MODIFICATION ON
Accession no.834668
THE PHOTO-STABILITY OF PIGMENTED
POLYETHYLENE FILMS
Item 63 Anna P; Bertalan G; Marosi G; Ravadits I; Maatoug M
Journal of Applied Polymer Science A
82, No.6, 7th Nov.2001, p.1382-90 Budapest,University of Technology & Economics
PROPERTIES AND MORPHOLOGY OF
Examination of the ageing characteristics of high density
POLY(ETHYLENE TEREPHTHALATE) AND
polyethylene films containing phthalocyanine green and
HIGH-DENSITY POLYETHYLENE BLEND
titanium white and other pigments with those of lightly
Guerrero C; Lozano T; Gonzalez V; Arroyo E
stabilised polymer film without pigments was carried out
Nuevo Leon,Universidad Autonoma
using tensile analysis, differential scanning calorimetry
Blends of polyethylene terephthalate (PET) and high and ultraviolet spectroscopy. The early failure of the
density polyethylene (HDPE), widely used in the soft phthalocyanine pigmented sample, and subsequent UV

© Copyright 2002 Rapra Technology Limited 61


References and Abstracts

spectroscopic examination showed that the cause was HIGH RESOLUTION SOLID-STATE CARBON 13
adsorption of stabilisers onto the pigment surface. NMR STUDY OF AS-CURED AND IRRADIATED
Reactive surfactant coating of pigments was shown to EPOXY RESINS
considerably extend the film stability by reducing their Ngono-Ravache Y; Foray M-F; Bardet M
adsorbency. 9 refs. Grenoble,University
EASTERN EUROPE; HUNGARY
Details are given of the effects of strong ionising
Accession no.831828 radiations on the physico-chemical modifications of
epoxy resins. The sensitivity of the epoxy resins to
Item 66 radiation was determined using carbon 13 NMR. 20 refs.
Polymer Degradation and Stability EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
73, No.3, 2001, p.387-92 WESTERN EUROPE
MECHANISM OF PHOTOSTABILIZATION OF Accession no.831124
PERFLUOROPOLYETHER COATINGS BY
HINDERED AMINE STABILISERS Item 69
Luda M P; Camino G; Laurenti E; Novelli S; Applied Spectroscopy
Temtchenko T; Turri S 55, No.8, Aug. 2001, p.984-91
Torino,Universita; Centro Ricerche Ausimont RAMAN AND INFRARED
The mechanism of operation of hindered amine stabilisers MICROSPECTROSCOPIC MAPPING OF
(HAS) against photodegradation in perfluoro polyethers PLASMA-TREATED AND GRAFTED POLYMER
incorporated into a coating material of polyurethane has SURFACES
been studied by infrared spectroscopy, gas Keen I; Rintoul L; Fredericks P M
chromatography-mass spectrometry and electron spin Queensland,University of Technology
resonance spectroscopy. Under curing conditions A section of the surface of a predominantly PP substrate
normally utilised for coil coating (280 degrees Centigrade containing a small amount of PE copolymer and a small
for 1 minute in air), the HAS was found to increase the amount of blended EPM was characterised before and
number of urea bridges in the polyurethane network, and after plasma treatment and after graft copolymerisation
reduce the amount of unreacted isocyanate, giving a with PS by means of Raman and ATR/IR mapping. The
structure which is more resistant to photooxidation. maps constructed indicated variations in crystallinity
Byproducts of the high temperature cure process, caused across the surface, the distribution of EPM and the
by partial transformation of the HAS into -NH derivatives distribution of hydroxy groups introduced onto the surface
act as antioxidants. The unreacted HAS was found to by plasma treatment. 24 refs.
slowly evaporate from the test film, but whilst present AUSTRALIA
acted as a radical scavenger. 8 refs.
Accession no.830453
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
WESTERN EUROPE
Accession no.831816 Item 70
POLYMER PROCESSING ENGINEERING. 01.
Proceedings of a conference held June 2001.
Item 67
London, IOM Communications Ltd., 2001, Paper 5,
Plast’ 21
p.46-58, 012
No.101, April 2001, p.77-9
AT-PROCESS RAMAN SPECTROMETRY OF
Spanish
POLYMER MELTS
INFRARED THERMOGRAPHY: THE COLOURS
Dhamdhere M; Li J; Deshpande B; Patil P; Hansen M G
OF HEAT
Tennessee,University
ASCAMM
(Institute of Materials; Interdisciplinary Research
The use of IR thermography in the study of injection Centre)
moulds and injection moulded plastics parts is discussed,
In-line monitoring of EVA extrusion was carried out using
and details are given of research and development projects
in-line fibre optic Raman spectroscopy. Vinyl acetate
being undertaken by ASCAMM of Spain using this
content in the random copolymer and melt indices of
technique.
various grades of the EVA were determined and vinyl
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
acetate content in the samples correlated using linear least
WESTERN EUROPE
squares and PLS analysis. Hierarchical Cluster analysis was
Accession no.831329 employed as a pattern recognition technique to follow the
natural clustering tendencies of the EVA samples. 10 refs.
Item 68 EUROPEAN COMMUNITY; EUROPEAN UNION; UK; USA;
Polymers for Advanced Technologies WESTERN EUROPE
12, No.9, Sept, 2001, p.515-23 Accession no.830358

62 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Item 71 FORMALDEHYDE NOVOLAC RESINS


Polymer Testing Markovic S; Dunjic B; Zlatanic A; Djonlagic J
20, No.7, 2001, p.729-40 Belgrade,University
DIRECT SOLID SAMPLING METHODS FOR
Using dynamic mechanical analysis the curing reactions
GAS CHROMATOGRAPHIC ANALYSIS OF
of typical phenol-formaldehyde novolac resins were
POLYMER/ADDITIVE FORMULATIONS
followed. The evolution of various rheological parameters
Bart J C J
was recorded for samples of the resins on cloth. A third-
Messina,University
order phenomenological equation described the curing
The present ‘state of the art’ in direct solid sampling reaction. The influences of the structure, composition and
methods for gas chromatographic analysis of additives physical treatment on the curing kinetics were evaluated.
encapsulated in polymers is reviewed. Techniques 20 refs.
considered are static and dynamic headspace methods, EASTERN EUROPE; YUGOSLAVIA
thermal desorption and solid phase microextraction. Accession no.829458
Applications for each method are discussed. 54 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
WESTERN EUROPE Item 74
Accession no.830211 Journal of Applied Polymer Science
81, No.11, 12th Sept.2001, p.2779-85
RIGID AMORPHOUS PHASE AND LOW
Item 72 TEMPERATURE MELTING ENDOTHERM OF
Antec 2001.Conference proceedings. POLY(ETHYLENE TEREPHTHALATE)
Dallas, Texas, 6th-10th May, 2001, paper 620 STUDIED BY MODULATED DIFFERENTIAL
DETERMINATION OF CONDENSABLE SCANNING CALORIMETRY
VOLATILES DURING POLYMER PROCESSING Song M
USING AN ANALYTICAL EXTRUDER Loughborough,University
Buzanowski W C; Gunderson J; Froelicher S
Dow Chemical Co. Three similar samples of polyethylene terephthalate (PET)
(SPE) prepared by isothermal cold crystallisation in the
differential scanning calorimetry (DSC) cell (PET1), melt
A method of collecting and analysing the volatiles created crystallisation at a steady cooling rate and annealing for
during extrusion is described, in which the extruder is part various times in the DSC cell (PET2), and quenching from
of the analytical instrumentation. A non-vented 19 mm (3/ 300 degrees centigrade to -20 degrees over a period of 5
4 in) single screw extruder was fitted with a right angle 3.2 minutes (PET3) were used to study the glass transition
mm single strand die, which in turn carried a glass tube effects in the rigid amorphous phase and the low
with a bulb near the die exit to allow for polymer swell, temperature melting endotherm using modulated DSC.
and a side arm for attachment of the sampling system. The As annealing time increased in PET2 the increment of
polymer extruded into the glass tube, the less volatile heat capacity (IHC) at annealing temperature increased
materials condensing in the tube, and the more volatile and the IHC at the glass transition temperature decreased.
materials being withdrawn by the side arm and trapped in It was deduced that the low temperature melting
a set of three impingers containing an appropriate chilled endotherm originated with transitions in the rigid
trapping solution. The volatiles from the glass tube were amorphous fraction, and it was noted that the glasslike
removed by rinsing and analysed by Fourier transform transition of this fraction occurred between glass transition
infrared spectroscopy and gas chromatography-mass and melting temperatures. 23 refs.
spectrometry. The trapping solutions were analysed directly. EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
The equipment was used to determine the influence of WESTERN EUROPE
extrusion time on volatile emissions from polycarbonate, Accession no.829381
the influence of melt temperature on volatile loss from a
polycarbonate/styrene-acrylonitrile copolymer blend, and Item 75
the influence of additives on volatile loss from a glass- Journal of Applied Polymer Science
filled polymer. 6 refs. 81, No.10, 6th Sept.2001, p.2387-98
USA COMPARISON OF THERMAL DEGRADATION
Accession no.830052 CHARACTERISTICS OF POLY(ARYLENE
SULFONE)S USING THERMOGRAVIMETRIC
Item 73 ANALYSIS/MASS SPECTROMETRY
Journal of Applied Polymer Science Li-Hsiang Perng
81, No.8, 22nd August 2001, p.1902-13 Ta Hwa,Institute of Technology
DYNAMIC MECHANICAL ANALYSIS STUDY Thermogravimetric analysis with gas chromatography and
OF THE CURING OF PHENOL- mass spectrometry were used in the analysis of the thermal

© Copyright 2002 Rapra Technology Limited 63


References and Abstracts

degradation of polyether sulphone (PES) and CHINA


polysulphone (PSF). Evolution of sulphur dioxide and Accession no.825682
phenol from random chain scission in a one stage
pyrolysis was observed in both cases with apparent initial
Item 78
thermal stability of the PES being lower than PSF, but
Journal of Thermal Analysis and Calorimetry
fire retardation of PES was better due to reduction of the
64, No.2, 2001, p.549-55
sulphone group by hydrogen radicals. More pyrolysis
CRYSTALLIZATION AND MELTING OF
products were identified from the PSF than from the PES.
POLYCARBONATE STUDIED BY
Thermal stability of ether and sulphone groups appeared
TEMPERATURE-MODULATED DSC (TMDSC)
similar in PES but in PSF the sulphone groups proved
Schick C; Wurm A; Merzlyakov M; Minakov A;
the more stable. A simple kinetic model was developed
Marand H
which showed good agreement between theoretical and
Rostock,University; Moscow,General Physics Institute;
experimental pyrolysis curves for both polymers. 20 refs.
Virginia,Polytechnic Institute & State University
TAIWAN
Accession no.829337 TMDSC measurements conducted at reasonably high
frequencies for bisphenol-A polycarbonate(PC, Lexan)
allowed for the determination of base-line heat capacity.
Item 76 Vitrification and devitrification of the rigid amorphous
Journal of Applied Polymer Science fraction(RAF) could be directly observed. 0.01 Hz
81, No.12, 19th Sept.2001, p.3064-8 appeared to be a reasonably high frequency for PC. The
TEMPERATURE AND ATMOSPHERE RAF of PC was established during isothermal
INFLUENCES ON SMOKE COMPOSITION crystallisation. Devitrification of the RAF seemed to be
DURING THERMAL DEGRADATION OF related to the lowest endotherm. For PC, the melting of
POLY(ETHYLENE TEREPHTHALATE) small crystals between the lamellae was expected to yield
Malgorzata Dzieciol; Jerzy Trzeszczynski the lowest endotherm. 27 refs.
Szczecin,Technical University
GENERAL ELECTRIC CO.
The less volatile compounds formed during the thermal EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
degradation of polyethylene terephthalate (PET) under RUSSIA; USA; WESTERN EUROPE
different conditions at 200-700 deg.C in nitrogen and air Accession no.825045
atmospheres were studied. The compounds were trapped
on a glass fibre filter and analysed by capillary gas Item 79
chromatography using a mass spectrometer (GC-MS), and Shawbury, Rapra Technology Ltd., 2001, p.iv, 174,
high performance liquid chromatography. The results 25cm, 91T
were tabulated, and plots were drawn of the degradation EASY IDENTIFICATION OF PLASTICS AND
temperatures in nitrogen and air atmospheres versus the RUBBERS
weight changes of terephthalic acid and monovinyl VERLAYE G A L; ROEGES N P G; DE MOOR MO
terephthalate evolved from PET. The effects of the KaHo Sint-Lieven
atmosphere and temperature on smoke emission and
composition during PET thermal degradation were This book presents an identification scheme developed
considered. 28 refs. over the last thirty years for thermoplastics, common
EASTERN EUROPE; POLAND
thermosets, a few copolymers and elastomers. The
techniques used are based on simple tests such as the
Accession no.826911
behaviour of polymers in liquids and in a flame. The book
also covers Infrared spectroscopy. Main headings are:
Item 77 Simple tests (melting, solubility, burning characteristics,
Macromolecules odour recognition, dripping, flotation, halogen test,
34, No.15, 17th July 2001, p.5224-8 nitrogen- and sulphur-test); Recording an IR spectrum;
STUDIES OF MISCIBILITY BEHAVIOUR AND Identification flow charts; Thermoplastics; Cellulose and
HYDROGEN BONDING IN BLENDS OF starch; Thermosets; Elastomers. (15 Refs)
POLYVINYLPHENOL AND BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
POLYVINYLPYRROLIDONE UK; WESTERN EUROPE
Kuo S W; Chang F C Accession no.824868
Taiwan,National Chiao Tung University
Blends of polyvinyl phenol with polyvinyl pyrrolidone Item 80
were prepared by solution casting from DMF solutions. UTECH 2000. Proceedings of a conference held The
DSC, FTIR, and NMR were used to investigate the Hague, Netherlands, 28th-30th March 2000.
hydrogen bonding and miscibility of the blend. The Tg London, 2000, Other Rigid Foam Developments
of the blend was determined. 22 refs. Session, Paper 1, pp.4, 012

64 © Copyright 2002 Rapra Technology Limited


References and Abstracts

LONG-TERM ENERGY EFFICIENCY OF PU- from different wood species was carried out. Studies were
INSULATION FOR REFRIGERATION carried out on Pine (Pino Eliottis), eucaliptus (Eucaliptus
Seifert H; Biedermann A Saligna) and marmelero (Ruprechia Laviflora), a
Elastogran GmbH softwood and two semi-hard woods, respectively. The
(Crain Communications Ltd.; European Isocyanate particles were used untreated and chemically modified
Producers’ Association) with maleic anhydride. For the characterisation of
untreated and treated flours, thermogravimetric analysis
The ageing behaviour of rigid PU foams was investigated
and analytical techniques were utilised. Dispersion of the
using gas chromatographic quantitative evaluation of the
fibrous particles, in addition to maximum fibre
cell gas composition in the foams. The change in thermal
concentration (accompanied by complete wetting of the
conductivity of the foams during ageing was also
wood fibres) was dependent on the treatment and on the
examined as was the dimensional stability of the foams
wood species utilised. Bending and compression tests
under diffusion open conditions and the results obtained
suggested some improvement in the performance of the
correlated with the K x A-values from refrigerator cabinets
composites, if the wood flour was previously esterified.
via the change in cell gas composition. The data obtained
Changes in the fracture surfaces due to maleic anhydride
revealed that the ageing process of appliances could be
treatment of the fibres were observed using scanning
simulated in a tenth of the time by measuring diffusion
electron microscopy. 12 refs.
opened PU foams. 2 refs.
ARGENTINA
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
NETHERLANDS; WESTERN EUROPE Accession no.824162
Accession no.824859
Item 83
Item 81 Polymer Degradation and Stability
International Polymer Science and Technology 73, No.2, 2001, p.251-7
28, No.5, 2001, p.T/79-80 THERMAL CHARACTERISTICS OF ADDITION-
STUDY OF POLYMER-FILLER INTERACTION CURED PHENOLIC RESINS
BY INVERSE GAS CHROMATOGRAPHY Reghunadhan C P; Bindu R L; Ninan K N
Gukasyan S Z Vikram Sarabhai Space Centre
The surface modification of fillers with polymeric The thermal cure characteristics, kinetics of thermal
substances is discussed with reference to improvement degradation and pyrolysis of four different addition cured
of the properties of filled polymers. When the fillers are phenolic resins were investigated using various
modified with polymers, the boundary layer contains not techniques, including DSC, DMA, FTIR spectroscopy,
only the matrix filler, but also the modifying polymer, TGA and X-ray diffraction. Resins investigated were
and when the modifying polymer interacts with the surface propargyl ether resins and phenyl azo-, phenyl ethynyl-
filler, the properties of both the mineral component and and maleimide-functional resins. A comparison of the data
the modifier are altered. One characteristic which reflects obtained for all the phenolic resins was made as a function
the result of polymer-filler interaction is the glass of molecular structure. 12 refs.
transition temperature of the modifier. To determine this INDIA
parameter for a very low content of polymer, the method Accession no.824043
of inverse gas chromatography was used using the
modified filler as the stationery phase. The study
investigated the use of travertine and tuff, the surfaces of Item 84
which were modified with latices of a copolymer of UTECH 2000. Proceedings of a conference held The
styrene and methacrylic acid. 3 refs. (Article translated Hague, Netherlands, 28th-30th March 2000.
from Plasticheskie Massy, No.8, 2000, p.36) London, 2000, Innovations: Flexible Foam
RUSSIA Developments Session, Paper 5, pp.4, 012
VOC DETECTION IN POLYURETHANE
Accession no.824324
FLEXIBLE FOAMS
Occhiello E; Tavan M; Pannocchia P; Fava F
Item 82
EniChem
Molecular Crystals & Liquid Crystals
(Crain Communications Ltd.; European Isocyanate
Vol.353, 2000, p.95-108
Producers’ Association)
COMPOSITES MADE FROM
LIGNOCELLULOSICS AND THERMOSET The detection of volatile organic compounds in polyols
POLYMERS and PU foams using SPME, gas chromatography and gas
Aramguren M I; Marcovich N E; Reboredo M M chromatography-mass spectroscopy is demonstrated.
INTEMA EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
NETHERLANDS; WESTERN EUROPE
Preparation and testing of composites from a styrene/
Accession no.823982
unsaturated polyester thermoset matrix and wood flours

© Copyright 2002 Rapra Technology Limited 65


References and Abstracts

Item 85 Quebec,Universite Laval; Pyrovac Institute Inc.; Petru


Polymer Degradation and Stability Poni,Institute of Macromolecular Chemistry
73, No.1, 2001, p.163-7
Vacuum pyrolysis was performed on HDPE, LDPE, PP,
THERMAL, PHYSICAL AND CHEMICAL
PS and PVC materials individually, and also on a mixed
STABILITY OF POROUS POLYSTYRENE-TYPE
plastics sample containing the five polymers. The main
BEADS WITH DIFFERENT DEGREES OF
gaseous and liquid products, including chlorinated
CROSSLINKING
hydrocarbons, were identified by chromatography, and
Yanhong Li; Yunge Fan; Jianbiao Ma
the yields and pyrolysis products were compared for the
Nankai,University
individual and mixed runs. The results suggested that the
The thermal decomposition of porous polystyrene beads pyrolysis yields of the plastics mixtures were similar to
with differing crosslinking degrees using divinyl benzene those calculated from the pyrolysis of the individual
were evaluated using thermogravimetry and differential polymers. However, the chlorine content was lower than
scanning calorimetry techniques. The test results showed expected indicating limited interaction during pyrolysis.
that the thermal stability of the beads increased with higher Full details of the experimental procedures are given
degrees of crosslinking. DSC analysis revealed that the including a detailed tabulation of all the pyrolysis
glass transition temperatures gradually increased with products. 54 refs.
crosslinking levels up to 30% crosslinking by weight, but CANADA; EASTERN EUROPE; RUMANIA
above this level beads were thermally stable as the glass Accession no.823939
transition temperature was replaced by an exothermic
peak. Complete details of the testing procedures and
results are given 15 refs. Item 88
Polymer Degradation and Stability
CHINA
73, No.1, 2001, p.15-22
Accession no.823950 THERMO-OXIDATIVE STABILITY OF PP
WASTE FILMS STUDIED BY IMAGING
Item 86 CHEMILUMINESCENCE
Polymer Degradation and Stability
The spread of oxidation in artificially recycled PP
73, No.1, 2001, p.69-74
materials, with and without stabilisation, was monitored
EXAMINATION OF A LOW DENSITY
using imaging chemiluminescence techniques. The results
POLYETHYLENE (LDPE) FILM AFTER 15
were compared with estimates made using Fourier
YEARS OF SERVICE AS AN AIR AND WATER
transform infrared spectroscopy and differential scanning
BARRIER
calorimetry techniques. It was concluded that although
Moller K; Gervert T; Holmstrom A
the conventional techniques gave residual lifetimes of five
Sweden,National Testing & Research Institute
cycles, imaging chemiluminescence showed that a
Comparisons between accelerated ageing tests and tests significant reduction in oxidative stability had occurred
on polymeric materials aged in actual service conditions after only two cycles. Full details of the imaging
to identify possible degradation mechanisms appear to chemiluminescence technique used are given with
be the only reliable method of predicting long term service detailed results. 12 refs.
lifetimes. A low density polyethylene film used as an air Accession no.823934
and water barrier for 15 years in an exterior wall
construction was characterised using tensile testing,
spectroscopy and chromatography techniques. Although Item 89
the mechanical properties of the film were unaffected by DEVELOPMENTS IN POLYMER ANALYSIS AND
ageing, its antioxidant stabilisers were severely degraded. CHARACTERISATION Proceedings of a conference
Full details of the ageing conditions, test methods and held Shawbury, UK, 10th May 1999.
results are given. 16 refs. Shawbury, 1999, Paper 4, p.1-15, 012
CHEMICAL CHARACTERISATION OF
EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERN
EUROPE POLYURETHANES
Forrest M J
Accession no.823940
Rapra Technology Ltd.
(Rapra Technology Ltd.)
Item 87
Polymer Degradation and Stability Polyurethane chemistry is briefly outlined, additives
73, No.1, 2001, p.47-67 generally used in polyurethanes are indicated and the
VACUUM PYROLYSIS OF COMMINGLED analytical techniques used to characterise the structure,
PLASTICS CONTAINING PVC. PART II. composition and properties of PUs and PU-based products
PRODUCT ANALYSIS are discussed in a comprehensive manner. Techniques
Miranda R; Pakdel H; Roy C; Vasile C covered include spectroscopic, chromatographic techniques
and miscellaneous techniques, such as wet chemistry

66 © Copyright 2002 Rapra Technology Limited


References and Abstracts

techniques. Sections are included dealing with the Item 92


characterisation of polymer structure and starting materials, Polymer Degradation and Stability
molecular weight determinations, characterisation of 72, No.1, 2001, p.175-86
additives and cure reaction studies. 14 refs. CHEMICAL AND MORPHOLOGICAL
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; MODIFICATIONS OF IRRADIATED LINEAR
WESTERN EUROPE LOW DENSITY POLYETHYLENE (LLDPE)
Accession no.822952 Guadagno L; Naddeo C; Vittoria V; Camino G;
Cagnani C
Salerno,University; Turin,University; Montell Italia
Item 90
SpA
Macromolecular Symposia
Vol. 169, May 2001, p.45-55 Spherilene technology produced films of linear low
CHARACTERIZATION OF THE density polyethylene which were exposed to UV
INTERACTIONS IN POLYMER/SILICA irradiation to simulate accelerated weathering.
SYSTEMS BY INVERSE GAS Comparison was made with a set of films annealed at
CHROMATOGRAPHY 60C and no irradiation. The resulting chemical structures
Voelkel A; Milczewsk K; Jeczalik J were examined using FTIR. The findings were that the
Poznan,University of Technology degradation is dominated by the formation of carbonyl
and vinyl species. 22 refs.
The inverse gas chromatography technique, (IGC) is
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
presented as a method of characterisation of the
WESTERN EUROPE
interactions in polymer-modified silica systems. The
authors propose to express the magnitude of modified Accession no.820850
filler/polymer interactions by means of the Flory-Huggins
parameter. Polyether-urethane/modified silica systems Item 93
containing different amounts of filler were investigated, Polymer Degradation and Stability
and information relating to the physicochemical properties 72, No.1, 2001, p.31-45
of oligomer and modified silicas were presented by means FACTORS AFFECTING THE ADSORPTION OF
of the solubility factor to describe the properties of the STABILISERS ON TO CARBON BLACK (FLOW
polymer layer, and the Flory-Huggins parameter which MICRO-CALORIMETRY STUDIES). IV.
describes the polymer-solute or mixture polymer/silica- SECONDARY ANTIOXIDANTS
solute interactions. These parameters are obtained from Pena J M; Allen N S; Edge M; Liauw C M; Valange B
inverse gas chromatography experiments. The influence Manchester,Metropolitan University; Cabot Corp.
of the IGC experiment temperature, the content of
Using flow micro-calorimetry, X-ray photoelectron
modified silica, and the nature of test solute on the
spectroscopy and Fourier transform infra-red
evaluated parameters are presented and discussed. 7 refs.
spectroscopy techniques the surface activity of different
EASTERN EUROPE; POLAND
types of carbon black with secondary antioxidants (aryl
Accession no.822644 phosphites and phosphonites) have been examined. Both
in the overall adsorption activity and the levels of probe
Item 91 adsorption significant differences were observed. Two
Journal of Applied Polymer Science factors were reported which were found to influence the
80, No.8, 23rd May 2001, p.1305-11 behaviour of phosphite stabilisers. 29 refs.
EFFECT OF RECYCLED POLYPROPYLENE ON BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
POLYPROPYLENE/HIGH DENSITY UK; WESTERN EUROPE
POLYETHYLENE BLENDS Accession no.820835
Bonelli C M C; Martins A F; Mano E B; Beatty C I
Rio de Janeiro,Universidade Federal; Item 94
Florida,University Polymer International
A study was made of the effects of addition of recycled 50, No.6, June 2001, p.635-42
polypropylene on the incompatible blends of virgin DEGRADATION OF HIGH BARRIER
polypropylene with high-density polyethylene. The ETHYLENE-VINYL ALCOHOL COPOLYMER
characteristics of the recycled polypropylene were UNDER MILD THERMAL-OXIDATIVE
determined by spectrographic and thermal analysis means. CONDITIONS STUDIED BY THERMAL
The mechanical properties of the blends were determined. ANALYSIS AND INFRARED SPECTROSCOPY
The 50/50 blend of the two virgin polymers benefited most Lagaron J M; Gimenez E; Suara J J
from the addition of the recycled polypropylene. 9 refs. Jaume I,Universitat
BRAZIL; USA The thermooxidative degradation of a solution cast
Accession no.821546 ethylene-vinyl alcohol copolymer (containing 32

© Copyright 2002 Rapra Technology Limited 67


References and Abstracts

mol.percent ethylene) used in barrier applications was polymers are analysed. The author’s own modification
studied at three temperatures immediately above the of PGC is presented, involving the use of a pyrolysis
melting point using thermogravimetric analysis, DSC and attachment with the mobile reaction zone. Resulting data
FTIR spectroscopy. The weight loss measured by are compared with those obtained by conventional
thermogravimetric analysis was fast at short times and pyrolysis gas chromatography. 34 refs.
slowed down progressively. The weight loss of about 3.6 Accession no.816530
percent measured by thermogravimetric analysis resulted
from chemical alterations in the polymer. DSC showed
small changes in crystallinity, melting point and glass Item 97
transition and broadening of the melting endotherms in New York, John Wiley & Sons, Inc., 1999, pp.xv,752
samples exposed to the more severe thermooxidative CHEMICAL SEPARATIONS- PRINCIPLES,
treatments. FTIR showed a transformation of the vinyl TECHNIQUES, AND EXPERIMENTS
alcohol hydroxyl groups into carbonyl groups and the MELOAN, C E
creation of double bonds. Changes in degradation kinetics, KANSAS STATE UNIVERSITY
and possibly mechanisms, were thought to occur with This combination laboratory manual and reference source
increasing time. FTIR measurements indicated that provides a working knowledge of an array of separation
transformation of the hydroxyl groups led to a weakening methods. In forty-two chapters, it explores all major
of the overall hydrogen bonding strength in the degraded categories of separation. With an emphasis upon everyday
samples so a reduction in the intermolecular cohesion, practice rather that theory, this book explains the
and hence the barrier properties of the copolymer, could principles and parameters of these methods and provides
be anticipated. 19 refs. 59 specific experiments to demonstrate proper procedures.
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; These experiments feature step-by-step protocols for each
WESTERN EUROPE separation scheme, precise instructions on setting up the
Accession no.819207 apparatus, and checklists for essential chemicals and
supplies. Main Headings include Separations involving
Item 95 phase changes; Separations involving extraction;
Polymer Science Series B Separations involving chromatography; Separations
43, Nos. 3-4,March/April 2001, p.105-8 involving ion exchange resins; Separations involving
TRANSFORMATIONS OF ANTIMONY- electric fields; Separations involving flotation;
HALOGEN- AND NITROGEN-PHOSPHORUS- Separations involving membranes; Separations involving
BASED FLAME RETARDANTS IN miscellaneous techniques.
POLYOLEFINS AND THEIR PERFORMANCE USA
Bogdanova V V Accession no.816497
Belorussian,State University
Degradation products from both antimony-halogen based Item 98
and nitrogen-phosphorus based flame retardants were Polymer Bulletin
studied using X-ray diffraction and atomic emission 46, No.2-3, April 2001, p.191-6
analysis. Evidence of the retardation mechanisms in use MISCIBILITY OF POLYETHERIMIDE AND
against combustion was obtained for each system and in POLYBUTYLENE NAPHTHALATE BLENDS
each case emission of volatile combustion inhibitors at Lin C H; Wang C S
the degradation temperature of the polymer matrix was Taiwan,Kung Shan Institute of Technology;
the critical factor. 11 refs Taiwan,National Cheng Kung University
BELARUS; BELORUSSIA DSC, optical microscopy, and SEM were performed to
Accession no.818458 characterise the miscibility of a blend of polybutylene
naphthalate and polyetherimide. Data were compared with
Item 96 theoretical predictions. 6 refs.
Polimery CHINA
45, Nos.11-12, 2000, p.51-8 Accession no.816205
Polish
PYROLYSIS GAS CHROMATOGRAPHY AND Item 99
NEW POSSIBILITIES OF ITS USE IN THE Journal of the National Institute of Materials and
ANALYSIS OF POLYMERS Chemical Research
Hetper J 8, No.4, 2000, p.149-59
Major conditions are formulated to ensure that pyrolysis Japanese
gas chromatography yields reliable and repeatable results, POSITRONIUM FORMATION AND DIFFUSION
particularly when non-volatile substances such as IN POLYMERS

68 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Hirata K; Kobayashi Y Kyoto,University


High-energy positrons injected into condensed matter Dynamic viscosity measurements were used to determine
quickly lose their energy, become thermalised and the physical ageing at 110C of polycarbonate using
annihilate with one of the electrons of the medium into samples quenched from the molten state. The test results
gamma rays. In polymers, some of the positrons form a showed that there was a memory effect in the
hydrogen-like bound state between a positron and an polycarbonate of the quenching processes, but as
electron prior to the annihilation. This bound state is called equilibrium is reached then the memory becomes lost.
positronium (Ps). Ps is formed by recombination of a Evidence is shown that the structure of the polymeric
positron and one of the electrons released from the chain in the glassy state relaxes over larger segment scale
molecules in terminal positron spur. Positron-electron lengths because the scale of the movable segments is
recombination in the positron spur competes with other related to temperature. 29 refs.
reactions, so that the Ps formation probability depends JAPAN
on various factors. The influence of additives, polar Accession no.814126
groups and external field on Ps formation in polymers is
discussed. A possibility of using Ps as a radiation chemical
probe for polymers is described. Ps formed as a result of Item 102
positron-electron recombination interacts with a Polymer
subnanometer-size free volume hole, and diffuses over a 42, No.13, 2001, p.5523-9
certain distance before annihilation. The diffusion SEC-FTIR CHARACTERIZATION OF SEMI-
coefficient of Ps is determined using a chemical reaction CRYSTALLINE HDPE AND PP
between Ps and an additive, and its diffusion length in Verdumen-Noel L; Baldo L; Bremmers S
amorphous polymers is estimated to be ca.1 nm. This DSM Research
result is of fundamental importance to apply Ps as a probe A pressure transducer in combination with the size
for studying free volume in polymers. 68 refs. exclusion chromatography-FTIR technique was used to
JAPAN characterise semi-crystalline materials such as HDPE and
Accession no.815833 random PP copolymers. The comonomer content (butene
for HDPE and ethylene for PP) decreased with increasing
molar mass. For two HDPE samples produced by the dual
Item 100
reactor process, this decrease occurred stepwise with a
Journal of Applied Polymer Science
constant comonomer amount on either side of the step.
80, No.11, 13th June 2001, p.2120-2
For all the HDPE samples, the amount of end
SOLID-STATE NMR AND XPS STUDIES OF PVA/
unsaturations decreased with molar mass. The
SUGARCANE COMPOSITES
concentration of side and trans unsaturations was too low
Tavares M I B; Stael G C; Gorelova M M; de Menezes
to be determined. 8 refs.
SMC
EUROPEAN COMMUNITY; EUROPEAN UNION;
Rio de Janeiro,Cidade Universitaria NETHERLANDS; WESTERN EUROPE
Bagasse, taken directly from the sugarcane mills, was Accession no.813974
dried, cut to lengths of 5 mm, and blended with
poly(ethylene-co-vinyl acetate) in proportions up to 60
Item 103
wt%. The composites were characterised by solid-state
Macromolecular Materials and Engineering
nuclear magnetic resonance spectroscopy and X-ray
286, No.3, 30th March 2001, p.161-7
photoelectron spectroscopy. A homogeneous copolymer
MATRIX-ASSISTED LASER DESORPTION/
covering on the surface of the fibres was achieved, the
IONIZATION MASS SPECTROMETRY OF
samples exhibiting homogeneity at the molecular level.
SYNTHETIC POLYMERS, 5A. ANALYSIS OF
The best physical interaction between the fibres and the
POLY(PROPYLENE OXIDE)S BY COUPLED
matrix was achieved with the sample containing 60 wt%
LIQUID CHROMATOGRAPHY AT THE
fibre. 10 refs.
CRITICAL POINT OF ADSORPTION AND
BRAZIL
MALDI-TOF MASS SPECTROMETRY
Accession no.814366 Keil C; Esser E; Pasch H
Darmstadt,Deutsches Kunststoff-Institut
Item 101 Poly(propylene oxide)s were analysed efficiently by
Journal of Polymer Science: Polymer Physics Edition coupled liquid chromatography and MALDI-TOF mass
39, No.3, 1st Feb.2001, p.337-41 spectrometry. The techniques were coupled via a robotic
PHYSICAL AGING OF POLYCARBONATE interface where the matrix was coaxially added to the
INVESTIGATED BY DYNAMIC eluate and spotted dropwise onto the MALDI target. Size
VISCOELASTICITY exclusion chromatography and liquid chromatography at
Apaki O; Horie M; Masuda T critical conditions of adsorption coupled to MALDI-TOF

© Copyright 2002 Rapra Technology Limited 69


References and Abstracts

gave useful structural information on oligomer masses Hyun J; Aspnes D E; Cuomo J J


and chemical composition; The technique showed the North Carolina,State University
presence of diols and monools in addition to the triols in
A non-destructive technique for characterisation of the
poly(propylene oxide) triols. The oligomer distributions
surface Tg in PETP is described which involves analysis
of all functionality fractions were determined. 23 refs.
of the variation of the ellipsometrically measured
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
refractive index with temp., using the spectral dependence
WESTERN EUROPE
of the penetration depth of light to discriminate between
Accession no.813967 surface and bulk transitions. The surface Tg is shown to
be lower than that of the bulk for spin-cast semicrystalline
Item 104 PETP films because of density variation and Tg is found
Polimery to be lowered further by plasma processing. 18 refs.
45, No.10, 2000, p.701-6 USA
Polish Accession no.813421
OXIDATION AND DESORPTION OF OXYGEN
FROM THE UPPER LAYER OF ACTIVATED
POLYPROPYLENE FILM Item 107
Zenkiewicz M Macromolecular Symposia
Vol.165, March 2001, p.91-8
Photoelectron spectroscopy was used to study oxidation RECENT DEVELOPMENTS IN POLYOLEFIN
of biaxially oriented polypropylene film. X-rays and CHARACTERISATION
ultrahigh vacuum associated with the method of study Pasch H
were found to promote oxygen desorption from the upper Deutsches Kunststoff-Institut
layer. 6 refs. Articles from this journal can be requested
for translation by subscribers to the Rapra produced A brief review is presented on techniques for the analysis
International Polymer Science and Technology. of polyolefins and additives in polyolefins. Techniques
considered include high-temperature GPC combined with
Accession no.813667
FTIR spectroscopy for the analysis of chemical
composition as a function of molar mass, crystallisation
Item 105 fractionation for the analysis of short-chain branching in
Macromolecules LLDPE and of polyolefin blends and pyrolysis-gas
34, No.8, 10th April 2001, p.2667-72 chromatography-mass spectrometry for the determination
SELF-FOCUSING IN GRADIENT LIQUID of additives, such as antioxidants, in polyolefins. 13 refs.
ADSORPTION CHROMATOGRAPHY OF (3rd Annual UNESCO School & IUPAC Conference on
POLYMERS Macromolecules and Materials Science, Stellenbosch,
Degoulet C; Perrinaud R; Ajdari A; Prost J; Benoit H; South Africa, 2000)
Bourrel M EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
TotalFinaElf; Atofina; Elf Atochem North America WESTERN EUROPE
Inc.; ESPCI; Institut Curie; Institut Charles Sadron Accession no.813085
The separation process occurring during liquid
chromatography of polymers in a gradient of composition Item 108
of the eluent was examined. The main feature was that, Vinyltec 2000. Conference proceedings.
after a transient regime, the concentration profile tended Philadelphia, Pa., 11th-12th Oct.2000, p.198-202
to move as a front, i.e. without diffusive spreading in time. USE OF ADVANCED ANALYTICAL METHODS
This results in relatively sharp peaks and the observation TO ENHANCE THE PERFORMANCE OF VINYL
that long columns were useless. A simple analytical model MATERIALS
was proposed for this self-focussing process that allowed Isner J D; Eiden R W
optimal conditions of operation to be determined. This Polymer Diagnostics Inc.
analysis was supported by experimental tests. 13 refs. (SPE,Vinyl Div.; SPE,Philadelphia Section)
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
USA; WESTERN EUROPE
Analytical laboratories are asked to perform a variety of
test methods in order to solve problems relating to the
Accession no.813456
performance or otherwise of vinyl materials, and whilst
there are many individual problems that need to be solved,
Item 106 they can be categorised, it is argued, by a relatively small
Macromolecules number of questions. Five of these questions are
34, No.8, 10th April 2001, p.2395-7 addressed, and ways in which a laboratory may answer
NONDESTRUCTIVE MEASUREMENT OF A them are discussed. Suggestions are made for techniques
GLASS TRANSITION TEMPERATURE AT SPIN- that may be used for each question, and examples of
CAST SEMICRYSTALLINE POLYMER SURFACES problems are given. Recent advances in analytical

70 © Copyright 2002 Rapra Technology Limited


References and Abstracts

techniques can be used to address topics such as lifetime temperatures and frequencies were used in the
prediction and failure analysis. Questions related to investigation. Results by each technique indicated that
identification, commercialisation, competitiveness, failure the degree of microphase separation of PUR into hard-
and performance. segment (HS) microdomains and soft-segment (SS)
USA microphase increases on addition of SAN. The various
Accession no.811310 techniques used were initially compared with each other.
Results showed that for the dynamic glass transition of
the PUR SS microphase the characteristic time scales at
Item 109 the same temperature are similar for DSC, TSDC and
Journal of Materials Science Letters DMTA and shorter for DRS. The PUR/SAN blends are
20, No.3, 1st Feb.2001, p.257-8 classified as fragile systems. 40 refs.
COMMENTS ON A NEW RAMAN PEAK IN A
EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE;
HIGH-DENSITY POLYETHYLENE WESTERN EUROPE
Rodriguez A B; Young R J Accession no.810314
Navarra,Universidad Publica; Manchester,University;
UMIST
Item 111
Raman spectroscopy yields information about the Macromolecular Rapid Communications
molecular structure of materials based on the observation 22, No.2, 8th Feb.2001, p.51-67
of scattered light spectra, and has been used extensively EVANESCENT WAVE LIGHT SCATTERING.
in the investigations of polymer structure and FUSION OF THE EVANESCENT WAVE AND
composition: chemical structure and interactions, LIGHT SCATTERING TECHNIQUES TO THE
morphology, crystalline and amorphous structure, STUDY OF COLLOIDS AND POLYMERS NEAR
processing effects and orientation, etc. As an analytical THE INTERFACE
technique, however, it is not free from artefacts, i.e. Matsuoka H
apparent experimental results that are not actually real Kyoto,University
but are due to the experimental methods or conditions.
One factor that may be responsible for the presence of The evanescent wave light scattering technique, which is
artefacts in Raman spectroscopy is external background produced by a fusion of the evanescent wave technique
light. There are numerous potential sources of external and light scattering technique, is a very powerful an useful
background light that lead to sharp spectral peaks. If they tool for investigation of colloidal particles and polymers
are not excluded from the collection optics of the Raman near the surface and interfaces. Two kinds of evanescent
instrument, they can lead to noise, or artefacts, wave light scattering apparatuses are developed. One is
superimposed on the Raman spectrum from the sample. the evanescent wave dynamic light scattering (EVDLS)
This background light can come from either the sample technique and the other is the evanescent wave light
or from the environment around the sample. A study of scattering microscope (EVLSM). By EVDLS, the diffusion
the latter is reported. 14 refs. behaviour of a colloidal particle near the interface can be
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK; extracted quantitatively as a function of the distance from
WESTERN EUROPE the interface. The diffusion coefficient is smaller than those
Accession no.811165 for particles in bulk, reflecting electrostatic and
hydrodynamic interactions. By EVLSM, the interaction
potential profile between a colloidal particle and the surface
Item 110 in dispersion can be directly evaluated. EVLSM will play
Journal of Applied Polymer Science an import role in colloidal interaction studies, especially at
80, No.7, 16th May 2001, p.1071-84 a low ionic strength. It is also shown that a particle dynamics
PHASE BEHAVIOUR AND MOLECULAR study is possible by the EVLSM technique. A new field
MOBILITY IN POLYURETHANE/STYRENE- will be developed in colloid science and polymer science
ACRYLONITRILE BLENDS by application of the evanescent wave light scattering
Vatalis A S; Kanapitsas A; Delides C G; Viras K; Pissis P technique, i.e. fusion of the evanescent light and a scattering
Kozani,Technological Education Institute; techniques. 41 refs.
Athens,University; Athens,Kapodistrian University JAPAN
The molecular mobility and microphase separation in Accession no.809623
blends of crosslinked polyurethane (PUR) and styrene-
acrylonitrile (SAN) copolymer were investigated. The
Item 112
PUR and SAN copolymer were prepared by reactive
Journal of Applied Polymer Science
blending with polymer polyols. DSC, thermally
79, No.6, 7th Feb.2001, p.1101-12
stimulated depolarisation currents (TSDC) techniques,
ULTRASONICATION AND MICROWAVE
dielectric relaxation spectroscopy (DRS) and dynamic
ASSISTED EXTRACTION OF DEGRADATION
mechanical thermal analysis over a wide range of
PRODUCTS FROM DEGRADABLE

© Copyright 2002 Rapra Technology Limited 71


References and Abstracts

POLYOLEFIN BLENDS AGED IN SOIL segments capable of establishing strong intermolecular


Contat-Rodrigo L; Haider N; Ribes-Greus A; Karlsson hydrogen bonds. Characterisation was carried out using
S proton NMR, size exclusion chromatography, DSC, and
Stockholm,Royal Institute of Technology; dynamic mechanical analysis. The influence of the ratio
Valencia,Polytechnical University of hard and soft segments on degree of crystallinity, Tg,
melting point, tensile strength, elongation and Young’s
Degradation in soil of samples of a polyolefin blend
modulus was examined. 24 refs.
treated with two different biodegradable additives (a
EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERN
starch/iron mixture and a commercial product (Mater-Bi
EUROPE
AF05H)) was studied using two non-conventional
extraction techniques. The period studied was from 0 to Accession no.808057
21 months, and extracted products were analysed by gas
chromatography mass spectroscopy. Molecular weight Item 115
changes were monitored using high-temperature size Journal of Applied Polymer Science
exclusion chromatography. Extraction techniques were 80, No.1, 4th April 2001, p.1-9
ultrasonication and microwave assisted extraction (MAE). CROSSLINKING AND ITS EFFECTS ON
Reproducibility of ultrasonification was found better with POLYANILINE FILMS
improved extraction of carboxylic acids and other Tan H H; Neoh K G; Liu F T; Kocherginsky N; Kang E T
products than MAE methods, but both were found faster Singapore,National University
than conventional (soxhlet) extraction techniques. Tables Polyaniline base films with varying degrees of
indicate the relative amounts of different extraction crosslinking were cast from methylpyrrolidone solutions
products and molecular weight changes in the polymer at different processing temperatures. The effects of
blend found over the 21-month period for both crosslinking on solubility, morphology, tensile strength,
biodegradable additive types. 17 refs doping characteristics and transport of ions across the
EUROPEAN COMMUNITY; EUROPEAN UNION; films were investigated. Characterisation was undertaken
SCANDINAVIA; SPAIN; SWEDEN; WESTERN EUROPE using UV visible spectroscopy, atomic force microscopy,
Accession no.808785 and elemental analysis. 18 refs.
SINGAPORE
Item 113 Accession no.807643
Polimeros: Ciencia e Tecnologia
10, No.4, Oct./Dec.2000, p.202-8 Item 116
Portuguese Macromolecular Symposia
ETHYLENE COPOLYMERS ANALYSIS BY Vol.162, Dec.2000, p.227-33
FRACTIONATION TECHNIQUES STUDY OF POLYMER COMPLEXES BY
Escher F F N; Silva L P; Galland G B; Benetti A EXCLUSION CHROMATOGRAPHY COUPLED
Rio Grande do Sul,Universidade Federal; Ipiranga WITH LIGHT SCATTERING IN COMBINATION
Petroquimica SA WITH FLUORESCENCE SPECTROSCOPY
Mrkvickova L; Pokorna V; Pecka J
Ethylene-butene copolymers were fractionated according
Czech Republic,Academy of Sciences
to molecular size by direct extraction by different solvents
and at different temperatures. Samples were also PMMA stereocomplexes prepared at different
fractionated by differences in crystallinity using DSC. concentration in dilute tetrahydrofuran solutions are studied
Fractions were characterised using carbon 13 NMR, FTIR, by size exclusion chromatography coupled with refractive
GPC and DSC. 9 refs. and light scattering detectors in combination with
BRAZIL fluorescence spectroscopy. A considerable increase in
Accession no.808128 segment density due to complexation compared with free
PMMA chain is only slightly affected by the polymer
concentration in solution where stereocomplexes are
Item 114 formed. At polymer concentrations up to 3 x 10-3 g cm-3,
Journal of Polymer Science: Polymer Chemistry an increase in non-uniformity of polymer complex
Edition molecular weight and size and a shift to higher values of
39, No.5, 1st March 2001, p.630-9 both are observed. In semidilute solutions stereocomplexes
NEW SEGMENTED POLYESTER-URETHANES virtually do not become heavier and larger. 6 refs.
FROM RENEWABLE RESOURCES CZECH REPUBLIC
Liu Y; Lindblad M S; Ranucci E; Albertsson A-C
Accession no.806260
Sweden,Royal Institute of Technology
The physical and mechanical properties of aliphatic Item 117
polyesters from propanediol and succinic acid were Polymer
improved by their combination with aromatic urethane 42, No.8, 2001, p.3859-66

72 © Copyright 2002 Rapra Technology Limited


References and Abstracts

STRUCTURE FORMATION DURING THE analytical data, including data on the relation between
ISOTHERMAL CRYSTALLISATION OF retention time and nitrile polarity, and the limiting yield on
ORIENTED AMORPHOUS POLY(ETHYLENE pyrolysis as a function of temperature were obtained. On
TEREPHTHALATE) FILMS the basis of these results, specific applications of PGCA and
Radhakrishnan J; Kaito A the usefulness of this method for studying the thermal
Japan,National Institute of Materials & Chemical degradation of acrylonitrile polymer are indicated. 20 refs.
Research JAPAN

A study was made of structure formation during the Accession no.804442


isothermal crystallisation of oriented, amorphous PETP
film from the glassy state using in situ FTIR spectroscopy, Item 120
in situ wide-angle X-ray diffraction and small angle X- West Conshohocken, Pa., 2000, pp.3. NALOAN
ray scattering. The PETP films were prepared by rolling ASTM D 3465-. TEST METHOD FOR PURITY OF
melt quenched films to a draw ratio of 2 and an evaluation MONOMERIC PLASTICISERS BY GAS
made of the changes in the conformation and orientation CHROMATOGRAPHY
order of the PETP chains during crystallisation along with American Society for Testing & Materials
the development of crystalline structure. Structure ASTM D 3465-
organisation before and during isothermal crystallisation Version 2000. Photocopies and loans of this document
is discussed and a comparison made of the crystallisation are not available from Rapra.
behaviour of oriented with that of isotropic PETP. 27 refs.
USA
JAPAN
Accession no.801052
Accession no.806185
Item 121
Item 118 Polymer News
Antec 2000.Conference proceedings. 25, No.10, Oct.2000, p.359-60
Orlando, Fl., 7th-11th May, 2000, paper 678 ANALYSIS OF AIRCRAFT COATING BY
USE OF CONTACT-ATOMIC FORCE SECONDARY ION MASS SPECTROSCOPY
MICROSCOPY IN PLASTIC MATERIAL Usmani A M; Donley M
SURFACES UDC; Wright-Patterson Air Force Base
Reyes E; Guerrero C
An analysis was made of a flat aircraft coating using
Nuevo Leon,Universidad Autonoma
secondary ion mass spectroscopy, which revealed that the
(SPE)
coating was a polyurethane C type based on isophorone
Using thin films of isotactic polypropylene, poly(ethylene diisocyanate, diethylene glycol and adipic acid. X-ray
terephthalate) and polystyrene, the range of atomic force photoelectron spectroscopy was employed to determine
microscopy contact forces and the scanning frequencies pigments and extenders. 10 refs.
required to obtain sharp and clear 3-D images of polymer USA
surfaces was determined, by systematically varying these Accession no.800157
parameters, starting with typical values used for rigid
surfaces. The optimum values were determined to be a Item 122
contact force of 88-150 nN, and a scanning frequency of Antec 2000.Conference proceedings.
1.0-1.5 Hz. 12 refs. Orlando, Fl., 7th-11th May, 2000, paper 441
MEXICO THERMODYNAMIC AND KINETIC ANALYSIS
Accession no.805686 OF SEMICRYSTALLINE RECYCLATES BY DSC
Cassel R B; Li L
Item 119 Perkin-Elmer Inc.
Journal of Applied Polymer Science (SPE)
79, No.3, 18th Jan.2001, p.473-8 Developments in differential scanning calorimetry (DSC)
PYROLYSIS GAS CHROMATOGRAPHIC for the characterisation of semicrystalline thermoplastics,
ANALYSIS OF POLYACRYLONITRILE including mixed recyclates are discussed. The techniques
Minagawa M; Onuma H; Ogita T; Uchida H include stepwise DSC for the accurate determination of
Yamagata,University specific heat capacity, rapid determination of crystallinity
In the pyrolytic gas chromatographic analysis (PGCA) of using the Gray-Mathot total enthalpy technique, and
acrylonitrile polymer under an inert atmosphere at 500-900 analysis of crystallisation kinetics. The techniques show
deg.C, lower nitriles, including methyl cyanide, HCN, and the influence of impurities on the glass transition
acrylonitrile were the main degradation products, but lower temperature, crystallinity and crystallisation. 6 refs.
hydrocarbons, e.g. methane and ethylene, resulting from USA
secondary decomposition, were also detected. Thermo- Accession no.799956

© Copyright 2002 Rapra Technology Limited 73


References and Abstracts

Item 123 PHASE SEPARATION IN MISCIBLE POLYMER


Antec 2000.Conference proceedings. BLENDS AS DETECTED BY MODULATED
Orlando, Fl., 7th-11th May, 2000, paper 439 TEMPERATURE DIFFERENTIAL SCANNING
NOVEL TECHNIQUE FOR THE DETECTION OF CALORIMETRY
A HINDERED AMINE LIGHT STABILIZER Dreezen G; Groeninckx G; Swier S; Van Mele B
(HALS), BASED ON SILICON TECHNOLOGY Leuven,Catholic University; Brussels,Free University
Narayan S; Lee R E; Hallberg D; Malatesta V
The phase separation of two partially miscible polymer
Great Lakes Chemical Corp.; Great Lakes Chemical
blends was studied using modulated temp.
Italia
DSC(MTDSC). The lower critical solution temp.
(SPE)
demixing behaviour of PEO blended with polyether
A technique for the determination of HALS in sulphone(PES) and with poly(3,4'-diphenylene ether
polypropylene was developed. The HALS, based on a isophthaloyl amide), as determined by cloud point temps.
polysiloxane backbone with tetramethyl piperidine side with optical microscopy, was in good agreement with
chains, was melt blended with the polypropylene which results obtained from non-isothermal MTDSC
was then spun into fibres. The chopped fibres were measurements. The non-isothermal MTDSC apparent
dissolved in toluene, the polymer precipitated using heat capacity evolution was time-dependent. It was
methanol, and the filtrate dried. A solution of the filtrate influenced by the endothermic demixing enthalpy and,
was then prepared and analysed by proton nuclear in the case of PEO/PES blends, by the vitrification of a
magnetic resonance spectroscopy. The peak at 0.1 ppm high-Tg phase formed. Quasi-isothermal MTDSC
was attributed to the methyl group on the silicon atom of measurements contained information on the kinetics of
the HALS, and was used for quantitative purposes. demixing and remixing, emphasising the added value
Polypropylene pellets were also prepared containing a of MTDSC to follow in situ the diffusion-controlled
lower concentration of HALS, which was subsequently phase separation processes of partially miscible polymer
subjected to direct extraction to prevent the loss which blends. 32 refs.
may occur during polymer reprecipitation. 3 refs. BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
USA WESTERN EUROPE

Accession no.799954 Accession no.798922

Item 124 Item 126


Antec 2000.Conference proceedings. Macromolecular Materials and Engineering
Orlando, Fl., 7th-11th May, 2000, paper 438 Vol.283, Nov.2000 p.153-62
ANALYTICAL METHODOLOGIES EMPLOYED CHARACTERIZATION OF FLAME-SPRAYED
IN A COMPREHENSIVE FDA FOOD CONTACT PEEK COATINGS BY FTIR-ATR, DSC AND
COMPLIANCE INVESTIGATION: ANALYSIS ACOUSTIC MICROSCOPY
FOR RESIDUAL MONOMERS, RESIN Simonin L; Liao H
OLIGOMERS, ADDITIVES AND MODIFIERS IN CREST; Belfort-Montbeliard,Universite de
SEVERAL FOOD SIMULATING SOLVENTS Technologie
Eberhard J S; McCort-Tipton M M Poly (aryl ether ether ketone) (PEEK) was utilised as a
Covance Laboratories name-sprayed coating because of its good mechanical
(SPE) properties, low friction coefficient and high thermal
The FDA considers that materials which come into contact stability. Fine polymeric powders were warmed up in
with food, such as processing machinery and packaging, oxyacetylene flame and sprayed onto a previously heated
to be indirect food additives, and the potential migration aluminium substrate. Investigation of the degree of
of materials into the food requires determination. Ethanol/ crystallinity of PEEK coatings was carried out using
water solutions and food oils are commonly used as food differential scanning calorimetry (DSC), according to
simulating solvents when determining migration. The the rate of cooling after the spraying process. Structural
subsequent determination of the migrating species (which modifications were revealed by FTIR-ATR, attributed
may include residual monomers, oligomers, additives and to interactions between the flame and the polymeric
modifiers) may be by liquid and gas chromatography, and powders. Ultrasonic methods were developed, especially
mass spectroscopy. acoustic microscopy, to study the variations of
USA mechanical properties at the surface and the defects
inside the material. In general terms, flame-sprayed
Accession no.799953
coatings contain a large amount of porosity. Particularly
suited to the observation of large defects (exceeding 50
Item 125 microns) inside the polymeric materials is low-frequency
Polymer microechography, a non-destructive technique. 19 refs.
42, No.4, 2001, p.1449-59 Accession no.798668

74 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Item 127 RAMAN SPECTRAL MAPPING OF


Polymer Preprints, Volume 40, Number 2, August PHOTOOXIDISED POLYPROPYLENE
1999, Conference proceedings. Blakey I; George G A
New Orleans, La., August 1999, p.1043-4 Queensland,University of Technology
MALDI/TOF/MS STUDY OF HOMOPOLYMERS
The photooxidation of unstabilised, isotactic PP was
AND AMPHIPHILIC DIBLOCK COPOLYMERS
investigated using Raman spectral mapping in
BASED ON SULPHONATED POLYSTYRENE
combination with SEM/energy dispersive X-ray analysis,
Yang A; Nonidez W K; Mays J W
which permitted the determination of Ziegler-Natta
Birmingham,University of Alabama
catalyst residue distribution throughout the PP. It was
(ACS,Div.of Polymer Chemistry)
found that oxidation was heterogeneous at a microscopic
Matrix-assisted laser desorption ionisation time of flight scale and that a high local concentration of catalyst
mass spectroscopy (MALDI/TOF/MS) provides a new residues resulted in the stabilisation of the polymer in the
way to probe polymers; it can provide information on immediate vicinity and the formation of mobile reactive
molecular weight, molecular weight distribution, mass species, which initiated oxidation at sites away from the
of end groups and mass of repeating units. Further catalyst. 30 refs.
information, such as reactivity ratios, individual block AUSTRALIA
chain length and its distribution, etc., can be obtained Accession no.795269
based on mass information. Polystyrene sulphonic acid
and its sodium salt form have been successfully
characterised by MALDI/TOF/MS, but no MALDI/TOF/ Item 130
MS study of diblock copolymers containing a polystyrene Macromolecules
sulphonic acid block appears to be evident. The results 33, No.19, 19th Sept.2000, p.7088-92
of such a study of amphiphilic diblock copolymers, SOLUTION CARBON-13 NMR
NaPSS-b-PtBS, and their precursors, PSb-PtBS, are CHARACTERIZATION OF NYLON 66:
reported. Number-average and weight-average molecular QUANTITATION OF CIS AMINE
weights (Mn and Mw), polydispersity indices and extents CONFORMERS, ACID AND AMINE GROUPS,
of sulphonation are obtained. 13 refs. AND CYCLIC UNIMERS
Southern Mississippi,University
USA
Edited by: Davis R D; Steadman S J; Jatterr W L;
Accession no.798428 Mathias L J
Item 128 Using a mixed 2,2,2-trifluoroethanol/deuteriochloroform
Polymer Degradation and Stability solvent system, well-resolved solution carbon-13 NMR
71, No.1, 2001, p.123-34 spectra of nylon-66 samples were obtained which showed
QUALITY-DETERMINATION OF RECYCLED several low intensity peaks which were not seen in more
PLASTIC PACKAGING WASTE BY acidic solvents. The low intensity peaks were correlated
IDENTIFICATION OF CONTAMINANTS BY GC- with the methylene carbons near cis amide conformers,
MS AFTER MICROWAVE ASSISTED acid and amine end groups and within cyclic oligomers.
EXTRACTION (MAE) The quantitative contents of these components for a
Camacho W; Karlsson S typical nylon-66 sample were 1.1 mol% cis amide
Sweden,Royal Institute of Technology conformers, 1.0 mol% acid end groups and 0.5 mol%
amine end groups. From end group concentrations, the
The resulted are reported of an investigation into the number-average molecular weight of the nylon-66 was
quality of recycled HDPE and PP separated from mixed calculated to be 30 177 g/mol. The chemical shift values
municipal solid waste carried out using gas of methylene carbons in the end groups and in cyclic
chromatography-mass spectrometry. The development of oligomers was pH sensitive and thus depended on the
a simple and rapid microwave assisted extraction method relative concentrations of acid and amine groups in each
for the systematic analysis of low molec.wt. compounds, sample. 12 refs.
such as decomposition products and additives, in
USA
polymers is also reported and successfully applied to the
analysis of contaminants in the above recycled plastics. Accession no.794402
15 refs.
EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERN Item 131
EUROPE Polymer Engineering and Science
Accession no.796627 40, No.11, Nov.2000, p.2442-55
EVALUATION OF THREE METHODS FOR THE
Item 129 MEASUREMENT OF CRYSTALLINITY OF PET
Polymer Degradation and Stability RESINS, PREFORMS, AND BOTTLES
70, No.2, Nov.2000, p.269-75 Bashir Z; Al-Aloush I; Al-Raqibah I; Ibrahim M

© Copyright 2002 Rapra Technology Limited 75


References and Abstracts

SABIC R & D EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;


WESTERN EUROPE
The crystallinity of PETP resins, preforms and bottles was Accession no.792350
investigated using DSC, modulated DSC and density
measurements. The PETP employed was a bottle-grade
PETP copolymer containing 1.5% isophthalic acid. The Item 134
accuracy, precision and validity of the techniques ICAC 99. Conference proceedings.
employed were evaluated and problems encountered in Bristol, UK, 23rd-24th Sept.1999, p.133-43
interpreting the results assessed. 47 refs. IDENTIFICATION OF KEY CURE STAGES IN
SAUDI ARABIA LIQUID MOULDING PROCESSES BY
PARALLEL PLATE DIELECTRIC ANALYSIS
Accession no.793608
McIlhagger A T; Matthews S T; Brown D; Hill B
Ulster,University
Item 132 (IOM Communications Ltd.; Ulster,University;
Kautchuk und Gummi Kunststoffe IMechE)
53, No.10, Oct.2000, p.574/81
The aerospace industry has recognised the major benefits
German
associated with fibre reinforced composite materials. The
DIRECT ANALYSIS OF ADDITIVES IN
more popular techniques available for composite
POLYMERIC MATERIALS BY PYROLYSIS-GAS
production are the traditional wet lay-up or autoclave and
CHROMATOGRAPHY-MASS SPECTROMETRY
resin transfer moulding (RTM). Efforts to further reduce
Meyer-Dulheuer T; Pasch H; Geissler M
processing time and improve part quality have focused
Deutsches Kunststoff-Institut
on improved process control. To date this has been based
This article describes the direct analysis of additives by on off-line techniques. The need for on-line cure
pyrolysis-gas chromatography-mass spectrometry. Using monitoring is widely recognised and this will require the
this method it is possible to identify additives quickly development of suitable in-mould sensors. The
and reliably without separation of the polymer matrix. A Engineering Composites Research Centre (ECKE) has
small specimen of the sample is pyrolysed, i.e. degraded investigated and concentrated on the specific problems
under inert gas atmosphere. The pyrolysis products are encountered in the aerospace industry. Of the available
separated by gas chromatography and ionised in the mass cure monitoring methods, parallel plate dielectric analysis
spectrometer by electron-impact ionisation. By comparing (DEA) appears to offer the greatest potential for
the results with library data it is possible to identify determining the through-thickness cure state of the resin
unknown additives unambiguously and with high during cure. A laboratory dielectric instrument is utilised
accuracy. 10 refs. to simulate RTM and autoclave cure cycles for composite
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; structures containing non-conductive and conductive
WESTERN EUROPE fibres and for different resin systems used in the aerospace
Accession no.792613 industry. Key resin cure stages are identified by an
appropriate dielectric signal and correlated with data from
Item 133 other thermal and mechanical techniques. Insulated
Journal of Thermal Analysis and Calorimetry parallel plate dielectric sensors are being developed for
61, No.2, 2000, p.589-96 use in the laboratory instrument with the potential for
CALORIMETRIC ANALYSIS OF AN ISOTACTIC incorporation into composite production tooling. 26 refs.
POLYPROPYLENE GAMMA-IRRADIATED IN EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
VACUUM
Spadaro G; Valenza A Accession no.790059
Palermo,University
The molecular modifications induced in an isotactic PP Item 135
gamma-irradiated in vacuum under a complete set of Polymer Journal (Japan)
experimental conditions are studied by means of calorimetric 32, No.7, 2000, p.610-5
analysis. The influence of the irradiation parameters, the total INFRARED SPECTROSCOPIC AND
absorbed dose, D, and the dose rate, I, has previously been MODULATED DIFFERENTIAL SCANNING
analysed and a simple kinetic model based on the rates of CALORIMETRY STUDY OF PHYSICAL AGING
the main reactions occurring during irradiation, i.e. beta- IN BISPHENOL A POLYCARBONATE
scission, addition to double bonds and termination, was also Jin Lu; Yong Wang; Deyan Shen
discussed. It is shown how thermal analysis confirms the Academia Sinica
model forecasts and in particular the existence of the FTIR spectroscopy was used to study the conformational
‘inversion conditions’: below them the main effect is changes in quenched bisphenol A polycarbonate films
molecular degradation, while above them the main effects during physical ageing. The conformation changed
are chain-branching and crosslinking. 12 refs. gradually from the high energy trans-cis conformation to

76 © Copyright 2002 Rapra Technology Limited


References and Abstracts

the low energy trans-trans conformation on sub-glass Item 138


transition temperature annealing. In-situ FTIR studies on Polymers Paint Colour Journal
the conformational changes of films quenched from the 190, No.4432, Sept.2000, p.25-6
rubbery and sub-glass transition temperature annealed for WATCHING PAINT DRY
different times were carried out while increasing the Middleton J
temperature through the glass transition region. The
The development of nuclear magnetic resonance imaging,
results indicated that incremental changes in the
a technique previously only used in medicine, to provide
population of trans-cis conformers in the quenched sample
various information, including the drying rate, position
were gradual, whereas rather abrupt changes occurred in
of water and curing in waterborne coatings, is discussed.
the sub-glass transition temperature annealed samples.
The principles of magnetic resonance imaging are outlined
The energy absorbed during the abrupt conformational
and work conducted at Surrey University in conjunction
change represented only part of the endothermic peak
with Resonance Instruments to design equipment for
observed by modulated DSC. The authors concluded that
coatings analysis is described.
some new cohesional entanglements may be formed
during physical ageing. 28 refs. SURREY,UNIVERSITY; RESONANCE
CHINA
INSTRUMENTS
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Accession no.789734 WESTERN EUROPE
Accession no.789465
Item 136
Polymer Journal (Japan) Item 139
32, No.7, 2000, p.560-6 Journal of Applied Polymer Science
CALORIMETRIC AND INFRARED 78, No.5, 31st Oct.2000 p.1009-16
SPECTROSCOPIC ANALYSIS OF MULTIPLE CRYSTALLIZATION OF LOW-DENSITY
MELTING ENDOTHERMS OF POLYETHYLENE- AND LINEAR LOW-DENSITY
POLY(ETHYLENE TEREPHTHALATE) POLYETHYLENE-RICH BLENDS
Yong Wang; Jin Liu; Deyan Shen Drummond K M; Hopewell J L; Shanks R A
Chinese Academy of Sciences RMIT University
The multiple melting behaviour of PETP was studied Using differential scanning calorimetry (DSC) the
using DSC, FTIR spectroscopy and temperature crystallisation of a series of low-density polyethylene
modulated DSC by examining PETP samples subjected (LDPE)- and linear low-density polyethylene (LLDPE)-
to special schemes of crystallisation and annealing rich blends was examined. After continuous slow cooling
treatment at different temperatures. On one-step and two- DSC analysis showed a broadening of the LLDPE melt
step annealing, a series of multiple endothermic minor peak and subsequent increase in the area of a second
peaks was observed, resulting from the melting of lower-temperature peak with increasing concentration of
imperfect crystals during crystallisation. Both dual LDPE. Melt endotherms following stepwise
morphology and melting-recrystallisation-remelting
crystallisation (thermal fractionation) detailed the effect
mechanisms were probably responsible for the observed
of the addition of LDPE to LLDPE, showing a nonlinear
multiple melting behaviour which was dependent on the
broadening in the melting distribution of lamellae, across
thermal history of the PETP samples. 34 refs.
the temperature range 80-140 degrees Celsius, with
CHINA
increasing concentration of LDPE. A rise in the population
Accession no.789727 of crystallites melting in the region between 110 and 120
degrees Celsius, a region was observed where as a pure
Item 137 component LDPE does not melt. A decrease in the
Analytical Chemistry crystallite population over the temperature range where
72, No.19, 1st Oct.2000, p.4550-4 LDPE exhibits its primary melting peaks (90-110 degrees
GPC SEPARATION OF POLYMER SAMPLES Celsius) was noted, indicating that a proportion of the
FOR MALDI ANALYSIS lamellae in this temperature range (attributed to either
Hanton S D; Liu X M LDPE or LLDPE) were shifted to a higher melt
Air Products & Chemicals Inc.; Lab Connections Inc. temperature. 30 refs.
MALDI mass spectrometry was combined with GPC Accession no.789066
analysis for broad polydispersity polymers with the use
of liquid chromatography interface. Results for PMMA Item 140
were compared with a blend of five narrow PMMA Polymer International
standards that mimic the broad dispersed material. 24 refs. 49, No.9, Sept.2000, p.1007-13
USA USING SPECTROSCOPY WITH
Accession no.789529 CHEMOMETRICS TO MEASURE POLYMER

© Copyright 2002 Rapra Technology Limited 77


References and Abstracts

MOLAR MASS polymethacrylic acid and polymethacrylonitrile. The


Shenton M J; Herman H; Stevens G C overall variation of the dispersive component of the
Surrey,University surface energy and the ratio of acceptor to donor
coefficients appear to group themselves into two
The ability to determine the molar mass of a polymer is
categories based upon the polarity of the polymer’s
of fundamental importance to describe polymer molecular
functional groups. In addition, the high loadings required
characteristics. Conventional methods for measuring
molar mass include viscometry, osmometry, light for stabilisation of the less polar polymers suggest that a
scattering and analytical gel permeation chromatography. relatively large volume of the matrix phase isaffected by
Although high quality data can be obtained by these the wood filler. 20 refs.
methods, the results can be significantly affected by USA
sample preparation, and they are often time consuming Accession no.786897
and unsuitable for real-time on-line processing. The
potential of determining polymer molar mass using optical Item 142
spectroscopy combined with chemometric analysis is Polymer Science Series B
demonstrated. This is technically attractive because 42, Nos.5-6, May-June 2000, p.169-74
optical spectroscopy is routinely used to collect process IR SPECTROSCOPY STUDY OF POLYMER
data on-line and some refineries routinely monitor and POROSITY
control blending using near-infrared spectroscopy. A Pakhomov P M; Kruglova E V; Khizhnyak S D
comparable development to monitor polymer molar Tver,State University
masses on-line from systems already being used to
measure density and melt index, would be of potential IR spectroscopic method is developed for evaluating the
value to many sectors of the polymer production and porosity (concentration and size of pores) in polymers.
processing industry. Chemometrics is a multivariate PE and PAN films of various porosity are prepared from
methodology that allows the information from entire the solutions in liquid and solid paraffins. The
spectra to be used; it can be considered as a maximal concentration and maximum pore size in the bulk and in
compression technique. Extracted ‘factors’ can then be a surface layer of the samples are determined by IR
regressed against property data by using a well- spectroscopy in the transmission and reflection modes,
characterised set of ‘training’ samples to produce respectively. The results obtained are in agreement with
predictive regression models. It is shown that simple the data of optical and atomic force microscopy. 12 refs.
spectroscopic methods, such as the Raman technique RUSSIA
discussed, when coupled with chemometrics, are capable Accession no.786845
of providing molar mass and distribution information.
This is illustrated with reference to polydimethylsiloxanes
in the liquid phase. 18 refs. Item 143
Iranian Polymer Journal
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE 9, No.2, April 2000, p.117-24
STUDY OF CRYSTALLINITY OF HIGH-
Accession no.787562
DENSITY POLYETHYLENE BY INVERSE GAS
CHROMATOGRAPHY
Item 141 Ghaemy M; Hadjmohammadi M R; Tabaraki R
Composite Interfaces Mazandaran,University
7, No.2, 2000, p.81-92
INVESTIGATING INTERPHASE The crystallinity of HDPE (Poliran-HD0035 and Irapol-
DEVELOPMENT IN WOOD-POLYMER 5620) was investigated using inverse gas chromatography.
COMPOSITES BY INVERSE GAS The effects of flow rate of carrier gas and sample size on
CHROMATOGRAPHY peak retention volume and of the amount of injection on
Rials T G; Simonsen J retention volume were evaluated. Retention diagrams and
USDA; Oregon,State University degrees of crystallinity of the HDPEs were determined
and compared with those of LDPE. 15 refs.
The influence of secondary interactions on the
IRAN
development of interfacial structure in composites of
wood and amorphous thermoplastic polymers is not well Accession no.786383
understood. Inverse gas chromatography is used to
investigate the effect of different polymers on the surface Item 144
energy of partially or fully coated white pine wood meal. Journal of Applied Polymer Science
In this way, the development of the interphase is 77, No.7, 15th Aug.2000, p.1419-31
monitored as a function of polymer depth on the wood CURE MODELING AND MONITORING OF
surface. The polymers are selected to provide a range of EPOXY/AMINE RESIN SYSTEMS. 1. CURE
functional groups and include PS, PMMA, PVC, KINETICS MODELING

78 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Karkanas P I; Partridge I K APPLICATION OF MODULATED-


Cranfield,University TEMPERATURE DIFFERENTIAL SCANNING
CALORIMETRY TO THE STUDY OF
An investigation using differential scanning calorimetry
CRYSTALLISATION KINETICS IN POLY(E-
was carried out under both isothermal and dynamic curing
CAPROLACTONE)-POLY(STYRENE-CO
conditions to determine the cure kinetics of four epoxy/
ACRYLONITRILE) BLENDS
amine resins. Various cure kinetic models were used to
Song M; Hourston D J
compare them with the results of the DSC results. Good
Loughborough,University
fits were found, in good agreement with the experimental
results for the resin systems. 22 refs. In order to evaluate the application of modulated-
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; temperature differential scanning calorimetry (M-TDSC)
WESTERN EUROPE to the study of the crystallisation kinetics of semi-
Accession no.786048 crystalline polymers, isothermal crystallisation kinetics
in poly(e-caprolactone)-SAN blends are investigated. The
temperature dependence of d ln G/dT (G =crystal growth
Item 145
rate), determined by M-TDSC agrees approximately with
International Polymer Science and Technology
previous experimental data and theoretical values. These
27, No.6, 2000, p.T/7-T/9. (Translation of Muanyag es
were obtained from direct measurements of spherulite
Gumi, No.3, 2000, p.89)
growth rate by optical microscopy. Here, theoretical and
APPLICATION OF STATE-OF-THE-ART
M-TDSC experimental results show that the d ln G/dT
METHODS IN ADHESION TECHNOLOGY. 1
versus temperature plots are not sensitive to the non-
Vabrik R; Czajlik I; Bertoti I; Keresztes Z; Ille A;
crystalline component in the poly(e-caprolactone)-SAN
Rusnak I; Vig A; Kalman E
blends. 15 refs.
The use is demonstrated of microscopic analysis EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
techniques for the investigation of adhesive failure. PVC WESTERN EUROPE
sheet was bonded to glass using a M35R hybrid UV Accession no.784242
curable adhesive based on epoxy resin. Atomic force
microscopy and X-ray induction photoelectron Item 148
spectroscopy were used for the chemical characterisation Polymer
of of failure surfaces. 11 refs. 41, No.22, Oct.2000, p.8151-4
EASTERN EUROPE; HUNGARY PORE DIMENSION OF WATER TREES IN PE:
Accession no.785593 NMR STUDIES
Judeinstein P; Carmo Lanca M; Marat-Mendes J; Rault J
Paris-Sud,Universite; Portugal,Universidade Nova de
Item 146
Lisboa
Journal of Applied Polymer Science
78, No.1, 3rd Oct. 2000, p.166-72 In PE films aged under electric field the crystallisation of
EFFECT OF POLY(VINYL CHLORIDE)/ water (and melting of ice) is studied by quadrupolar NMR,
CHLORINATED POLYETHYLENE BLEND this technique allows determination of water concentration
COMPOSITION ON THERMAL STABILITY as low as 10 -4. It is shown that the pore dimensions of
Klaric I; Vrandecic N S; Roje U the tracks forming the water trees of the order of 2.5 nm
Split,University are independent of the ageing time. The mobility of water
in these water trees and in porous glass, of similar pore
The miscibility of PVC and chlorinated PE and the effect
dimensions, are compared. 17 refs.
of the blend composition on the heat stability of the PVC
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
were investigated using several techniques, including PORTUGAL; WESTERN EUROPE
TGA and DSC. The apparent activation energy of PVC
Accession no.784240
dehydrochlorination in the blends was calculated and
experimental TGA curves compared with those predicted
using the additivity rule. It was found that the blends were Item 149
heterogeneous and that addition of chlorinated PE in a Journal of Applied Polymer Science
specific temperature range resulted in an improvement 77, No.10, 6th Sept.2000, p.2178-8
in the heat stability of the PVC. 22 refs. CURE MODELLING AND MONITORING OF
EPOXY/AMINE RESIN SYSTEMS. II.
CROATIA
NETWORK FORMATION AND
Accession no.784861 CHEMOVISCOSITY MODELLING
Karkanas P I; Partridge I K
Item 147 Cranfield,University
Polymer The glass transition temperature (Tg) advancement and
41, No.22, Oct.2000, p.8161-5 the chemoviscosity development under isothermal

© Copyright 2002 Rapra Technology Limited 79


References and Abstracts

conditions are investigated for four epoxy/amine systems, filter parameters and the most suitable sampling lines in
including commercial RTM6 and F934 resins. Differential terms of flow rate, diameter, construction material and
scanning calorimetry is the thermoanalytical technique operating temperature have been specified. In the large
used to determine the Tg advancement, and rheometry scale, special concern was given to the probe design and
for determination of the chemoviscosity profiles of these the effects of the probe location as well as practical
resin systems. The complex cure kinetics are correlated considerations of the sampling line length. Quantitative
to the Tg advancement via a one-to-one relationship using calibration and prediction methods have been constructed
Di Benedetto’s formula. It is revealed that the three- for different components present in smoke gases.
dimensional network formation follows a single activated Recommendations on how to deal with interferents, non-
mechanism independent of whether the cure kinetics linearities and outliers have been provided and a
follow a single or several activation mechanisms. The verification method for the spectrometer for unexpected
viscosity profiles show the typical characteristics of variations and for the different models have been
epoxy/amine cure. A modified version of the Williams- described. FTIR measurement procedures in different fire
Landel-Ferry equation (WLF) is adequate to model the test scenarios are studied using the recommendations of
viscosity profiles of all the resin systems, in the this project for measurement techniques and analysis and
temperature range 130 to 170 deg.C, with a very good an interlaboratory trial of the FTIR technique in smoke
degree of accuracy. The parameters of the WLF equation gas analysis is carried out to define the repeatability and
are found to vary in a systematic manner with cure reproducibility of the method in connection with a small
temperature. Further correlation between Tg and viscosity scale fire test method, the cone calorimeter. 9 refs.
shows that gelation, defined as the point where viscosity BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
reaches 10 4 Pas, occurs at a unique Tg value for each FINLAND; FRANCE; ITALY; SCANDINAVIA; SWEDEN; UK;
resin system, which is independent of the cure conditions. WESTERN EUROPE
16 refs. Accession no.784096
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
Item 151
Accession no.784172 Polymer
41, No.23, Nov.2000, p.8241-5
Item 150 USE OF RAMAN SPECTROSCOPY TO STUDY
Fire & Materials THE REACTION BETWEEN AN AMINE-
24, No.2, March/April 2000, p.101-12 TERMINATED THERMOPLASTIC AND EPOXY
SMOKE GAS ANALYSIS BY FOURIER RESINS
TRANSFORM INFRARED SPECTROSCOPY - van Overbeke E; Carlier V; Devaux J; Carter J T;
SUMMARY OF THE SAFIR PROJECT RESULTS McGrail P T; Legras R
Hakkarainen T; Mikkola E; Laperre J; Gensous F; Louvain,Universite Catholique; ICI Plc
Fardell P; Le Tallec Y; Bajocchi C; Paul K; Simonson Reactive thermoplastics are often used as toughening
M; Deleu C; Metcalfe E modifiers for epoxy resins. Raman spectroscopy was used
VTT Building Technology; Centexbel; Elf Atochem to follow the reaction of aromatic amines with epoxide
SA; UK,Building Research Establishment; CEMATE; monomers through the evolution of an amine-substituted
LSF SUD srl; Rapra Technology Ltd.; Sweden,National aromatic vibration. A double shift of this peak was correlated
Testing & Research Institute; Ghent,University; with the formation of secondary and tertiary amines. Band
Greenwich,University assignment was confirmed by the study of model
The determination of toxic components from fire gases compounds. Using this method, qualitative observation of
is difficult because the environment is hot, reactions are the reaction between an amine-terminated copolyether-
often temperature dependent, and a lot of soot may be sulphone thermoplastic and epoxide was performed.
produced. Due to the different properties of the gas Unfortunately, in the blend studied containing the curing
components, a different time-consuming procedure for agent, a band appearing upon curing overlapped with the
each species has traditionally been used. The use of FTIR band characterising the end group reaction. 17 refs.
(Fourier transform infrared) spectrometers as a continuous BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
UK; WESTERN EUROPE
monitoring technique overcomes many of the problems
in smoke gas analyses. FTIR offers an opportunity to set Accession no.783075
up a calibration and prediction method for each gas
showing a characteristic spectral band in the infrared Item 152
region of the spectrum. The objective of the SAFIR project Polymer Degradation and Stability
was to further develop the FTIR gas analysis of smoke 68, No.3, 2000, p.437-43
gases to be an applicable and reliable method for the SEMI-QUANTITATIVE ANALYSIS OF
determination of toxic components in combustion gases THERMAL DEGRADATION IN
related to fire test conditions. The optimum probe design, POLYPHENYLENE ETHER

80 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Kinoshita M; Nemoto T; Souda T; Takeda K Wunderlich B


Koito Mfg.Co.Ltd.; Shibaura,Institute of Technology Tennessee,University; Oak Ridge National Laboratory
(ACS,Div.of Polymeric Materials Science & Engng.)
The use of simple computer simulation and analysis of
the thermal degradation products of differently thermally Semicrystalline, polymeric materials consist usually of
aged samples of melt processed polyphenylene ether film metastable aggregates of strongly coupled microphases or
gave information on possible degradation routes for this nanophases with their constituent, micrometre-long, flexible
polymer. An increase in dimeric products was noted with molecules traversing multiple phase domains. Some 40 years
increased thermal ageing, but not in monomeric products. ago it was established that well-formed crystals are often
To explain the distribution of scission products found lamellar with a thickness of only about 10 nm. Between these
experimentally, the simple computer model was arranged lamellae one can find the remaining amorphous phase with
to simulate cleavage rates of methylene bridge, ether and even smaller dimensions. Less perfect crystallisation can
sidechain links. Although results were not totally decrease the crystal dimensions to as little as 1-2 nm in all
conclusive, it was noted that both ether bridge and side dimensions. An operational definition of the microphase is
chain cleavage rates were similar, and approximately nine its having at least one dimension smaller than a micrometre,
times lower than cleavage rates of the methylene bridge. while nanophases are approached when the small dimension
It is suggested that quantitative results determined will approaches 10 nm. Characteristic of the microphases is the
give detailed information on flame retardance due to the need to consider the surface properties for their description,
understanding of rates of volatile product generation at i.e. the melting temperature depends on the surface free
the polymer surface. 28 refs. energy. Nanophases, in turn, show an interaction between
JAPAN opposing surfaces, i.e. they may show no bulk properties. If
Accession no.782776 the dimensions decrease below 1 nm, the macroscopic phase
description has reached its limit. Many macromolecules can,
Item 153 however consist of alternating sequences of nanometer-
Polymer Degradation and Stability length chain segments that are immiscible, so that in all their
68, No.3, 2000, p.321-6 phase structures there is a strong tendency of nanophase
COMPARATIVE ANALYSIS OF THE PHOTO- separation. It is shown that special tools must be developed
OXIDATION OF POLYSTYRENE AND to probe the nanophase structures and properties of polymers.
POLY(ALPHA-METHYLSTYRENE) Some new information available by using three rather new
Mailhot B; Jarroux N; Gardette J-L techniques their combinations are described. 10 refs.
Ensemble Universitaire des Cezeaux USA

Fourier transform infrared spectroscopy (FTIR) and mass Accession no.780666


spectroscopy were used to study the photo-oxidation of
both poly(alpha-methylstyrene) (PMS) and polystyrene Item 155
(PS) films which had been irradiated at different ACS, Polymeric Materials Science & Engineering Fall
temperatures and with different radiation sources under Meeting 1999. Volume 81. Conference proceedings.
an oxygen atmosphere. The oxidised films were treated New Orleans, La., 22nd-26th Aug.1999, p.236-7
with ammonia or sulphur tetrafluoride and photolysis CRYSTALLISATION AND MELTING OF
carried out under vacuum. Photoproducts from both POLYMER CRYSTALS REVEALED BY T-M DSC
polymers were broadly similar, but aromatic ketone Toda A; Oda T; Tomita C; Hikosaka M; Arita T;
concentration was higher from the PMS and a new ketone Saruyama Y
was also identified from this source. Routes for formation Hiroshima,University; Kyoto,Institute of Technology
of identified photoproducts are proposed. 13 refs. (ACS,Div.of Polymeric Materials Science & Engng.)
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; Temperature-modulated differential scanning calorimetry
WESTERN EUROPE
(T-MDSC) applies a thermal modulation in temperature
Accession no.782763 to a conventional DSC run and determines a dynamic heat
capacity from the relationship between the modulation
Item 154 components of temperature and of heat flow. Primary
ACS, Polymeric Materials Science & Engineering Fall application of this technique has been the measurement
Meeting 1999. Volume 81. Conference proceedings. of specific heat capacity and the examination of the
New Orleans, La., 22nd-26th Aug.1999, p.242-3 anomaly in a relaxation process such as alpha process
ANALYSIS OF THE NANOPHASE STRUCTURE related to the glass transition. An application to the first-
OF SEMICRYSTALLINE POLYMERS WITH order phase transitions of crystallisation and melting of
ATOMIC FORCE MICROSCOPY (AFM), polymer crystals has recently been suggested. The method
MICROCALORIMETRY (MC) AND and typical results are described. 13 refs.
TEMPERATURE-MODULATED JAPAN
CALORIMETRY (TMC) Accession no.780663

© Copyright 2002 Rapra Technology Limited 81


References and Abstracts

Item 156 Item 158


ACS, Polymeric Materials Science & Engineering Fall Analytical Chemistry
Meeting 1999. Volume 81. Conference proceedings. 72, No.11, 1st June 2000, p.2490-8
New Orleans, La., 22nd-26th Aug.1999, p.173-4 CHARACTERISATION OF POLYETHER AND
FILM FORMATION IN POLYMER LATEX POLYESTER POLYURETHANE SOFT BLOCKS
BLENDS: MICROSPECTROSCOPIC 3D STUDIES USING MALDI MASS SPECTROMETRY
Zhao Y; Urban M W Mehl J T; Murgasova R; Dong X; Hercules D M;
North Dakota State University Nefzger H
(ACS,Div.of Polymeric Materials Science & Engng.) Vanderbilt University; Bayer Corp.
A series of previous studies on latex films indicates that Selective degradation reactions combined with MALDI
mobility of low molecular weight species in particular analysis were applied for molecular weight determination
surfactant molecules, may be affected by latex glass of polyether and polyester polyurethane soft blocks. Size
transition temperature, and subsequently, by free volume exclusion chromatography was combined with MALDI to
of a polymer matrix, surface tension at the film/air and provide accurate molecular weight determination. 44 refs.
film/substrate interfaces, compatibility and coalescence USA
times, to name just a few. It appears that there are other Accession no.778970
factors that not only influence distribution of individual
components including distribution of surfactants, but also
may significantly affect film formation. In an effort to Item 159
enhance understanding of these multi-phase latex blends Macromolecular Symposia
and their coalescence, a series of experiments on latexes Vol.152, March 2000, p.267-78
containing PS and poly-n-butyl acrylate (p-nBA) blends ANALYSIS OF COMPLEX POLYMERS BY
is presented. An attempt is made to identify factors MALDI-TOF MASS SPECTROMETRY
affecting film formation of PS/p-nBA latex blends using Pasch H; Ghahary R
multi-dimensional vibrational spectroscopic methods, and German Plastics Institute
these findings are compared with respective copolymers. The results are reported of an analysis of the functionality,
The effects of SDOSS exudation by latex composition, molar mass and chemical composition of complex
particle and annealing temperatures are also addressed in polymers, using MALDI-TOF mass spectrometry and a
terms of phase separation and dynamics of combination of MALDI-TOF mass spectrometry and
macromolecular segments. 21 refs. liquid chromatography. Polymers investigated included
USA polyamide-12, bisphenol A polycarbonate, methoxylated
Accession no.780632 melamine-formaldehyde resin, carboxy-terminated PS
and PMMA. 33 refs.
Item 157 EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
ACS, Polymeric Materials Science & Engineering Fall WESTERN EUROPE
Meeting 1999. Volume 81. Conference proceedings. Accession no.778702
New Orleans, La., 22nd-26th Aug.1999, p.387-8
FAILURE STUDIES OF ADHESION BY UV Item 160
REFLECTION AND FLUORESCENCE Journal of Injection Molding Technology
TECHNIQUES 4, No.2, June 2000, p.84-91
Kim N-J; Jeong C N; Sung C S P; Sung N-H ANALYSIS OF STYRENE PLASTIC RESIDUES
Connecticut,University; Tufts University ON INJECTION MOULDING TOOLS
(ACS,Div.of Polymeric Materials Science & Engng.) Makinen M; Astola J; Poutanen J; Alen R; Paakkonen E
Various techniques such as optical and electron microscopy, Tampere,University of Technology;
IR-ATR ESCA and SIMS have been used for failure mode Jyvaskyla,University
analysis in polymeric adhesive joints. However, these The contaminating substances formed during the injection
techniques are not amenable for in situ, non-destructive moulding of ABS and PS parts were removed from the
examination of the failure surfaces as failure occurs. In mould surface. The residues were characterised using
order to develop in situ techniques, UV reflection and FTIR, gas chromatography, pyrolysis gas
fluorescence methods are evaluated, as they can be applied chromatography, elemental analysis, detection reaction
via optical fibres to the actual failure surface. Failure test of bromine, and different dissolving tests. The
surfaces of two types of adhesive joints are examined by chemical composition of the contamination was clarified
UV reflection and fluorescence, complemented by FT-IR and suitable solvents for dissolving these products were
ATR studies. The first joint studied is PU on epoxy-coated selected. 6 refs.
steel. The second is PETP/PE/PETP. 8 refs.
EUROPEAN UNION; FINLAND; SCANDINAVIA; WESTERN
USA EUROPE
Accession no.780560 Accession no.776471

82 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Item 161 CHARACTERISATION OF POLYURETHANE


Polymer COATINGS USING THERMOANALYTICAL
41, No.15, 2000, p.5949-55 TECHNIQUES
UNDERSTANDING VITRIFICATION DURING Ginic-Markovic M; Choudhury N R; Matisons J G;
CURE OF EPOXY RESINS USING DYNAMIC Williams D R G
SCANNING CALORIMETRY AND South Australia,University; Adelaide,University
RHEOLOGICAL TECHNIQUES
A two-pack PU coating was analysed using
Lange J; Altmann N; Kelly C T; Halley P J thermoanalytical techniques. The curing reaction was
Queensland,University monitored using pressure differential calorimetry,
The gelation and vitrification transitions during cure of rheometry and dynamic mechanical analysis. The
an epoxy resin-amine system were examined using decomposition behaviour was examined using TGA. 13
rheological, modulated DSC and FTIR techniques. The refs.
results of DMA showed that gelation was observed before AUSTRALIA
vitrification at all temps. where it could be rheologically Accession no.776090
defined. By comparing different rheological criteria for
vitrification, it was seen that the vitrification transition
Item 164
was a gradual process that extended over a large part of
Injection Molding
cure at all temps. where it occurred. Results from
8, No.6, June 2000, p.42/50
modulated DSC measurements showed that the
MATERIALS ANALYST: PART 33 -
calorimetric vitrification times were longer than the
DETERMINING COMPOSITION
vitrification times obtained from rheological
Sepe M
measurements at cure temps. above 100C, but that at lower
Dickten & Masch Mfg.
temps. calorimetric vitrification occurred before, or at the
same time as, rheological vitrification. Theoretical This article focuses on the problems associated with
gelation times, estimated from FTIR conversion data, identifying a polymer. There are three major techniques
were found to be consistently shorter than the observed that are particularly helpful in identifying the type of
gelation times. Theoretical vitrification times agreed well polymer used in a compound. These are DSC, TGA and
with the observed times. The magnitude of the vitrification IR spectroscopy. Each of these techniques has its
transition, expressed either as amount of change in heat strengths, and in determining the composition of the
capacity or as maximum value of loss tangent, was found polymer, the task is to highlight properties and behaviour
to decrease approximately linearly with increasing cure that are distinctive.
temp. 34 refs. USA
AUSTRALIA Accession no.775805
Accession no.776348
Item 165
Item 162 Polymer
Macromolecules 41, No.11, 2000, p.4361-5
33, No.8, 18th April 2000, p.3180-3 RAPID MICROWAVE INDUCED
COMPLETE ASSIGNMENT OF PROTON AND DEPOLYMERISATION OF POLYAMIDE 6
CARBON 13 NMR SPECTRA OF Klun U; Krzan A
POLYVINYLCARBAZOLE Ljubljana,National Institute of Chemistry
Karali A; Froudakis G E; Dais P; Heatley F Polyamide 6 depolymerisation was performed using
Crete,University; Manchester,University microwaves as the energy source for the acid catalysed
Details are given of the assignment of the proton and hydrolysis, with phosphoric acid as the catalyst. The
carbon 13 spectra of polyvinylcarbazole by using a product mixture was analysed by chromatographic and
number of modern gradient two-dimensional NMR spectroscopic methods. 19 refs.
experiments. The relationship between the assignments SLOVENIA
and the conformational and dynamic properties of the Accession no.774158
polymer is discussed. 13 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE; UK;
WESTERN EUROPE Item 166
Polymer
Accession no.776167
41, No.11, 2000, p.4039-46
MATRIX-ASSISTED LASER DESORPTION/
Item 163 IONISATION MASS SPECTROMETRY OF
Journal of Thermal Analysis and Calorimetry SYNTHETIC POLYMERS. IV. COUPLING OF
59, Nos.1-2, 2000, p.409-24 SIZE EXCLUSION CHROMATOGRAPHY AND

© Copyright 2002 Rapra Technology Limited 83


References and Abstracts

MALDI-TOF USING A SPRAY-DEPOSITION Persian


INTERFACE KINETIC STUDY OF THE AUTO-OXIDATION
Esser E; Keil C; Braun D; Montag P; Pasch H OF POLYURETHANE
Darmstadt,Deutsches Kunststoff-Institut Semsarzadeh M A; Salehi H
Size exclusion chromatography and MALDI-TOF mass Tarbiat Modarres University
spectrometry was coupled via a robotic interface. For Gel permeation chromatography was used to study the
polydisperse synthetic polymers a continuous track of kinetics of the auto-oxidation of polyurethane. The
matter was deposited onto the matrix surface. Spectra stationary state rate and the induction time were
were taken from different positions of the polymer track. determined at various temperatures. FTIR and H NMR
Data are presented for PS, PMMA and butyl methacrylate- were used to determine the alcohol, acetate and formate
methyl methacrylate copolymers. 20 refs. compounds in the auto-oxidation products.
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; IRAN
WESTERN EUROPE
Accession no.773140
Accession no.774127

Item 167 Item 170


Muanyag es Gumi Journal of Macromolecular Science B
37, No.3, 2000, p.89-91 B39, No.2, 2000, p.279-96
Hungarian TIME-RESOLVED FTIR STUDY OF
APPLICATION OF STATE-OF-THE-ART CRYSTALLISATION BEHAVIOUR OF MELT-
METHODS IN ADHESION TECHNOLOGY. I. CRYSTALLISED POLYPHENYLENE SULPHIDE
Vabrik R; Czajlik I; Bertoti I; Keresztes Zs; Ille A; Yu J; Asai S; Sumita M
Rusznak I; Vig A; Kalman E Tokyo,Institute of Technology; China,Textile
University
Atomic force microscopy (AFM) and X-ray photoelectron
spectroscopy (XPS) were used to study the nature of the The crystallisation behaviour of polyphenylene sulphide
failure interface and the failure mechanism in a PVC film/ was studied using time-resolved FTIR spectroscopy and
adhesive/glass system. The failure mode was found to be the results obtained correlated with DSC measurements.
mostly interfacial, occurring at the glass/adhesive interface, The 1073 cm/1 amorphous band was selected for the time-
and also partially cohesive, located in the adhesive layer resolved measurements. The procedure provided details
very close to the interface. The results are discussed in on the microstructure of the PPS, including heterogeneity
relation to the chemical nature of the interface and the of the amorphous phase above and below Tg. A method
failure mechanism. 11 refs. Articles from this journal can is proposed for calculating the rigid, amorphous fraction
be requested for translation by subscribers to the Rapra in terms of the increase in the slope of the absorbance
produced International Polymer Science and Technology. variation with temperature at the glass transition. 43 refs.
CHINA; JAPAN
Accession no.773793
Accession no.772147
Item 168
Revista de Plasticos Modernos Item 171
78, No.521, Nov.1999, p.541-6 Journal of Applied Polymer Science
Spanish 76, No.6, 9th May 2000, p.938-46
STRUCTURAL CHARACTERISATION OF OPTIMIZATION OF EXPERIMENTAL
MULTILAYER POLYMERIC MATERIALS BY PARAMETERS FOR THE QUANTIFICATION OF
MICRORAMAN SPECTROSCOPY POLYMER ADDITIVES USING SFE/HPLC
Sanz R; Martin B; Merino J C; Pastor J M Thilen M; Shishoo R
Valladolid,Universidad Swedish Institute for Fibre & Polymer Research
Results are presented of a study in which confocal A study was conducted with the aim of extracting the
microRaman spectroscopy was used to determine the antioxidants Irganox 1010 and Irgafos 168 from a PP
structure of the individual polymers present in a series of matrix by using the supercritical fluid extraction(SFE)
multilayer food packaging films. 8 refs. technique and by subsequent analysis using high-
AMCOR FLEXIBLES ESPANA SA performance liquid chromatography(HPLC). The
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; experimental parameters of temp., pressure and modifiers
WESTERN EUROPE
were varied to find the best extraction conditions. The
Accession no.773260 optimum temp. and pressure for extraction of these
polymer additives were found to be 120 and 384 bar, with
Item 169 methanol as the modifier. The quantitative extractions
Iranian Journal of Polymer Science & Technology were significantly faster than those reported previously
12, No.2, Summer 1999, p.1-8 in the literature. The results showed that the SFE/HPLC

84 © Copyright 2002 Rapra Technology Limited


References and Abstracts

technique used in these experiments was a reliable and conditions. Within this project, optimal working
environmentally-friendly alternative to the commonly- conditions including sampling, calibration and analysis
used liquid extraction and analytical methods. 22 refs. for FTIR fire gas method are defined and verified under
EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERN a variety of fire test scenarios. The FTIR method are
EUROPE shown to be a repeatable and reproducible method for
Accession no.770687 the determination of the most important toxic gas
components of real fires. Moreover, the findings of this
Item 172 project concerning sampling techniques are most relevant
Macromolecular Symposia for other methods used for defining fire gases. 5 refs.
Vol.148, Dec.1999, p.463-81 EUROPEAN UNION; FINLAND; SCANDINAVIA; WESTERN
CHARACTERIZATION OF ACRYLIC DENTAL EUROPE
POLYMERS Accession no.768669
Vera-Graziano R; Martinez-Richa A; Palacios-Alquisira
J; Barcelo-Santana F; Castano-Meneses V Item 174
Mexico,Universidad Nacional Autonoma; Surface Coatings International
Guanajuato,Universidad 83, No.3, March 2000, p.111-8
DETERMINATION OF VOC EMISSIONS FROM
The chemical composition, dimensions and the molecular
LATEX PAINTS DURING AND AFTER
parameters of four dental acrylic polymer materials and
APPLICATION; METHODS, PERFORMANCE
two polyacrylic acids of different molec.wt. used as model
AND PRECISION
compounds were studied by NMR and IR spectroscopies,
Zeh H
GPC, intrinsic viscosity and light scattering
Wacker Polymer Systems GmbH
measurements. Two of the dental polymers were shown
to be mainly polyacrylic acid, while one showed the peak VOC emissions from indoor latex paints during and after
pattern for an acrylic acid/methyl acrylate copolymer of application is determined by four different test methods:
about 2:1 composition and one was an oligomer derived a chamber method in which an emission chamber is
from 2-hydroxyethyl methacrylate. The steric hindrance combined with gas chromatography, two practical
parameter, molecular stiffness and second virial methods in which VOC emitted in a room is measured
coefficient were calculated using different thermodynamic either by the determination of the total organic carbon or
models. The Flory-Fox-Shafgagen and the Stockmayer- by infrared spectroscopy, and an ‘in-can-individual-VOC
Fixman models fitted the experimental data reasonably method’ which determines the VOC of a liquid paint by
well and could be use to describe the molecular parameters the quantitative analysis of each volatile component. VOC
of the acrylic polymers. 18 refs. (7th International emission data gathered by these methods are compared
Conference on Polymer Characterization (POLYCHAR- with calculations from a dynamic computer model
7), Denton, Texas, USA, Jan.1999) describing the time-dependence of the VOC emission in
MEXICO the room atmosphere. This comparison indicates that the
Accession no.770356 ‘in-can-individual-VOC method’ with computer
calculation allows variations in the size of the room, the
Item 173 application rate, VOC content of the paint and the rate of
Flame Retardants 2000. Conference proceedings. air change, without the necessity of additional
London, 8th-9th Feb.2000, p.185-92 experiments, and therefor, offers an approach with a
PRACTICE OF FTIR ANALYSIS FOR FIRE reduction in costs. 10 refs.
GASES (SAFIR) EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
Mikkola E WESTERN EUROPE
VTT Building Technology Accession no.768107
(BPF; Interscience Communications Ltd.; APME;
European Flame Retardant Assn.; Fire Retardant Item 175
Chemicals Assn.) Journal of Coatings Technology
72, No.902, March 2000, p.53-61
The use of FTIR (Fourier transform infrared)
ACID ETCH OF AUTOMOTIVE CLEARCOATS.
spectrometers as a continuous monitoring technique
II. COMPARISON OF DEGRADATION
overcomes many of the problems associated in analyses
CHEMISTRY IN LABORATORY AND FIELD
of hot fire gases. FTIR offers an opportunity to set up a
TESTING
calibration and prediction method for each gas showing
Schmitz P J; Holubka J W; Xu L-F
a characteristic spectral band in the infrared region of the
Ford Motor Co.
spectrum. A European project, SAFIR, aims to further
develop the FTIR gas analysis of smoke gases to be an X-ray photoelectron spectroscopy was used to determine
applicable and reliable method for the determination of whether exposure conditions used in the laboratory
toxic components in combustion gases related to fire test gravimetric etch testing of acrylic melamine clearcoats

© Copyright 2002 Rapra Technology Limited 85


References and Abstracts

simulated field degradation pathways. The surface The fibre-matrix interface in carbon fibre-reinforced
chemistry of the field exposed panels was examined and epoxy resin composites was studied by time of flight
the results compared with those for laboratory treated secondary ion mass spectrometry (ToF-SIMS) using novel
powders having identical technologies. Consistency in the preparation techniques. The initial adsorption between
formation of a melamine salt and ammonium sulphate uncured resin or amine curing agent and the fibre was
upon field exposure and laboratory acid treatment investigated by the use of adsorption isotherms obtained
indicated that the laboratory treatment conditions by the analysis of fibre surfaces following immersion in
simulated the field exposure conditions. 7 refs. liquid solutions of the resin. The intact interphase of a
USA composite could be examined by ToF-SIMS following
Accession no.767768 mode I or mode II failure within the spectrometer by the
use of carefully designed in-situ fracture stages. 11 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Item 176 WESTERN EUROPE
Journal of Adhesion Science and Technology Accession no.765326
14, No.5, 2000, p.745-64
XPS ANALYSIS OF THE COVERAGE AND
COMPOSITION OF COATINGS ON GLASS Item 179
FIBRES Adhesion ’99. Conference Proceedings.
Thomason J L; Dwight D W Cambridge, UK, 15th-17th Sept.1999, p.347-50
Owens-Corning Science & Technology Center MICRO THERMAL ANALYSIS AT
INTERPHASES
The use of X-ray photoelectron spectroscopy as a method
Hassler R; zur Muhlen E
for characterising different sizings on glass fibres was
Dresden,Institut fuer Polymerforschung; TA
evaluated. A model, based on a patchy sizing overlay
Instruments GmbH
hypothesis, was developed to aid in the reduction of data
(IOM Communications Ltd.)
obtained from the X-ray photoelectron spectroscopic
analysis. It is shown that the spectroscopic results, when Details are given of a thermal analysis technique, referred
combined with the weight fraction of the sizing, provide to as micro thermal analysis, which combines the high
a quantitative value for the coverage of the fibre surface resolution positioning of scanning probe microscopy with
by the sizing. 25 refs. some of the quantitative analysis capabilities of conventional
USA thermal analysis. The application of this technique in
Accession no.767755 characterising the thermal properties of interfaces in
aluminium/epoxy resin adhesive joints and in glass fibre-
reinforced epoxy resin composites is described. 7 refs.
Item 177 EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
Polymer News UK; WESTERN EUROPE
25, No.2, Feb.2000, p.56-8 Accession no.765322
POLYMER ANALYSIS AND
CHARACTERISATION
Garbassi F Item 180
EniChem SpA Macromolecules
33, No.1, 11th Jan.2000, p.120-4
Analytical techniques, such as mass spectroscopy, atomic BRANCHING AND CROSSLINKING IN
absorption spectroscopy and atomic emission RADIATION-MODIFIED PTFE. A SOLID-STATE
spectroscopy, for the detection of trace elements, mainly NMR INVESTIGATION
metal trace elements, in polymers, used particularly in Fuchs B; Scheler U
food, are briefly considered. The disadvantages and Dresden,Institute of Polymer Research
suitability of such techniques are summarised. 10 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
High-resolution fluorine 19 NMR was used to investigate
WESTERN EUROPE the structural changes resulting from PTFE electron
Accession no.766702 irradiation under vacuum. A quantitative analysis of the
data was used to establish the density of side groups and
branches. 20 refs.
Item 178 EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
Adhesion ’99. Conference Proceedings. WESTERN EUROPE
Cambridge, UK, 15th-17th Sept.1999, p.369-73 Accession no.764731
INTERPHASE CHEMISTRY OF CARBON FIBRE
COMPOSITE MATERIALS
Prickett A C; Vickers P E; Smith P A; Watts J F Item 181
Surrey,University Color and Appearance Retec 1999. Conference
(IOM Communications Ltd.) proceedings.

86 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Nashville, Tn., 27th-29th Sept.1999, p. 178-87 drinking water in contact with PP pipes was studied.
USING MICROSCOPY AS A PROBLEM Austrian, German and International Standard methods
SOLVING TOOL IN PLASTICS were used for water at 23C and 60C. The low molecular
Compton C degradation product 2,4-di-tert-butylphenol, rather than
Sun Chemical Corp. the high molecular antioxidants, was detected in the
(SPE,Color & Appearance Div.) aqueous extracts. In warm water extracts, the
concentration of phenols, the total organic carbon content
Microscopy is a valuable tool for pigment evaluation and
and the effect on odour and flavour were considerably
problem solving in plastics and other applications. The
higher than in cold. Alkaline water extracted higher
organic pigments used in plastic applications are typically
amounts of phenols but acidic drinking water showed no
sub-micron in size. Pigment performance is greatly affected
effect. Thermal loading of PP during the extrusion process
by how well the pigment particles are incorporated in the
significantly increased the extractable phenols, total
polymer medium. Various microscopic evaluation
organic carbon content and flavour number/threshold
techniques that can be used to investigate dispersion quality,
odour. 7 refs.
strength development and thermal stability are reviewed.
AUSTRIA; EUROPEAN UNION; WESTERN EUROPE
In addition, various microscopic techniques for identifying
contaminants are discussed. 7 refs. Accession no.763574
USA
Accession no.764247 Item 184
West Conshohocken, PA, 1999, pp.6. NALOAN.
ASTM D 2124-. METHOD FOR ANALYSIS OF
Item 182
COMPONENTS IN POLY (VINYL CHLORIDE)
Composites Part A: Applied Science and
COMPOUNDS USING AN INFRARED
Manufacturing
SPECTROPHOTOMETRIC TECHNIQUE
31A, No.2, 2000, p.165-71
American Society for Testing & Materials
FAILURE PHENOMENA IN TWO-
ASTM D 2124-
DIMENSIONAL MULTI-FIBRE
MICROCOMPOSITES. PART IV: A RAMAN Version 99. Photocopies and loans of this document are
SPECTRASCOPIC STUDY ON THE INFLUENCE not available from Rapra.
OF THE MATRIX YIELD STRESS ON STRESS USA
CONCENTRATIONS Accession no.760789
van den Heuval P W J; Peijs T; Young R J
Eindhoven,University of Technology; UMIST; Queen
Mary & Westfield College Item 185
Journal of Coatings Technology
Raman spectroscopy is used to study the influence of shear 72, No.900, Jan.2000, p.69-74
yield stress of the matrix on stress situations in carbon ANALYSIS OF EXEMPT PAINT SOLVENTS BY
fibre/epoxy resin composites containing a planar fibre GAS CHROMATOGRAPHY USING SOLID-
array. A mixture of two curing agents, with different PHASE MICROEXTRACTION
functionality and molecular weights, are used to cure the Bodrian R R
epoxy resin in order to obtain a matrix with varying cross- California,Polytechnic University
linked density. The carbon fibres are surface treated to
give good fibre-matrix adhesion. Three matrix systems Acetone, methyl acetate and parachlorobenzotrifluoride
are investigated in the study, each with a different yield have been exempted as VOC solvents by the EPA. In
stress. The mechanical properties of each material are measuring coating VOC content, separate methods for
measured under tension and shear conditions. 35 refs. determining exempt solvents are required. One such
EUROPEAN COMMUNITY; EUROPEAN UNION;
method utilises solid-phase microextraction to sample the
NETHERLANDS; UK; WESTERN EUROPE headspace of solvent-based coatings to which the
Accession no.763633 surrogates acetone-d6, methyl acetate-d3 and/or
metachlorbenzotrifluoride have been added. The sampled
exempt coating solvents are thermally desorbed and
Item 183 analysed using gas chromatography with flame ionisation
Journal of Macromolecular Science A or mass spectral detection. This paper presents the results
A36, No.11, 1999, p.1751-8 obtained for acetone and toluene in a large number of
POLYPROPYLENE PIPES FOR DRINKING aerosol paints. Additionally, the results from a round-robin
WATER SUPPLY study for acetone, methyl acetate and
Hametner C parachlorobenzotrifluoride in commercial solvent-based
Austrian Plastics Institute coatings are reported. 17 refs.
The migration of phenolic antioxidants (which are USA
typically used for the stabilisation of PP pipes) into Accession no.760572

© Copyright 2002 Rapra Technology Limited 87


References and Abstracts

Item 186 Toronto,University


Journal of Thermal Analysis and Calorimetry
Near-infrared inline monitoring of polymer processing
57, No.3, 1999, p.847-51
means using an optical fibre-assisted spectrometer to
IDENTIFICATION OF POLYETHYLENE BY
obtain spectra of the polymer melt flowing through
DIFFERENTIAL SCANNING CALORIMETRY
commonly used processing equipment (an extruder).
Tsukame T; Kutsuzawa M; Sekine H; Saitoh H;
Conditions in the extruder are typically 200 deg.C and
Shibasaki T
20 MPa. The design of interfaces between the
Saitama,Criminal Investigation Laboratory;
spectrometer and the molten polymer is shown. Three
Saitama,University
designs are shown, each permitting monitoring at a
A forensic sample consisting of melt-recrystallised different location in the process: a melt-at-die interface,
polymers recovered from the scene of a fire in a factory a melt-in-barrel interface and a strand interface. These
is identified by differential scanning calorimetry. The designs are for monitoring just before the extruder exit,
factory commonly used two kinds of film sheets, A and in the main barrel of the extruder and after the product
B, made by different manufacturers. It is necessary to exits from the extruder as a strand, respectively. All these
decide whether the forensic sample related to material A interfaces protect the inserted optical fibre probe from
or B. The forensic sample and reference samples of the harsh environment within the extruder while
materials A and B are subjected to IR spectroscopy and permitting easy replacement or a probe without
pyrolysis gas chromatograph mass spectrometry interrupting the process. This latter characteristic is very
measurements, which reveal their PE nature. The thermal important because it permits easy probe repair as well as
behaviour of the samples is examined by differential the use of other types of probes (for monitoring colour or
scanning calorimetry (DSC) and they are found to be particles, for example) to be used during a run. Examples
blends of two kinds of PEs, LDPE and LLDPE. The of near-infrared spectra obtained with each of the
samples can be identified and distinguished from each interfaces used with an immiscible blend of PE and PP
other via the DSC measurements. 6 refs. are shown. Large differences in the spectra demonstrate
JAPAN
that the design of the interface will affect multivariate
analysis directed at composition prediction. Subsequent
Accession no.760331
papers are directed at using the melt-at-die interface for
composition prediction and accounting for nonlinear
Item 187 relationships between absorbance and concentration. 6
Journal of Thermal Analysis and Calorimetry refs.
58, No.1, 1999, p.13-8 CANADA
THERMAL CHARACTERISATION OF Accession no.760231
POLYURETHANE ACRYLATE RESINS
Ledru J; Saiter J M; Grenet J; Yuossef B; Burel F;
Bunel C Item 189
Rouen,University; Rouen,Institut National des Sciences Applied Spectroscopy
Appliquees 53, No.11, Nov.1999, p.1403-11
THERMAL VOLATILISATION ANALYSIS: A
Polyurethane acrylate resins cured by two different VERSATILE PLATFORM FOR
methods, thermally and photochemically, are investigated SPECTROSCOPIC INVESTIGATION OF
by means of differential scanning calorimetry and POLYMER DEGRADATION PROCESSES
thermally stimulated depolarisation currents. Even if both Guo X; Huang B; Dyakonov T; Chen Y; Padron L;
curing methods lead to the same material from a chemical Vickstrom T; Kuhn J; Hodkiewicz J; Stevenson W T K
point of view, important differences exist between the Wichita,State University; Harrick Scientific Co.;
thermocured resin and the photocured resin in terms of Oklahoma State University; Koch Industries Inc.; ATI
molecular relaxation behaviour. 8 refs. Instruments
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
WESTERN EUROPE Thermal volatilisation analysis (TVA) and sub-ambient
thermal volatilisation analysis (SATVA) techniques are
Accession no.760327
described. In addition to rate profiling of the volatile
product flux of thermal degradation under high-vacuum
Item 188 conditions through measurement of pressure in the
Applied Spectroscopy vacuum line as a function of sample temperature, the TVA
53, No.11, Nov.1999, p.1412-8 technique is shown to afford a convenient method for an
IN-LINE NEAR-INFRARED MONITORING OF on the basis of volatility under high-vacuum conditions,
POLYMER PROCESSING. I. PROCESS/ of product fractions of thermal degradation for subsequent
MONITOR INTERFACE DEVELOPMENT spectroscopic analysis. The capacity and flexibility of
Reshadat R; Desa S; Joseph S; Mehra M; Stoev N; TVA as a platform for these analyses are illustrated in a
Balke S T case study format by degrading poly(bisphenol A, 2-

88 © Copyright 2002 Rapra Technology Limited


References and Abstracts

hydroxy propylether). The overall degradation process is mode atomic force microscopy (AFM). The
quantified, and most significant pathways of thermolysis microfibrils feature is observed with an average width
are identified through subsequent spectroscopic analysis of 500 nm, composed of various types of periodical
of products of decomposition. The design and construction units of an average size 50 nm in a pleating appearance.
of a modified vacuum-tight long-path gas IR cell, as an At the less crystalline spot on the Kevlar fibre surface,
interface allowing for the application of Fourier transform the periodical organisations exhibit the skin core-like
infrared spectroscopy (FT-IR) for the online analysis of differentiation. In contrast, at the highly crystalline
volatile products of polymer degradation, is described. spot, the periodicity is more uniformly arranged by a
Proof of concept and application of this new analytical rectangular network manner. Inverse gas
technique, subsequently referred to as TVA/FT-IR, is chromatography (IGC) is used as a tool to investigate
illustrated through the examination of appropriate aspects the surface structure heterogeneity by calculating the
of the thermal degradation of PMMA polymers. 49 refs. surface energy of different types of probes adsorbed
USA on the Kevlar fibre surface. The energy sites
Accession no.760230 distribution plot of n-hexylamine adsorption at finite
dilution exhibits a two-adsorbing-peaks curve. At the
Item 190 higher energy site, a possible hydrogen bonding
Analytical Chemistry interaction is proposed between n-hexylamine and
71, No.21, 1st Nov.1999, p.4793-9 oxygen-containing groups formed at the less crystalline
GEL PERMEATION CHROMATOGRAPHY surface. According to the AFM and IGC results, a
COUPLED TO FOURIER TRANSFORM MASS Kevlar fibre surface organisations model at the
SPECTROMETRY FOR POLYMER nanometer scale is proposed. 19 refs.
CHARACTERIZATION EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
SWITZERLAND; WESTERN EUROPE
Aaserud D J; Prokai L; Simonsick W J
Florida,University Accession no.758987

On-line coupling of GPC to Fourier transform(FT) mass


spectrometry(MS) using a modified commercial Item 192
electrospray ionisation(ESI) interface was studied. Macromolecular Chemistry & Physics
Selected oligomer profiles for the sodiated oligomer ions 200, No.10, Oct.1999, p.2345-55
of a narrow molec.wt. PMMA were generated and used THERMAL DEGRADATION MECHANISMS OF
for obtaining a calibration curve. Using the MS-generated POLYETHERIMIDE INVESTIGATED BY
calibration curve and the refractive index response for DIRECT PYROLYSIS MASS SPECTROMETRY
quantification, an accurate MWD was calculated and Carroccio S; Puglisi C; Montaudo G
shown to be in good agreement with the value specified Istituto per la Chimica e la Tecnol.dei Mat.Pol.;
by the supplier. GPC/ESI/FT-MS also allowed for an Catania,University
unequivocal end group determination and characterisation The thermal degradation of poly(2,2'-bis(3,4-
of a secondary distribution due to the formation of cyclic dicarboxyphenoxy)phenylpropane-2-phenylenediimide)
reaction products. A glycidyl methacrylate/butyl was investigated by TGA and direct pyrolysis mass
methacrylate copolymer with a broad MWD was spectrometry and the pyrolysis of this polyimide
analysed, fractionation and high resolving power being compared with that of an aromatic polyamide (NOMEX).
required for adequate characterisation. MWD data showed The structure of preformed oligomers from the purified
the advantages of coupling high-resolution MS and GPC polyetherimide and the structure of high temperature
to overcome the difficulty of analysing polydisperse pyrolysis products obtained at 620C were examined and
polymers with MS alone. 34 refs. the thermal degradation pathways involved in the
USA degradation elucidated. 32 refs.
Accession no.759794 EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
WESTERN EUROPE
Item 191 Accession no.757742
Polymer
40, No.26, 1999, p.7341-50 Item 193
SURFACE STRUCTURE OF KEVLAR FIBRE Macromolecular Chemistry & Physics
STUDIED BY ATOMIC FORCE MICROSCOPY 200, No.10, Oct.1999, p.2205-7
AND INVERSE GAS CHROMATOGRAPHY COLLECTION OF SOLID-STATE CARBON-13
Rebouillat S; Peng J C M; Donnet J-B CP/MAS NMR SPECTRA OF COMMON
Du Pont de Nemours International SA; Haute- POLYMERS
Alsace,Universite Wilhelm M; Neidhoefer M; Spiegel S; Spiess H W
Kevlar fibre surface structure is primarily and directly Max-Planck-Institut fuer Polymerforschung; Wiley-
observed in the filament configuration by the tapping VCH Verlag GmbH

© Copyright 2002 Rapra Technology Limited 89


References and Abstracts

A collection of high resolution solid-state Carbon-13 Item 196


NMR spectra of a wide range of polymers is presented. It Polymer International
is useful for reference purposes in case of unknown or 48, No.10, Oct.1999, p.1042-5
partly unknown samples, such as polymer blends, block EFFECTS OF UV RADIATION ON SEVERAL
copolymers or polymeric latices. 16 refs. HIGH-PERFORMANCE POLYIMIDE
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; COMPOSITES
WESTERN EUROPE Kiefer R L; Herring K; Wylie B J; Orwoll R A;
Accession no.757725 Thibeault S A
Williamsburg,College of William & Mary; NASA
Item 194 Langley Research Center
Polymer Degradation and Stability Three carbon fibre-reinforced polyimides were exposed
66, No.1, 1999, p.107-25 to UV radiation at 177C, at three different intensities for
VACUUM PYROLYSIS OF PVC. II: PRODUCT three different times, so that the product of intensity and
ANALYSIS time was a constant. Intensities of 1, 2 and 3 suns, where
Miranda R; Pakdel H; Roy C; Darmstadt H; Vasile C one sun is the power in space at one earth-sun distance,
Quebec,Universite Laval; Institut Pyrovac Inc.; Petru were used, for a time periods of 500, 250 and 167 h. The
Poni,Institute of Macromolecular Chemistry samples were characterised by X-ray photoelectron
Vacuum pyrolysis of pure PVC was carried out at various spectroscopy (XPS), thermogravimetric analysis,
temperatures between 220 and 520C and under a total thermomechanical analysis and dynamic mechanical
pressure of 2 kPa. The main gaseous and liquid pyrolysis analysis. Measurement of bulk properties showed no
products obtained during the different stages of thermal difference between samples exposed to heat and UV
degradation were identified and quantified by radiation, and control samples. Surface analysis by XPS
chromatographic methods. Global mass balance and showed an apparent decrease in carbonyl concentration
chlorine mass balance were determined and different on the surface of some exposed samples. This was
methods of capturing hydrogen chloride under vacuum correlated to surface contamination by a silicone-
conditions were tested. The elemental composition, containing material. 3 refs.
surface properties and calorific value of the solid residue USA
were determined. 43 refs. Accession no.756185
CANADA; EASTERN EUROPE; RUMANIA
Accession no.757340 Item 197
Composites Part A: Applied Science and
Item 195 Manufacturing
Polymer Recycling 30A, No.12, 1999, p.1401-13
4, No.1, 1999, p.13-25 USE OF XPS FOR CHARACTERISATION OF
COMPOSITIONAL ANALYSIS AND GLASS FIBRE COATINGS
FEASIBILITY STUDY OF RECYCLED HDPE Thomason J L; Dwight D W
FOR DIRECT FOOD CONTACT APPLICATIONS Owens-Corning Science & Technology Center
Salafranca J; Cacho J; Nerin C
Zaragoza,University X-ray photoelectron spectroscopy was applied to a study
of commercial and experimental glass fibres using three
Five HDPE samples, consisting of a virgin HDPE for different instruments. A protocol for plotting ratios of
food-contact applications, three samples of this polymer appropriate atom concentrations was developed and the
taken after each of the three sequential recycling cycles plots used to estimate the surface coverage of the coating
and a real post-consumer sample were analysed. Two on the glass fibres and provide data on the chemical
different extraction methods were applied: a combination composition of the coating. The relationships between
of maceration and sonication; and the total dissolution of the spectroscopic data and coated glass fibre parameters
the polymer. In order to evaluate both the feasibility of are demonstrated using an overlay model and data from
using these polymers in food-contact applications and the the three instruments are compared. 22 refs.
evolution of HDPE composition through the recycling USA
process, samples were analysed by both qualitative and
Accession no.755993
quantitative GC-MS. Furthermore, GC-FID was applied
to the determination of alpha-alkenes, the most
representative compounds as indicators of polymer matrix Item 198
degradation. Finally, antioxidants were analysed by Analytical Chemistry
reversed phase HPLC. 34 refs. 71, No.20, 15th Oct.1999, p.4776-80
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; COMPOSITION AND MICROSTRUCTURE
WESTERN EUROPE DETERMINATION OF A LATEX SYSTEM BY
Accession no.756660 PYROLYSIS GAS CHROMATOGRAPHY

90 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Frank Cheng-Yu Wang of branching and determination of refractive index


Dow Chemical Co. increment. 19 refs.
CZECH REPUBLIC
The composition and microstructure of polymers in a
latex system were studied by pyrolysis gas Accession no.755647
chromatography. The composition and microstructure
of a polymer in the emulsion phase were identified by Item 201
direct pyrolysis of the latex system, followed by Journal of Vinyl and Additive Technology
comparing the trimer peak pattern with appropriate 5, No.3, Sept.1999, p.148-58
microstructure standards. The polymer in the aqueous NMR SPECTRA OF LEAD STABILISERS
phase was pre-pyrolysis derivatised with Grossman R F
tetrabutylammonium hydroxide to convert the acid to Halstab Corp.
its butyl ester. Similar procedures were then used to High resolution proton and 13C NMR spectra of lead-
explore the composition and microstructure of the based heat stabilisers and their reaction products, obtained
polymer in the aqueous phase. Polymers analysed using the magic angle spinning technique, support
included SCX-2660 (probably a styrene-methyl structural assignments inferred from IR spectra. These
methacrylate-butyl acrylate terpolymer), styrene-butyl demonstrate that lead stabilisers are unique compounds,
acrylate copolymer and styrene-alpha-methylstyrene- rather than the double salts of lead oxide found in
butyl acrylate terpolymer. 17 refs. textbooks. 8 refs.
JOHNSON S.C.,& SON INC. USA
USA Accession no.755491
Accession no.755899
Item 202
Item 199 Polymers for Advanced Technologies
Oxford, Butterworth-Heinemann Ltd., 1999, 10, No.4, April 1999, p.237-43
pp.xxvii,920. 24cms. 12/1/00. 011 CHARACTERISATION OF THE SURFACE OF
PLASTICS MATERIALS. 7TH EDN. BULK-MOULDED COMPOUNDS
Brydson J A Vallat M F; Schultz J; Mauzac C; Jacquin M
The latest edition, now the seventh, of this reputable text Institut de Chimie des Surfaces et Interfaces; PSA
book, provides an overview of the scientific, technological Etudes et Recherches Centre Technique de Belchamp
and economic aspects of currently available plastics and The surface characterisation of bulk moulding compound
related materials, and also focuses on new materials - (BMC) automotive parts using complementary techniques
many based on metallocene catalyst technology. of surface analysis, i.e. SEM, X-ray photoelectron
Developments with condensation polymers, including spectroscopy, time of flight secondary ion mass
several new polyester-type materials of interest for bottle spectroscopy, glow discharge spectroscopy and contact
blowing and/or degradable plastics, are also covered. This angle is described. Similarities and differences between
edition also attempts to explain the basis of metallocene BMC surfaces and sheet moulding compound (SMC)
polymerisation. The commercial importance of the surfaces are pointed out. Particular emphasis is placed on
materials discussed is also noted. mould release agents (polymeric and stearate) on the surface
Accession no.755818 which can influence future bonding behaviour. 14 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
Item 200 WESTERN EUROPE
Journal of Applied Polymer Science Accession no.754736
74, No.10, 5th Dec.1999, p.2432-8
CHARACTERIZATION OF BISPHENOL A- Item 203
BASED EPOXY RESINS BY HPLC, GPC, GPC- Macromolecular Chemistry & Physics
MALLS, VPO, VISCOMETRY, AND END GROUP 200, No.9, 1999, p.2074-9
ANALYSIS: ON THE IDENTIFICATION OF 2,3- INVESTIGATION OF MOLECULAR
DIHYDROXYPROPYL-CONTAINING DIMENSIONS OF POLYSTYRENE AS A
COMPOUNDS, DETERMINATION OF MOLAR FUNCTION OF SOLVENT COMPOSITION:
MASS DISTRIBUTION, AND BRANCHING APPLICATION TO LIQUID
Podzimek S; Kastanek A CHROMATOGRAPHY AT THE EXCLUSION-
SYNPO ADSORPTION TRANSITION POINT
Baran K; Laugier S; Cramail H
Results of the above characterisation are presented and
ENSCPB
discussed with particular reference to determination of
alpha-glycol-containing compounds, determination of Liquid chromatography was used to study PS standards at
molar mass and molar mass distribution, determination the exclusion-adsorption transition point using silica

© Copyright 2002 Rapra Technology Limited 91


References and Abstracts

adsorbents having differing porosities in various eluents. The Item 206


behaviour of model PS chains in solvent mixtures LCGC International
corresponding to the critical adsorption conditions was 12, No.9, Sept.1999, p.577/87
evaluated using viscometry and light scattering. It was found LC-MS ANALYSIS OF POLYMER ADDITIVES
that critical adsorption conditions could be achieved if the BY EL AND API: IDENTIFICATION AND
polymer chains entered the pores of the stationary phase and QUANTIFICATION
that the characteristics of the elution mode could be defined Yu K; Block E; Balogh M
with the aid of the polarity index of the eluent. 20 refs. Waters Corp.
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
Mass spectrometry can be the ideal detector for liquid
WESTERN EUROPE
chromatography because it offers both universality and the
Accession no.752269 required selectivity for complex analytical problems. The
two most popular types of interface for the benchtop single
Item 204 quadrupole LC-mass spectrometer are the particle beam
Macromolecular Symposia interface and the atmospheric pressure ionisation interface.
Vol.141, 1999, p.95-101 The particle beam interface is used to generate electron
RECENT ADVANCES IN THE ANALYSIS OF ionisation spectra and the API interface is used to generate
POLYMERS AND COPOLYMERS BY MASS either electrospray or atmospheric pressure chemical
SPECTROMETRY ionisation. This comprehensive article supplies a detailed
Montaudo M S analysis of a study in which organic extractable from
Istituto per la Chimica e la Tecnol.dei Mat.Pol. polypropylene was used as the model analyte to
demonstrate how the information obtained separately from
Progress which has been made in the use of MALDI mass
EI and API can be complementary. Seven compounds were
spectroscopy to provide reliable molec.wt. and MWD
separated and detected by both MS detectors. 35 refs.
values is reported. Molec.wt. averages and MWD of
USA
polydisperse samples (PMMA, siloxanes, polyesters and
copolyesters) were obtained by off-line coupling of SEC Accession no.747567
equipment with the MALDI mass spectrometer. SEC
traces of the samples were recorded, selected fractions Item 207
were analysed by MALDI-TOF and the average Macplas International
molec.wts. of the fractions were determined from the mass No.10, Aug.1999, p.64-70
spectrum. A method for analysing unknown copolymers, DIFFERENTIAL SCANNING COLORIMETRY
which involves the use of Markoffian statistics, is also AND INFRARED SPECTROSCOPY IN
presented. 26 refs. POLYMER ANALYSIS
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; Panarotto A; Bertucci M
WESTERN EUROPE Cesap
Accession no.752091
Differential scanning calorimetry is one of the most
commonly used methods for characterising the thermal
Item 205 properties of polymers. This method, particularly if
Polimery complemented by IR spectroscopic analysis, also allows
44, No.4, 1999, p.246-54 the nature of the materials under test to be determined.
Polish The principles involved in DSC and IR spectroscopy are
USE OF PHOTOELECTRON SPECTROSCOPY discussed.
IN STUDIES OF THE DEPTH PROFILE OF EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
POLYPROPYLENE FILM WESTERN EUROPE
Zenkiewicz M; Golebiewski J Accession no.745360
Metalchem Plastics Processing Institute
The physical fundamentals of photoelectron spectroscopy Item 208
are reviewed and the range of applications is given. Three Polimery Tworzywa Wielkoczasteczkowe
PP films were examined and the depth of oxidation was 44, No.3, 1999, p.218-21
found to be in the nanometer range. The oxidation level Polish
of the external layer increases as the specific energy of DETERMINATION OF MIGRATION OF
corona discharges is increased. 27 refs. Articles from this DIMETHYL TEREPHTHALATE AND
journal can be requested for translation by subscribers to DIMETHYL ISOPHTHALATE FROM PLASTICS
the Rapra produced International Polymer Science and Stareczek T; Kaminska G; Ermel J; Kortylewska
Technology. Edited by: Gliwice,Institute of Plastics & Paint Industry
EASTERN EUROPE; POLAND A gas chromatographic method is described for
Accession no.747688 determining dimethyl terephthalate and dimethyl

92 © Copyright 2002 Rapra Technology Limited


References and Abstracts

isophthalate in food simulants. The method consists in proposed and tested liquid chromatographic elution of
extracting DMT and DMIP from the food simulants with homopolymers under limiting conditions of desorption
chloroform and analysing of the compounds by GC with and takes into account the simultaneous effect of
the use of calibration curves and diethyl terephthalate as adsorption and exclusion of macromolecules onto/from
an internal standard. 3 refs. Articles from this journal can the column packing. 17 refs.
be requested for translation by subscribers to the Rapra SLOVAK REPUBLIC; SLOVAKIA
produced International Polymer Science and Technology. Accession no.743327
EASTERN EUROPE; POLAND
Accession no.745025 Item 211
Polymer Recycling
Item 209 3, No.4, 1997/1998, p.263-7
Journal of Applied Polymer Science PROCEDURES FOR THE COMPOSITIONAL
73, No.2, 11th July 1999, p.221-6 ANALYSIS OF REINFORCED POLYESTER
EVALUATION OF EVA-PVAC BLEND RECYCLATE
BEHAVIOUR BY 1-D AND 2-D SOLID-STATE Bream C E; Hornsby P R
NMR Brunel University
De Souza C M G; Pacheco C R; Tavares M I B
In order to consider effective strategies for the recovery
Rio de Janeiro,Universidade Federal; PETROBRAS
and reuse of plastics recyclates, a quantitative method is
Ethylene-co-vinyl acetate and poly(vinyl acetate) blends described for the characterisation of polyester-based
were prepared in different proportions by melting in a moulding compounds. Analytical procedures are
HAAKE Rheomix mixer. The blends were prepared at a described for the quantification of fibre, filler and fire
fixed temperature, rotation rate, and processing time. retardant contents in polyester moulding compounds
High-resolution solid state NMR was used to characterise containing calcium carbonate filler, glass fibre
the blends with respect to structure-mobility-compatibility reinforcement, and aluminium hydroxide flame retardant.
using magic angle spinning with cross-polarisation and 3 refs.
high power hydrogen decoupling and measurements of EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
the proton spin-lattice relaxation time in the rotating WESTERN EUROPE
frame. Miscibility between polymer chains was also Accession no.742796
studied by two-dimensional hydrogen ion/carbon-13 shift
correlation (HETCOR). 21 refs.
Item 212
BRAZIL
High Performance Plastics
Accession no.743489 Aug.1999, p.10
IDENTIFICATION OF PLASTICS IN WASTE
Item 210 A review is presented of the methods used in the
Macromolecules identification of plastics waste prior to recycling
32, No.11, 1st June 1999, p.3671-3 operations, which was published in International Polymer
LIQUID ADSORPTION CHROMATOGRAPHY Science and Technology, and translated from a Polish
OF COPOLYMERS: MOLAR MASS source. Rapid spectroscopic methods are indicated, and
(IN)DEPENDENT RETENTION their use in packaging and automotive recycling are
Berek D discussed.
Slovak Academy of Sciences EASTERN EUROPE; POLAND
Liquid adsorption chromatography with a continuous Accession no.742675
solvent gradient elution was shown by several previous
authors to be capable of separating random and graft
Item 213
copolymers according to their chemical composition, with
Journal of Polymer Science: Polymer Physics Edition
their molar masses not playing an important role. A
37, No.13, 1st July 1999, p.1485-94
tentative explanation of this finding is presented. It is
GLASS TRANSITION AND MISCIBILITY IN
assumed that the copolymer species travel along the
BLENDS OF TWO SEMI-CRYSTALLINE
column with a velocity which exactly corresponds to that
POLYMERS: POLYARYL ETHER KETONE AND
of the eluent composition, exhibiting a displacing power
POLYETHER ETHER KETONE
just necessary to prevent a fast progress of the
Woo E M; Tseng Y C
macromolecules due to their exclusion. Under specific
Taiwan,National Cheng Kung University
conditions, retention of macromolecules at this adsorption
promoting ‘barrier’ depends almost exclusively on the A study was made of the miscibility in the amorphous
copolymer composition and not on its molar mass. This region of melt mixed blends composed of a novel polyaryl
hypothesis is based on the mechanism of the recently- ether ketone (PK99) and PEEK using various methods,

© Copyright 2002 Rapra Technology Limited 93


References and Abstracts

including optical microscopy, DSC, SEM, FTIR Sano K; Shimoyama M; Ohgane M; Higashiyama H;
spectroscopy and wide-angle X-ray diffraction. Samples Watari M; Tomo M; Ninomiya T; Ozaki Y
were physically aged in order to resolve any possible Kwansei-Gakuin,University; Hyogo,Prefectural Police
overlapping Tg’s but only one single Tg was detected over Headquarters; Yokogawa Electric Co.
the entire composition range. No evidence for
FTIR spectra were measured for pellets of sixteen kinds
isomorphism was found and the crystal forms of the
of LLDPE with short branches and one kind of PE without
respective polymers remained distinct and unchanged by
any branch to explore the effects of the branches on the
miscibility in the amorphous region. 14 refs.
physical properties and the Raman spectrum. Partial least
TAIWAN
squares analysis regression was applied to the Raman
Accession no.742306 spectra after multiplicative scatter correction to propose
a calibration model that predicts the density of LLDPE.
Item 214 38 refs.
Applied Spectroscopy JAPAN
53, No.6, June 1999, p.672-81 Accession no.740338
POST-CONSUMER PLASTIC IDENTIFICATION
USING RAMAN SPECTROSCOPY Item 217
Allen V; Kalivas J H; Rodriguez R G Journal of Coatings Technology
Idaho,State University 71, No.893, June 1999, p.53-60
The suitability of Raman spectroscopy, when used with INVERSE GAS CHROMATOGRAPHY, SURFACE
K-nearest neighbours, library searching or cyclic subspace PROPERTIES, AND INTERACTIONS AMONG
regression, for computerised classification of post- COMPONENTS OF PAINT FORMULATIONS
consumer plastics was evaluated. Plastics investigated Ziani A; Xu R; Schreiber H P; Kobayashi T
were PETP, PP, PS, PVC, HDPE AND LDPE. Ecole Polytechnique de Montreal; Nippon Paint Co.
Modifications were made to the original cyclic subspace Inverse gas chromatography analysis at very high dilution
regression algorithm for modelling multiple sample and at finite concentrations of probe injection was carried
properties and the adapted algorithm employed to directly out on a series of polymers and pigments used in paint
compare the mechanisms of principal component formulations. Values of dispersion surface energies, and
regression and the PLS2 form of partial least-squares. It of acid-base interaction parameters were obtained for the
was found that Raman spectroscopy could be used to materials, and pair interaction parameters were calculated
identify both HDPE and LDPE. 33 refs. from the results. The dispersion stability of each pigment/
USA polymer combination was measured and correlated with
Accession no.741260 the acid-base interaction parameters of the materials, and
is shown to justify the availability of fundamental
thermodynamic interaction data to optimise performance
Item 215
aspects of protective coatings. 23 refs.
Applied Spectroscopy
CANADA; JAPAN
53, No.5, May 1999, p.557-64
COMPARISON OF NEAR-INFRARED AND Accession no.739845
RAMAN SPECTROSCOPY FOR THE
DETERMINATION OF CHEMICAL AND Item 218
PHYSICAL PROPERTIES OF NAPHTHA Analytical Chemistry
Min-Sik Ku; Hoeil Chung 71, No.10. 15th May 1999, p.2037-45
SK Corp. ANALYSIS OF POLYMERIC FLAME
RETARDANTS IN ENGINEERING
Near-infrared and FTIR Raman spectroscopy were
THERMOPLASTICS BY PYROLYSIS GAS
compared and evaluated for the quantitative analysis of
CHROMATOGRAPHY WITH AN ATOMIC
naphtha using partial least-squares regression. 19 refs.
EMISSION DETECTOR
SOUTH KOREA
Wang F C Y
Accession no.740339 Dow Chemical Co.
Halogen-containing polymeric flame retardants in
Item 216 engineering thermoplastics were analysed by pyrolysis
Applied Spectroscopy gas chromatography(Py-GC) with an atomic emission
53, No.5, May 1999, p.551-6 detector(AED) and a mass selective detector(MSD). The
FOURIER TRANSFORM RAMAN SPECTRA OF AED was very effective in monitoring halogen-containing
LINEAR LOW-DENSITY POLYETHYLENE AND pyrolysates after Py-GC. The type of polymeric flame
PREDICTION OF THEIR DENSITY BY retardant used in thermoplastics could be identified by
MULTIVARIATE DATA ANALYSIS peak pattern recognition through an AED halogen element

94 © Copyright 2002 Rapra Technology Limited


References and Abstracts

trace. A set of thermoplastic resins containing different were poly(vinyl acetate)/poly(methyl acrylate),
brominated polymeric flame retardants was studied. After poly(phenylene oxide)/PS and two poly(styrene-co-
generation of the pyrogram by Py-GC/AED, those acrylonitrile)/PMMA blends, the last two containing
pyrolysates produced from polymeric flame retardants different acrylonitrile contents. Specific molecular
were identified by MSD analysis of a complex total ion interactions determined whether the glass transition
chromatogram generated by the thermoplastic resins. The temperature and the increment of heat capacity versus
results demonstrated the effectiveness of the AED in the composition showed positive or negative deviations
tasks of specific element monitoring and component from linearity for the blend systems. In the non-
pattern recognition. The advantages and disadvantages interacting system (poly(vinyl acetate)/poly(methyl
of using the AED are also discussed. 11 refs. acrylate)), the glass transition temperature and increment
USA of heat capacity showed linear behaviour with
Accession no.738049 composition. Thermodynamic theories for the observed
results were discussed. 17 refs.
Item 219 EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
ACS, Polymeric Materials Science and Engineering. WESTERN EUROPE
Vol.76. Conference proceedings. Accession no.737361
San Francisco, Ca., Spring 1997, p.128-9. 012
ATOMIC FORCE MICROSCOPY STUDY OF Item 221
INTRAOCULAR LENS IMPLANTS - LCGC International
TOPOGRAPHY AND SURFACE PROPERTIES 12, No.7, July 1999, p.432/6
Kowalewski T; Ravi V N
QUANTITATIVE ANALYSIS OF
Washington,University; St.Louis,Veterans Affairs
POLY(METHYLMETHACRYLATE) IN DRUGS
Medical Center
BY CURIE-POINT PYROLYSIS GAS
(ACS,Div.of Polymeric Materials Science & Engng.)
CHROMATOGRAPHY
Cataracts are one of the most common causes of Muguruma S; Uchino S; Oguri N; Kiji J
worldwide blindness. They are presently corrected by Japan Analytical Industry Co.Ltd.; Tottori,University
surgery in which the natural cataractous lens is replaced
Curie-point pyrolysis gas chromatography was used for
by a synthetic intraocular lens. Successful visual
the quantitative analysis of residual synthetic adsorbent
rehabilitation is not only a function of patients’ health
crosslinked PMMA used in drug purification. Levels of
and the surgical technique, but it also depends on the
PMMA adsorbent below 0.15% in drug substances were
optical, mechanical and bioperformance of the intraocular
successfully measured quantitatively by Py-GC using
lens. Visual deterioration after surgery has been attributed
to cellular debris deposited on the lens surface and characteristic peaks that reflect the structure of the
capsular opacification resulting from inflammation. adsorbent, demonstrating that this analytical technique
Although the exact sequence of events that take place can be used to monitor compliance with the limit of 0.1%
when an implant is exposed to the ocular environment in organic impurity in drug substances stipulated by ICH
vivo is not known, protein adsorption, complement guidelines. 12 refs.
activation and cellular adhesion have been implicated and JAPAN
believed to be influenced by the surface properties of the Accession no.736647
implants. The surface characteristics (surface topography
and viscoelasticity) of intraocular lenses are investigated Item 222
using tapping-mode atomic force microscopy. 9 refs. Journal of Applied Polymer Science
USA 72, No.7, 16th May 1999, p.913-25
Accession no.737604 HIGH-PERFORMANCE LIQUID
CHROMATOGRAPHY-MASS SPECTROMETRY
Item 220 OF EPOXY RESINS
Polymer Fuchslueger U; Rissler K; Stephan H; Grether H J;
40, No.17, 1999, p.4763-7 Grasserbauer M
MODULATED DIFFERENTIAL SCANNING Ciba Specialty Chemicals Inc.; Vienna,Technical
CALORIMETRY: 14. EFFECT OF MOLECULAR University
INTERACTIONS ON GLASS TRANSITION
The application of liquid chromatography coupled to
BEHAVIOUR AND INCREMENT OF HEAT
mass spectrometry for the analysis of epoxy resins was
CAPACITY IN MISCIBLE POLYMER BLENDS
shown in two examples. Electrospray (ESI) and
Song M; Hourston D J; Pollock H M; Hammiche A
atmospheric pressure chemical ionisation (APCI) were
Loughborough,University; Lancaster,University
compared with respect to the ionisation of diglycidyl
Modulated differential scanning calorimetry was used ether of bisphenol A (DGEBA)-based epoxy resins. By-
to study miscible polymer blends. The blends studied products in a typical modified solid DGEBA-based

© Copyright 2002 Rapra Technology Limited 95


References and Abstracts

epoxy resin and in a new weatherable crosslinker for Item 225


powder coating applications were characterised and Coloring Technology for Plastics.
discussed. 26 refs. New York, N.Y., Plastics Design Library, 1999, p.197-
AUSTRIA; SWITZERLAND; WESTERN EUROPE 207. 52
Accession no.734831 MEASURING STABILISERS IN PIGMENTED
PLASTICS WITH NEAR-INFRARED
SPECTROSCOPY
Item 223 Solera P; Nirsberger M; Castillo N
Journal of Adhesion Science and Technology Ciba Specialty Chemicals Corp.
13, No.5, 1999, p.629-45 Edited by: Harris R M
ADHESION CHARACTERISATION OF
PROTECTIVE ORGANIC COATINGS BY Near-infrared (NIR) spectroscopy has become a
ELECTROCHEMICAL IMPEDANCE commonplace analytical tool in the plastics industry. NIR
SPECTROSCOPY techniques have made quantification of many organic
Deflorian F; Fedrizzi L components in polymer processing easy and quick. The
Trento,University work presented outlines the methodology for using NIR
to measure stabiliser levels in colour concentrates and
This review describes in detail the influences on adhesion natural polymer formulations. Advantages and limitations
of different pretreatments or organic coatings, considering are considered as well as particle size and product form.
aluminium, galvanised steel, and stainless steel substrates, 4 refs.
and it was shown that the information obtained using an
USA
electrochemical approach can be used for adhesion
evaluation, with particular attention to monitoring of Accession no.732217
adhesion in an aqueous environment, which is the most
detrimental for protective organic coatings. 40 refs. Item 226
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; Coloring Technology for Plastics.
WESTERN EUROPE New York, N.Y., Plastics Design Library, 1999, p.191-
Accession no.733531 5. 52
PRACTICAL ANALYSIS TECHNIQUES OF
POLYMER FILLERS BY FOURIER
Item 224
TRANSFORM INFRARED SPECTROSCOPY
Macromolecular Chemistry & Physics
(FTIR)
200, No.5, May 1999, p.1134-42
Coles B J; Hall C J
POSSIBILITIES AND LIMITS OF PHOTON
Hauser Inc.
CORRELATION SPECTROSCOPY IN
Edited by: Harris R M
DETERMINING POLYMER MOLECULAR
WEIGHT DISTRIBUTIONS The identification of polymers by FTIR is often
Faraone A; Magazu S; Maisano G; Villari V; Maschio G complicated by the presence of fillers. However, for kaolin
Messina,University clay, FTIR analysis should be able to identify the filler
and predict its concentration using a standard curve. The
The effect of concentration and polydispersity on the
resulting percentage is more reliable than a simple ash,
collective diffusion coefficient(Dc) evaluated using
which may change the chemical composition of the filler.
photon correlation spectroscopy was investigated on
2 refs.
PMMA in acetone solutions. The concentration
USA
dependence of the Dc followed a linear regression law,
the slope being fairly independent of polydispersity, Accession no.732216
molec.wt. and temp. The diffusion coefficient at infinite
dilution obeyed a given scaling law. The inversion of the Item 227
scattered intensity autocorrelation data by the Pitture e Vernici
regularisation method CONTIN permitted the evaluation 75, No.5, March 1999, p.7-8
of the MWD function of the polymeric samples. Although English; Italian
this algorithm gave valuable information on average E.I.S. EVALUATION OF ATTACHED AND FREE
amounts or on the widths of the distribution, it had limited POLYMER FILMS
resolution power. A comparison with the results obtained Castela A S; Simoes A M P
by size exclusion chromatography was therefore carried
Evaluation of the volume fraction of water in organic
out for a set of samples having monomodal and bimodal
coatings in immersion is often made by electrochemical
distribution functions. 22 refs.
impedance spectroscopy, EIS, and based upon the
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
evolution of the coating capacitance. Among the several
WESTERN EUROPE
models and equations proposed for this determination,
Accession no.733222 the most frequently used is the Brasher equation. Most

96 © Copyright 2002 Rapra Technology Limited


References and Abstracts

frequently these determinations are made with applied GENERATION SPECTROSCOPY


coatings, although studies can be found in the literature Zhang D; Dougal S; Yeganeh M S
using free films. The behaviour of a commercial coating Exxon Research & Engineering Co.
- PVC plastisol - is studied, both applied on a metallic (ACS,Div.of Polymer Chemistry)
substrate and as a free film.
The effects of UV light and oxygen plasma on PS surfaces
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
is investigated using SFG spectroscopy. The observed
WESTERN EUROPE
spectral changes provide strong support for the
Accession no.731759 photooxidation of the aromatic ring at the PS surface, as
observed by the dramatic decrease in the aromatic C-H
Item 228 vibration during photo irradiation and plasma treatment.
Journal of Thermal Analysis and Calorimetry It is also found that the kinetics of the photooxidation of
55, No.2, 1999, p.559-63 the PS surface, monitored by SFG, is much faster than
TG/FT-IR STUDIED OF POLY(VINYL similar process observed by other techniques, such as
CHLORIDE) BLENDS FTIR or SIMS. 13 refs.
Pielichowski K USA
Krakow,Technical University Accession no.730043
Thermogravimetry coupled with FTIR was used to
investigate the stabilising action of 3-(2,4- Item 231
dibromophenylazo)-9-(2,3-epoxypropane)carbazole on Polymer Composites
the degradation of PVC. This secondary stabiliser 20, No.2, April 1999, p.314-20
increased the initial temperature of hydrogen chloride CHARACTERISATION OF MIXED FIBRE
evolution (the main process responsible for PVC NYLON COMPOSITES INCORPORATING
decomposition), thereby allowing its application for novel COMPOSITE SCRAP
PVC systems with enhanced thermal stability. 10 refs. Licea-Claverie A; Carrillo F J U; Alvarez-Castillo A;
EASTERN EUROPE; POLAND Castano V M
Accession no.731454 Tijuana,Instituto Tecnologico; Zacatepec,Instituto
Tecnologico; UNAM
Item 229 Recycling of engineering thermoplastics and their
Analytical Chemistry composites is discussed. A study on nylon-6,6 based
71, No.9, 1st May 1999, p.1809-14 composites with mixed glass fibre and carbon fibre
POLYMER ANALYSIS BY LIQUID reinforcement, including nylon composite scrap in their
CHROMATOGRAPHY/ELECTROSPRAY formulation, were reported. Several formulations were
IONISATION TIME-OF-FLIGHT MASS prepared by injection moulding and were characterised
SPECTROMETRY by stress-strain measurements, impact testing,
Nielen M W F; Buijtenhuijs F A simultaneous DTA and TGA, density measurements and
Akzo Nobel Central Research SEM. Mechanical and thermal properties of the resulting
composites are presented, discussed, and compared with
Different liquid chromatography modes in polymer
a virgin standard composite. 26 refs.
analysis were successfully interfaced with electrospray
MEXICO
ionisation time-of-flight mass spectrometry in a single
experimental set-up: the mass spectrometry data from size Accession no.729302
exclusion chromatography/mass spectrometry of PMMA
were used as absolute calibration points in the size Item 232
exclusion chromatography/refractive index Analytical Chemistry
chromatogram, and monomer mass and end groups were 71, No.7, 1st April 1999, p.1316-22
inferred from the isotopically resolved mass spectra. 44 CHARACTERIZATION OF NATURAL RESIN
refs. SHELLAC BY REACTIVE PYROLYSIS-GAS
EUROPEAN COMMUNITY; EUROPEAN UNION; CHROMATOGRAPHY IN THE PRESENCE OF
NETHERLANDS; WESTERN EUROPE ORGANIC ALKALI
Accession no.731446 Wang L; Ishida Y; Ohtami H; Tsuge S; Nakayama T
Nagoya,University; Gifu Shellac Manufacturing
Item 230 Co.Ltd.
Polymer Preprints. Volume 40. Number 1. March 1999. A method for determining the chemical composition of
Conference proceedings. natural resin shellac was developed based on reactive
Boston, Ma., March 1999, p.226-7. 012 pyrolysis-gas chromatography(Py-GC) in the presence of
SURFACE MODIFICATION OF POLYSTYRENE an organic alkali, tetramethylammonium
STUDIED BY IR-VISIBLE SUM FREQUENCY hydroxide(TMAH). Py-GC using 25% TMAH aqueous

© Copyright 2002 Rapra Technology Limited 97


References and Abstracts

solution permitted the highly sensitive determination of RAPRA COLLECTION OF INFRARED SPECTRA
terpenic acids, aleuritic acid, several minor fatty acids and OF RUBBERS, PLASTICS AND
the wax components of shellac as their methyl derivatives THERMOPLASTIC ELASTOMERS. SECOND
on the resulting pyrograms with less than 2.0 % relative EDITION
standard deviations without using any cumbersome Sidwell J A
pretreatment. The observed average distributions of each
This book provides a set of transmission and pyrolysate
resin acid component determined by reactive Py-GC for
spectra of a comprehensive range of technically important
shellac samples from India and Thailand showed that the
rubber and plastics materials including copolymers and
average ratios among terpenic acids, aleuritic acid and the
blends which are in current use. Materials are indexed
other fatty acids were about 53:24:14 for Indian shellac
under both polymer and trade name.
and 51:35:14 for Thailand shellac, respectively, suggesting
a slightly significant difference. Clearer discrimination of Accession no.725345
the shellac samples from the two different countries was,
however, achievable by applying principal component Item 235
analysis for the mole percent distributions of all the acidic Polymer
components determined by reactive Py-GC. 24 refs. 40, No.12, 1999, p.3479-85
INDIA; JAPAN; THAILAND INVERSE GAS CHROMATOGRAPHIC
Accession no.727139 CHARACTERIZATION OF POLY(ETHYLENE
OXIDE)
Al-Saigh Z Y
Item 233
Columbus,State University
ACS Polymeric Materials Science and Engineering.
Fall Meeting 1997. Volume 77. Conference The inverse gas chromatography method was used to
proceedings. obtain the thermodynamic properties and the surface
Washington, D.C., 1997, p.594-5 .012 energy of a semicrystalline polymer, PEO. PEO was used
EFFECT OF SECOND DIMENSION SAMPLING as a stationary phase in the chromatographic column and
RATE AND PARTICLE SIZE ON RESOLUTION 16 solutes with a different chemical nature were used as
AND RUN TIME IN TWO DIMENSIONAL eluents. Alkanes showed endothermic interaction
LIQUID CHROMATOGRAPHY FOR THE parameters and the molar heat of mixing in a temp. range
ANALYSIS OF POLYMERS of 70-130C. Acetates and alcohols showed better
Murphy R E; Schure M R; Foley J P interactions with the PEO layer and butanol was found to
Rohm & Haas Co.; Villanova,University be the best solvent for PEO among all solutes used. The
(ACS,Div.of Polymeric Materials Science & Engng.) variation in molec.wt. of PEO above 400 g/mol showed
no apparent effect on the interaction coefficients. The
The optimisation of a two dimensional high performance
dispersive contribution of the surface energy of PEO was
liquid chromatography (HPLC) (reverse phase liquid
measured as a function of temp., which ranged from 8.00
chromatography/gel permeation chromatography (GPC))
and 13.00 mJ/sq m, indicating a poor surface energy of
system for the analysis of low molecular weight polymers
PEO. 43 refs.
is described. A test mixture of polyethylene glycols and a
USA
commercial surfactant was used. The analysis time of the
second dimension, GPC, was varied by using different Accession no.721885
columns. The columns had different particle sizes and
lengths, and the two dimensional resolution was compared Item 236
by varying the run time in the second dimension. Journal of Adhesion
Following the optimisation, it was possible to complete a 68, Nos.1-2, 1998, p.117-42
two dimensional analysis in the time normally taken for QUANTIFICATION OF COATING ADHESION
a normal gradient HPLC run. It was established that USING LASER INDUCED DECOHESION
conventional columns could be run with higher flow rates SPECTROSCOPY
without a significant loss of resolution. The combination Meth J S; Sanderson D; Mutchler C; Bennison S J
of shorter and smaller particle GPC columns resulted in DuPont Co.
lower sampling periods at lower flow rates than
conventional columns. The highest sampling rate into the A new technique, laser induced decohesion spectroscopy,
second dimension gave the best resolution. 7 refs. is presented, which is capable of measuring the practical
work of adhesion between a transparent polymer coating
USA
or substrate. A laser pulse directed onto the sample creates
Accession no.726180 a blister at the transparent/opaque interface. The blister’s
internal pressure depends on the laser pulse energy, and
Item 234 at a critical pressure the sample fractures, creating an
Shawbury, Rapra Technology Ltd., 1997, pp.315. annular debond similar to that obtained in the standard
220.00. 30cms. 9922 blister test. By measuring physical variables such as the

98 © Copyright 2002 Rapra Technology Limited


References and Abstracts

curvature of the blister, and its radius and thickness, it is Kuo C; Grieser M D; Robinson D
possible to deduce the practical work of adhesion. 19 refs. Henkel Corp.
USA (ACS,Div.of Polymeric Materials Science & Engng.)
Accession no.721348 Applications are given of the use of size exclusion
chromatography and high performance liquid
Item 237 chromatography for the characterisation of coatings
Journal of Adhesion Science and Technology systems which either use water as the major solvent or
13, No.3, 1999, p.379-91 utilise low molecular weight polymers, oligomers, and
DETERMINATION OF THE ADHESION reactive additives which are then reacted to produce high
PROPERTIES OF AN ALKYD PIGMENTED molecular weight and crosslinked films. 6 refs.
COATING BY ELECTROCHEMICAL USA
IMPEDANCE SPECTROSCOPY Accession no.720838
Gonzalez J E G; Rosca J C M
Gran Canaria,University
Item 240
Impedance measurements were performed in different ACS Polymeric Materials Science and Engineering.Fall
frequency ranges at open circuit potential for an alkyd Meeting 1997.Volume 77.Conference proceedings.
coating with titanium dioxide as a mineral pigment in Washington, D.C., 1997, p.35-6 012
3% sodium chloride. The most probable impedance LIQUID CHROMATOGRAPHY OF
equivalent circuit method was considered for data MACROMOLECULES UNDER LIMITING
analysis. The interpretation of the impedance spectra CONDITIONS OF SOLUBILITY: FIRST
permitted the determination of water permeation, the EXPERIMENTAL OBSERVATIONS
formation of blisters, swelling of the coating, and the loss Bartkowiak A; Hunkeler D; Murgasova R; Berek D
of adhesion. 17 refs. Szczecin,Technical University; Swiss Federal Institute
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; of Technology; Slovak Academy of Sciences
WESTERN EUROPE (ACS,Div.of Polymeric Materials Science & Engng.)
Accession no.721335 Liquid chromatography at the critical adsorption point
(LC LCS) was investigated. The solubility of
Item 238 macromolecules, the sensitivity of LC LCS to such
ACS Polymeric Materials Science and Engineering.Fall variables as the injection volume, concentration injected,
Meeting 1997.Volume 77.Conference proceedings. mobile phase flow rate and mixing between the injection
Washington, D.C., 1997, p.48-9 012 zone, were investigated, using polymethyl methacrylate
QUANTITATION IN THE ANALYSIS OF (PMMA) and polyacrylamide standards. It is proposed
OLIGOMERS BY HPLC WITH ELSD that using tetrahydrofuran and n-hexane as eluents for
Trathnigg B; Kollroser M; Maier B; Berek D; Janco M PMMA, at the LC LCS, limited polymer insolubility or
Graz,Karl-Franzens-Universitat; Slovak Academy of even local precipitation is combined with the size
Sciences exclusion of macromolecules. 12 refs.
(ACS,Div.of Polymeric Materials Science & Engng.) EASTERN EUROPE; POLAND; SLOVAK REPUBLIC;
SLOVAKIA; SWITZERLAND; WESTERN EUROPE
The influence of the operating parameters used when
Accession no.720833
operating evaporative light scattering detectors in
conjunction with high performance liquid
chromatography for the characterisation of oligomers was Item 241
investigated, using polyether samples. It was concluded ACS Polymeric Materials Science and Engineering.Fall
that the instrument was useful because it provided gradient Meeting 1997.Volume 77.Conference proceedings.
elution, however, very careful calibration was required Washington, D.C., 1997, p.31-2 012
to obtain reliable quantitative data. 16 refs. LIQUID CHROMATOGRAPHY OF
AUSTRIA; WESTERN EUROPE MACROMOLECULES AT THE CRITICAL
Accession no.720839 ADSORPTION POINT: PROBLEMS AND
PITFALLS
Berek D; Janco M
Item 239 Slovak Academy of Sciences
ACS Polymeric Materials Science and Engineering.Fall (ACS,Div.of Polymeric Materials Science & Engng.)
Meeting 1997.Volume 77.Conference proceedings.
Washington, D.C., 1997, p.46-7 012 The role of column packing pore size in liquid
APPLICATION OF SEC AND HPLC TO THE chromatography at the critical adsorption point was
CHARACTERIZATION OF POLYMERS, investigating using three silica gels and a series of
OLIGOMERS, AND SMALL MOLECULES USED polymethyl methacrylates (PMMA), using toluene,
IN COATINGS AND INKS tetrahydrofuran (THF) or their mixtures as eluents.

© Copyright 2002 Rapra Technology Limited 99


References and Abstracts

Toluene strongly promotes adsorption of PMMAs on the Dallas, Tx., Spring 1998, p.102-3. 012
silica surface, whereas THF suppresses adsorption. It was COUPLED PROGRAMMED PYROPROBE-MASS
established that the pore size of the column packings SPECTROMETRY AND
played an important role in liquid chromatography at the THERMOGRAVIMETRIC-MASS
critical adsorption point. The column with the smallest SPECTROMETRY
pores largely determined the behaviour of the whole set. Carraher C E; Molloy H M; Louda J W; Baker E
The feasibility of using silica gel as column packings for Florida,Atlantic University; Florida,Center for
liquid chromatography at the critical adsorption point is Environmental Studies; Midwest Research Institute
questioned. 14 refs. (ACS,Div.of Polymeric Materials Science & Engng.)
SLOVAK REPUBLIC; SLOVAKIA In 1977, a thermogravimetric analysis unit was
Accession no.720831 successfully coupled with a mass spectrophotometer, TG-
MS. More recently, a coupled programmed pyroprobe-
Item 242 mass spectrophotometry system, also utilising IR
ACS Polymeric Materials Science and Engineering.Fall spectroscopy, was employed as a means of describing
Meeting 1997.Volume 77.Conference proceedings. degradation sequences as a function of temperature. The
Washington, D.C., 1997, p.22-3 012 application of these tools as a means to define polymer
2D-LC OF FUNCTIONAL POLYETHERS structure and degradation products is described. 9 refs.
Trathnigg B; Kollroser M; Parth M USA
Graz,Karl-Franzens-Universitat Accession no.719193
(ACS,Div.of Polymeric Materials Science & Engng.)
A combination of liquid chromatography under critical Item 245
conditions using coupled density and RI detection in one ACS Polymeric Materials Science & Engineering,
dimension, and gradient high performance liquid Spring Meeting 1998. Volume 78. Conference
chromatography in the second dimension, was used in proceedings.
the two-dimensional chromatographic analysis of the Dallas, Tx., Spring 1998, p.219-20. 012
oligomers present in fatty alcohol ethoxylates. Full SECONDARY TRANSITIONS IN POLYMERS
resolution was achieved. 6 refs. PROBED BY DIFFERENTIAL SCANNING
CALORIMETRY
AUSTRIA; WESTERN EUROPE
Bertolucci P R H; Harmon J P
Accession no.720827 South Florida,University
(ACS,Div.of Polymeric Materials Science & Engng.)
Item 243
The use of differential scanning calorimetry to identify
ACS Polymeric Materials Science and Engineering.Fall
secondary transitions in thermoplastics is studied. The
Meeting 1997.Volume 77.Conference proceedings.
temperature and breadth of the secondary transition are
Washington, D.C., 1997, p.20-1 012
related to the those of the alpha transition in a variety of
MOLECULAR CHARACTERIZATION OF
methacrylate, acrylate and styrene polymers, as well as
COMPLEX POLYMERS BY COUPLED LIQUID
polycarbonate. The effect of thermal history and the
CHROMATOGRAPHIC PROCEDURES
position and sharpness of these endothermic transitions
Berek D is discussed. Some comparisons are made between this
Slovak Academy of Sciences technique and results obtained via dielectric analysis and
(ACS,Div.of Polymeric Materials Science & Engng.) dynamic mechanical analysis obtained in the laboratory.
Size exclusion chromatography alone cannot characterise 7 refs.
the constituents of complex polymer systems. Separation USA
selectivity and characterisation of complex systems may Accession no.718740
be enhanced with liquid chromatographic (LC) methods
utilising combinations of different separation
Item 246
mechanisms. These are termed coupled LC procedures.
Macromolecular Chemistry & Physics
The applications of a variety of coupled LC procedures
200, No.2, Feb.1999, p.413-21
are discussed. 16 refs.
THERMAL PROPERTIES AND
SLOVAK REPUBLIC; SLOVAKIA
CRYSTALLISATION BEHAVIOUR OF
Accession no.720826 POLYHYDROXYBUTYRIC ACID IN BLENDS
WITH CHITIN AND CHITOSAN
Item 244 Ikejima T; Yagi K; Inoue Y
ACS Polymeric Materials Science & Engineering, Tokyo,Institute of Technology
Spring Meeting 1998. Volume 78. Conference Films of blends of polyhydroxybutyric acid with chitin
proceedings. and chitosan were prepared as completely biodegradable

100 © Copyright 2002 Rapra Technology Limited


References and Abstracts

polyester-polysaccharide composites. Crystallisation was systems under elongational interactions in polymer bilayer
examined using DSC. Data are given from FTIR and systems under elongational deformations and changes in
carbon 13 NMR. 31 refs. potential energy, leading to determination of the work of
JAPAN adhesion. This research expands the scope of previous
Accession no.716972 findings and provides a relationship between the C-H
stretching vibrational energy changes for acrylic/PE,
epoxy/PE, acrylic/PP, and epoxy/PP bilayer systems and
Item 247 the interfacial forces responsible for adhesion. 39 refs.
Journal of Biomedical Materials Research (Applied
USA
Biomaterials)
48, No.1, 1999, p.5-8 Accession no.715972
EXTRACTABLE FREE MONOMERS FROM
SELF-CURED DENTAL SEALANTS RESULTING Item 250
FROM DISPENSING ERRORS Analytical Chemistry
Vaubert V M; Moon P C; Love B J 71, No.2, 15th Jan.1999, p.468-75
Virginia,Polytechnic Institute IDENTIFICATION AND DETERMINATION OF
CROSSLINKERS IN CROSSLINKED
HPLC experiments were performed on a series of self-
POLYVINYLPYRROLIDONE(PVP) BY
curing polybisglycidyl methacrylate dental sealants that
PYROLYSIS-GAS CHROMATOGRAPHY(GC)/
were deliberately mismixed. The amount of extractable
MASS SPECTROMETRY(MS)
sealant under conditions of nonideal processing was
Cheng T M H; Malawer E G
measured. 13 refs.
International Specialty Products
USA
Accession no.716163 Pyrolysis-GC and pyrolysis-GC/MS were used to identify
and quantify specific nitrogen-containing crosslinker
compounds incorporated into the structures of crosslinked
Item 248 PVP polymers which appeared to be identical by FTIR
Macromolecular Rapid Communications spectroscopy. The pyrolyser regenerated and volatilised
20, No.2, Feb. 1999, p.95-7 specific crosslinkers which could be distinguished from
CURING OF MONOMER COMPOSITES. II. USE other pyrolysate compounds by either peak retention time
OF NMR TO MONITOR REAL TIME CURING or mass spectral release. Individual compounds studied
DYNAMICS included 3-ethylidene-1-vinyl-2-pyrrolidone, 3,3'-
Martin S J; McBrierty V J; Dowling J; Douglass D C ethylidenebis(1-vinyl-2-pyrrolidone) and N,N’-
Dublin,Trinity College; Bausch & Lomb Inc. divinylimidazolidone. In general, the level of specific
Details are given of a method for monitoring the real- crosslinkers in various commercial products ranged from
time curing dynamics of composite monomers, exploiting 1.8 to 2.5% w/w. The effect of pyrolysis temp. on this
site specific information provided by high resolution level varied with the crosslinkers studied. The crosslinker
NMR. Data using polyvinylpyrrolidone, polyhydroxy- content obtained by this technique correlated with the
ethyl methacrylate and polybutylhydroxycyclohexyl swell volume data for a specific series of crosslinked PVP
methacrylate are compared with results from a computer samples made with a single crosslinker and having similar
simulation based on a multicomponent kinetic model. particle size distributions. The pyrolysis methodology
7 refs. could not distinguish the level of crosslinker which was
EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND; incorporated as a pendant functionality from that portion
WESTERN EUROPE which was incorporated through both vinyl groups. 26
Accession no.716161 refs.
USA

Item 249 Accession no.715578


Journal of Adhesion Science and Technology
13, No.1, 1999, p.19-34 Item 251
RHEO-PHOTOACOUSTIC (RPA) FTIR Polymer Testing
SPECTROSCOPIC STUDIES OF THE 17, No.8, Dec.1998, p.533-41
ADHESION OF THERMOSETS TO NMR STUDY OF COMMERCIAL
POLYOLEFINS POLYETHYLENE-CO-VINYL ACETATE
Pennington B D; Urban M W de Souza C M G; Tavares M I B
North Dakota State University Rio de Janeiro,Cidade Universitaria
Rheophotoacoustic FTIR analysis and previously Two EVA materials with distinct vinyl acetate ratios are
developed theory were utilised in an attempt to correlate studied by nuclear magnetic resonance using solution and
the molecular level interactions in polymer bilayer solid techniques. These studies are made in order to obtain a

© Copyright 2002 Rapra Technology Limited 101


References and Abstracts

relation between the structure-properties-mobility and this Item 254


response can be utilised in order to have precise information Muanyag es Gumi
for new applications as well as better understanding of the 34, No.12, 1997, p.A12-4
material behaviour. The results show that these polymers Hungarian
present characteristic mobilities as a function of vinyl acetate ASSESSMENT OF THE THERMAL HISTORY OF
in the copolymer. Thus, as the quantity of vinyl acetate EXTRUDED UPVC
increases the dyads and tryads distribution and the molecular Marossy K
mobility in the copolymer change, as a consequence of the BorsodChem Rt.
different commercial applications. 13 refs.
The paper deals with the investigation by differential
BRAZIL
scanning calorimetry of extruded rigid PVC formulations.
Accession no.714141 The DSC traces of processed UPVC depend on the
thermal history of the melt. The DSC tests can be used to
Item 252 estimate extrusion conditions e.g. of failed products. 16
Journal of Thermal Analysis and Calorimetry refs. Articles from this journal can be requested for
54, No.2, 1998, p.565-76 translation by subscribers to the Rapra produced
METHOD FOR ANALYSIS OF THE MEASURED International Polymer Science and Technology.
CURVES OF TEMPERATURE-MODULATED
EASTERN EUROPE; HUNGARY
DIFFERENTIAL SCANNING
CALORIMETRY(TMDSC) INVESTIGATION IN Accession no.713264
THE MELTING REGION OF POLYMERS
Schawe J E K; Bergmann E; Winter W Item 255
Ulm,University; IFA GmbH Surface Coatings International
The measured signal of the TMDSC was examined for the 82, No.1, Jan.1999, p.26-30
case of polymer melting. Fourier transform analysis was USE OF ELECTROCHEMICAL IMPEDANCE
used to evaluate the data, the resulting information being SPECTROSCOPY FOR THE DETERMINATION
the amplitude and the phase shift of the first harmonic of OF THE PROTECTIVE PROPERTIES OF
the periodic heat flow component. It was shown that this SOLVENT- AND WATER-BASED PAINT
procedure was not sufficient for quantitative discussions if SYSTEMS
deviations from the symmetric curve shape occurred in the Al-Hashem A; Carew J A; Hasan A
measured heat flow curves. For polymer melting, it was Kuwait,Institute for Scientific Research
shown that asymmetric curves would be measured if the In this work, electrochemical impedance spectroscopy
experimental temp. amplitude was too large. 15 refs. was used to evaluate the corrosion protection properties
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; of the solvent-based coatings and water-based coating
WESTERN EUROPE
systems currently being proposed for use in the industrial
Accession no.713454 installations in the Arabian Gulf region. Evaluation of
corrosion damage levels for three coating systems after
Item 253 90 day immersion in 0.5M NaCl was performed using
Journal of Thermal Analysis and Calorimetry the EIS and visual observations. 22 refs.
54, No.2, 1998, p.477-99 KUWAIT
APPLICABILITY OF TEMPERATURE-
Accession no.713236
MODULATED DIFFERENTIAL SCANNING
CALORIMETRY(TMDSC) TO POLYMERIC
SYSTEMS. GENERAL THEORETICAL Item 256
DESCRIPTION BASED ON THE FULL HEAT Journal of Materials Science
CAPACITY FORMULATION 33, No.19, 1st Oct.1998, p.4721-5
Scherrenberg R; Mathot V; Steeman P RAMAN SPECTRA OF HIGH MODULUS
DSM Research POLYETHYLENE FIBRES BY RAMAN
MICROSCOPY
An overview is presented of the different aspects of
Lu S; Russell A E; Hendra P J
TMDSC, using a general theoretical description based
Southampton,University
on the full heat capacity formulation. It is demonstrated
that processes studied with the aid of TMDSC can be Raman microscopy was used to analyse a series of high
simply classified into three distinct regimes, depending modulus PE fibres, relating the Raman scattering
on the time scale and the susceptibility of the process to anisotropy to the mechanical performance of the
the temp. modulation. 47 refs. filaments. Measurements of the band intensity ratio of
EUROPEAN COMMUNITY; EUROPEAN UNION; the fibres were made and related to their Young’s modulus.
NETHERLANDS; WESTERN EUROPE This relationship is useful in morphological studies of
Accession no.713453 PE fibres. 10 refs.

102 © Copyright 2002 Rapra Technology Limited


References and Abstracts

EUROPEAN COMMUNITY; EUROPEAN UNION; UK; Details are given of the range of physical and chemical
WESTERN EUROPE properties of flame-sprayed ethylene-methacrylic acid
Accession no.711133 copolymer following different processing conditions.
Coatings were produced at a range of specific
Item 257 temperatures by varying the propane flow rate and gun
Applied Spectroscopy traverse rate. Coatings were scanned using dielectric
52, No.12, Dec.1998, p.1498-504 relaxation spectroscopy. 24 refs.
MEASUREMENT OF ORIENTATION AND AUSTRALIA; USA
CRYSTALLINITY IN UNIAXIALLY DRAWN Accession no.709520
POLY(ETHYLENE TEREPHTHALATE) USING
POLARISED CONFOCAL RAMAN
Item 260
MICROSCOPY
Polymer Journal (Japan)
Everall N J
30, No.10, 1998, p.771-4
ICI Wilton Research Centre
CRYSTALLITE SIZES AND LATTICE
Polarised confocal Raman microscopy was used to DISTORTIONS OF GEL-SPUN ULTRA-HIGH
measure molecular orientation in uniaxially drawn PETP MOLECULAR WEIGHT POLYETHYLENE
films, prepared with draw ratios from 1 to 3.5. The FIBRES
orientation of both polarised Raman microscopy and Xiao-Ping Hu; You-Lo Hsieh
polarised attenuated total reflection IR spectroscopy. California,University
Crystallinity profiles were measured through the thickness
A detailed method is reported for deriving the lattice
of the film samples and compared with the orientation
distortions and crystallite sizes of UHMWPE fibres using
gradients existing in the films. This procedure was to
a full wide angle X-ray diffraction patterns. The
determine whether the intuitive assumption that
instrumental broadening and the background scattering
orientation and crystallinity would be positively correlated
is represented by a binomial. A discussion is included
actually holds true on the microscopic scale for these
about the diffraction trace, peak assignments, and unit
samples. 18 refs.
cell dimensions. 26 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
USA
WESTERN EUROPE
Accession no.711041 Accession no.709342

Item 258 Item 261


Plasticheskie Massy (USSR) Chinese Journal of Polymer Science
No.3, 1997, p.30-3 16, No.4, 1998, p.332-8
Russian DETECTION OF TG BY MODULATED
BREAKDOWN OF AMMONIUM SALTS WITH DIFFERENTIAL SCANNING CALORIMETRY
REFERENCE TO THEIR INTRODUCTION INTO Rui Song; Jing Chen; Jingui Gao; Xin Lin; Qingrong Fan
WOOD-BASED COMPOSITES Chinese Academy of Sciences
Vigdorovich A I; Efremov V N The glass transition of PETP samples which were
The possibility was studied of using ammonium salts as subjected to solvent induced crystallisation (SINC) was
plasticisers for wood-based composites, and the investigated by modulated differential scanning
breakdown of the ammonium salts during heating was calorimetry (MDSC) and density measurements. The
studied by differential thermal gravimetry. 15 refs. Articles differential heat capacity signal from MDSC was used to
from this journal can be requested for translation by monitor the SINC process. 16 refs.
subscribers to the Rapra produced International Polymer CHINA
Science and Technology. Accession no.709335
RUSSIA
Accession no.710456 Item 262
Journal of Applied Polymer Science
Item 259 71, No.1, 3rd Jan.1999, p.1-6
Polymer Engineering and Science MICROWAVE PLASMA REACTIONS OF
38, No.11, Nov.1998, p.1873-81 IMIDAZOLE ON POLY(VINYL CHLORIDE)
PHYSICAL AND RELAXATION PROPERTIES SURFACES: A SPECTROSCOPIC STUDY
OF FLAME-SPRAYED ETHYLENE- Schmitt B R; Heung Kim; Urban M W
METHACRYLIC ACID COPOLYMER North Dakota State University
Brogan J A; Berndt C C; Simon G P; Hewitt D A closed-system microwave plasma reactor was used to react
Stony Brook,University; Monash,University imidazole molecules to PVC surfaces. Newly created

© Copyright 2002 Rapra Technology Limited 103


References and Abstracts

surfaces were analysed using ATR FTIR spectroscopy. The use of NMR to probe the in-situ curing of monomer
Surface reactions on PVC were heavily dependent on a prior mixtures commonly encountered in the manufacture of
thermal history of the PVC substrate. A mechanism for the contact lenses was studied. Spectral lines were identified
PVC-imidazole reactions was also presented. The PVC was which monitored curing with time of individual
useful as an implant for biomedical applications. 10 refs. components in the monomer mix. This information can
USA aid in gaining an understanding of the overall curing
Accession no.709309 dynamics and provide important guidance in establishing
suitable protocols in the manufacturing process. As a
precursor to this goal, several commonly-used component
Item 263 materials were characterised by high resolution proton
Applied Spectroscopy and carbon-13 NMR spectroscopies. The efficacy of the
52, No.11, Nov.1998, p.1483-7 overall procedure is demonstrated. 20 refs.
SAMPLING CONSIDERATIONS FOR FT- EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND;
RAMAN SPECTROSCOPY OF POLYMERS AND WESTERN EUROPE
SOLUTIONS Accession no.706520
Barrerra B A; Sommer A J
Miami,University
Item 266
Details are given of the determination of apparent Polimeros: Ciencia e Tecnologia
absorption coefficients and optimal sample thickness of 8, No.1, Jan./March 1998, p.46-53
PE, PETP, cellulose, and cyclohexane by FT-Raman Portuguese
analysis. A relationship was developed that permits the THERMAL STABILITY OF POLYETHYLENE
optimal sample thickness for FT-Raman measurements TEREPHTHALATE PACKAGING:
to be determined by measuring the absorbance spectrum DETERMINATION OF OLIGOMERS
of a sample whose thickness is known. Results are Freire M T de A; Reyes F G R; Castle L
discussed in the context of scattering theory, sampling Campinas,Universidade Estadual; UK,Min.of
considerations, and spectral artifacts. 9 refs. Agriculture,Fisheries & Food
USA
PETP food packaging materials were subjected to
Accession no.709038 different heating conditions (50 minutes at 120-230C),
and oligomers were identified by HPLC coupled with
Item 264 mass spectrometry and used as a parameter for evaluating
Journal of Applied Polymer Science the thermal stability of PETP. Small changes in oligomer
71, No.3, 18th Jan.1998, p.371-5 distribution were observed only for samples heated at
PROPYLENE OLIGOMERS: EXTRACTION 230C, suggesting that PETP was thermally stable under
METHODS AND CHARACTERISATION BY the heating conditions employed. The results also
FTIR, HPLC, AND SEC suggested the suitability of PETP as a food packaging
El Mansouri H; Yagoubi N; Scholler D; Feigenbaum A; material for use in conventional and microwave ovens,
Ferrier D and for secondary recycling under controlled conditions.
INRA 28 refs.
BRAZIL; EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Details are given of the isolation of propylene oligomers WESTERN EUROPE
from polymer matrix by dissolution precipitation and
Accession no.706082
Soxhlet methods. Characterisation was undertaken by
FTIR, UV spectroscopy, HPLC, and GPC. Data were used
to explain their behaviour toward packaged food products Item 267
in PP packaging. 18 refs. Journal of Thermal Analysis and Calorimetry
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; 52, No.2, 1998, p.261-74
WESTERN EUROPE THERMAL ANALYSIS OF SOME
Accession no.708984 ENVIRONMENTALLY DEGRADABLE
POLYMERS
Day M; Cooney J D; Shaw K; Watts J
Item 265 Canada,National Research Council
European Polymer Journal
34, No.12, Dec.1998, p.1817-28 The thermal characteristics of a series of degradable
CURING OF POLYMER COMPOSITES. I. NMR polymers for use in commercial composting facilities was
CHARACTERIZATION OF COMPONENT investigated using TGA and DSC. Phase changes
MONOMERS associated with some of the polymers investigated may
Martin S J; O’Brien J E; Dowling J; McBrierty V J cause problems in the interpretation of data from
Dublin,Trinity College; Bausch & Lomb Inc. composting degradation studies. Several biodegradable

104 © Copyright 2002 Rapra Technology Limited


References and Abstracts

polymers were observed to have melt transitions at DETERMINATION OF VINYL ACETATE


temperatures similar to those found in a composting CONTENT IN EVA COPOLYMERS. FACILITIES
environment. 19 refs. AND LIMITS OF APPLICATIONS OF MASS
CANADA SPECTROMETRY ANALYSIS METHODS
Accession no.705674 Haussler L; Pompe G; Albrecht V; Voigt D
Dresden,Institut fuer Polymerforschung
Item 268 Ethylene-vinyl acetate copolymers were investigated by
Journal of Applied Polymer Science simultaneous thermal analysis and pyrolysis gas
70, No.12, 19th Dec.1998, p.2457-61 chromatography. Both devices were coupled to a mass
NUCLEAR MAGNETIC RESONANCE STUDY spectrometer. Calibration with polyvinyl acetate led to
OF COMMERCIAL POLY(VINYL ACETATE) sufficient accuracy in relation to the vinyl acetate content,
De Souza C M G; Tavares M I B because of the linear calibration plot. Quantitative
Rio de Janeiro,Universidade Federal determination of vinyl acetate was carried out at both 500
and 700 C. The calibration plot was linear provided that
The commercial poly(vinyl acetate) bulk was studied by
the mass of vinyl acetate did not exceed a critical value.
NMR at solution and solid state to understand the
18 refs.
behaviour of this polymer to obtain information on
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
structure, sample molecular mobility, and heterogeneity. WESTERN EUROPE
To analyse the behaviour of this polymer, NMR
Accession no.705281
techniques were chosen, such as carbon-13 solution,
magic angle spinning, cross-polarisation/magic angle
spinning, proton spin-relaxation time in the rotating frame Item 271
parameter and dipolar dephasing experiment. 13 refs. Composites Science & Technology
BRAZIL 58, No.10, 1998, p.1641-7
CHEMICAL ANALYSIS OF A FIELD-FAILED
Accession no.705529
COMPOSITE SUSPENSION INSULATOR
Chughtai A R; Smith D M; Kumosa M S
Item 269
Denver,University
Journal of Thermal Analysis and Calorimetry
52, No.1, 1998, p.145-55 The type of corrosive environment responsible for brittle
German fracture of suspension composite insulators was
THERMOANALYTICAL CHARACTERISING established. A series of FTIR experiments was performed
UV-CURED POLYMER FILMS to identify chemical functionalities formed during the
Hosselbarth B; Friese K; Geyer W degradation process of composite insulators affected by
Institut fuer Oberflaechenmodifizierung eV; Leipzig- brittle fracture. It was shown that the brittle fracture
Halle Ltd.; Umweltforschungzentrum process was caused by the formation of nitric acid either
outside or inside an insulator leading to stress corrosion
Thermooxidative and thermomechanical stabilities of cracking of the glass/polymer composite rod material.
radiation-cured acrylates and epoxides were examined by Nitrate was detected on the composite fracture surfaces
TGA, DMA and DSC. The polymeric trifunctional inside a 115 kV suspension composite insulator which
acrylates PETIA, TMPTA and THEIC displayed the failed in service by brittle fracture. 17 refs.
highest temperatures of onset of degradation. The high USA
crosslinking density of the films resulted in an almost
Accession no.705241
temperature-independent complex E-modulus, as
measured by DMA. With increasing degree of
ethoxylation or propoxylation of the monomers, decreases Item 272
in thermal stability and strength were found. For International Journal of Adhesion & Adhesives
difunctional polymeric acrylates and epoxides, the TG 18, No.5, 1998, p.319-31
temperature was measured. The average degree of curing LOW RESOLUTION PULSED NMR AND
of UV-cured epoxy films could be determined from the ULTRASOUND STUDY TO MONITOR THE
temperature of the maximum in the loss modulus. 13 refs. CURE OF AN EPOXY RESIN ADHESIVE
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; Cocker R P; Chadwick D L; Dare D J; Challis R E
WESTERN EUROPE Keele,University; Manchester,Metropolitan University
Accession no.705282 The cure of an epichlorohydrin-bisphenol A resin and
curing agent containing a primary diamine and an amido-
Item 270 polyamine was studied using two complementary
Journal of Thermal Analysis and Calorimetry techniques, low resolution pulsed NMR spectroscopy and
52, No.1, 1998, p.131-43 measurement of pulsed broad bandwidth ultrasound
German propagation velocity and absorption changes. The two

© Copyright 2002 Rapra Technology Limited 105


References and Abstracts

techniques independently gave a similar picture of the Item 274


cure process, predicting cure events at the same times. Revista de Plasticos Modernos
The results obtained indicated that the cure followed 74, No.495, Sept.1997, p.255-61
distinct phases, i.e. an initial liquid stage where short Spanish
polymer chains were formed, followed by a second stage FTIR SPECTROPHOTOMETRY FOR THE
where longer molecules developed, a third stage where DETECTION OF MICROSTRUCTURAL
crosslinking between chains occurred and the adhesive CHANGES IN A POLYPROPYLENE/
began to solidify, and a final stage when solidification POLYETHYLENE COPOLYMER CAUSED BY
was completed. 19 refs. ARTIFICIAL AGEING
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; Romeu J; Pages P; Carrasco F
WESTERN EUROPE Cataluna,Universidad Politecnica; Girona,Universidad
Accession no.704884 A study was made of microstructural changes occurring
in blue and red samples of an ethylene-propylene
Item 273 copolymer exposed to artificial ageing in a Xenotest
Polymer Degradation and Stability chamber for up to 5000 hours. The effects of ageing
62, No. 1, Oct. 1998, p.41-8 were quantified by Fourier transform IR
MECHANISMS OF THERMAL DEGRADATION spectrophotometry. By calculating the reduced
OF A POLYESTER FLAME-RETARDED WITH absorption in selected spectral bands, it was possible
ANTIMONY OXIDE/BROMINATED to detect oxidation and chain scission reactions and
POLYCARBONATE STUDIED BY variations in isotacticity which differed in the
TEMPERATURE-PROGRAMMED ANALYTICAL differently coloured specimens. 8 refs.
PYROLYSIS EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
Sato H; Kondo K; Tsuge S; Ohtani H; Sato N WESTERN EUROPE
Nagoya,University; Toray Research Center Inc. Accession no.702522
Thermal degradation of a flame-retarded PBTP consisting
of PBTP and a synergistic flame-retardant system based Item 275
on brominated polycarbonate (copolycarbonate Journal of Applied Polymer Science
containing units from bisphenol A and tetrabrominated 70, No.7, 14th Nov.1998, p.1307-10
bisphenol A plus tribromophenoxy end groups) and MULTIDIMENSIONAL SPECTROMETRY AND
antimony trioxide was studied by means of various MAPPING
temperature-programmed analytical pyrolysis techniques Fateley W G; Deverse R A; Hammaker R M
such as temperature-programmed pyrolysis-mass Kansas State University
spectrometry, temperature-programmed pyrolysis-atomic
A new inexpensive approach is described for mapping
emission detection and temperature-programmed
molecular structure in polymeric materials which includes
pyrolysis-gas chromatography. During the degradation of
the combination of interferometers and Hadamard
the flame-retarded PBTP, brominated phenols were first
transform techniques to perform multidimensional
observed to evolve at temperatures slightly lower than
spectometry and mapping. 17 refs.
those for the flammable product evolution from the
USA
substrate polymer PBTP, followed by the evolution of
hydrogen bromide over the whole range of degradation Accession no.702159
temperatures for the substrate polymer. These degradation
processes were closely related to the synergistic effects Item 276
of antimony trioxide on the decomposition of brominated Journal of Materials Science.Materials in Medicine
polycarbonate in the flame-retardant system to promote 9, No.9, Sept.1998, p.529-33
the thermal degradation of brominated polycarbonate at INVESTIGATION OF GLASS-IONOMER
lower temperatures than those for pure brominated CEMENTS USING DIFFERENTIAL SCANNING
polycarbonate. Furthermore, the evolution of the flame CALORIMETRY
poisoning antimony tribromide formed through the Khalil S K H; Atkins E D T
reaction between brominated polycarbonate and antimony Bristol,University
trioxide could also be monitored directly by temperature-
programmed pyrolysis techniques. On the basis of the Six commercial glass-ionomer cements commonly used
data obtained by these temperature-programmed pyrolysis for various dental applications were investigated using
techniques, the thermal degradation of the flame-retarded DSC. Heat flow behaviour and heat capacity of the
PBTP and synergistic flame-retarding mechanisms are cements were measured during isothermal (at 37 C) setting
discussed. 10 refs. reactions. All materials underwent an exothermic setting
process, but with different enthalpies of reactions and
JAPAN
different heat capacities; there were no remaining endo-
Accession no.704607 or exothermic reactions after the setting of the cement.

106 © Copyright 2002 Rapra Technology Limited


References and Abstracts

All materials examined were effective thermal insulators. Popovici D; Sacher E; Meunier M
18 refs. Montreal,Ecole Polytechnique
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Teflon, type AF1600, which contains perfluorinated
WESTERN EUROPE
dioxole rings, was found to suffer significant degradation
Accession no.702142 when exposed to X-rays whilst undergoing investigation
by X-ray photoelectron spectroscopy. The degradation
Item 277 mechanism was significantly different to that of
Journal of Materials Science fluoropolymers which contain only carbon and fluorine.
33, No.14, 15th July 1998, p.3511-7 It was established that oxygen was at least as twice as
MOLECULAR ORGANISATION IN susceptible as fluorine, and that the amounts of oxygen
STRUCTURAL PVDF loss were equal to those of fluorine. Oxygen could be
Glennon D; Cox P A; Nevell R T; Nevell T G; Smith J degraded by the breaking of only one bond, the oxygen
R; Tsibouklis J; Ewen R J then forming a free radical. The free radicals produced
Portsmouth,University; West of England,University by scission of carbon-carbon bonds participated in
reactions leading to degradation and crosslinking. 9 refs.
Poly(vinylidene fluoride) containing 10% dibutyl sebacate
CANADA
plasticiser, as used in the construction of flexible oil and
gas pipelines, was exposed to raised temperatures for Accession no.700200
prolonged periods of time, to acid etching and to various
tensile deformation regimes. The effects of these Item 280
treatments on crystallinity and surface properties of this Polymer International
material were examined in the light of analytical data 47, No.1, Sept.1998, p.72-5
obtained by FTIR, DSC, X-ray diffraction, X-ray TEMPERATURE-MODULATED DIFFERENTIAL
photoelectron spectroscopy, goniometry and a variety of SCANNING CALORIMETRY. II.
microscopy techniques. 36 refs. DETERMINATION OF ACTIVATION ENERGIES
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; Zhong Jiang; Hutchinson J M; Imrie C T
WESTERN EUROPE Aberdeen,University
Accession no.701984
Alternating differential scanning calorimetry (ADSC), a
commercial development of temperature-modulated
Item 278 differential scanning calorimetry, was used to determine the
Food Additives and Contaminants activation energy associated with the relaxation processes
15, No.3, 1st April 1998, p.346-54 in polycarbonate in the region of the glass transition. In this
PARTS-PER-TRILLION DETERMINATION OF procedure the frequency of the temperature modulation is
STYRENE IN YOGHURT BY PURGE-AND-TRAP varied over a range of approximately one decade, and the
GAS CHROMATOGRAPHY WITH MASS mid-point of the step change in the complex heat capacity is
SPECTROMETRY DETECTION evaluated. In these experiments, two different amplitudes
Nerin C; Rubio C; Cacho J; Salafranca J of temperature modulation were employed. The results were
Zaragoza,University in agreement with each other, and in good agreement with
Headspace sampling methods prior to capillary gas published values. Ripples seen on the Fourier-transformed
chromatography are widely used for the determination signals are attributed to the mode of the data analysis, and
of volatile compounds present in very different types of not to noise on the data. 7 refs.
samples. An automated and rapid system for EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
determination of volatiles from yoghurt was developed.
Thirty-five volatile organic compounds(VOCs) were Accession no.700165
identified in PS cups used for yoghurt packaging and 42
VOCs from yoghurt samples. Quantitative analysis of Item 281
styrene in several samples from the Spanish retail market Materials World
was carried out. 16 refs. 6, No.10, Oct.1998, p.617-9
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; THROWING LIGHT ON FIBRES AND
WESTERN EUROPE COMPOSITES
Accession no.700270 Young B
Manchester,University
Item 279 The use is discussed of Raman spectroscopy to monitor
Journal of Applied Polymer Science the stresses and strains on individual fibres in composite
70, No.6, 7th Nov.1998, p.1201-7 materials. New instrumentation has caused rapid growth
PHOTODEGRADATION OF TEFLON AF1600 in the use of Raman spectroscopy for materials
DURING XPS ANALYSIS characterisation, including the introduction of charged-

© Copyright 2002 Rapra Technology Limited 107


References and Abstracts

coupled device cameras which offer significant London, Chapman & Hall, 1997, p.181-233. 9
improvements in sensitivity and very low noise, and also INFRARED DICHROISM, POLARISED
holographic notch filters which are used to remove the laser FLUORESCENCE AND RAMAN
line and allow single monochromators to be used. Both SPECTROSCOPY
these developments are incorporated in the Raman imaging Bower D I
microscope developed by Renishaw in collaboration with Leeds,University
Leeds University Physics Department. Its use is described Edited by: Ward I M
with reference to aramid fibre reinforced PP. 5 refs. (Leeds,University)
RENISHAW PLC
The three spectroscopic techniques for studying
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE molecular orientation in polymers described in detail
Accession no.699334 use polarised electromagnetic radiation. The principles
of the techniques are outlined, relevant theory and
Item 282 experimental details described, and a selection of results
Farbe und Lack presented. 79 refs.
104, No.10, 1998, p.93/8 EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
German
MODULATED DIFFERENTIAL SCANNING Accession no.697738
CALORIMETRY
Haessler R Item 285
Dresden,Institut fuer Polymerforschung Polymer
The use of modulated DSC for improved interpretation 39, No.20, 1998, p.4973-6
of product characteristics under thermal effects was EFFECTS OF SUBSTRATE INTERACTIONS IN
investigated. Tgs, for example, which are masked by post- THE LIQUID CHROMATOGRAPHY OF
curing or enthalpy relaxation, could be detected in a single POLYMERS
measurement and compared. The separation of complex Kosmas M K; Bokaris E P; Georgaka E G
transitions in multicomponent systems into individual Ioannina,University
parts such as melts, transition temps. and relaxations was The elution behaviour of PMMA samples was studied
shown to be feasible. The potential for use of modulated through two liquid chromatographic columns, one
DSC in the field of epoxy resins was demonstrated using
containing a substrate of silica covered with trimethylsilyl
examples of the determination of Tg near the regions of
groups and the other a substrate of pure silica. Both
enthalpy relaxation, melt and post-curing. 7 refs.
substrates had the same pore size and the solvent was the
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
WESTERN EUROPE
same for both columns. The results were discussed and
they showed that the polymer-surface interactions
Accession no.699054
changed when the nature of the substrate was changed.
14 refs.
Item 283
EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE;
Structure and properties of Oriented Polymers. Second WESTERN EUROPE
Edition.
Accession no.696588
London, Chapman & Hall, 1997, p.234-68. 9
NUCLEAR MAGNETIC RESONANCE
Speiss H W Item 286
Max-Planck-Institut fuer Polymerforschung Food Additives and Contaminants
Edited by: Ward I M 15, No.1, 1st Jan.1998, p.93-9
(Leeds,University) SYSTEMATIC STUDY ON THE STABILITY OF
SELECTED POLYMER ANTIOXIDANTS IN EU
The basics of solid state NMR are outlined and the site-
OFFICIAL AQUEOUS AND ALTERNATIVE
selective information available from multi-dimensional
FOOD SIMULANTS USING HPLC
NMR spectra about molecular order and dynamics in
Demertzis P G; Franz R
oriented polymers is illustrated with specific experimental
examples. 55 refs. Fraunhofer Institute for Food Technol. & Packag.
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; Details are given of the stability of five commercial
WESTERN EUROPE antioxidants in food simulants and in an alternative fat
Accession no.697739 simulant. Analysis was performed using a rapid HPLC
method with UV detection. 23 refs.
Item 284 EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
WESTERN EUROPE
Structure and properties of Oriented Polymers. Second
Edition. Accession no.695963

108 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Item 287 discussed include the use of SEM in studying fracture in


Colloid & Polymer Science mineral filled thermoplastics, secondary electron imaging
276, No.7, July 1998, p.565-9 in obtaining information on sample topography,
DESCRIPTION OF THE GLASS TRANSITION backscattered electron imaging in studying filler
MEASURED BY TEMPERATURE MODULATED dispersion in polymer matrices, and energy dispersive X-
DIFFERENTIAL SCANNING CALORIMETRY ray spectroscopy in determining the chemical composition
Schawe J E K of the fillers or contaminants responsible for fracture
Ulm,University initiation. 5 refs.
BRAZIL
The temp. modulated DSC (TMDSC) technique could be
used for heat capacity spectroscopy in the low frequency Accession no.695299
range. The measured property was the complex heat
capacity. The frequency-dependent relaxation transition Item 290
measured by TMDSC occurred in the temp. range of the Journal of Polymer Science : Polymer Physics Edition
thermal Tg. The non-equilibrium of the glassy state thus 36, No.12, 15th Sept.1998, p.2165-75
influenced the TMDSC curves. Experimental evidence DESCRIPTION OF THERMAL RELAXATION OF
was the dependence of the shape of the heat capacity curve POLYSTYRENE CLOSE TO THE THERMAL
on the thermal history. A theoretical description of the GLASS TRANSITION
influence of the non-equilibrium state on the spectroscopic Schawe J E K
curves, based on the Tool-Narayanaswamy-Moynihan Ulm,University
model, is presented. 23 refs.
Using spectroscopic methods at relatively high frequency,
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
WESTERN EUROPE the alpha-relaxation was measured in the thermodynamic
Accession no.695591 equilibrium. In the caloric case this phenomenon is called
thermal relaxation transition. Using a conventional
differential scanning calorimeter, the transition of the
Item 288 equilibrium (the melt) into a nonequilibrium (the glassy
Composites Plastiques Renforces Fibres de Verre state) was measured. This effect is called thermal glass
Textile transition. Temperature-modulated DSC curves in the
No.21, May/June 1997, p.48-54 glass transition region were described using the Tool-
French Narayanaswamy-Moynihan model. 54 refs.
DURABILITY OF COMPOSITES: HOW TO EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
ACHIEVE RELIABLE ACCELERATED AGEING WESTERN EUROPE
Siampiringue N; Gaumet S; Lemaire J Accession no.694872
Centre National d’Evaluation de Photoprotection
The use of accelerated ageing tests and Item 291
spectrophotometric techniques in studying the Journal of Polymer Science : Polymer Physics Edition
photooxidative degradation of unsaturated polyester resins 36, No.12, 15th Sept.1998, p.2103-9
and glass fibre-reinforced composites is examined. RAPID DETERMINATION OF COMONOMER
Results of accelerated and natural ageing tests are CONTENT, CRYSTALLINITY, AND LONG
compared, and criteria to be taken into account in SPACING BY MULTIPLE-PULSE PROTON NMR
achieving accelerated test results representative of reality IN ETHYLENE-VINYL ALCOHOL
are discussed. 5 refs. COPOLYMERS
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; Perez E; Cerrada M L; Vanderhart D L
WESTERN EUROPE Instituto de Ciencia y Tecnologia de Polimeros;
Accession no.695308 US,National Institute of Standards & Technology
Capitalising on the superior sensitivity of proton NMR,
Item 289 relatively rapid estimates of three parameters, namely,
Polimeros: Ciencia e Tecnologia comonomer content, crystallinity, and long spacing, were
7, No.3, July/Sept.1997, p.19-23 determined for three ethylene-vinyl alcohol copolymers
Portuguese using solid state proton NMR measurements. Multiple-pulse
FAILURE ANALYSIS OF MATERIALS BY techniques were utilised (a) in conjunction with magic angle
ADVANCED MICROSCOPIC TECHNIQUES spinning for measuring comonomer content, (b) in
Chinaglia C R; Correa C A conjunction with a relaxation time measurement for
Sao Carlos,Universidade Federal determining crystallinity, and (c) in conjunction with a
Failure analysis techniques allowing the determination relaxation time-based spin diffusion measurement for
of the chemical composition of a sample and its correlation determining the long spacing. These three parameters,
with the observed fracture mode are examined. Topics extracted from data collected in a total spectrometer time of

© Copyright 2002 Rapra Technology Limited 109


References and Abstracts

about 20 min., and were compared with similar parameters Item 295
obtained using more conventional DSC, small angle X-ray Macromolecular Chemistry & Physics
scattering (including synchrotron), and solution-state NMR 199, No.8, 1998, p.1623-9
measurements, with good agreement. 23 refs. THERMAL STABILITY AND
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; USA; CRYSTALLISATION KINETICS OF PEEK
WESTERN EUROPE Chen J-Y; Chen M; Chao S-C
Accession no.694867 Taiwan,National Sun Yat-Sen University
TGA, dynamic rheological analysis and polarised light
Item 292 microscopy were used to assess thermal stability of PEEK.
Smart Materials & Structures Emphasis is given to the effect of melting temperature on
7, No.4, Aug. 1998, p.557-68 thermal stability. 23 refs.
IN SITU CURE MONITORING USING OPTICAL CHINA
FIBRE SENSORS. A COMPARATIVE STUDY Accession no.694246
Powell G R; Crosby P A; Waters D N; France C M;
Spooncer R C; Fernando G F Item 296
Brunel University; Cranfield,University Injection Molding
A comparative study is presented for different types of 6, No.8, Aug. 1998, p.56/9
optical fibre sensor developed to monitor the cure of an MATERIALS ANALYST: PART 13.
epoxy resin system. The sensors were based on PERFORMANCE PROBLEMS: WHEN THE
transmission spectroscopy, evanescent wave spectroscopy PELLETS DON’T MATCH THE PARTS
and refractive index monitoring. 19 refs. Sepe M
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; Dickten & Masch Mfg.
WESTERN EUROPE The use of differential scanning calorimetry and
Accession no.694840 thermogravimetric analysis as analytical tools in part
failure determination is applied. Problems are examined
Item 293 in part performance of moulded 30% glass-reinforced,
Polymer Testing ’97. Day 3: Chemical Analysis. low-viscosity PEI and a second part moulded from PPS
Conference proceedings. with proprietary additives to improve wear resistance. The
Shawbury, 7th-11th April 1997, Paper 4. 9T importance of checking the composition of the basic
RAMAN SPECTROSCOPY OF POLYMERS material is stressed.
Williams K P J; Wilcock I C USA
Renishaw plc Accession no.693205
(Rapra Technology Ltd.; Plastics & Rubber Weekly;
European Plastics News) Item 297
Raman spectroscopy is now coming of age as a routine Journal of Applied Polymer Science
analytical method. Advances in Raman technology have 69, No.11, 12th Sept.1998, p.2175-85
meant that robust, user-friendly equipment can be IR SPECTROSCOPY AS A QUANTITATIVE AND
manufactured at a reasonable cost. These advances are PREDICTIVE ANALYSIS METHOD OF
described, together with applications of Raman imaging PHENOL-FORMALDEHYDE RESOL RESINS
microscope systems to polymer analysis. 11 refs. Holopainen T; Alvila L; Rainio J; Pakkanen T T
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Joensuu,University; Dynoresin Oy
WESTERN EUROPE A set of resin samples was characterised by IR and carbon-
Accession no.694712 13 NMR spectroscopy. The suitability of IR spectroscopy
for the quantitative analysis of resins was evaluated by
Item 294 statistical methods using the NMR reference data as
International Polymer Processing calibration. The values of interesting properties, e.g. the
13, No.2, July 1998, p.142-8 amount of free phenol and the formaldehyde-to-phenol
PEROXIDE INDUCED CROSSLINKING AND molar ratio, of the resins being similar to the calibration
DEGRADATION OF POLYAMIDE resins were predicted from the IR spectra. The predicted
Yu Q; Zhu S results were compared with those observed by carbon-13
McMaster University NMR spectroscopy. 15 refs.
FINLAND; SCANDINAVIA; WESTERN EUROPE
Peroxide-induced crosslinking and degradation of nylon
12 were investigated using ESR. Various reaction Accession no.692990
mechanisms are proposed. 20 refs.
Item 298
CANADA
Journal of Materials Science
Accession no.694268 33, No.13, 1st July 1998, p.3245-9

110 © Copyright 2002 Rapra Technology Limited


References and Abstracts

XPS MONITORING OF THE REMOVAL OF AN transform-Raman spectroscopy was proposed as a


AGED POLYMER COATING FROM A METAL qualitative tool to follow the degree of crosslinking in this
SUBSTRATE BY TEA-CARBON DIOXIDE high-ortho novolac. 54 refs.
LASER ABLATION BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
Cottam C A; Emmony D C; Cuesta A; Bradley R H WESTERN EUROPE
Loughborough,University; Aberdeen,Robert Gordon Accession no.689414
University
X-ray photoelectron spectrometry was used to observe Item 301
the changes in surface chemistry during the removal of Antec ’98. Volume II. Conference proceedings.
paint from a zinc coated steel substrate using TEA-carbon Atlanta, Ga., 26th-30th April 1998, p.1415-7. 012
dioxide laser ablation. Laser ablation at both plasma and IN SITU SPECTROSCOPY OF CO2-INDUCED
sub-plasma fluences were investigated and their relative PLASTICISATION OF GLASSY POLYMERS
merits discussed. The laser was shown to be effective in Kazarian S G; Brantley N H; Eckert C A
paint removal and was not impaired by ageing in the paint. Georgia,Institute of Technology
32 refs. (SPE)
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
In situ spectroscopy is used to study the plasticisation of
WESTERN EUROPE
glassy polymers by high-pressure and supercritical CO2.
Accession no.692055 The methodology for in situ spectroscopic analysis of the
interactions between CO2 and polymers is described. The
Item 299 changes in IR spectra of CO2 incorporated into various
Analytical Chemistry polymers indicate a specific interaction between CO2 and
70, No.15, 1st Aug.1998, p.3298-303 polymer functional groups. Increased polymer segmental
IMPROVEMENTS IN POLYMER mobility is also observed, indicative of the plasticisation
CHARACTERIZATION BY SIZE-EXCLUSION phenomenon. Implications of these discovered molecular
CHROMATOGRAPHY AND LIQUID interactions are discussed. 25 refs.
CHROMATOGRAPHY AT THE CRITICAL USA
CONDITION BY USING ENHANCED-FLUIDITY Accession no.687565
LIQUID MOBILE PHASES WITH PACKED
CAPILLARY COLUMNS
Hao Yun; Olesik S V; Marti E H Item 302
Ohio,State University; Ashland Chemical Co. Antec ’98. Volume II. Conference proceedings.
Atlanta, Ga., 26th-30th April 1998, p.1860-4. 012
The use of the above combination of techniques is QUANTITATIVE ANALYSIS OF CHEMICAL
described and results obtained for samples of PS, PMMA, BLOWING AGENTS BY DSC
styrene-methyl acrylate copolymers and functionalised Prasad A; Shanker M
PS are presented and discussed. 32 refs. Millennium Petrochemicals Inc.
USA (SPE)
Accession no.691471
It is shown that differential scanning calorimetery (DSC)
can be used to determine quantitatively the level and
Item 300 composition of chemical blowing agents such as
Polymer azodicarbonamide (azo) in commercial formulations.
39, No.22, 1998, p.5293-300 DSC can also be used to obtain the onset of decomposition
QUANTITATIVE CARBON-13 SOLID-STATE temperature and the rate of decomposition of azo in the
NMR AND FT-RAMAN SPECTROSCOPY IN presence of group II and group IV metal salt activators.
NOVOLAC RESINS DSC has the potential to detect the level of undecomposed
Ottenbourgs B; Adriaensens P; Carleer R; Vanderzande blowing agents present in processed foam products and
D; Gelan J to qualitatively determine the degree of dispersion of the
Limburg,University blowing agent and the activators in commercial
formulations. Advantages of DSC over the currently used
A qualitative and quantitative study of the curing behaviour
EGA technique are ease of operation, shorter analysis time
of a high-ortho novolac resin with paraformaldehyde under
and detection of azo concentrations as low as 1%. 12 refs.
different conditions was conducted. The degree of cure as
USA
a function of the formaldehyde/phenol ratio, the degree of
conversion and the final structure after curing were Accession no.687551
determined on the basis of a quantitative carbon-13 solid
state NMR with cross-polarisation and magic angle Item 303
spinning. The spin-lattice relaxation time was measured Antec ’98. Volume II. Conference proceedings.
as a probe to follow the evolution of cure. Fourier Atlanta, Ga., 26th-30th April 1998, p.2114-8. 012

© Copyright 2002 Rapra Technology Limited 111


References and Abstracts

APPLICATION OF GC/MS IN epoxy-anhydride thermosetting system is used as an


THERMOPLASTICS PROBLEM SOLVING example. Vitrification and devitrification steps are
Shaker D C; Kim H C observed. The heat flow phase during isothermal and
LNP Engineering Plastics nonisothermal cure is always small, but its evolution
(SPE) contains information on relaxation phenomena, vitrification
and devitrification, in the course of the chemical reaction.
The use of GC/MS (gas chromatography/mass spectrometry)
Modelling of the (heat flow related) chemical kinetics and
in the thermoplastics problem solving area is outlined. GC/
the (heat capacity related) mobility restrictions contributes
MS is a hyphenated technique; i.e. it combines the two
to a better understanding of the reaction mechanism and
techniques, chromatography and spectroscopy. In this
reaction kinetics up to a high degree of chemical
procedure, a material is introduced into the GC, components
conversion. The use of MTDSC as a tool for a quantitative
are separated and sent to the MS where they are ionised, and
construction of the vitrification curve in Temperature-Time-
the resulting particles are separated by mass. The applications
Transformation and Continuous-Heating-Transformation
of GC/MS to solving complex problems are discussed
diagrams is illustrated. 20 refs.
through positive identification of base resins, contamination,
BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;
odours and solvents.
WESTERN EUROPE
USA
Accession no.687483
Accession no.687499

Item 306
Item 304 Antec ’98. Volume II. Conference proceedings.
Antec ’98. Volume II. Conference proceedings. Atlanta, Ga., 26th-30th April 1998, p.2215-8. 012
Atlanta, Ga., 26th-30th April 1998, p.2101-5. 012 PRACTICAL ANALYSIS TECHNIQUES OF
TEMPERATURE GRADIENT INTERACTION POLYMER FILLERS BY FOURIER
CHROMATOGRAPHY OF POLYMERS TRANSFORM INFRARED SPECTROSCOPY
Chang T; Lee W; Lee H C; Mays J W; Harville S; (FTIR)
Frater D J Coles B J; Hall C J
Pohang,University of Science & Technology; Hauser Inc.
Alabama,University at Birmingham (SPE)
(SPE)
The identification of polymers by FTIR is often
Temperature gradient interaction chromatography (TGIC) complicated by the presence of fillers. However for kaolin
is a conventional reversed phase BPLC technique, but the clay, an FTIR analysis should be able to identify the filler
column temperature is varied during elution. A very fine and predict its concentration using a standard curve. The
and reproducible control of interaction between polymer resulting percentage is more reliable than a simple ash,
chains and the stationary phase can be achieved by changing which may change the chemical composition of the filler.
the column temperature. Under a suitable temperature 2 refs.
programming, this method provides a far superior resolution
USA
to conventional size exclusion chromatography. In addition,
elution in TGIC is more sensitive to molecular weight alone. Accession no.687418
Thus it provides an excellent route to separating branched
polymer molecules of similar hydrodynamic volume but Item 307
differing molecular weight. 8 refs. Polymer Engineering and Science
KOREA; USA 38, No.6, June 1998, p.922-5
Accession no.687496 IDENTIFICATION OF OFF-FLAVOUR
COMPOUNDS IN HDPE WITH DIFFERENT
AMOUNTS OF ABSCENTS
Item 305 Villberg K; Veijanen A; Gustafsson I
Antec ’98. Volume II. Conference proceedings. Jyvaskyla,University; Borealis AB
Atlanta, Ga., 26th-30th April 1998, p.2037-41. 012
MODULATED DIFFERENTIAL SCANNING Details are given of the addition of zeolite to HDPE
CALORIMETRY TO STUDY REACTING drinking water pipes in an attempt to eliminate odours
POLYMER SYSTEMS and to remove odour-causing compounds. The system
Van Mele B; Van Assche G; Van Hemelrijck A used for analysis of volatile organic compounds was a
Brussels,Free University gas chromatographic/mass spectrometric sniffing system.
(SPE) Purge and trap techniques were used to introduce the
volatile, off-flavour components into the gas
Modulated (temperature) differential scanning calorimetry chromatograph. 16 refs.
(MTDSC or MDSC) is used to simultaneously study the
FINLAND; SCANDINAVIA; SWEDEN; WESTERN EUROPE
evolution of heat flow and heat capacity for the isothermal
and non-isothermal reactions of polymer systems. An Accession no.686400

112 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Item 308 15, No.2, 1998, p.217-28


Polymer EFFECTS OF PACKAGING AND STORAGE
39, No.19, 1998, p.4665-73 CONDITIONS ON VOLATILE COMPOUNDS IN
SURFACE GLASS TRANSITION BEHAVIOUR GAS-PACKED POULTRY MEAT
OF AMORPHOUS POLYMER FILM BY Eilamo M; Kinnunen A; Latva-Kala K; Ahvenainen R
SCANNING FORCE MICROSCOPY AND VTT Biotechnology & Food Research;
SURFACE SPECTROSCOPY Finland,Technical Research Centre
Kakiyama T; Tanaka K; Takahara A
Volatile compounds released by raw chicken legs packed
Kyushu,University
in modified atmosphere packages were determined to
The surface molecular motion of amorphous polymeric develop a spoilage indicator for monitoring the shelf life
solids was measured by lateral force microscopy, scanning of raw chicken. The effects of four packaging factors
viscoelasticity microscopy, and differential X-ray (headspace volume, oxygen transmission rate of the
photoelectron spectroscopy. Data are given for PS and package, residual oxygen and carbon dioxide
styrene-methyl methacrylate copolymers. 35 refs. concentration) and three storage factors (temperature,
JAPAN illumination and storage time) on the amounts of volatile
Accession no.686392 compounds in the headspace of gas packages containing
two chicken legs were studied. Statistical experimental
design was applied and a linear screening design
Item 309 comprising 18 experiments (fractional factorial) was
Revista de Plasticos Modernos utilised. Volatile compounds in package headspace were
73, No.487, Jan.1997, p.26-31 determined by gas chromatography/mass spectrometry.
Spanish The results were compared with the results of sensory
TEMPERATURE MODULATED DIFFERENTIAL evaluation and microbial determinations. 8 refs.
SCANNING CALORIMETRY: A STEP FORWARD
FINLAND; SCANDINAVIA; WESTERN EUROPE
IN STUDYING THE THERMAL PROPERTIES
OF POLYMERS Accession no.686119
Perena J M
Instituto de Ciencia y Tecnologia de Polimeros Item 312
International Journal of Adhesion & Adhesives
The principles of temperature modulated DSC are
18, No.3, 1998, p.193-8
described, and a number of examples are presented of its
USE OF XPS AND TOF-SIMS TO INVESTIGATE
application to studies of the thermal properties of plastics.
ADHESION FAILURE OF A CATIONIC
Some limitations of the technique are also examined. 6
RADIATION CURED COATING ON
refs.
GALVANISED STEEL
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
WESTERN EUROPE
Leadley S R; Watts J F; Rodriguez A; Lowe C
Surrey,University; Becker Industrial Coatings
Accession no.686251
Details are given of coating delamination in a hot, humid
environment for a cationic radiation cured coating of
Item 310
cycloaliphatic epoxy resin. X-ray photoelectron
Analytical Chemistry
spectroscopy and time-of-flight mass spectroscopy of the
70, No.13, 1st July 1998, p.456A-61A
delaminated surface showed that the phosphorus
CHARACTERISING SYNTHETIC POLYMERS
hexafluoride anion of the photoinitiator segregates to the
BY MALDI MS
interface. The durability of the coating was improved by
Kuang Jen Wu; Odom R W
reformulation with a reduced concentration of
Evans C.,& Associates
photoinitiator. 7 refs.
An review is given of the use of matrix-assisted laser EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
desorption/ionisation time-of flight (MALDI TOF) mass WESTERN EUROPE
spectroscopy to determine MWDs and structures of Accession no.684932
synthetic organic polymers, including the ion desorption
mechanism, synthetic polymer analysis, molecular weight
Item 313
analysis, and its use in calibration of GPC profiles. 30
Antec ’98. Volume I. Conference proceedings.
refs.
Atlanta, Ga., 26th-30th April 1998, p.816-20. 012
USA
METHODS FOR THE MEASUREMENT OF
Accession no.686157 CRYSTALLINITY OF PREFORMS AND
BOTTLES MADE FROM PETP
Item 311 Bashir Z; Al-Alouish I; Al-Raqibah I; Ibrahim M
Food Additives and Contaminants SABIC Corp.

© Copyright 2002 Rapra Technology Limited 113


References and Abstracts

(SPE) focusing on the prediction of ESC and assessment by


testing, factors that influence ESC and data on specific
PETP has established itself as a material for making
plastics. Methods for the experimental evaluation of
lightweight, clear and tough bottles. Ideally, a preform
environmental stress are described. This book is
with zero or very low crystallinity (for purposes of clarity)
available for purchase from Publication Sales, Rapra
is sought, while the final bottle should have high
Technology Ltd.
crystallinity (for enhancing gas barrier and mechanical
properties). Monitoring crystallinity is thus important. An Accession no.683806
attempt is made to evaluate methods of crystallinity
measurement using density, differential scanning Item 316
calorimetry and modulated differential scanning Journal of Adhesion Science and Technology
calorimetry to study the crystallinity of preforms and 12, No.5, 1998, p.507-21
bottles. The applicability and appropriateness of each EFFECT OF CURING TEMPERATURE ON THE
technique for different PETP sample types, and ADHESION STRENGTH OF POLYAMIDEIMIDE/
interpretation problems are also discussed. 20 refs. COPPER JOINTS
SAUDI ARABIA Cho J H; Kong D I; Park C E; Jin M Y
Accession no.684627 Pohang,University of Science & Technology;
Korea,Research Institute of Chemical Technology
Item 314 The adhesion strength of polyamideimide/copper joints
Polymer Journal (Japan) was investigated as a function of the curing temperature
30, No.5, 1998, p.439-43 and time. The effects of copper oxide formed by thermal
DIRECT DETERMINATION OF MOLECULAR treatment and alkaline treatment on the adhesive strength
WEIGHT DISTRIBUTION BY SIZE EXCLUSION of the joints were examined. The locus of failure of the
CHROMATOGRAPHY(SEC) WITH 750 MHZ joints was also studied by SEM and X-ray photoelectron
PROTON NMR DETECTION (ON-LINE SEC- spectroscopy. 21 refs.
NMR) KOREA
Ute K; Niimi R; Hongo S; Hatada K Accession no.682955
Osaka,University
The above on-line SEC-NMR technique was used to Item 317
analyse MWDs of isotactic PMMAs with Mn ranging Polymer Engineering and Science
from 3270 to 22,200. The molec.wt. of the polymer in 38, No.4, April 1998, p.566-72
flowing eluate was determined directly (without a DYNAMIC AND ISOTHERMAL
conventional calibration procedure) from he relative THERMOGRAVIMETRIC ANALYSIS OF A
intensity of NMR signals due to the end group and POLYCYANURATE THERMOSETTING SYSTEM
repeating units. The MWD determined in this manner was Zacharia R E; Simon S L
proved to be accurate by SEC-NMR experiments on Pittsburgh,University
uniform isotactic PMMAs consisting of exactly 23, 40 Isothermal and dynamic thermogravimetric analysis
and 80 repeating units. Investigation was also undertaken (TGA) were performed on a polycyanurate thermosetting
to optimise flow rate and NMR parameters for quantitative material. The effects on thermal stability of the copper
SEC-NMR measurements. The signal-to-noise ratio of naphthenate catalyst were studied by comparing two
750 MHz SEC-NMR spectra was 9.2 times that obtained systems with different amounts of catalyst. Tests were
previously with 500 MHz SEC-NMR operated under performed isothermally at temperatures ranging from 200-
similar conditions. 17 refs. 240C for times up to one week. Dynamic tests were also
JAPAN performed at rates of 0.1 C/min to 40 C/min at
Accession no.684613 temperatures ranging from 180 to 600C. Results
demonstrate the difficulties of extrapolating dynamic TGA
data to use conditions to predict long-term thermal
Item 315
stability. 14 refs.
Shawbury, Rapra Technology Ltd., 1996, pp.150.
USA
95.00. 30cms. 9511
ENVIRONMENTAL STRESS CRACKING OF Accession no.681689
PLASTICS
Wright D C Item 318
Rapra Technology Ltd. European Polymer Journal
This book reviews the factors which influence 34, No.2, Feb.1998, p.163-70
environmental stress cracking, and examines the current STUDY OF TALC-ADDITIVE INTERACTIONS
state of knowledge regarding specific categories of BY COMBINED TGA-FTIR SYSTEM
plastics. The book is divided into three main sections Bertin D; Boutevin B; Rigal G; Fourty G

114 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Montpellier,Ecole Nationale Superieure de Chimie; composites. The interaction and chemical reaction of
Talcs de Luzenac SA functional groups in the matrix with functional groups at
the fibrer surface contribute to the adhesion. Direct
By using combined TGA/FTIR thermogravimetric
analysis of the fibre/matrix interface by surface analytical
analysis, accurate real time qualitative and quantitative
methods such as X-ray photoelectron spectroscopy is not
data can be obtained for thermal decomposition of
trivial due to the thickness of a matrix layer over fibres
polymers. It was used to study interactions between an
and the complexity of the matrix system. Indirect analysis
additive and a filler (talc), highlighting a degradation
of the matrix/fibre interface is possible using model
phenomenon of additive by talc, and this phenomenon
compounds which represent functional groups where
depended on the structure and chemical composition of
differences in results are indicative of reaction between
talc. This procedure also applied to analysis of degradation
fibre and matrix. The matrix functional groups that may
of other additives by talc. Thus, polymer formulations
chemically react with the fibre surface can be separated
will rapidly be optimised in various areas of filled
and investigated individually. Mixtures of model
polymers. 12 refs.
compounds can be used to investigate functional groups
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
WESTERN EUROPE
reactions between the components, and with the fibre
surface. Model compounds based on epoxy, polyimide,
Accession no.681630
polyphenylene sulphide and vinyl ester matrices are
investigated to characterise the chemical reactions at the
Item 319 fibre/matrix interface. XPS is used to characterise both
Journal of Polymer Science : Polymer Chemistry the carbon fibre surfaces and the reacted carbon fibre
Edition surfaces. The model compounds representative of each
36, No.9, 15th July 1998, p.1363-71 of these matrices demonstrate the range of possible
LIQUID CHROMATOGRAPHY OF reactions and interactions possible between the fibre and
MACROMOLECULES AT THE CRITICAL matrix, ranging from no reaction to distinct chemical
ADSORPTION POINT. II. ROLE OF COLUMN reactions. 4 refs.
PACKING: BARE SILICA GEL USA
Berek D; Janco M; Meira G R Accession no.681439
Slovak,Academy of Sciences; INTEC CONICET
Data are presented manifesting the role of column Item 321
packings from the point of view of both their pore size Cleanrooms
and surface chemistry. Bare silica gels that are the most 12, No.5, Suppl. May 1998, p.S13/20
commonly used LC CAP column packings and model APPLICATION OF FTIR FOR MONITORING
macromolecules, viz. narrow PMMA, were investigated. CLEANROOM AIR AND PROCESS EMISSIONS
20 refs. Zazzera L; Reagen W
ARGENTINA; SLOVAK REPUBLIC; SLOVAKIA 3M Co.
Accession no.681599
The use of FTIR monitoring methods for HAP, VOC, PFC
and HFC emissions for identification and quantification
Item 320 in process exhaust and in clean room air, is discussed. A
20th Annual Anniversary Meeting of the Adhesion summary is included of the various protocols, test methods
Society. Conference proceedings. and references for the use of FTIR spectroscopy to
Hilton Head Island, S.C., 23rd-26th Feb.1997, p.519- generate verifiable data. Results of field trials and
21. 8(10) laboratory study trials are presented, which demonstrate
USING XPS TO INVESTIGATE FIBRE/MATRIX its value as a monitoring method in the semiconductor
CHEMICAL INTERACTIONS AT THE industry
INTERFACE IN CARBON FIBRE REINFORCED USA
COMPOSITES Accession no.679498
Weitzsacker C L; Xie M; Drzal L T
Michigan,State University
Edited by: Drzal L T; Schreiber H P Item 322
(US,Adhesion Society) Analytical Chemistry
70, No.8, 15th April 1998, p.1563-8
With composites expanding into areas from aerospace to POLYMER ANALYSIS BY MICRO-SCALE SIZE-
recreation, different matrices are being investigated to EXCLUSION CHROMATOGRAPHY(SEC)/
tailor composites to specific uses. The degree of adhesion MALDI TIME-OF-FLIGHT MASS
between the fibre and matrix, influenced by chemical SPECTROMETRY WITH A ROBOTIC
reactions, mechanical interactions and topography at the INTERFACE
fibre/matrix interface, has been recognised as a critical Nielen M W F
factor in determining the performance of fibre-reinforced Akzo Nobel Central Research

© Copyright 2002 Rapra Technology Limited 115


References and Abstracts

A report is presented on the development of a micro-scale greatest improvement, while fine grades and talc had little
SEC system in which the MALDI matrix solution is effect. Micrographs revealed the level of interparticle
coaxially added to the column effluent and directly spotted contact and alignment of anisotropic particles which gave
onto the MALDI targets in a robotic interface. Each spot rise to the observed differences. Filler type and content
corresponds to the 10-s elution window from the micro- did not significantly influence shear rheology at the shear
SEC column, thus yielding a narrow polymer distribution rates associated with film extrusion. 17 refs.
which is amenable to characterisation by MALDI mass CANADA; EUROPEAN COMMUNITY; EUROPEAN UNION;
spectroscopy. The performance of the system is UK; USA; WESTERN EUROPE
demonstrated by the characterisation of a polybisphenol Accession no.677503
A carbonate and a complex dipropoxylated bisphenol A/
adipic acid/isophthalic acid copolyester resin. 29 refs. Item 325
EUROPEAN COMMUNITY; EUROPEAN UNION; TAPPI 1997 Polymers, Laminations and Coatings
NETHERLANDS; WESTERN EUROPE Conference. Conference Proceedings. Book 1.
Accession no.679150 Toronto, Ontario, 24th-28th Aug.1997, p.35-44. 012
EFFECT OF TITANIUM DIOXIDE ON
Item 323 EXTRUSION STABILITY
Polymer Engineering and Science Merkley J H
38, No.2, Feb.1998, p.265-73 Eastman Chemical Co.
DSC STUDIES ON THE CRYSTALLISATION (TAPPI)
CHARACTERISTICS OF POLY(ETHYLENE Rheological techniques for following the degradation and
TEREPHTHALATE) FOR BLOW MOULDING changes in molecular weight and MWD of titanium
APPLICATIONS dioxide-filled polyolefins during extrusion coating are
Daw-Ming Fann; Huang S K; Jiunn-Yih Lee examined. These include measurements of the crossover
Taiwan,National University of Science & Technology point between loss modulus and storage modulus and the
The crystallisation behaviour of blow moulded PETP variation in complex viscosity versus frequency curves
bottles, which helps determine the product’s transparency, seen in the rotational mechanical spectrometer curves,
was investigated by DSC dynamic cooling experiments variations in viscosity versus shear rate seen in the
that simulated the cooling that occurs in the injection blow capillary extrusion rheometer curves, and shifts in the
moulding manufacturing process. DSC measurements DMTA curves.
were used to obtain information on related aspects, such CANADA; USA
as the ease of crystallisation from glassy and molten states Accession no.677489
and crystallinity in the products. An Avrami equation was
used for calculation of the crystallisation kinetic Item 326
parameters. 40 refs. Journal of Polymer Science : Polymer Chemistry
TAIWAN Edition
Accession no.678858 36, No.5, 15th April 1998, p.851-60
PEROXIDE INDUCED CROSSLINKING AND
DEGRADATION OF PVC
Item 324
Yu Q; Zhu S; Zhou W
TAPPI 1997 Polymers, Laminations and Coatings
McMaster University
Conference. Conference Proceedings. Book 1.
Toronto, Ontario, 24th-28th Aug.1997, p.173-82. 012 Peroxide induced crosslinking and degradation of PVC
INFLUENCE OF MINERAL FILLERS ON THE were investigated using an on-line ESR technique. The
PROCESSING OF LLDPE FILMS reaction variables included temperature, peroxide type and
Ansari D M; Higgs R P concentration. The mechanism involved in the reaction
ECC International Ltd. was determined base on the radical information. The gel
(TAPPI) content and swelling ratio were also measured. 38 refs.
A study was made of the thermal properties and melt CANADA
rheology of linear LDPE masterbatches filled with Accession no.674965
calcium carbonate, talc and calcined clay. Films were
prepared by extrusion blowing and temperature changes Item 327
were monitored along the bubble. Filler distribution within Journal of Materials Science Letters
the films was assessed by optical and electron microscopy. 17, No.6, 15th March 1998, p.511-3
Rheological properties of the diluted masterbatches were EVIDENCE OF MOLECULAR ORIENTATION IN
evaluated over four decades of shear rate. The mineral POLY(3-BUTYLTHIOPHENE) FILMS BY
fillers increased cooling rates and improved bubble ELECTRON SPIN RESONANCE
stability. Coarser calcium carbonate grades gave the MEASUREMENTS

116 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Pawlicka A; Walmsley L; Faria R M; Nascimento O R SHEATH-CORE DIFFERENCES CAUSED BY


Sao Paulo,University; Paulista,Universidade Estadual RAPID THERMOOXIDATION DURING MELT
BLOWING OF FIBRES
It was demonstrated that ESR could show evidence of
Kelley S L; Shambaugh R L
molecular orientation in films of poly(3-butyl thiophene),
Oklahoma,University
making ESR useful to study orientation in conjugated
polymers when it is wished to avoid radiation damage or A technique based on intrinsic viscosity measurements
for a non-destructive investigation before X-ray was developed for measuring sheath and core molecular
measurements. 11 refs. weights during melt blowing of fibres. A mathematical
BRAZIL
model is described which accounts for rapid diffusion and
thermooxidation. Experimental molecular weight
Accession no.674766
measurements for PP fibres were compared with
theoretical predictions. 29 refs.
Item 328
USA
Macromolecules
30, No.25, 15th Dec.1997, p.7970-6 Accession no.670584
DSC, FT-IR, AND ENERGY DISPERSIVE X-RAY
DIFFRACTION APPLIED TO THE STUDY OF Item 331
THE GLASS TRANSITION OF POLY(P- Polymer Bulletin
PHENYLENE SULPHIDE) 40, No.2-3, Feb./March 1998, p.227-34
Caminiti R; D’Ilario L; Martinelli A; Piozzi A; Sadun C COMPATIBILISATION OF POLYSULPHONE/
Roma,Universita La Sapienza; Roma,Istituto Nazionale POLYAMIDE BLENDS BY REACTIVE
per la Fisica della Materia POLYSULPHONES. EVIDENCE FOR
COPOLYMER FORMATION
The glass transition of PPS was studied by means of DSC, Weber M; Heckmann W
FTIR spectroscopy and energy dispersive X-ray diffraction. BASF AG
All of the techniques showed the alpha-transition of the
Melt blending studies using polysulphone with different
polymer. The results of the different techniques were
functional groups and polyamide were performed in a batch
consistent if the onset temperature for the DSC experiments
type mixer. Blends were investigated by solvent extraction
was taken as representative of the glass transition. The glass
and TEM. Model experiments revealed the possibility to
transition temperature was found to vary as a function of
compatibilise these blends by reactive blending techniques
the heating rate. The activation energy of the glass transition using functionalised polysulphones. 14 refs.
process was calculated by means of a theoretical model.
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
The results were discussed. 47 refs. WESTERN EUROPE
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
Accession no.670478
WESTERN EUROPE
Accession no.672088
Item 332
Journal of Polymer Science : Polymer Physics Edition
Item 329 36, No.1, 15th Jan.1998, p.133-41
Kunststoffe Plast Europe NEW APPROACH FOR ESTIMATING THE
88, No.2, Feb.1998, p.34-5 RECRYSTALLISATION RATE AND
WHAT HAS GONE WRONG? EQUILIBRIUM MELTING TEMPERATURE
Sass A Hong Gyun Kim; Robertson R E
NRW GmbH Michigan,University
Practical case studies are used to demonstrate how useful A method was described for measuring the heat and rate
differential scanning microscopy analysis can be for of crystallisation following partial melting. The method
material testing and damage analysis on plastics and plastic uses a specific sequence of temperatures with a differential
parts. It measures the physical and chemical properties of scanning calorimeter, and the melting and recrystallisation
the plastic as a function of temperature. Information gained processes were confirmed by optical observations. The
by use of the analytical tool is examined, and case studies method was applied to poly(butylene terephthalate). The
relating to fluctuating material quality through the use of melting temperatures obtained from recrystallisation were
recyclate, and the oxidation of PP water pipes are discussed. used in the Hoffman-Weeks equation to deduce 236 C as
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; the equilibrium melting temperature for PBTP. 22 refs.
WESTERN EUROPE USA
Accession no.671875 Accession no.669994

Item 330 Item 333


Industrial & Engineering Chemistry Research Composites Science & Technology
37, No.3, March 1998, p.1140-53 57, No.8, Aug.1997, p.975-83

© Copyright 2002 Rapra Technology Limited 117


References and Abstracts

EFFECTS OF SILANE COUPLING AGENTS ON Rashidzadeh H; Baochuan Guo


THE INTERPHASE AND PERFORMANCE OF Cleveland,State University
GLASS-FIBRE REINFORCED POLYMER
Using PMMA samples, some of the causes of mass
COMPOSITES
discrimination encountered in the MALDI-TOF analysis
Wu H F; Dwight D W; Huff N T
of polydisperse polymers were investigated. It was found
Owens-Corning Science & Technology Center
that detector saturation could be a major instrumental
A single filament model of a commercial glass fibre- factor causing mass discrimination. This was due to the
reinforcement manufacturing process was used to apply strong signals of matrix-related ions and low-mass
methacryloxy and amino silanes with one, two and three oligomer ions. The matrix effect as another source of mass
silanols to two different glass fibres in a molecular model. discrimination was analysed quantitatively. 34 refs.
Surface analyses by angular-dependent X-ray USA
photoelectron spectroscopy, electric-kinetic analysis, and Accession no.666829
contact-angle measurements were used to characterise the
surface coatings. The micro-indentation technique was Item 336
used to evaluate fibre-matrix interfacial adhesion. Polymer
Changes observed in surface chemistry, micromechanics, 39, Nos.6-7, 1998, p.1439-43
and composite properties as functions of silanol type are TEMPERATURE MODULATED DSC STUDY OF
correlated. Data includes molecular models of coupling POLYETHYLENE TEREPHTHALATE
agent on E-glass surface, chemisorption of coupling agent CRYSTALLIZATION. II. APPLICABILITY TO
into glass surface, isoelectric point values for each NON-ISOTHERMAL PROCESS
treatment, composite flexural strength, composite TS, and Toda A; Tomita C; Hikosaka M; Saruyama Y
composite interfacial shear strength before and after 3- Hiroshima,University; Kyoto,Institute of Technology
days in boiling water. Matrix was polyester resin (E-701
from Owens Corning). 22 refs. (Presented at 6th Int. Conf. The non-isothermal crystallisation of PETP was examined
on Composite Interfaces, Microphenomena in Advanced by temp. modulated DSC(TMDSC). A new analytical
Interfaces, Zichron Yaacov, Israel, 5th-8th May 1996). model of TMDSC was applied to the process, taking
USA account of the response of exothermic heat flow to temp.
modulation in an apparent heat capacity of complex
Accession no.669950
quantity. By examining the frequency dependence of the
apparent heat capacity, the applicability was successfully
Item 334 examined for the non-isothermal process. The method was
Polymer Bulletin capable of determining the temp. dependence of crystal
39, No.6, Dec.1997, p.721-7 growth rate from TMDSC data analysis. The results were
COMPARISON OF CALIBRATION WITH PPG in good agreement with the dependence determined from
AND PS STANDARDS IN SIZE EXCLUSION literature values of spherulite growth rate measured by
CHROMATOGRAPHY MEASUREMENTS FOR optical microscopy. 12 refs.
CHARACTERISATION OF OLIGOLACTONE JAPAN
MACROMONOMERS Accession no.666765
Schoch M; Gopp U; Steurich S; Sandner B
Halle,Martin-Luther-Universitat
Item 337
The calibration of size exclusion chromatography Polymer Journal (Japan)
measurements for the determination of the molecular 29, No.11, 1997, p.910-3
weights of oligolactone macromonomers was carried out FRACTIONATION OF PEO STAR SAMPLES BY
using PPG and PS as standards. Results are compared SUPERCRITICAL FLUIDS
with those obtained by end-group analysis with proton Cansell F; Botella P; Six J-L; Garrabos Y; Tufeu R;
NMR14 refs. Gnanou Y
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; CNRS
WESTERN EUROPE
Details are given of the use of supercritical fluids for the
Accession no.669429 fractionation of PEO. The fractionation of a binary mixture
of star and linear chains of PEO was studied. 25 refs.
Item 335 EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
Analytical Chemistry WESTERN EUROPE
70, No.1, 1st Jan.1998, p.131-5 Accession no.666545
USE OF MALDI-TOF TO MEASURE
MOLECULAR WEIGHT DISTRIBUTIONS OF
Item 338
POLYDISPERSE POLYMETHYL
Polymer
METHACRYLATE
39, No.2, 1998, p.255-66

118 © Copyright 2002 Rapra Technology Limited


References and Abstracts

INVESTIGATION OF PHYSICAL AGEING IN 67, No.3, 18th Jan.1998, p.449-53


POLYMETHYLMETHACRYLATE USING COMPATIBILITY STUDY OF
POSITRON ANNIHILATION, DIELECTRIC POLYCARBONATE-POLYVINYL
RELAXATION AND DYNAMIC MECHANICAL PYRROLIDONE BLEND USING HIGH
THERMAL ANALYSIS RESOLUTION SOLID STATE NUCLEAR
Davis W J; Pethrick R A MAGNETIC RESONANCE
Strathclyde,University da Silva E P; Tavares M I B
Rio de Janeiro,Universidade Estadual do Norte
Physical ageing of PMMA was studied using positron
Fluminense; Rio de Janeiro,Universidade Federal
annihilation lifetime spectroscopy (PALS), dielectric
relaxation spectroscopy (DRS) and dynamic mechanical The combining NMR techniques in the solid state permit
thermal analysis (DMTA) and the results obtained from the evaluation of the polymeric systems homogeneity. In
these techniques were compared. A correlation existed polycarbonate-polyvinyl pyrrolidone blends, the response
between the free volume as measured by PALS and the of proton spin-lattice relaxation time in the rotating frame
changes which occurred in the DRS and DMTA data. It was the determinant to obtain information on the transition
was concluded that “thermorheologically simplicity” was when the quantity of polyvinyl pyrrolidone is close to 40
probably an oversimplification for this system and that wt% and a better organisation of amorphous phase was
physical ageing was associated with a redistribution, not detected. 13 refs.
just a shift, of molecular relaxation processes. The BRAZIL
relaxation distribution changed as the glass transition Accession no.665732
temperature was approached. The free volume distribution
probably changed during ageing, but it was not possible Item 341
to quantify these changes from the PALS study. 43 refs. Applied Spectroscopy
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; 51, No.12, Dec.1997, p.1823-5
WESTERN EUROPE INVESTIGATION OF CHEMICAL
Accession no.665913 INTERACTIONS AT THE STEEL/POLYMER
INTERFACE BY FT-IR DIFFUSE
Item 339 REFLECTANCE SPECTROSCOPY
Journal of Applied Polymer Science Bistac S; Vallat M F; Schultz J
67, No.3, 18th Jan.1998, p.487-500 Institut de Chimie des Surfaces et Interfaces
SURFACE ENERGY MAPPING OF KEVLAR
Interactions between a steel surface and an ethylene-vinyl
FIBRES BY INVERSE GAS
acetate copolymer grafted with maleic anhydride were
CHROMATOGRAPHY
investigated by FTIR diffuse reflectance spectroscopy.
Rebouillat S; Donnet J B; Guo H; Wang T K
The failed surfaces obtained after a mechanical separation
Du Pont (UK) Ltd.; Ecole Nationale Superieure de
of the polymer/steel assemblies were analysed. A two-
Chimie de Mulhouse
step mechanism was proposed: the opening of the
The surface energy characteristics of three Kevlar fibres anhydride cycle by a hydrolysis reaction, leading to the
were systematically studied using two inverse gas formation of a carboxylic diacid, followed by the reaction
chromatography (IGC) techniques, i.e. at an infinite probe of the acid with some oxidised metallic elements present
dilution and at a finite probe concentration, with the latter at the metal surface. This study underlines the contribution
allowing a unique mapping of the surface energy levels, of FTIR reflectance techniques to the understanding of
which complements greatly the more traditional adhesion mechanisms. 7 refs.
characterisation of the highest energy sites. The standard EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
thermodynamic parameters, such as the free energy and WESTERN EUROPE
the adsorption enthalpy and entropy, as well as the Accession no.665698
dispersive and the specific component of the fibre surface
energy, were determined from the retention behaviour at Item 342
zero coverage of selected molecules of various polarity. Applied Spectroscopy
Using the second IGC approach, i.e. at finite 51, No.12, Dec.1997, p.1784-90
concentration, the isotherms for the adsorption of n-octane DEPTH PROFILING STUDY OF EFFECT OF
and n-hexylamine on the three selected Kevlar fibres were ANNEALING TEMPERATURE ON POLYMER/
constructed by the one peak method. 29 refs. POLYMER INTERFACES IN LAMINATES
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; USING CONFOCAL RAMAN
WESTERN EUROPE MICROSPECTROSCOPY
Accession no.665736 Hajatdoost S; Olsthoorn M; Yarwood J
Sheffield,Hallam University; Utrecht,University
Item 340 The effect of annealing temperature on molecular
Journal of Applied Polymer Science interactions at the interface of polymer laminates was

© Copyright 2002 Rapra Technology Limited 119


References and Abstracts

reported. Depth profiling was carried out using confocal Item 345
Raman microspectroscopy to study polyacrylonitrile/ Applied Spectroscopy
polyvinyl alcohol and polyacrylonitrile/polyacrylic acid 51, No.11, Nov.1997, p.1668-77
laminates. The laminates were annealed at 65, 75 and 90C. RAPID-SCAN TWO-DIMENSIONAL FT-IR: AN
It was demonstrated that the degree of hydrogen bonding EFFICIENT APPROACH TO DYNAMIC
interaction between the nitrile and alcohol groups near INFRARED SPECTROSCOPY
the interfacial region changes between laminates annealed Steeman P A M
at different temperatures. For comparison, Raman DSM Research
mapping of a polyacrylonitrile-polyvinyl alcohol blend
A new and efficient mode of operation is presented that
was used to study the interactions between the polymers
involves a continuous rapid-scan FTIR spectrometer, the
in this (disordered) system. 29 refs.
measurement technique relying completely on the
EUROPEAN COMMUNITY; EUROPEAN UNION;
utilisation of the digital signal processor for data
NETHERLANDS; UK; WESTERN EUROPE
acquisition and manipulation. Experimental and
Accession no.665697 mathematical details were discussed. Application of the
rapid-scan technique was illustrated with some results for
Item 343 a styrene-acrylonitrile/butadiene copolymer. 17 refs.
Applied Spectroscopy EUROPEAN COMMUNITY; EUROPEAN UNION;
51, No.11, Nov.1997, p.1741-4 NETHERLANDS; WESTERN EUROPE
CHARACTERISATION OF DENTURE ACRYLIC Accession no.665692
RESIN SURFACES MODIFIED BY GLOW
DISCHARGES
Item 346
Suzer S; Ozden N; Akaltan F; Akovali G
Applied Spectroscopy
Bilkent,University; Ankara,University; Middle
51, No.11, Nov.1997, p.1593-6
East,Technical University
RAMAN IMAGING OF DENTAL ADHESIVE
Resin samples prepared by compression moulding using DIFFUSION
a PMMA denture base material were exposed to radio Wieliczka D M; Kruger M B; Spencer P
frequency glow discharges to improve the wettability of Missouri,University
the material. FTIR reflectance, X-ray photoelectron
Using micro-Raman spectroscopy, chemical and
spectroscopy and contact angle measurements were used
morphological information on the dentin/adhesive
to characterise the changes introduced by the glow
interface was collected with minimal sample preparation.
discharge plasma. 18 refs.
Results provided direct evidence of an adhesive
TURKEY
preparation and demineralisation depth for two adhesive
Accession no.665695 systems. 17 refs.
USA
Item 344 Accession no.665691
Applied Spectroscopy
51, No.11, Nov.1997, p.1736-40
Item 347
GENERALISED TWO-DIMENSIONAL FOURIER
Injection Molding
TRANSFORM INFRARED PHOTOACOUSTIC
5, No.12, Dec. 1997, p.44-5
SPECTRAL DEPTH-PROFILING ANALYSIS
MATERIALS ANALYST: PART 3. LOT-TO-LOT
Jiang E Y; McCarthy W J; Drapcho D L; Crocombe R
VARIATION
A
Sepe M
Bio-Rad Laboratories Inc.
Dickten & Masch Mfg.Co.
A new application of generalised two-dimensional
The use is examined of thermogravimetric analysis as an
correlation spectroscopy in photoacoustic depth-profiling
analytical tool for the diagnosis of part failure in injection
analysis. Both rapid-scan and step-scan photoacoustic
moulding. The consistent performance of an ethylene
spectroscopy (obtained by using the software-based
vinyl acetate copolymer was evaluated and the need to
digital signal processing technique) of multilayer samples
separate the component parts of the material to test for
were used to calculate generalised two-dimensional
the amount of vinyl acetate in the compound is discussed
correlation maps. Advantages of this unambiguous
in order to develop a thermal history. Once this history is
analysis method in enhancing spectral as well as depth
established, a customer can institute an incoming QC test
resolutions, over conventional two-dimensional
on the material’s composition rather than by adjusting
correlation and other spectral depth-profiling methods,
the process for each new lot and performing product
were discussed. 31 refs.
testing after the parts have been produced.
USA
USA
Accession no.665694
Accession no.664180

120 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Item 348 Item 351


Polymer Degradation and Stability Analytical Chemistry
57, No.3, 1997, p.313-24 69, No.23, 1st Dec.1997. p.4872-7
THERMOANALYTICAL STUDY OF THE SAMPLE PRECONCENTRATION USING ION-
EFFECT OF EAA AND STARCH ON THE EXCHANGE POLYMER FILM FOR LASER
THERMOOXIDATIVE DEGRADATION OF ABLATION SAMPLING INDUCTIVELY
LDPE COUPLED PLASMA ATOMIC EMISSION
Bikiaris D; Prinos J; Perrier C; Panayiotou C SPECTROMETRY
Thessaloniki,University Wing Tat Chan; Yip H H G
Hong Kong,University
The effect of ethylene-acrylic acid copolymer (EAA) and
plasticised starch (PLST) on the thermooxidative An efficient sample pretreatment/introduction technique
degradation of LDPE was examined. The course of for the inductively coupled plasma atomic emission
oxidation was followed using TGA to monitor the weight spectrometry (ICP-AES) using ion exchange for analyte
changes during heating and DSC to study the heat changes preconcentration and matrix separation and laser ablation
taking place during oxidation. Three types of blend were sampling for sample introduction was developed.
examined: LDPE-plasticised starch, LDPE-EAA and Ammonium pyrrolidone dithiocarbamate-PS films were
LDPE-starch-EAA blends. All blends contained cobalt coated on glass plates for analyte preconcentration. 32 refs.
stearate as prooxidant. 36 refs. HONG KONG
EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE; Accession no.662915
WESTERN EUROPE
Accession no.664073
Item 352
Pigment & Resin Technology
Item 349 26, No.6, 1997, p.370-7
Pitture e Vernici FTIR SPECTROSCOPY OF LAC RESIN AND ITS
73, No.17, 1997, p.38-43 DERIVATIVES
English; Italian Sarkar P C; Shrivastava A K
RELEASE OF VOLATILE DERIVATIVES FROM Indian Council of Agricultural Research; Ranchi
INITIATORS IN RADIATION CURING College
Visconti M; Cattaneo M; Li Bassi G
Lamberti SpA Fourier transform infrared spectroscopy was applied to
the study of lac resin, a complex natural resin of insect
Details are given of the development of a technique for origin, and some of its derivatives. The results obtained
the direct evaluation of volatile organic compounds during by this method are compared with those from earlier
the radiation curing process. This method was used to studies that used classical methods of chemical analysis.
evaluate the release of benzaldehyde from commercially Experiments include the preparation of hard and soft
available alpha-hydroxyketones during curing. 8 refs. resins, dewaxed lac, ammoniated lac, lac acetal,
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; halogenated lac, hydrolysed lac, rebuilt lac (rebulac), and
WESTERN EUROPE the preparation of lac metal salts. It is found that FTIR
Accession no.663242 has several advantages over classical methods, but that
FTIR data requires supplementing by other instrumental
Item 350 techniques such as FT-Raman spectroscopy and solid state
Iranian Journal of Polymer Science & Technology nuclear magnetic resonance. 21 refs.
10, No.2, Summer 1997, p.35-46 INDIA
Persian Accession no.662758
APPLICATIONS OF HIGH-RESOLUTION
SOLID-STATE CARBON 13 NMR Item 353
SPECTROSCOPY TO POLYMERS Journal of Vinyl and Additive Technology
Farahmand F G; Morshedian J 3, No.3, Sept.1997, p.249-55
Iran,Polymer Research Centre PRACTICAL GUIDE TO THE IDENTIFICATION
A brief review is given of the theory and applications of OF MONOMERIC PLASTICIZERS IN
carbon 13 NMR to polymer analysis. Mention is made of FLEXIBLE PVC COMPOUNDS
conformational analysis, polymer reactions in solid state, Kozlowski R R; Gallagher T K
analysis of crosslinked systems, homogeneity of polymeric Aristech Chemical
blends, analysis of surface species, and variable temperature The performance of a flexible PVC compound is often
carbon 13 NMR solid state spectroscopy. 37 refs. defined by its plasticiser content and composition and a
IRAN simple, accurate and fast method of plasticiser
Accession no.663219 identification could, therefore, be an effective quality

© Copyright 2002 Rapra Technology Limited 121


References and Abstracts

control and benchmark performance test in new product MEASUREMENT OF POLYDISPERSE


development studies. Gas chromatography was shown to POLYMERS FROM THEIR MATRIX-ASSISTED
provide the most effective identification method and it LASER DESORPTION/IONISATION TIME-OF-
was demonstrated that it could be complemented by IR FLIGHT MASS SPECTRA
spectroscopy, liquid chromatography and physical Vitalini D; Mineo P; Scamporrino E
observations to confirm identity. 4 refs. Istituto per la Chimica e la Tecnol.dei Mat.Pol.;
USA Catania,Universita
Accession no.661993 A recently reported off-line procedure to estimate
molecular weight averages and MWD index, also for
Item 354 polydisperse polymers, directly from their matrix-assisted
Macromolecules laser desorption/ionisation time-of-flight mass spectra
30, No.21, 20th Oct.1997, p.6674-6 (MALDI-TOF) was applied to poly(bisphenol A-
HIGH-RESOLUTION CALORIMETRY STUDY carbonate), a poly(ether-sulphone resin) and
OF THE ORDER-DISORDER TRANSITION IN A poly(dimethylphenylene oxide), all having a wide
DIBLOCK COPOLYMER MELT polydispersity index. The molecular weight and MWD
Voronov V P; Buleiko V M; Podneks V E; Hamley I W; obtained values were compared with those determined
Fairclough J P A; Ryan A J; Mai S M; Liao B X; Booth C by GPC or supplied by makers. A structural
Russian Academy of Sciences; Leeds,University; characterisation of these polymers was also performed
UMIST; Manchester,University by examining their MALDI-TOF mass spectra. 29 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
A new method is reported for locating the order-disorder WESTERN EUROPE
transition in a diblock copolymer, namely high-resolution
Accession no.657168
calorimetry, and the result compared with determinations
by small-angle X-ray spectroscopy and rheology. 13 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; RUSSIA; UK; Item 357
WESTERN EUROPE Injection Molding
Accession no.658801 5, No.10, Oct. 1997, p.60/2
MATERIALS ANALYST: PART 2. BRITTLE PPO
Item 355 Sepe M
Polymer Science Series A Dickten & Masch Mfg.
39, No.8, Aug.1997, p.953-7 The use is described of differential scanning spectroscopy
STUDY OF SOLUBLE POLYAMIC ACIDS AND (DSC) as an analytical tool in the diagnosis of part failure.
POLYESTER IMIDES BY METHODS OF Degradation of the polymer during processing is
EXCLUSION LIQUID CHROMATOGRAPHY examined, and the example is investigated of a 30% glass
Nesterov V V; Kudrysvtsev V V; Svetlichnyi V M; reinforced PPO which showed brittleness and for which
Gazdina N V; Bel’nikevich N G; Kurenbin O I; the causes of failure were revealed by means of DSC
Zhukova T I analysis.
St.Petersburg,Institute of Macromol.Compounds USA

The molecular and conformation characteristics of a series Accession no.655661


of polyamic acids and polyester imides, obtained by high-
temp. imidisation of polyamic acids in N- Item 358
methylpyrrolidinone or m-cresol, were studied by Macromolecular Symposia
viscometry and exclusion liquid chromatography. The Vol.119, July 1997, p.317-24
differences in the molec.wts. of the products of polyamic CHEMICAL ANALYSIS OF POLYMERS USING
acid imidisation in N-methylpyrrolidinone and m-cresol TRANSMISSION ELECTRON MICROSCOPY/
were explained by the different characters of inactivation ELECTRON ENERGY-LOSS SPECTROSCOPY:
of the anhydride groups. 20 refs. (Full translation of THE EXAMPLE OF POLY(ETHYLENE
Vys.Soed.A, 39, No.8, 1997, p.1387-91) TEREPHTHALATE)
RUSSIA Varlot K; Martin J M; Quet C; Kihn Y
Accession no.658622 Lyon,Ecole Centrale; CEMES-LOE
Electron energy-loss spectroscopy analysis of PETP was
Item 356 performed in the analytical TEM to evaluate the
Macromolecules possibility of chemical analysis of the polymer at sub-
30, No.18, 8th Sept.1997, p.5285-9 micrometre scale. Due to irradiation damage, it was
FURTHER APPLICATION OF A PROCEDURE necessary to work at the lowest possible electron dose,
FOR MOLECULAR WEIGHT AND and with the specimen cooled to liquid nitrogen
MOLECULAR WEIGHT DISTRIBUTION temperature. In the acquired spectra, an identification of

122 © Copyright 2002 Rapra Technology Limited


References and Abstracts

the different chemical bondings in agreement with X-ray OF POLYETHYLENE AND N-ALKANES
absorption near-edge spectroscopy experiments is Parker S F
proposed. 14 refs. Rutherford Appleton Laboratory
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
High quality inelastic neutron scattering (INS) spectra of
WESTERN EUROPE
randomly oriented polycrystalline PE, polydeutero-
Accession no.653745
polyethylene and highly oriented polyethylene are
presented and a number of new features described. 9 refs.
Item 359 EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Macromolecular Symposia WESTERN EUROPE
Vol.119, July 1997, p.309-15 Accession no.653736
CARBON-13, MAGNESIUM-25 AND BORON-11
SOLID STATE NMR STUDY OF A FIRE
Item 362
RETARDED ETHYLENE-VINYL ACETATE
Macromolecular Symposia
COPOLYMER
Vol.119, July 1997, p.157-64
Pecoul N; Bourbigot S; Revel B
INFRARED ABSORPTION SPECTRA OF
Ecole Nationale Superieure de Chimie de Lille; Centre
POLYMERS FROM CLASSICAL MOLECULAR
Commun de Mesures RMN
SIMULATION
Flame retardance of ethylene-vinyl acetate copolymer can Soldera A; Dognon J P
be achieved using magnesium hydroxide incorporated in CEA/Le Ripault
the polymeric matrix. The adduct of a small amount of
A method is proposed to predict the IR spectra of
zinc borate as synergistic agent in the formulation
amorphous polymers. Based on classical molecular
increases the fire-proofing properties. Multinuclei solid-
state NMR appears as a means to characterise materials simulation and Kramers-Kronig relations, it allows the
before and after combustion. It was shown that computations of absorption and transmittance spectra of
endothermic dehydration, water vapour evolved and polymer films in near and middle infra-red domains with
formation of a glassy coating provided the flame good agreement with experimental data. 22 refs.
retardancy of interest to the polymer matrix. 12 refs. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
WESTERN EUROPE
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
WESTERN EUROPE Accession no.653730
Accession no.653744
Item 363
Item 360 Macromolecular Symposia
Macromolecular Symposia Vol.119, July 1997, p.79-87
Vol.119, July 1997, p.269-76 CREEP RATE SPECTROSCOPY USING A LASER
QUANTITATIVE ATR-FTIR SPECTROSCOPY AT INTERFEROMETER AS ULTRA-HIGH
POLYMER SURFACES: SORPTION AND RESOLUTION TECHNIQUE FOR STUDY OF
MOLECULAR CONFORMATION RELAXATIONS
Mueller M; Schmitt F J Peschanskaya N N; Yakushev P N; Sinani A B;
Dresden,Institute of Polymer Research Bershtein V A
Russian Academy of Sciences
Adsorption and diffusion phenomena at or within polymer
systems were investigated by surface sensitive ATR-FTIR An original laser interferometry creep rate spectroscopy
spectroscopy. For a systematic description, a study was (CRS) method was developed and used as the low-
made of (1) the competitive adsorption and desorption frequency and high-resolution technique for studying
behaviour of proteins on polymer surfaces, (2) swelling microplasticity and relaxations in different materials
of hydrophilic polymers by water molecules, which can including brittle ones. New possibilities for CRS for
be accompanied by conformational changes, and (3) polymers are demonstrated. 13 refs.
induced orientational changes of hydrophobically RUSSIA
modified polypeptides by apolar solvents. 10 refs. Accession no.653722
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
WESTERN EUROPE
Item 364
Accession no.653740 Macromolecular Symposia
Vol.119, July 1997, p.49-63
Item 361 POTENTIAL OF TWO-DIMENSIONAL NEAR-
Macromolecular Symposia INFRARED CORRELATION SPECTROSCOPY
Vol.119, July 1997, p.227-34 IN STUDIES OF PRE-MELTING BEHAVIOUR OF
INELASTIC NEUTRON SCATTERING STUDIES NYLON 12

© Copyright 2002 Rapra Technology Limited 123


References and Abstracts

Ozaki Y; Yongliang Liu; Noda I g PE; and 0.125 mg dioctadecyl-beta,beta’-thiodipropionate


Kwansei-Gakuin,University; Procter & Gamble Co. (Irganox PS 802) /1 g PE. 23 refs.
AUSTRIA; WESTERN EUROPE
This review paper discusses the potential of generalised
two-dimensional near-infrared correlation spectroscopy Accession no.653220
in studies of pre-melting behaviour and hydrogen bonds
of nylon 12. A study on dissociation and hydrogen bonds Item 367
of N-methylacetamide is also reviewed as a model Macromolecular Symposia
compound study of nylon 12. FTIR spectra were measured Vol.118, June 1997, p.383-8
over a temperature range of 30-150C where gradual FREE VOLUME STUDIES IN MISCIBLE
weakening of inter- or intramolecular associative POLYMER BLEND SYSTEMS
interactions and decrease of local order leading to the Campbell J A; Goodwin A A; Ardi M S; Simon G P;
eventual fusion of nylon 12 crystals are observed. 24 refs. Landry-Coltrain C J T
JAPAN; USA Monash,University; Eastman Kodak Co.
Accession no.653720
A brief review is presented of the published literature
relating to the use of positron annihilation lifetime
Item 365 spectroscopy in studying the effects of miscibility on the
Macromolecular Symposia free volume of miscible, amorphous polymer blends.
Vol.119, July 1997, p.25-48 Studies of a fully miscible polyvinyl phenol/PVAC blend,
UNDERSTANDING POLYMERS BY a partially miscible polyphenyl methacrylate/
VIBRATIONAL SPECTROSCOPY: SOME polycarbonate blend and a largely immiscible PS/PVAC
RECENT ADVANCES IN THEORY AND blend are reported. The results indicate that miscible
EXPERIMENT blends tend to show a negative deviation of free volume
Meier R J size, and to a lesser degree free volume fraction, on mixing
DSM Research due to the intimacy of packing of the blend component
A rapid scan version of two-dimensional spectroscopy is macromolecules. The largely immiscible blend shows
introduced and applied to study the phases of an positive deviation of free volume size which is ascribed
acrylonitrile-butadiene-styrene polymer system. Some to additional free volume at the interface. 13 refs.
recent advances in the application of computational AUSTRALIA; USA
chemistry to the evaluation of vibrational spectra are Accession no.652994
presented. Some specific applications are discussed. 31 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION;
NETHERLANDS; WESTERN EUROPE Item 368
Journal of Polymer Science : Polymer Chemistry
Accession no.653719
Edition
35, No.12, 15th Sept.1997, p.2431-9
Item 366 ESR STUDY ON CHEMICAL CROSSLINKING
International Journal of Polymer Analysis and REACTION MECHANISMS OF PE USING A
Characterization CHEMICAL AGENT. II. EFFECT OF PHENOLIC
3, No.4, 1997, p.369-79 ANTIOXIDANTS
HPLC QUANTIFICATION OF THIOETHER Yamazaki T; Seguchi T
ANTIOXIDANTS IN POLYETHYLENE AFTER Hitachi Cable Ltd.; Japan,Atomic Energy Research
DISSOLUTION OF POLYMER UNDER Institute
PRESSURE IN ALIPHATIC SOLVENT
The effect of antioxidant on the reaction mechanism of
Macko T; Furtner B; Lederer K
chemical crosslinking of PE with dicumyl peroxide at high
Leoben,Montan-Universitat
temperatures was investigated by ESR. The antioxidant
A new method is described for the quantitative reacted with the alkyl radicals in PE formed by the thermal
determination of some sulphur-containing antioxidants in decomposition of dicumyl peroxide above 120C and
PE. The polymer matrix is dissolved in hot n-heptane/ disturbed the crosslinking. 10 refs.
isopropyl alcohol, 97/3 v/v at 160 deg.C under elevated JAPAN
pressure (0.33 MPa) and precipitated by cooling. The Accession no.652659
solution is injected directly into a normal-phase silica gel
column flushed with the same solvent as used for the
dissolution of the polymer. This method gives high recovery Item 369
of the antioxidants, good repeatability of the analysis and Applied Spectroscopy
a low detection limit of 0.011 mg 4,4'-thiobis(3-methyl-6- 51, No.8, Aug.1997, p.1176-8
tert-butylphenol) (Santonox R) /1 g PE; 0.074 mg QUANTITATION OF POLYETHYLENE GLYCOL
ditetradecyl-beta,beta’-thiodipropionate (Chimox 14) / 1 CONCENTRATION USING RAMAN

124 © Copyright 2002 Rapra Technology Limited


References and Abstracts

SPECTROSCOPY industry is explored with a view to the quantification of


Melendez Y; Schrum K F; Ben-Amotz D finishing oils in acrylic fibres by partial least-squares
Purdue,University; Maryville College regression, using a rotary cuvette system for recording
spectra. Calibration is performed with a set of samples
Raman spectroscopy is used to quantitate the amount of
that encompasses every source of variability, and the
polymer in solution, in particular polyethylene glycol
wavelength region where absorption is mostly due to the
dissolved in chloroform. For various chain lengths and
oil is used to construct several models from which that
polymer weight fraction ranges, it is shown that the ratios
leading to the minimum relative standard error for a
of peak intensifies in the C-H stretching region may be
sample test set is selected. The results provided by various
used to quantitate polymer weight fraction with about 1%
mathematical treatments used to minimise scattering
uncertainty. For low polymer weight fraction ranges (0-
resulting from the differential linear density of the samples
10%), the relationship between Raman intensity and
reveal no significant differences between prediction
polymer weight fraction is essentially linear, while at
errors. The model is used to quantify levels of finishing
higher ranges (0-50%) the intensity follows a nonlinear
oil in routinely manufactured samples for a period of six
function derived from basic concentration relationships
months, during which time two batches show poor
and indicates a universal scaling with polymer chain
predictions due to a new component appearing in the
length. 10 refs.
product. Modification of the calibration model to account
USA
for this component substantially increases robustness and
Accession no.652414 allows the accurate quantification of all batches
manufactured after the model is developed. 28 refs.
Item 370 EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
Polymer WESTERN EUROPE
38, No.17, 1997, p.4381-5 Accession no.651451
SEPARATION AND IDENTIFICATION OF
ETHYLENE-PROPYLENE BLOCK Item 372
COPOLYMER Analyst
Junting Xu; Linxian Feng; Shilin Yang; Yinan Wu; 122, No.9, Sept.1997, p.101R-15R
Yiqing Yang; Xiangming Kong ANALYTICAL EXTRACTION OF ADDITIVES
Zhejiang,University; Shanghai,Research Institute of FROM POLYMERS
Petrochemical Technology Vandenberg H J; Clifford A A; Bartle K D; Carroll J;
A commercial impact resistant PP alloy was fractionated Newton I; Garden L M; Dean J R; Costley C T
using the temperature rising elution fractionation Leeds,University; ICI; Newcastle,University of
technique and several ethylene-propylene block Northumbria
copolymers with different ethylene contents were Plastics contain many other small molecules as well as
obtained. The block structure of the fractions was the polymer itself. These include additives to alter the
identified by combining the fractionation results with polymer properties or prolong the life of the polymer,
carbon-13 NMR spectroscopy and DSC results. Some such as plasticisers, antioxidants and UV light absorbers.
transition segments were found between PE and PP There may also be processing aids, residual monomers,
segments in the block copolymers. With increasing elution
low molecular weight oligomers and inadvertent
temperature, the number and kind of transition segments
contaminants present. It is important for the manufacturer
decreased, together with the length and melting
and regulators to know the level of these materials in the
temperature of the PE segment in the block copolymer
polymer to ensure the product is fit for its intended
fractions. 18 refs.
purpose. Food contact plastics are regulated by maximum
CHINA
concentrations allowable in the plastic, which applies to
Accession no.651909 residual monomers and processing aids as well as
additives. There are some methods for determining
Item 371 concentrations of additives without extraction from the
Analyst polymer, such as nuclear magnetic resonance
122, No.8, Aug.1997, p.777-81 spectrometry, UV spectrometry and UV desorption-mass
DETERMINATION OF FINISHING OILS IN spectrometry. However, in order to determine the levels
ACRYLIC FIBRES BY NEAR-INFRARED in the polymer, it is usually necessary to extract the
REFLECTANCE SPECTROMETRY compounds quantitatively from the plastic before analysis.
Blanco M; Coello J; Fraga J M G; Iturriaga H; A review is presented of the available extraction
Maspoch S; Pages J techniques. 102 refs.
Barcelona,Universidad Autonoma EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
The potential of near-infrared diffuse reflectance
spectrometry for quality control analyses in the textile Accession no.651430

© Copyright 2002 Rapra Technology Limited 125


References and Abstracts

Item 373 chromatography, is described. Fine and reproducible


Analytical Chemistry control of interaction between polymer chains and the
69, No.16, 15th Aug.1997, p.3304-13 alkyl chain bonded silica packing material can be achieved
QUANTITATIVE ANALYSIS OF PESTICIDES IN by varying the column temperature. The method can be
POST-CONSUMER RECYCLED PLASTICS used to characterise binary polymer mixtures, where one
USING OFF-LINE SUPERCRITICAL FLUID component is separated by the size exclusion mechanism
EXTRACTION(SFE)/GAS and the other is simultaneously separated by the
CHROMATOGRAPHY-ECD interaction mechanism in a single isocratic elution. The
Nerin C; Batlle R; Cacho J application of this technique to the characterisation of PS
Zaragoza,University and PS/PMMA mixtures is examined. 12 refs.
KOREA
The SFE of several organochlorine and organophosphorus
pesticides and two metabolites from recycled plastics was Accession no.649987
studied. The recycled plastics, used as agricultural soil covers,
were a mixture of LDPE and EVA. The SFE was optimised Item 376
and compared with the classical sonication and total Macromolecules
dissolution extraction methods. The plastic was extracted 30, No.13, 30th June 1997, p.3781-7
with supercritical carbon dioxide under different extraction CHARACTERISATION OF POLYESTERS BY
conditions, depending on the physical matrix characteristics. MATRIX-ASSISTED LASER DESORPTION
Average recoveries of the eleven chemicals studied ranged IONISATION MASS SPECTROMETRY
from values greater than 90% with an overall relative Williams J B; Gusev A I; Hercules D M
standard deviation of 4.3% for plastics films to values lower Pittsburgh,University
than 40% with an overall standard deviation of 7.2% for A series of aliphatic polyesters, characterised by
plastics pellets. The variables affecting the whole extraction asymmetric oligomer distributions, heteroterminated linear
process and the results obtained in the comparison between chains, and cyclic oligomers, were studied using MALDI.
the three extraction methods are discussed. 45 refs. Structural characterisation results were compared with
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; those from fast atom bombardment mass spectrometry,
WESTERN EUROPE
electrospray ionisation mass spectrometry, NMR and end-
Accession no.650545 group titration. MALDI molecular weight determination
was contrasted with those from GPC and NMR. 23 refs.
Item 374 USA
European Polymer Journal Accession no.649761
33, No.7, July 1997, p.1135-42
FOURIER TRANSFORM INFRARED Item 377
SPECTROSCOPY APPLIED TO THE STUDY OF Shawbury, Rapra Technology Ltd., 1997, pp.120. 12
PVC DECOMPOSITION ins. 15/4/97. Rapra Review Rept. No.95, vol.8, No. 11
Beltran M; Marcilla A 1997,
Alicante,Universidad THERMAL ANALYSIS OF POLYMERS
The process of PVC decomposition was studied by FTIR Sepe M P
under dynamic conditions. The IR spectra were directly Dickten & Masch Mfg.Co.
obtained from PVC films pyrolysed in-situ in a specially Edited by: Dolbey R
designed infra red cell. A qualitative description of the (Rapra Technology Ltd.)
changes observed in the spectra was presented. 35 refs. Rapra Review Report No.95
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; A review is presented of the techniques involved in the
WESTERN EUROPE thermal analysis of polymers. Techniques discussed
Accession no.650382 include differential scanning calorimetry, differential
photocalorimetry, thermogravimetric analysis,
Item 375 thermomechanical analysis, dynamic mechanical analysis,
Macromolecular Symposia dielectric, thermally stimulated current/relaxation map
Vol.118, June 1997, p.261-5 analysis analysis, and thermal conductivity analysis. 381
HIGH PERFORMANCE LIQUID refs.
CHROMATOGRAPHY CHARACTERIZATION EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
OF MACROMOLECULES
Chang T; Lee H C; Lee W Accession no.647258
Pohang,University of Science & Technology
Item 378
A new chromatographic method for polymer molecular Journal of Applied Polymer Science
weight characterisation, temperature gradient interaction 65, No.3, 18th July 1997, p.595-600

126 © Copyright 2002 Rapra Technology Limited


References and Abstracts

MOLECULAR WEIGHT OF POLYETHYLENE interpretation methods were applied to the data. The wide
GLYCOLS BY VAPOR PRESSURE temperature range used in this work (45-580C)
OSMOMETRY: AN ALTERNATIVE DATA encompassed a change in the decomposition mechanism
TREATMENT and this greatly limited the utility of the methods. To
Sabadini E; Assano E M; Atvars T D Z accommodate this mechanism change, the data were
Campinas,Universidade Estadual treated as a pseudo-first order reaction. The lower
activation energy occurring at lower degradation
The number-average molec.wt. of some polyethylene
temperatures was attributed to scission of the ‘weak links’
glycols was analysed using vapour pressure osmometry.
in the polymer. The higher activation energy was similar
This technique generally worked with a plot of the
to the carbon-carbon dissociation energy and was
difference in electrical resistance/concentration versus
associated with random scission throughout the polymer.
concentration and the molec.wt. was determined by the
47 refs.
calibration constant obtained from the curve intercept. It
CANADA
was demonstrated that this method induced a high
dispersion of the data, which could be minimised using a Accession no.645116
plot of difference in electrical resistance versus
concentration.. More precise values of molec.wt. could Item 381
thus be obtained and the number-average molec.wt. of Polymer Degradation and Stability
several polyethylene glycols could be directly obtained 57, No.2, 1997, p.113-25
from the ratio between the curve slopes obtained for a THERMAL DEGRADATION KINETICS OF
standard and the polymer sample. 10 refs. POLYPROPYLENE. I. MOLECULAR WEIGHT
BRAZIL DISTRIBUTION
Accession no.645677 Chan J H; Balke S T
Toronto,University
Item 379 A kinetic model for the thermal degradation of PP was
Speciality Chemicals developed and fitted to MWD data obtained by high
17, No.5, June/July 1997, p.165/70 temperature size exclusion chromatography. In a series
MAKING LIQUID CHROMATOGRAPHY MORE of ampoule experiments, reaction temperatures of 275-
ACCESSIBLE 315C were examined with reaction times of up to 48 h. A
Kuehler T C; Sellen M; Lavold T; Batt J; Langridge J; single-parameter version of the model, containing an
Raso R; Rontree J A apparent rate constant, was found to provide excellent
Astra Hassle AB; Micromass AB; Micromass UK Ltd. fits of all MWDs. Values of the parameter varied with
Until recently, mass spectrometry was regarded as a highly both temperature and reaction time. 35 refs.
sophisticated technique requiring careful use of the CANADA
instrument by a sole operator, and demanding meticulous Accession no.645114
sample preparation by the chemist. However, moves
towards open-access, chemist-operated systems have been
Item 382
reported on mass spectrometers equipped with a variety
Analytical Chemistry
of ionisation modes. The reliability and robustness of
69, No.13, 1st July 1997, p.2485-95
atmospheric pressure ionisation, the ease and speed of
MASS SPECTROMETRIC INVERSE GAS
source tuning, the fact that it is unnecessary to optimise
CHROMATOGRAPHY: INVESTIGATION OF
the source conditions for each sample individually and
POLYMERIC PHASE TRANSITIONS
the reproducibility of results have made API techniques
Panda S; Bu Q; Huang B; Edwards R R; Liao Q; Yun K
the ionisation methods of choice. Details are given. 5 refs.
S; Parcher J F
EUROPEAN COMMUNITY; EUROPEAN UNION;
SCANDINAVIA; SWEDEN; UK; WESTERN EUROPE Mississippi,University
Accession no.645281 An improved inverse gas chromatographic method
involving the use of a mass-specific detector for
Item 380 determination of the Tg of polymeric materials is
Polymer Degradation and Stability described. This new method allows the use of several
57, No.2, 1997, p.135-49 probe solutes simultaneously with an automated, closed-
THERMAL DEGRADATION KINETICS OF loop injector and stepped temperature programming. The
POLYPROPYLENE. III. result is a single continuous chromatogram for each probe
THERMOGRAVIMETRIC ANALYSIS solute over a range of temperatures encompassing the Tg.
Chan J H; Balke S T Several different methods for the exact determination of
Toronto,University Tg from the chromatogram were investigated. Two new
methods were also proposed for the evaluation of Tg from
Thermogravimetric data were obtained for the pyrolysis
either the temperature dependence of the second moments
of polypropylene, and several previously published

© Copyright 2002 Rapra Technology Limited 127


References and Abstracts

of the elution peaks for probe solutes or simple inspection When coupled with an automated mapping stage, it can
of the variation of elution peak height (width) with offer unique evaluation capabilities. A number of
temperature. 51 refs. applications of FTIR spectroscopy mapping to the vinyl
USA siding industry are described. Examples focus on
Accession no.645093 determining, in single sample mapping experiments, the
compositional changes associated with capstock to
substrate transition and evaluating the degradation species
Item 383 and level observed during weathering exposure
Analytical Chemistry throughout the thickness of the siding panel. 4 refs.
69, No.12, 15th June 1997, p.15R-28R
USA
COATINGS
Anderson D G Accession no.639927
Witco Corp.
Item 386
A review is presented of analytical techniques applicable
Antec 97. Volume II. Conference proceedings.
to the examination of coatings, raw materials and
Toronto, 27th April-2nd May 1997, p.2310-4. 012
substrates since 1995. The most highly referenced areas
QUANTITATIVE ANALYSIS OF LDPE/LLDPE
were found to be IR spectroscopy, NMR, HPLC, thermal
BLEND USING DSC AND FTIR METHODS
analysis and gas chromatography. 704 refs.
Prasad A; Mowery D
USA
Quantum Chemical Co.
Accession no.640310 (SPE)
A blend of LDPE and LLDPE is widely used for blown
Item 384 film applications. For quality control an accurate and rapid
Polymer Bulletin method is required to identify the type and composition
38, No.6, June 1997, p.681-8 of alpha-olefin in an LDPE/LLDPE blend. A rapid,
SEPARATION OF BLOCK COPOLYMERS FROM accurate and new test method is developed which utilises
PARENT HOMOPOLYMERS BY MEANS OF DSC and FTIR techniques. The melting point of LDPE
LIQUID CHROMATOGRAPHY AT THE varies with density and usually is in the range of 106 deg.C
CRITICAL ADSORPTION POINT to 112 deg.C for film grade resins. The DSC thermogram
Janco M; Berek D; Onen A; Fischer C H; Yagci Y; of LLDPE is characterised by a broad range of melting
Schnabel W with a lower melting peak around 106 deg.C to 110 deg.C
Slovak Academy of Sciences; Istanbul,Technical and a higher one in the range of 120 deg.C to 124 deg.C.
University; Hahn-Meitner-Institut Berlin GmbH In the blend with LDPE, the ratio of the two endothermic
The principle underlying the above method is described peak heights changes. At a given weight percent of LDPE,
and results of its application to block copolymers this ratio depends on the type of LLDPE. The separate
consisting of methyl methacrylate and tetrahydrofuran calibrations for butene-1, hexene-1, and octene-1 LLDPEs
blocks are presented and discussed. The technique is are developed to quantify the blend composition from
shown to be suitable for characterisation of block DSC thermograms provided the alpha-olefin type is
copolymers with regard to the presence of homopolymer identified by a rapid method such as FTIR. 17 refs.
and multiblock (triblock) fractions. 5 refs. USA
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; Accession no.638387
SLOVAK REPUBLIC; SLOVAKIA; TURKEY; WESTERN
EUROPE
Accession no.640169 Item 387
Shawbury, Rapra Technology Ltd., 1992, pp.112. 12ins.
30/6/97. Rapra Review Rept. No.61, Vol.6, No.1, 1992.
Item 385 FOOD CONTACT POLYMERIC MATERIALS
Antec 97. Volume III. Conference proceedings. Sidwell J
Toronto,27th April-2nd May 1997,p.3588-92. 012 Rapra Technology Ltd.
FOURIER TRANSFORM INFRARED MICRO Edited by: Dolbey R
SPECTROSCOPY MAPPING. APPLICATIONS (Rapra Technology Ltd.)
TO VINYL SIDING INDUSTRY Rapra Review Report No.61
Garcia D; Black J
Elf Atochem North America Inc. A review is presented of the current and proposed
(SPE) European legislation on materials in contact with food,
as well as the latest technological advances. With
Fourier transform IR (FTIR) spectroscopy is a powerful reference to legislation, details are given of EC directives
analytical technique capable of yielding high quality issued, their implementation, FDA regulations, recycling
information with a spacial resolution as low as 10 microns. and waste management legislation. Technical

128 © Copyright 2002 Rapra Technology Limited


References and Abstracts

developments in food contact materials cover barrier 5, No.3, March 1997, p.97-102
polymers in multilayer packaging films, migration of CHARACTERISATION OF POLYMER BLENDS
species from food contact materials, and methods of BY INVERSE GAS CHROMATOGRAPHY
analysis of multilayer food contact materials. 485 refs. Al-Saigh Z Y
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; Ohio,State University
WESTERN EUROPE
A brief review is presented of the use of inverse gas
Accession no.637749 chromatography to characterise polymer blends.
Comparisons between data from inverse gas
Item 388 chromatography and DSC are discussed. 23 refs.
Polymer
USA
38, No.12, 1997, p.3035-43
CHARACTERIZATION OF POLYETHYLENE Accession no.632110
TEREPHTHALATE AND POLYETHYLENE
TEREPHTHALATE BLENDS Item 391
Fox B; Moad G; van Diepen G; Willing I; Cook W D Polymer News
CSIRO,Div.of Chemicals & Polymers; 22, No.1, Jan.1997, p.15
Monash,University POLYMER ANALYSIS AND
CHARACTERISATION. SOLID STATE NMR: IS
A method was developed for direct determination of the
IT BECOME TRULY POPULAR?
molec.wt. of the PETP component in PETP/ABS blends
Garbassi F
by GPC. The technique was used to demonstrate that an
EniChem SpA
observed deterioration in the mechanical properties, e.g.
Izod impact strength, of PETP/ABS blends on processing A very brief review is presented of specific areas where
could be correlated with a decrease in the molec.wt. of solid state NMR can contribute to polymer analysis.
the PETP component. Various methods for evaluating the Mention is made of polymer morphology, interactions,
molec.wt. and the chemical microstructure of PETP were dynamics and polymer reactions. 10 refs.
examined. The use of NMR spectroscopy as a means of EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
quantitatively identifying end groups and comonomers WESTERN EUROPE
that were present at the 1-4% level in commercial PETP Accession no.632071
was critically evaluated with reference to the stability of
PETP and PETP end groups in various NMR solvents.
Item 392
New proton NMR chemical shift assignments for
Analytical Chemistry
cyclohexanedimethanol units are presented and the
69, No.4, 15th Feb.1997, p.618-22
reactivity of hydroxy end groups in trifluoroacetic acid
COMPOSITION AND MICROSTRUCTURE
mixtures is examined. 34 refs.
ANALYSIS OF CHLORINATED
AUSTRALIA
POLYETHYLENE BY PYROLYSIS GAS
Accession no.636573 CHROMATOGRAPHY AND PYROLYSIS GAS
CHROMATOGRAPHY/MASS SPECTROMETRY
Item 389 Cheng-Yu Wang F; Smith P B
Polymer Testing Dow Chemical Co.
16, No.2, 1997, p.193-8 A pyrolysis gas chromatography method was developed
NMR CARBON-13 HIGH RESOLUTION STUDY to determine the composition and microstructure of
OF POLY(ETHYLENE-CO-VINYL ACETATE) chlorinated PE (CPE). The method used specific aromatic
Stael G C; Tavares M I B compounds which were formed through
CCT/UENF dehydrochlorination of trimers after pyrolysis of CPE
EVA was analysed by carbon-13 high-resolution using polymers at elevated temperatures. The composition and
NMR employing solution and solid state techniques. The microstructure calculation was based on the difference
analyses of this copolymer by solution NMR permitted between the levels of ethylene and vinyl chloride trimers
the copolymer composition to be obtained, and using formed. The composition of CPE polymers used in this
solid-state NMR, a study of molecular mobility was study was corroborated with carbon-13 NMR results and
carried out. Both studies were made to correlate the the manufacturers product specification. 23 refs.
structure and properties. 9 refs. USA
BRAZIL Accession no.629089
Accession no.634101
Item 393
Item 390 Biomaterials
Trends in Polymer Science 18, No.5, March 1997, p.415-9

© Copyright 2002 Rapra Technology Limited 129


References and Abstracts

DETECTION OF PEROXY SPECIES IN ULTRA- compared for THF/carbon dioxide and other common liquid
HIGH MOLECULAR WEIGHT mixtures. As enhanced-fluid liquids were highly
POLYETHYLENE BY RAMAN SPECTROSCOPY compressible, it was possible to reach the critical condition
Chenery D H by changing the pressure of the THF/carbon dioxide
Smith & Nephew Group Research Centre mixture. Approaching the critical condition by pressure
variation was compared with that possible with temp.
Samples of gamma-sterilised UHMWPE were examined
changes. Pressure variation was a more accurate and
using infra-red and Raman spectroscopies. The purpose
reproducible means of reaching the critical condition than
of this study was to detect the peroxy intermediates by
temp. variation. Finally, THF/carbon dioxide mixtures were
the novel use of Raman spectroscopy to confirm that
used as mobile phases at the critical condition for PS to
oxidation proceeded by this mechanism. 16 refs.
characterise styrene-methyl acrylate copolymers. 25 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE USA

Accession no.625483 Accession no.620015

Item 396
Item 394 Shawbury, Rapra Technology Ltd., 1995, pp.108. 12ins.
Polymer 18/7/95. Rapra Review Rept. Vol.7, No.11, 1995,
38, No.1, 1997, p.1-7 MOLECULAR WEIGHT CHARACTERISATION
MODULATED DIFFERENTIAL SCANNING OF SYNTHETIC POLYMERS
CALORIMETRY: 6. THERMAL Holding S R; Meeham E
CHARACTERISATION OF MULTICOMPONENT Rapra Technology Ltd.; Polymer Laboratories Ltd.
POLYMERS AND INTERFACES Edited by: Dolbey R
Hourston D J; Song M; Hammiche A; Pollock H M; (Rapra Technology Ltd.)
Reading M Rapra Review Report No. 83
Loughborough,University of Technology;
Lancaster,University; ICI Paints Techniques are examined for the determination of the
molecular weight distribution and molecular weight averages
A quantitative thermal method, based on the differential of synthetic polymers. The use is discussed of gel permeation
of heat capacity signal from modulated temperature chromatography in combination with other techniques such
differential scanning calorimetry, was described for as light scattering and viscometry to provide information
determining the weight fraction of interface and the extent about the molec.wt. of a polymer and potentially significant
of phase separation in polymer materials. The interface information on the composition of copolymers and blends.
was modelled as discrete fractions, each with its own The use of solution viscosity is also examined as a valuable
characteristic increment of heat capacity. The materials quality control technique. 411 refs.
used to demonstrate the range of the method were PS
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
blended with poly(phenylene oxide) (PPO), pure PS, pure WESTERN EUROPE
PPO, a styrene-isoprene-styrene triblock copolymer (SIS),
Accession no.556661
SIS blended with PPO, PMMA/poly(vinyl acetate) blends
and PVC sandwiched with poly(n-butyl acrylate). Two-
Item 397
phase and four-phase systems were used. The calculated
Analytical Chemistry
results agreed well with experimental results for two- and
60,No.9,1st May 1988,p.932-7
four-phase systems. 20 refs.
IDENTIFICATION OF DYES IN SOLID
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
POLYMETHYL METHACRYLATE BY MEANS
OF LASER DESORPTION FOURIER
Accession no.621625
TRANSFORM ION CYCLOTRON RESONANCE
MASS SPECTROMETRY
Item 395 Hsu A T;Marshall A G
Analytical Chemistry OHIO STATE,UNIVERSITY
69, No.1, 1st Jan.1997, p.66-71
It is demonstrated that the above technique can detect and
LIQUID CHROMATOGRAPHY AT THE
identify (by chemical formulae) dyes in solid PMMA
CRITICAL CONDITION USING ENHANCED-
commercial plastics at concentrations at least on order of
FLUIDITY LIQUID MOBILE PHASES
magnitude lower (0.1% vs 1-2wt%) than those obtained
Souvignet I; Olesik S V
by the best currently-available alternative method (ATR
Ohio,State University
Fourier transform IR spectrometry). Both untreated and
The use of enhanced-fluidity liquid mixtures of THF and redissolved PMMA can be characterised, in the presence
carbon dioxide for liquid chromatography at the critical and absence of up to three dyes in a single sample. 44 refs.
condition was examined. For PS polymers, the molec.wt. USA
range that could be analysed at the critical condition was Accession no.357996

130 © Copyright 2002 Rapra Technology Limited


References and Abstracts

Item 398 processing aids are presented. Over 1300 IR spectra and
Oxford, Pergamon Press Ltd., 1984, pp.ix,445. 60 UV spectra are included. The functions and
LS.24.50. 9ins. 2copies. 12/7/85. Analytical Chemistry compositions as well as the physical and chemical
Vol.8. 91T methods of identification of the following materials are
ANALYSIS OF PLASTICS discussed: plasticisers, fillers, pigments, antioxidants, UV
Crompton T R stabilisers, optical brighteners, antistatic agents,
biostabilisers, flame retardants, lubricants, accelerators,
This book covers all aspects of the analysis of plastics by
hardeners and blowing agents. 608 refs.
chemical and physical methods. It is divided into eight
chapters which each deal with a particular polymer or Accession no.211056
group of polymers:- polyolefins, polypropylene, higher
alkene polymers, styrene polymers, chlorine-containing Item 400
polymers, methacrylates, polybutadienes, polyesters and Members Rept.49 Shawbury, 1980, pp.12. 12ins.
polyethers. The techniques discussed include 2copies. 26/6/80. 91T
spectroscopy, chromatography, fractionation,, X-ray HIGH PERFORMANCE LIQUID
diffraction, autoradiography, DTA, TGA and DSC. CHROMATOGRAPHY - ANALYTICAL
UK APPLICATIONS IN THE RUBBER AND
Accession no.280400 PLASTICS INDUSTRIES
Sidwell J A
Rubber & Plastics Research Assn.of Gt.Britain
Item 399
RUBBER & PLASTICS RA.MEMBERS REPT.049
Weinheim, Verlag Chemie GmbH, 1981, pp.XV,687.
12ins. 22/3/82. R.ROOM. 91T This report details some of the high-performance liquid
ATLAS OF POLYMER AND PLASTICS chromatography work carried out at RAPRA and reviews
ANALYSIS. VOL.3....ADDITIVES AND reported in the literature. 11 refs.
PROCESSING AIDS: SPECTRA AND METHODS RUBBER & PLASTICS RESEARCH ASSN.OF
OF IDENTIFICATION. 2ND REV.EDN. GT.BRITAIN
Scholl F Accession no.154074
The spectroscopic and chromatographic data that are
required for the identification of plastics additives and

© Copyright 2002 Rapra Technology Limited 131


References and Abstracts

132 © Copyright 2002 Rapra Technology Limited


Subject Index

Subject Index
A ALKYD RESIN, 237 BAND STRUCTURE, 262
ALPHA TRANSITION, 245 290 BARIUM SULPHATE, 40
ABS, 160 164 207 225 345 365 388 328 BARRIER PROPERTIES, 56 57 86
398 ALUMINIUM, 126 168 179 223 266 94 168 387
ABSORPTION, 56 226 297 306 374 ALUMINIUM HYDROXIDE, 211 BENZENE, 382
382 ALUMINIUM OXIDE, 6 BETA RELAXATION, 325
ABSORPTION SPECTRA, 274 AMINE, 36 48 130 151 161 178 272 BIAXIALLY ORIENTED, 104
ABSORPTION SPECTROSCOPY, AMMONIUM PYRROLIDONE BIOCOMPATIBLE, 42
358 362 DITHIOCARBAMATE, 351 BIODEGRADABLE, 37 112 267
ACCELERATOR, 399 AMMONIUM SALT, 258 387
ACCURACY, 131 AMORPHOUS, 14 54 74 78 99 117 BIODETERIORATION, 5 37 112
ACETIC ACID, 76 266 141 170 207 213 274 283 340 246 267 387
ACETONE, 185 224 266 311 362 367 BIOMATERIAL, 42 46 246 262
ACETONITRILE, 21 266 ANISOTROPY, 13 256 324 BIOMEDICAL APPLICATION,
ACID, 277 288 ANNEALING, 24 54 74 101 135 262
ACOUSTIC MICROSCOPY, 126 136 277 308 338 342 BIREFRINGENCE, 257 284
ACRYLATE, 269 ANTI-STICK AGENT, 6 BISPENTAMETHYLPIPERIDYL
ACRYLIC, 199 ANTIMONY, 95 SEBACATE, 66
ACRYLIC ACID COPOLYMER, ANTIOXIDANT, 65 86 93 107 132 BISPHENOL A, 200 222 272 356
172 217 348 171 183 195 286 288 366 368 BISPHENOL A COPOLYMER,
ACRYLIC POLYMER, 33 172 255 372 387 399 189
299 314 335 371 384 397 ANTISTATIC AGENT, 399 BISPHENOL A DIGLYCIDYL
ACRYLIC-MELAMINE RESIN, 44 AQUEOUS, 46 198 223 232 ETHER, 178
175 ARAMID FIBRE, 281 BISPHENOL A EPOXY RESIN,
ACRYLONITRILE, 119 AROMA, 56 57 11
ACRYLONITRILE COPOLYMER, AROMATIC, 48 125 192 278 288 BISPHENOL A
57 299 392 POLYCARBONATE, 4 29 78
ACRYLONITRILE-STYRENE ATMOSPHERIC PRESSURE, 50 135 159 322 367
COPOLYMER, 72 110 220 345 206 222 BISPHENOL DIGLYCIDYL
ACTIVATION ENERGIES, 49 75 ATOMIC ABSORPTION ETHER, 178
146 169 280 288 317 328 380 SPECTROSCOPY, 177 BLEND, 11 12 15 25 47 58 60 63
381 ATOMIC EMISSION 64 69 72 77 91 98 107 110 112
ADDITIVE, 29 36 71 89 99 107 108 SPECTROSCOPY, 95 177 218 125 137 139 146 147 151 156
112 124 128 132 151 161 171 273 351 186 188 193 209 213 220 228
178 181 199 201 206 225 226 ATOMIC FORCE MICROSCOPY, 234 246 309 331 340 347 348
250 272 288 289 302 306 318 30 38 44 58 59 62 108 115 118 363 367 375 377 386 388 390
324 325 353 366 372 377 387 142 145 154 167 179 191 219 391 394
391 397 399 277 BLOCK COPOLYMER, 127 193
ADHESION, 32 61 62 145 157 167 ATTENUATED TOTAL 274 354 370 384 394
176 202 223 231 236 237 247 REFLECTANCE BLOW MOULDING, 313 323
249 312 316 341 346 SPECTROSCOPY, 43 61 69 126 BLOWING AGENT, 302 399
ADHESIVE, 9 20 62 167 168 179 257 262 301 360 BLOWN FILM, 324 386
272 346 AUGER ELECTRON BODY ARMOUR, 281
ADSORPTION, 46 56 65 93 103 SPECTROSCOPY, 13 BOILING POINT, 120 185 266
178 203 210 221 241 285 319 AUTOMATION, 46 50 212 278 382 BONDING, 32 168 202
339 360 384 AUTOMOTIVE APPLICATION, 44 BONDING AGENT, 168 179
ADSORPTION 56 62 67 175 202 212 236 329 BONNET, 329
CHROMATOGRAPHY, 105 210 AUTOOXIDATION, 169 BOTTLE, 57 131 212 266 313 323
AEROPLANE, 36 62 121 BOUND WATER, 51
AFFINITY CHROMATOGRAPHY, BOUNDARY LAYER, 81
50 97
B BRANCHING, 18 35 60 102 200
AGEING, 66 80 86 88 112 148 152 BACKSCATTERED ELECTRON 216
274 288 298 309 338 377 IMAGING, 289 BRITTLE, 41 62 271 289 357 363
ALCOHOL, 56 235 288 BAG, 266 BROMINE CONTAINING
ALCOHOLYSIS, 39 BAGASSE, 100 COPOLYMER, 273

© Copyright 2002 Rapra Technology Limited 133


Subject Index

BUCKET, 67 CHEMICAL COMPOSITION, 25 CLOUD POINT, 12 98 125


BUILDING APPLICATION, 7 385 72 80 89 103 107 146 159 172 COATED FIBRE, 179
BULK MOULDING 197 198 211 213 229 232 289 COATED METAL, 157 227
COMPOUND, 202 318 COATING, 19 27 44 62 66 121 126
BUMPER, 67 CHEMICAL FORCE 138 163 168 174 175 185 217
BUTYL ACRYLATE MICROSCOPY, 58 222 223 227 236 237 239 255
COPOLYMER, 28 198 CHEMICAL IONISATION MASS 259 266 298 312 325 359 383
BUTYL METHACRYLATE SPECTROSCOPY, 222 COBALT STEARATE, 348
COPOLYMER, 166 190 CHEMICAL REAGENT, 53 334 COHESION, 94 145 167
BUTYLENE COPOLYMER, 102 CHEMICAL RECYCLING, 39 COLOUR, 274 288
113 CHEMICAL RESISTANCE, 57 COLOURANT, 181
175 COLUMN CHROMATOGRAPHY,
CHEMICAL STRUCTURE, 1 8 12 233 375
C 16 25 31 47 49 51 53 56 66 68 COLUMN PACKING, 50 203 235
CALCINED CLAY, 324 73 77 83 89 93 98 102 103 114 241 319 375
CALCIUM CARBONATE, 65 211 130 133 140 152 158 159 164 COMBUSTION, 359
289 324 166 168 180 200 222 228 229 COMPATIBILITY, 63 90 209 331
CALCULATION, 8 14 77 98 114 243 264 268 269 274 275 277 340
149 162 172 190 227 276 277 283 284 286 291 300 301 308 COMPLEX VISCOSITY, 325
285 290 310 323 328 330 337 310 317 318 328 331 334 337 COMPOSITE, 10 13 17 36 62 79
344 362 382 390 392 394 355 356 364 365 368 370 376 81 82 90 100 134 141 176 178
CALIBRATION, 6 47 173 190 208 382 391 179 182 196 197 199 202 211
216 229 238 270 297 309 310 CHEMILUMINESCENCE, 88 231 234 258 265 271 281 288
319 334 378 392 CHEMOMETRIC ANALYSIS, 140 289 296 318 320 333 339 357
CALORIMETRY, 9 61 64 65 74 88 216 377
133 150 154 186 290 302 305 CHINA CLAY, 226 306 COMPOSITION, 72 73 100 122
313 354 359 CHITIN, 246 123 130 220 241 243 389 392
CAPILLARY CHLORINATED 394
ELECTROPHORESIS, 46 50 POLYETHYLENE, 146 392 COMPUTER AIDED ANALYSIS,
97 CHLORINE, 17 194 373 46 67 108 173 174 214 309
CAPILLARY GAS CHLORODIFLUOROETHANE, COMPUTER MODEL, 144 152
CHROMATOGRAPHY, 76 337 174 338
CAPILLARY RHEOMETRY, 324 CHLOROFORM, 3 208 369 382 COMPUTER SIMULATION, 248
325 CHROMATOGRAPHIC 367
CAR, 56 67 ANALYSIS, 66 81 86 89 96 97 CONCENTRATION, 55 102 105
CARBON 13, 130 193 209 265 105 112 119 137 141 152 171 129 130 183 197 215 224 250
268 297 359 370 389 392 191 194 229 235 303 304 366 262 283 300 311 317 339 353
CARBON BLACK, 40 93 375 382 384 378
CARBON DIOXIDE, 57 298 301 CHROMATOGRAPHY, 3 21 25 28 CONE CALORIMETER, 150 359
311 373 395 29 30 34 35 39 40 46 50 52 53 CONFOCAL RAMAN
CARBON DISULPHIDE, 311 55 56 60 66 71 72 75 80 81 84 MICROSPECTROSCOPY, 168
CARBON FIBRE-REINFORCED 86 87 89 96 97 102 103 105 342
PLASTIC, 36 178 182 196 231 107 108 112 113 114 116 119 CONFORMATIONAL
320 120 124 128 137 141 152 158 ANALYSIS, 360
CARBONYL GROUP, 274 288 159 160 166 169 171 172 174 CONTACT ANGLE, 37 61 202
CARBOXYLIC ACID, 288 341 183 185 186 190 191 194 195 217 277 333 343
CASTING, 94 262 367 200 203 204 206 208 210 218 CONTACT LENS, 265
CELLULAR MATERIAL, 80 84 222 229 233 235 239 240 241 CONTAINER, 57 266 278
85 97 302 242 243 259 264 273 278 285 CONTAMINATION, 17 128 160
CELLULOSE, 43 82 263 295 299 303 304 307 310 311 181 289 357
CELLULOSE ACETATE, 79 314 319 322 325 334 349 353 COOLING, 57 67 139 309 323 324
CELLULOSE NITRATE, 46 79 355 356 366 372 373 375 376 358
185 379 381 382 383 384 388 395 COOLING RATE, 57 126 207 309
CEMENT, 276 398 399 323 324
CHAIN LENGTH, 272 274 CHROMIC ACID, 61 COPOLYESTER, 204 322
CHAIN SCISSION, 274 380 CHROMOGEN, 16 288 COPOLYETHERSULPHONE, 47
CHAR, 194 CLAY, 324 COPOLYMER COMPOSITION,
CHEMICAL BONDING, 358 CLEARCOAT, 27 44 175 28 57 70 94 198 210 220 370

134 © Copyright 2002 Rapra Technology Limited


Subject Index

COPPER, 61 316 317 DEFECT, 67 88 126 289 329 INTERFERENCE


CORONA TREATMENT, 205 DEFORMATION, 41 59 67 249 MICROSCOPY, 324
CORRELATION 277 283 DIFFERENTIAL
SPECTROSCOPY, 344 364 DEGRADABLE, 37 112 267 387 PHOTOCALORIMETRY, 377
CORROSION, 255 271 DEGRADATION, 4 16 39 44 58 DIFFERENTIAL SCANNING
CREEP RATE SPECTROSCOPY, 65 66 80 85 86 87 88 92 94 101 CALORIMETRY, 2 6 7 8 10 11
363 112 119 135 148 152 164 175 12 15 17 18 20 22 24 29 36 41
CRESOL, 355 183 189 194 195 213 228 244 51 54 56 63 64 65 74 77 78 83
CRITICAL CONCENTRATION, 258 266 267 274 279 288 294 85 88 94 95 98 101 110 113 114
241 298 302 309 311 318 325 326 122 125 126 131 133 134 135
CRITICAL POINT, 103 395 330 338 347 357 374 377 380 136 139 144 146 147 149 154
CRITICAL SOLUTION 385 155 161 163 164 170 186 187
TEMPERATURE, 125 DEGRADATION PRODUCT, 4 17 207 211 213 220 245 246 252
CROSS-POLARISATION, 193 209 34 75 87 112 128 152 175 183 253 254 258 261 267 269 276
268 300 194 274 279 288 277 280 282 287 290 291 296
CROSSLINK, 83 279 DEGRADATION 302 305 309 313 323 324 328
CROSSLINK DENSITY, 179 269 TEMPERATURE, 194 269 380 329 332 336 348 357 367 370
CROSSLINKED, 110 179 221 250 DEGREE OF BRANCHING, 18 35 377 382 386 387 390 394 398
CROSSLINKING, 9 10 20 24 27 DEGREE OF CROSSLINKING, 9 DIFFERENTIAL THERMAL
36 46 48 49 73 85 115 134 161 27 300 377 ANALYSIS, 2 6 7 8 10 12 15
180 187 265 272 279 288 294 DEGREE OF CRYSTALLINITY, 17 18 20 22 24 29 36 41 54 56
300 309 326 368 377 143 313 63 64 65 74 77 78 83 88 94 95
CROSSLINKING AGENT, 222 DEGREE OF CURE, 10 36 269 98 101 110 113 114 122 125
288 DEHYDROCHLORINATION, 146 126 131 133 134 136 139 144
CRYSTALLINE, 2 59 143 147 283 392 146 147 149 154 155 161 163
313 DELAMINATION, 255 312 164 170 186 187 207 211 213
CRYSTALLINITY, 2 13 24 42 54 DENSITY, 18 52 56 106 131 168 231 245 246 252 253 254 258
57 62 63 64 69 94 102 113 114 179 216 231 261 289 313 367 267 269 276 277 280 287 290
117 122 126 131 139 143 147 DENTAL APPLICATION, 172 247 291 296 302 309 313 323 324
168 257 260 274 277 281 291 276 343 346 328 329 332 336 348 357 367
309 313 323 357 364 367 377 DEPOLYMERISATION, 39 165 370 377 382 386 387 390 398
391 266 DIFFUSE REFLECTANCE
CRYSTALLISATION, 2 9 12 13 DEPTH PROFILING, 205 333 342 SPECTROSCOPY, 341
22 24 26 52 54 57 59 74 78 107 344 DIFFUSION, 9 56 80 99 124 125
117 122 131 136 139 147 148 DERIVATIVE 264 274 346 351 360 372 387
155 170 246 261 295 309 323 THERMOGRAVIMETRY, 380 394
329 332 336 386 DESORPTION, 71 93 104 210 310 DIFFUSION COEFFICIENT, 56
CRYSTALLISATION 360 99 111 224
TEMPERATURE, 136 309 DETECTION LIMIT, 56 174 289 DIGITAL ANALYSIS, 10
CRYSTALLITE, 57 139 260 DIACID, 288 341 DIGLYCIDYL ETHER
CURE TEMPERATURE, 2 48 161 DIBUTYL PHTHALATE, 76 BISPHENOL A, 200
CURE TIME, 36 265 309 DIBUTYL SEBACATE, 277 DIMETHYL FORMAMIDE, 21 77
CUREMETER, 134 DICHLOROXYLENE, 48 DIMETHYL ISOPHTHALATE,
CURING, 8 20 27 36 68 73 83 89 DICHROISM, 284 208
138 144 149 161 163 178 182 DICUMYL PEROXIDE, 368 DIMETHYL SULPHOXIDE, 342
187 247 248 265 269 272 300 DICYANATE POLYMER, 11 DIMETHYL TEREPHTHALATE,
305 309 312 316 349 377 DIELECTRIC ANALYSIS, 9 377 39 208
CURING AGENT, 36 151 161 178 DIELECTRIC CONSTANT, 46 DIPHENYLMETHANE
182 222 250 272 288 317 237 338 DIISOCYANATE, 9
CYCLOHEXANE, 21 263 285 DIELECTRIC PROPERTIES, 46 DISCOLOURATION, 288
245 338 DISPERSION, 181 217 289 361
DIELECTRIC RELAXATION DISTILLED WATER, 56
D SPECTROSCOPY, 49 110 259 DISTORTION, 20 260
DATA ANALYSIS, 13 216 237 267 338 DISTRIBUTION, 60 102 338
291 319 DIELECTROMETRY, 9 DOMESTIC APPLIANCE, 80
DATA COLLECTION, 291 345 DIETHYLENE GLYCOL, 26 121 DOUGH MOULDING
DEBONDING, 236 266 COMPOUND, 211
DECANE, 382 DIFFERENTIAL DRAW RATIO, 117 257 283 284

© Copyright 2002 Rapra Technology Limited 135


Subject Index

DRINKING WATER, 183 307 ELECTRONIC APPLICATION, 5 ETHYLENE GLYCOL, 39 266


DUCTILE FAILURE, 289 ELECTROPHORESIS, 46 50 97 ETHYLENE-HEXENE
DYE, 16 397 ELECTROSPRAY IONISATION, COPOLYMER, 52
DYNAMIC, 71 144 317 323 374 190 222 229 376 ETHYLENE-PROPYLENE
DYNAMIC DIFFERENTIAL ELEMENTAL ANALYSIS, 15 115 COPOLYMER, 69 274 370
SCANNING CALORIMETRY, 160 194 351 ETHYLENE TEREPHTHALATE
11 ELUENT, 203 235 375 COPOLYMER, 131
DYNAMIC INFRARED ELUTION, 35 46 203 210 266 285 ETHYLENE-VINYL ACETATE
SPECTROSCOPY, 345 370 375 382 COPOLYMER, 57 70 100 209
DYNAMIC LIGHT ELUTION CHROMATOGRAPHY, 226 251 270 306 341 347 359
SCATTERING, 111 50 373 389
DYNAMIC MECHANICAL ELUTION FRACTIONATION, 52 ETHYLENE-VINYL ALCOHOL
ANALYSIS, 36 56 73 83 92 ELUTION VOLUME, 35 285 310 COPOLYMER, 56 57 94 291
114 134 161 196 245 269 309 356 387
377 EMISSION, 56 87 174 321 ETHYLIDENE VINYL
DYNAMIC MECHANICAL END GROUP, 36 102 130 151 229 PYRROLIDONE, 250
THERMAL ANALYSIS, 325 274 314 EVANESCENT WAVE
338 367 END-GROUP ANALYSIS, 190 SPECTROSCOPY, 111 292
DYNAMIC PROPERTIES, 179 200 334 376 388 EXCLUSION
317 325 ENDOTHERM, 54 56 74 78 94 CHROMATOGRAPHY, 28 29
DYNAMIC SPECTROSCOPY, 125 136 139 34 35 40 41 50 52 55 60 97 102
345 ENDOTHERMIC, 235 245 276 103 108 112 114 116 158 166
DYNAMIC VISCOELASTIC 309 329 359 204 210 229 239 240 243 299
PROPERTIES, 101 ENERGY ABSORPTION, 207 314 322 334 355 375 381
ENERGY CONTENT, 357 EXOTHERM, 85 323
ENERGY DISPERSIVE X-RAY EXOTHERMIC, 54 276 309 329
E ANALYSIS, 108 129 289 328 336
ELECTRICAL CONDUCTIVITY, ENGINEERING APPLICATION, EXTENDER, 121
38 309 367 EXTRACTION, 71 97 128 171 185
ELECTRICAL INSULATOR, 271 ENTHALPY, 36 64 74 125 179 187 195 266 331 372 373
ELECTRICAL PROPERTIES, 38 276 282 309 339 354 375 EXTRACTION
46 338 378 ENTROPY, 339 375 CHROMATOGRAPHY, 97
ELECTROCHEMICAL ENVIRONMENTAL SCANNING EXTRUSION, 6 7 40 70 72 183
IMPEDANCE ELECTRON MICROSCOPY, 188 195 225 254 266 324 325
SPECTROSCOPY, 5 223 227 324
ENVIRONMENTAL STRESS
237 255
CRACKING, 315
F
ELECTRODIALYSIS, 97
ELECTROKINETIC EPICHLOROHYDRIN, 272 FADING, 288
CHROMATOGRAPHY, 46 EPOXY NOVOLAC RESIN, 11 FAILURE, 17 30 36 167 178 182
ELECTROKINETIC EPOXY RESIN, 10 11 20 32 36 47 254 271 289 296 341 347 357
POTENTIAL, 333 62 68 144 145 149 151 157 161 FAILURE ANALYSIS, 36 108 145
ELECTRON DISPERSIVE X-RAY 178 179 182 199 200 222 249 167 254 289 329
ANALYSIS, 6 255 269 272 282 292 305 309 FAST ATOM BOMBARDMENT
ELECTRON ENERGY LOSS 312 320 MASS SPECTROSCOPY, 376
SPECTROSCOPY, 13 358 EQUIPMENT, 6 46 138 194 197 FATTY ACID, 232
ELECTRON IONISATION MASS 218 309 335 379 FIBRE, 31 33 43 82 100 178 179
SPECTROMETRY, 206 ERROR ANALYSIS, 13 182 231 256 260 330 339 371
ELECTRON MICROSCOPY, 2 5 ETHANOL, 56 311 FIBRE GLASS, 76 176 197
13 63 82 108 129 181 289 324 ETHERSULPHONE FIBRE OPTIC, 36
ELECTRON SCANNING COPOLYMER, 47 FIBRE-REINFORCED PLASTIC,
MICROSCOPY, 2 5 13 63 82 ETHYLENE ACRYLIC ACID 36 100 141 178 231 258 281
108 129 181 COPOLYMER, 51 348 320
ELECTRON SPECTROSCOPY ETHYLENE-BUTYLENE FIELD EMISSION SCANNING
FOR CHEMICAL ANALYSIS, COPOLYMER, 52 TRANSMISSION ELECTRON
61 ETHYLENE CONTENT, 370 392 MICROSCOPY, 289
ELECTRON SPIN RESONANCE ETHYLENE COPOLYMER, 22 60 FIELD-FLOW
SPECTROSCOPY, 45 66 294 63 102 113 154 209 259 348 FRACTIONATION, 35 97
326 327 368 359 389 FILLED, 179 318 325

136 © Copyright 2002 Rapra Technology Limited


Subject Index

FILLER, 17 43 45 65 81 90 93 184 FRACTURE, 67 82 98 178 236 149 155 161 163 164 170 179
207 211 226 289 306 307 318 271 289 207 213 220 249 261 269 280
324 325 399 FRACTURE MORPHOLOGY, 2 282 287 290 305 308 309 323
FILLER CONTENT, 81 90 324 13 54 61 98 115 191 319 346 328 338 357 367 377 382 390
FILLER DISTRIBUTION, 289 324 391 394 394
FILM, 1 3 16 27 37 38 40 41 49 56 FREE ENERGY, 339 GLOW DISCHARGE, 343
57 61 62 65 86 92 102 104 106 FREE RADICAL, 45 266 GLOW DISCHARGE
115 117 118 135 142 148 156 FREE VOLUME, 18 56 99 338 SPECTROSCOPY, 202
167 168 186 205 246 257 262 367 382 GRAVIMETRIC ANALYSIS, 23
266 269 288 289 308 324 327 FREEZING POINT, 324 82 85 93 94 152 189 196 211
349 351 362 373 374 386 387 FREQUENCY, 78 118 179 255 256 244 258 296 317 347 377 380
FINITE ELEMENT ANALYSIS, 287 309 325 336
108 FUEL TANK, 56
FIRE RETARDANT, 359 FUNCTIONAL GROUP, 36 83 274
H
FLAME IONISATION, 185 331 HEADSPACE ANALYSIS, 311
FLAME RETARDANT, 95 152 FUNGUS, 5 HEADSPACE
211 218 273 FURAN RESIN, 199 CHROMATOGRAPHY, 185
FLAMMABILITY, 150 173 273 FURNITURE, 274 HEAT CAPACITY, 20 74 78 125
359 161 179 220 253 261 276 280
FLASH CHROMATOGRAPHY,
97
G 287 290 309 324 336 394
HEAT DEGRADATION, 23 26 29
FLASH PYROLYSIS, 4 GAMMA-IRRADIATION, 4 99 75 76 83 152 160 163 189 192
FLAVOUR, 183 133 393 194 196 244 266 273 318 325
FLEXIBLE, 84 277 283 353 GAS, 67 80 277 311 380 381
FLOATATION, 97 GAS BARRIER, 56 57 168 HEAT FLOW, 36 155 245 252 261
FLOW INJECTION ANALYSIS, GAS CHROMATOGRAPHY, 3 4 276 309 324
50 30 34 39 53 56 66 71 72 75 76 HEAT INSULATION, 80 276
FLOW MICROCALORIMETRY, 80 81 84 87 90 96 107 112 119 HEAT RESISTANCE, 11 24 26 57
93 120 124 128 132 141 143 160 85 126 163 196 228 266 267
FLOW RATE, 50 143 233 324 372 174 183 185 186 191 194 195 269 295 317 377
FLUORESCENCE, 17 293 198 208 217 218 221 232 235 HEAT STABILITY, 146 196
FLUORESCENCE 250 270 273 278 303 307 311 HEAT TREATMENT, 57 119
SPECTROSCOPY, 108 116 157 339 349 353 373 382 383 390 HEATING, 36 179 187 244 266
FLUOROPOLYMER, 279 387 392 398 309 323 348 354
FOAM, 80 84 97 302 GAS DIFFUSION, 274 HEATING RATE, 36 54 144 179
FOOD-CONTACT GAS LIQUID 309 328 332 348 380
APPLICATION, 124 177 195 CHROMATOGRAPHY, 97 HELIUM, 57
208 264 286 387 GAS-PHASE, 67 80 277 311 HETEROGENEITY, 25 217 268
FOOD PACKAGING, 57 124 168 GAS PIPE, 277 HETEROGENEOUS, 129 146 170
195 266 278 311 GAS TRANSMISSION, 311 HEXANE, 240 319
FORMULATION, 30 108 164 174 GEL, 46 319 326 HIGH DENSITY
217 312 GEL ELECTROPHORESIS, 97 POLYETHYLENE, 52 56 57 63
FOURIER TRANSFORM GEL PERMEATION 87 91 102 109 112 128 132 143
INFRARED SPECTROSCOPY, CHROMATOGRAPHY, 50 107 164 195 212 214 307 357 372
1 3 6 8 11 24 25 26 29 30 34 36 113 137 152 169 172 190 200 392
40 41 60 63 64 72 77 83 88 92 233 259 264 295 310 325 334 HIGH IMPACT PS, 48
93 94 98 102 107 108 113 117 356 376 383 388 396 399 HIGH PERFORMANCE LIQUID
126 135 136 150 153 156 160 GELATION, 7 73 134 161 294 CHROMATOGRAPHY, 21 35
161 163 165 169 170 173 181 GLASS, 145 167 276 351 39 46 76 97 165 171 183 195
189 190 213 215 216 226 228 GLASS CONTENT, 296 200 222 233 238 239 242 247
246 249 250 252 259 262 264 GLASS FIBRE, 76 176 197 264 266 286 304 337 366 375
271 274 275 277 288 300 306 GLASS FIBRE-REINFORCED 383 399 400
309 316 318 321 328 341 343 PLASTIC, 17 179 202 211 231 HIGH TEMPERATURE, 62 107
344 345 352 360 364 374 381 271 288 296 333 277 381
385 386 397 GLASS TRANSITION HIGH RESOLUTION, 179 209
FRACTION, 35 170 204 394 TEMPERATURE, 12 15 18 20 289 340 354 363 389
FRACTIONATION, 28 52 97 107 29 36 49 51 56 74 77 81 85 94 HINDERED AMINE, 3 31 66 123
113 337 370 398 101 106 110 114 117 122 135 225

© Copyright 2002 Rapra Technology Limited 137


Subject Index

HINDERED PHENOL, 41 250 256 257 259 262 264 269 KEVLAR, 191
HIP JOINT, 42 271 274 275 277 284 294 297 KINETIC, 8 10 45 73 83 125 377
HOMOGENEITY, 100 289 340 301 306 316 318 321 328 341 KINETICS, 3 23 52 73 75 94 144
HOT STAGE MICROSCOPY, 2 343 344 345 353 360 362 364 149 302 317 323 332 363 380
181 365 371 374 381 383 385 386 381
HUMIDITY, 44 56 57 309 387 393 399
HYDROFLUOROCARBON, 321 INFRARED THERMOGRAPHY,
HYDROGEN BONDING, 77 94 67
L
99 114 342 364 INJECTION MOULDING, 67 160 LAC RESIN, 352
HYDROGEN CHLORIDE, 34 48 231 296 357 LACQUER, 185
194 228 INK, 239 LAMELLAE, 78 139
HYDROLYSIS, 34 58 59 165 319 INSULATION, 80 276 LAMINATE, 56 57 168 182 266
341 352 INTERACTION, 90 167 178 235 342
HYDROPHILICITY, 46 51 360 249 285 311 318 341 342 364 LAMINATED FILM, 57 168 266
HYDROPHOBICITY, 37 46 360 INTERACTION PARAMETER, 293
375 220 235 285 LANGIVIN EQUATION, 3 46 50
HYDROXYBENZENE, 75 297 INTERCHAIN PACKING, 135 60 75
300 INTERFACE, 178 179 182 206 229 LASER, 62 212 236 298 351 397
HYDROXYETHYL 236 322 341 342 346 367 394 LASER INDUCED
METHACRYLATE INTERFACIAL ADHESION, 333 DECOHESION
COPOLYMER, 46 INTERFACIAL DEBONDING, 167 SPECTROSCOPY, 236
HYDROXYL GROUP, 36 69 INTERFACIAL INTERACTION, LASER INTERFEROMETRY, 363
90 167 178 LASER IONISATION MASS
INTERFACIAL PROPERTIES, 81
I 90 111 141 167 178 249 320 342
SPECTROMETRY, 6
LASER LIGHT SCATTERING, 35
IDENTIFICATION, 30 79 121 128 INTERFEROMETRY, 13 275 363 200
132 212 214 353 370 397 INTERNAL MOULD RELEASE, LASER RAMAN
ILLUMINATION, 311 202 SPECTROSCOPY, 168
IMAGING, 13 67 88 168 179 275 INTRINSIC VISCOSITY, 29 172 LATERAL FORCE
289 346 266 330 MICROSCOPY, 308
IMIDAZOLE, 262 INVERSE GAS LATEX, 46 156 174 193 198
IMIDISATION, 8 355 CHROMATOGRAPHY, 81 90 LEACHING, 183
IMMERSION, 178 223 237 141 143 191 217 235 339 382 LEAD, 201
IMMISCIBLE, 188 367 394 390 LEAST-SQUARES ANALYSIS,
IMMUNOELECTROPHORESIS, ION CHROMATOGRAPHY, 97 70 214 345
97 218 LENS, 219 265
IMPACT PROPERTIES, 56 63 231 ION CYCLOTRON RESONANCE, LIFETIME PREDICTION, 108
370 388 397 255 377
IMPLANT, 219 262 393 ION EXCHANGE, 50 97 351 LIGHT ABSORPTION, 229 274
IMPURITY, 221 IONISATION, 46 50 206 222 379 LIGHT DEGRADATION, 3 40 129
INDUCTION PERIOD, 41 88 IRON OXIDE, 112 153 196 274 288
INDUCTIVELY COUPLED IRRADIATION, 4 40 92 153 358 LIGHT MICROSCOPY, 181 295
PLASMA SPECTROMETRY, IRRADIATION DEGRADATION, LIGHT SCATTERING, 111 116
351 133 117 172 203 238 260 310 396
INELASTIC NEUTRON ISOELECTRIC POINT, 46 333 LIGHT STABILISER, 3 31 123
SCATTERING, 361 ISOMERISATION, 11 288 132 288
INFRARED ABSORPTION, 36 ISOPHORONE DIISOCYANATE, LIGHT STABILITY, 3 288
274 362 121 LIGNOCELLULOSE, 82
INFRARED CAMERA, 67 ISOTACHOPHORESIS, 46 LINEAR LOW DENSITY
INFRARED DICHROISM, 284 ISOTACTIC, 129 133 274 314 POLYETHYLENE, 57 92 107
INFRARED SPECTROSCOPY, 1 3 ISOTHERM, 67 178 309 339 139 186 216 225 324 386
8 11 14 17 24 26 29 33 34 36 39 ISOTHERMAL, 36 78 117 125 276 LINEAR REGRESSION
41 43 51 60 63 66 69 72 77 79 317 338 348 375 ANALYSIS, 144
85 88 92 93 94 98 108 113 126 ISOTROPY, 117 LIQUID CHROMATOGRAPHY,
135 142 150 153 156 160 161 21 25 35 39 46 50 55 76 97 103
163 164 165 169 172 173 181 K 105 108 124 159 165 171 183
184 186 188 189 207 215 216 195 200 203 206 210 222 229
225 226 228 230 244 246 249 KAOLIN, 226 306 233 238 239 240 241 242 243

138 © Copyright 2002 Rapra Technology Limited


Subject Index

247 264 266 285 286 299 304 325 288 387
319 337 353 355 366 375 379 MEDICAL APPLICATION, 42 262 MINERAL FILLER, 45 288 289
383 384 395 MELAMINE-FORMALDEHYDE 324
LIQUID CRYSTAL POLYMER, RESIN, 159 365 MISCIBILITY, 12 64 77 98 125 146
309 367 387 MELT, 54 170 254 282 290 354 209 213 220 309 367 390 391
LIQUID NITROGEN, 358 MELT TRANSITION, 267 394
LOW DENSITY MELTING, 2 24 54 78 79 136 155 MOBILE PHASE, 50 375 395
POLYETHYLENE, 3 57 86 87 179 209 252 309 332 MODEL, 28 105 149 152 172 216
139 143 164 168 186 207 214 MELTING POINT, 12 52 56 63 94 290 311 319 336 341 360 381
266 324 325 348 372 373 386 114 164 266 295 324 382 394
LOW FREQUENCY, 126 363 MELTING TEMPERATURE, 20 57 MODULATED DIFFERENTIAL
LOW MOLECULAR WEIGHT, 179 207 309 323 332 370 SCANNING CALORIMETRY,
128 375 MEMBRANE OSMOMETRY, 396 10 36 74 125 131 135 161 220
METAL, 177 179 298 341 261 282 309 377 394
METAL ADHESION, 62 223 341 MODULATED TEMPERATURE
M METAL COATING, 62 255 THERMOMECHANICAL
MAGIC ANGLE, 209 268 283 291 METAL SALT, 352 ANALYSIS, 20
300 340 METALLISED FILM, 168 266 387 MOISTURE CONTENT, 6 51 148
MAGNESIUM-25, 359 METHACRYLATE COPOLYMER, 266 309
MALDI-TOF SPECTROSCOPY, 190 MOLAR MASS, 25 35 102 103 107
28 103 127 137 158 159 166 204 METHACRYLIC ACID 140 159
310 322 335 356 376 COPOLYMER, 15 63 259 MOLECULAR
MALEIC ANHYDRIDE, 82 METHACRYLIC ESTER CONFIGURATION, 117 130
MALEIC ANHYDRIDE COPOLYMER, 190 135 168 328 338 355 367
COPOLYMER, 28 341 METHACRYLIC ESTER MOLECULAR INTERACTION,
MAPPING, 69 275 289 339 342 POLYMER, 45 245 178 220 342 375
344 METHANOL, 39 56 76 171 266 MOLECULAR MOBILITY, 26 268
MASS SELECTIVE DETECTOR, METHANOLYSIS, 39 301 389
76 218 METHYL ACETATE, 185 MOLECULAR ORIENTATION,
MASS SPECTROMETRY, 4 6 13 METHYL ACRYLATE 257 281 284 327 360
28 30 50 75 103 107 112 127 COPOLYMER, 33 172 299 395 MOLECULAR STRUCTURE, 1 8
132 178 186 192 194 204 222 METHYL ETHYL KETONE, 285 12 16 25 31 47 49 51 53 56 66
229 266 278 307 311 376 379 METHYL METHACRYLATE, 288 68 72 73 77 80 83 89 93 98 101
382 392 396 397 398 METHYL METHACRYLATE 102 103 107 114 130 133 140
MASS SPECTROSCOPY, 28 66 72 COPOLYMER, 28 33 166 198 146 152 158 159 164 166 168
84 86 103 121 124 127 128 137 308 384 172 180 197 198 200 211 213
153 158 159 166 177 185 190 METHYLBENZENE, 56 185 241 222 228 229 232 243 264 268
195 202 204 206 244 250 270 261 269 274 275 277 283 284 286
273 303 310 312 322 335 356 METHYLENE CHLORIDE, 266 289 291 300 301 308 310 317
376 399 MICROANALYSIS, 179 231 289 318 328 331 334 337 355 356
MATRIX, 36 82 141 178 182 351 MICROBIAL DEGRADATION, 5 364 365 368 370 376 382 391
359 MICROCALORIMETRY, 154 MOLECULAR WEIGHT, 1 28 29
MATRIX-ASSISTED LASER MICRODIELECTROMETRY, 9 42 46 50 52 54 55 62 73 89 102
DESORPTION, 28 103 127 137 MICROEXTRACTION, 71 185 112 113 114 116 120 127 128
158 159 166 204 310 322 335 MICRORAMAN 130 158 164 166 172 185 190
356 376 SPECTROSCOPY, 168 346 200 204 210 222 224 235 239
MDI, 9 MICROSCOPY, 2 13 16 27 38 41 243 285 310 314 319 322 323
MECHANICAL DEGRADATION, 58 59 61 98 111 125 126 142 325 330 332 334 337 355 356
266 145 168 179 181 213 231 256 375 376 378 381 382 388 395
MECHANICAL PROPERTIES, 9 257 277 289 295 308 324 387 396
40 41 56 61 62 63 65 67 82 84 MICROSTRUCTURE, 13 58 60 MOLECULAR WEIGHT
86 91 114 115 126 151 163 168 168 170 198 274 370 388 392 DISTRIBUTION, 102 116 190
178 179 182 207 231 249 256 MICROTOMY, 168 200 204 224 310 314 319 322
269 271 277 281 288 289 296 MICROWAVE, 112 128 262 325 356 375 381 396
309 315 316 324 325 333 353 MICROWAVEABLE, 266 387 MONITORING, 5 70 149 174 188
365 370 388 MID-INFRARED 223 261 272 298 311 321 348
MECHANICAL RECYCLING, 195 SPECTROSCOPY, 362 MONOETHYLENE GLYCOL, 39
MECHANICAL SPECTROSCOPY, MIGRATION, 46 65 183 264 266 266

© Copyright 2002 Rapra Technology Limited 139


Subject Index

MONOMER, 124 229 269 270 387 OIL, 194 277 PERMITTIVITY, 338
MORPHOLOGY, 2 13 54 61 63 98 OLIGOMER, 26 46 103 124 172 PEROXIDE, 294 326
115 118 136 191 213 256 309 190 192 238 242 264 266 335 PEROXY COMPOUND, 393
319 346 367 391 394 ON-LINE MEASUREMENT, 314 PESTICIDE, 373
MOULDING, 134 225 343 OPTICAL FIBRE, 36 188 292 PH, 46 50 130 183
MULTI-ANGLE LASER LIGHT OPTICAL MICROSCOPY, 2 13 41 PHARMACEUTICAL
SCATTERING, 35 200 98 125 142 181 213 289 324 APPLICATION, 46 221
MULTILAYER, 168 266 344 387 387 PHASE BEHAVIOUR, 267 340
MULTILAYER FILM, 57 168 OPTICAL PROPERTIES, 1 3 47 365
MULTIPLE PULSE NMR, 291 57 162 181 199 200 206 263 PHASE SEPARATION, 110 125
MULTIVARIATE ANALYSIS, 216 274 288 292 293 323 332 350 156 391 394
MUNICIPAL WASTE, 128 362 375 PHENOL, 75 297 300
OPTIMISATION, 50 102 105 171 PHENOL-FORMALDEHYDE
233 318 373 RESIN, 73 297 300
N ORGANOLEPTIC PROPERTIES, PHENOLIC ANTIOXIDANT, 183
N-METHYL-2-PYRROLIDONE, 57 183 PHENOLIC RESIN, 83 199 300
355 ORIENTED, 104 117 283 284 361 PHOSPHORUS, 95 312 373
NANOCOMPOSITE, 62 387 PHOTOACOUSTIC
NAPHTHA, 215 ORTHOPAEDIC APPLICATION, SPECTROSCOPY, 249 288 344
NATURAL FIBRE, 82 393 PHOTOCALORIMETRY, 377
NATURAL FIBRE-REINFORCED OSCILLATING DIFFERENTIAL PHOTOCHEMICAL
PLASTIC, 141 SCANNING CALORIMETRY, DEGRADATION, 288
NATURAL POLYMER, 232 352 7 PHOTOCROSSLINKING, 45 187
NEAR-INFRARED OSMOMETRY, 29 46 200 378 PHOTODEGRADATION, 16 19
CORRELATION OVEN STABILITY, 266 65 66 274 279
SPECTROSCOPY, 364 OXIDATION, 40 41 61 66 88 94 PHOTOELECTRON
NEAR-INFRARED 104 129 152 153 205 266 269 SPECTROSCOPY, 13 37 48
SPECTROSCOPY, 14 36 215 274 288 325 329 348 381 393 100 104 121 167 175 176 196
225 362 371 OXYGEN, 57 104 153 262 274 197 202 205 277 279 298 308
NITROCELLULOSE, 46 79 185 311 312 316 320 333 343
NITROGEN, 57 76 95 OXYGEN ABSORPTION, 104 PHOTOINITIATOR, 27 312
NITROGEN-CONTAINING 387 PHOTOISOMERISATION, 288
POLYMER, 250 OXYGEN BARRIER, 56 57 168 PHOTOLYSIS, 153
NON-DESTRUCTIVE TEST, 19 PHOTON CORRELATION
SPECTROSCOPY, 224
32 67 106 126 157 327 P PHOTOOXIDATION, 40 129 153
NOVOLAC RESIN, 73 300
NUCLEAR MAGNETIC PACKAGING, 5 57 128 131 168 274 288
RESONANCE, 1 22 28 30 31 212 264 266 278 323 387 PHOTOVOLTAIC PROPERTIES,
32 34 57 60 68 73 77 100 108 PACKAGING FILM, 57 168 266 38
113 114 123 130 138 148 162 387 PHTHALATE, 288
169 172 180 189 193 201 209 PAINT, 62 174 185 217 255 298 PHTHALOCYANINE GREEN, 65
212 246 248 251 265 268 272 PAPER, 266 387 PHYSICAL AGEING, 101 135 213
283 291 297 300 314 331 334 PAPER CHROMATOGRAPHY, 97 309 338
340 350 359 370 372 376 383 PARACRYSTALLINE, 102 207 PHYSICAL PROPERTIES, 12 42
388 389 391 392 213 315 52 56 63 94 114 164 188 215
NUMBER-AVERAGE PARTIAL LEAST SQUARES, 215 216 236 259 266 295 324 353
MOLECULAR WEIGHT, 130 216 382
375 378 PARTICLE BEAM ANALYSIS, PIGMENT, 65 121 181 217 225
NYLON, 33 56 57 79 125 164 168 206 236 237 325 399
192 199 207 225 231 309 331 PARTICLE PACKING, 324 PIPE, 52 183 277 307 329
NYLON 1010, 24 PARTICLE SIZE, 13 45 50 81 225 PLANT FIBRE, 82
NYLON-12, 294 364 233 319 324 372 375 PLASMA TREATMENT, 61 69
NYLON-6, 33 56 57 132 207 387 PARTICLE SIZE 106 230 262 298 343
NYLON-6,6, 17 33 57 130 231 329 DISTRIBUTION, 62 324 PLASTICISATION, 36 56 301 348
PEAK INTENSITY, 168 178 260 PLASTICISER, 33 34 120 184 258
289 392 277 353 387 399
O PELLET, 216 266 296 373 PLASTICS WASTE, 87 211 212
PERMEABILITY, 56 57 168 237 PLATE-OUT, 6
ODOUR, 57 183 307

140 © Copyright 2002 Rapra Technology Limited


Subject Index

POLARISATION, 256 257 284 POLYCYANATE, 11 207 212 214 257 261 263 266
POLARISED CONFOCAL POLYCYANURATE, 317 269 283 293 309 323 336 357
RAMAN MICROSCOPY, 257 POLYDEUTEROPOLYETHYLENE, 358 382 388 398
POLARISED FLUORESCENCE, 361 POLYFLUOROETHYLENE, 79
284 POLYDICYANATE, 11 164 180 279 296
POLARISED LIGHT POLYDIMETHYLPHENYLENE POLYHYDROXYBUTYRATE, 59
MICROSCOPY, 181 OXIDE, 356 POLYHYDROXYBUTYRIC
POLARISED OPTICAL POLYDIMETHYLSILOXANE, ACID, 246
MICROSCOPY, 13 140 POLYHYDROXYETHYL
POLARISING MICROSCOPY, POLYDISPERSITY, 29 35 127 137 METHACRYLATE, 172 248
168 204 224 325 335 356 POLYHYDROXYKETONE, 349
POLARITY, 50 203 339 POLYEPICHLOROHYDRIN, 390 POLYHYDROXYSTYRENE, 77
POLYACETAL, 164 POLYEPOXIDE, 10 20 32 36 47 367
POLYACRYLAMIDE, 46 240 62 68 144 145 149 151 157 161 POLYIMIDE, 5 23 79 196 199 320
POLYACRYLATE, 245 269 178 179 182 199 200 222 249 355
POLYACRYLIC, 249 343 255 269 272 282 292 305 309 POLYIONENE, 57 276
POLYACRYLIC ACID, 46 172 342 312 320 POLYISOCYANATE, 9
POLYACRYLIC IMIDE, 387 POLYESTER RESIN, 199 204 288 POLYKETONE, 54
POLYACRYLONITRILE, 33 79 POLYESTER-URETHANE, 114 POLYLACTIC ACID, 267
119 342 POLYESTERIMIDE, 355 POLYMERIC FLAME
POLYALPHA- POLYETHER, 54 66 158 235 238 RETARDANT, 218 273
METHYLSTYRENE, 153 242 384 398 POLYMERIC MOULD RELEASE
POLYAMIC ACID, 355 POLYETHER SULPHONE, 75 AGENT, 202
POLYAMIDE, 33 56 57 79 125 125 151 356 POLYMETHACRYLATE, 45 245
164 168 192 199 207 225 231 POLYETHER-ETHERKETONE, 398
309 331 54 79 126 213 295 315 POLYMETHACRYLIC ACID, 15
POLYAMIDE-1010, 24 POLYETHER-URETHANE, 90 141
POLYAMIDE-12, 159 POLYETHERETHERKETONE, 79 POLYMETHACRYLONITRILE,
POLYAMIDE-6, 33 56 57 132 165 126 141
207 387 POLYETHERIMIDE, 64 79 98 192 POLYMETHYL
POLYAMIDE-6,6, 17 130 296 367 387 METHACRYLATE, 14 21 116
POLYAMIDE-IMIDE, 316 POLYETHERSULPHONE, 75 125 132 137 141 159 166 178 204
POLYAMINE, 46 272 151 356 219 220 221 224 229 240 241
POLYANILINE, 46 115 POLYETHYL ACRYLATE, 58 284 285 289 299 301 304 314
POLYARAMIDE, 191 339 POLYETHYL METHACRYLATE, 319 335 338 343 363 375 382
POLYARYL ETHER KETONE, 390 384 394 397 398
213 POLYETHYLENE, 42 52 56 57 60 POLYMETHYLENE OXIDE, 79
POLYARYLATE, 367 61 63 65 79 87 91 92 99 102 POLYOL, 84 110
POLYBENZIMIDAZOLE, 79 107 109 112 128 132 139 143 POLYOXYETHYLENE, 154
POLYBENZYL 146 148 154 157 164 168 181 POLYOXYMETHYLENE, 79
METHACRYLATE, 35 186 188 195 199 207 212 214 POLYPHENYLENE, 398
POLYBIBENZOATE, 309 216 225 249 256 260 263 266 POLYPHENYLENE ETHER, 79
POLYBISGLYCIDYL 267 283 293 307 315 324 325 152 220 367
METHACRYLATE, 247 344 348 357 361 365 366 368 POLYPHENYLENE OXIDE, 79
POLYBUTYL ACRYLATE, 156 370 372 373 386 392 393 398 152 220 357 367 394
394 400 POLYPHENYLENE SULPHIDE,
POLYBUTYL METHACRYLATE, POLYETHYLENE GLYCOL, 46 79 170 296 320 328
21 376 233 310 369 378 POLYPHENYLENE
POLYBUTYL THIOPHENE, 327 POLYETHYLENE GLYCOL TEREPHTHALAMIDE, 339
POLYBUTYLENE TEREPHTHALATE, 26 POLYPHENYLMETHACRYLATE,
NAPHTHALATE, 98 POLYETHYLENE 367
POLYBUTYLENE NAPHTHALATE, 387 POLYPHENYLSULPHONE, 79
TEREPHTHALATE, 164 273 POLYETHYLENE OXIDE, 125 POLYPROPYLENE, 31 41 57 59
POLYCAPROLACTONE, 147 267 154 235 337 79 87 88 91 102 104 109 112
390 POLYETHYLENE 118 123 128 129 132 133 168
POLYCARBONATE, 14 57 62 72 TEREPHTHALATE, 2 12 26 171 183 188 205 206 207 212
79 99 101 199 207 245 273 280 39 40 57 63 64 74 76 79 106 214 249 264 281 284 289 293
309 340 356 363 367 382 398 117 118 131 136 157 164 168 329 330 370 380 381 398

© Copyright 2002 Rapra Technology Limited 141


Subject Index

POLYPROPYLENE GLYCOL, POWDER COATING, 222 30 33 42 47 69 70 108 109 129


334 PRE-TREATMENT, 176 197 215 140 151 168 182 212 214 215
POLYPROPYLENE GLYCOL 223 351 216 256 257 263 281 284 288
MALEATE, 288 PRECIPITATION, 35 266 293 300 342 346 365 369 393
POLYPROPYLENE OXIDE, 103 PRESSURE, 50 56 171 194 206 RAPID SCAN, 344 345
POLYPYRROLE, 46 222 236 395 REACTIVITY, 151 274 388 392
POLYSTYRENE, 14 21 35 46 48 PRINCIPAL COMPONENTS REARVIEW MIRROR, 67
57 58 79 82 85 87 118 141 153 ANALYSIS, 216 RECLAIM, 289
156 159 160 164 166 203 207 PROBE, 179 339 382 RECOVERY, 319
212 214 220 230 245 278 290 PROBLEM PREVENTION, 30 RECRYSTALLISATION, 54 136
299 304 308 315 334 351 363 181 296 303 309 332
367 375 382 394 395 398 PROCESSING, 115 168 199 207 RECYCLABILITY, 57 88 266 387
POLYSULPHONE, 75 79 99 125 209 231 254 261 323 325 329 RECYCLATE, 64 91 122 195 329
331 373 388 373
POLYTETRAFLUOROETHYLENE, PROPYLENE, 264 RECYCLING, 39 57 64 88 91 122
79 164 180 279 296 363 PROPYLENE COPOLYMER, 18 128 165 195 211 212 231 266
POLYTETRAMETHYLENE 22 69 102 373 387
OXIDE, 384 PROPYLENE-ETHYLENE REFLECTANCE
POLYTHIOPHENE, 38 COPOLYMER, 69 274 370 SPECTROSCOPY, 257 343
POLYURETHANE, 19 66 79 80 84 PROTECTIVE COATING, 217 REFRACTIVE INDEX, 1 106 190
89 110 157 158 163 169 187 255 200 229 292 375
199 207 255 PROTON MAGNETIC REFRIGERATOR, 80
POLYVINYL ACETATE, 79 199 RESONANCE, 265 291 314 REGRESSION ANALYSIS, 144
209 220 268 270 367 394 388 214 215 216 224 345
POLYVINYL ALCOHOL, 1 46 51 PROTON SPIN RELAXATION, REINFORCED PLASTIC, 13 17
57 284 342 209 268 36 79 81 90 100 134 141 176
POLYVINYL CARBAZOLE, 162 PULSED NMR, 272 178 179 182 196 197 199 202
POLYVINYL CHLORIDE, 6 7 17 PURITY, 120 192 211 231 234 271 281 288 296
57 79 87 108 141 145 146 167 PYROLYSIS, 4 75 83 87 119 192 318 320 333 339 357 377
184 194 201 207 212 214 227 194 212 234 270 273 296 303 RELATIVE HUMIDITY, 44 56 57
228 254 262 315 326 353 374 374 380 392 309
385 392 394 PYROLYSIS GAS RELAXATION, 74 282 287 290
POLYVINYL ESTER, 320 CHROMATOGRAPHY, 4 96 309 363
POLYVINYL METHYL ETHER, 107 132 198 218 221 232 250 RELAXATION MAP ANALYSIS
363 270 392 SPECTROSCOPY, 377
POLYVINYL PHENOL, 77 367 PYROLYSIS-IR RELAXATION SPECTRA, 325
POLYVINYL PYRROLIDONE, 46 SPECTROPHOTOMETRY, 4 RELAXATION TIME, 209 291
77 248 250 340 PYROLYSIS MASS 340
POLYVINYLBENZENE, 79 85 87 SPECTROMETRY, 4 192 RELAXATION TRANSITION,
118 153 212 290 315 290
POLYVINYLCARBAZOLE, 162 RELEASE AGENT, 202
POLYVINYLIDENE CHLORIDE,
Q REPEATABILITY, 347
57 168 387 QUALITATIVE ANALYSIS, 195 REPRODUCIBILITY, 6 46 347
POLYVINYLIDENE FLUORIDE, QUALITY, 183 311 361 375
12 79 277 390 QUALITY CONTROL, 67 131 329 RESIDENCE TIME, 266 325 357
POLYVINYLPYRROLIDONE, 46 347 353 357 386 RESIDUAL ADDITIVE, 221
77 248 250 340 QUANTITATIVE ANALYSIS, 102 RESIDUAL CATALYST, 129
PORE SIZE, 50 241 285 319 375 171 179 184 195 221 278 373 RESIDUAL STRESS, 67 316
POROSITY, 50 126 142 203 241 QUENCHING, 101 117 135 261 RESOLUTION, 50 118 229
285 319 367 375 363 RETENTION TIME, 119 222
POSITRON ANNIHILATION RETENTION VOLUME, 143 375
LIFETIME SPECTROSCOPY, REVERSE OSMOSIS, 97
19 99 338 367 R REVERSE-PHASE
POST-CONSUMER, 195 214 266 CHROMATOGRAPHY, 50 195
RADIATION CURING, 269
373 233
RADIO FREQUENCY
POTABLE WATER, 183 307 REVIEW, 13 55 59 71 79 107 199
DISCHARGE, 343
POTASSIUM BROMIDE, 262 271 205 212 283 284 310 350 363
RADIOLYSIS, 4
POWDER, 126 175 194 364 365 367 372 377 383 387
RAMAN SPECTROSCOPY, 16 27

142 © Copyright 2002 Rapra Technology Limited


Subject Index

390 391 396 SILICA, 6 21 40 45 46 90 203 289 CHROMATOGRAPHY, 71


RHEOLOGICAL PROPERTIES, 319 375 STATIONARY PHASE, 50 203
10 20 29 41 46 73 149 161 163 SILICA GEL, 241 319 235 375
217 266 295 324 325 338 354 SILICATE, 65 81 STEEL, 223 341
RHEOMETRY, 10 324 325 SILICONE POLYMER, 204 284 STEP-SCAN PHOTOACOUSTIC
RHEOPHOTOACOUSTIC SIMULATED BODY FLUID, 34 SPECTROSCOPY, 344
SPECTROSCOPY, 249 SIMULATION, 34 134 149 323 STEREOREGULARITY, 168
ROPE, 281 362 367 STERIC EXCLUSION
ROTATING FRAME, 209 268 340 SIZE EXCLUSION CHROMATOGRAPHY, 41
ROUND ROBIN TEST, 173 CHROMATOGRAPHY, 28 29 STERILISATION, 42 393
34 35 40 50 52 55 60 97 102 STORAGE, 309 311
103 108 112 114 116 158 166 STORAGE TIME, 311
S 204 229 239 240 243 299 314 STRAIN, 315 325 365
SAMPLE PREPARATION, 13 72 322 334 375 381 STRENGTH, 9 167 269 315
123 124 207 SIZING, 176 STRESS, 67 168 182 281 289 315
SAMPLE SIZE, 72 124 143 SMALL-ANGLE, 117 291 354 316 325
SAMPLING, 13 71 72 123 124 207 SMOKE EMISSION, 76 150 173 STRESS CRACKING, 271
233 351 SOFTENING TEMPERATURE, STRESS-STRAIN PROPERTIES,
SAN, 110 147 207 220 284 315 179 61 231 281 325
345 SOFTWARE, 67 195 344 STRUCTURAL ADHESIVE, 62
SATURATED POLYESTER, 26 49 SOL-GEL, 53 STRUCTURAL ANALYSIS, 168
106 114 204 229 267 322 336 SOLAR ENERGY STRUCTURE-PROPERTY
367 376 388 398 APPLICATION, 38 RELATIONSHIP, 209 269 389
SCANNING ELECTRON SOLID STATE, 193 209 268 283 STYRENE, 199 278 288
MICROSCOPY, 2 5 6 13 59 61 291 300 340 359 389 STYRENE-ACRYLONITRILE
62 63 82 98 108 129 181 202 SOLUBILITY, 56 79 90 97 114 COPOLYMER, 72 110 147 207
231 289 316 324 358 115 160 372 375 220 284 315 345
SCANNING PROBE SOLUTE, 50 235 382 STYRENE COPOLYMER, 28 69
MICROSCOPY, 59 179 SOLUTION, 21 46 55 77 115 116 127 198 299 308 363 395
SCISSION, 4 152 274 380 130 178 224 268 291 351 367 STYRENE-ISOPRENE-
SCRAP POLYMER, 122 128 214 389 STYRENE BLOCK
231 SOLUTION CASTING, 94 262 COPOLYMER, 394
SEALANT, 247 367 STYRENE-METHACRYLIC
SEALING, 387 SOLUTION VISCOSITY, 396 ACID COPOLYMER, 81
SEAT, 274 SOLVENT, 21 29 35 56 113 124 SUB-GLASS TRANSITION, 170
SECONDARY AMINE, 36 151 130 185 203 210 235 259 261 SUBSTRATE, 126 223 236 262
SECONDARY ANTIOXIDANT, 266 285 349 360 366 369 375 285 298
93 388 SULPHUR DIOXIDE, 75
SECONDARY ION MASS SOLVENT EXTRACTION, 266 SUPERCRITICAL, 39
SPECTROSCOPY, 13 121 178 331 SUPERCRITICAL FLUID
202 312 SOLVENT PERMEABILITY, 56 CHROMATOGRAPHY, 50 372
SECONDARY STABILISER, 228 SOXHLET EXTRACTION, 112 SUPERCRITICAL FLUID
SEMICONDUCTOR, 321 SPECIFIC HEAT, 20 122 207 309 EXTRACTION, 97 171 372
SEMICRYSTALLINE, 102 106 324 354 373
122 207 213 235 315 SPECIFIC VOLUME, 18 SUPERCRITICAL GAS, 301
SENSITIVITY, 118 291 SPIN-PROBE ANALYSIS, 45 SURFACE ANALYSIS, 19 30 37
SENSOR, 20 292 SPIN RELAXATION, 209 268 300 38 44 58 59 62 67 69 118 175
SEPARATION, 35 55 97 105 128 SPOILAGE INDICATOR, 311 178 179 202 219 289 324 333
243 341 351 370 375 384 STABILISER, 3 40 41 66 86 183 SURFACE AREA, 197 324
SEQUENCE ANALYSIS, 50 184 201 225 228 288 372 SURFACE CHEMISTRY, 93 298
SHEAR, 9 178 182 324 325 333 STABILITY, 24 26 57 85 126 163 319
SHEET, 186 196 228 266 267 269 295 317 SURFACE ENERGY, 52 141 217
SHEET MOULDING 324 377 235 277 339
COMPOUND, 202 211 STANDARD, 120 183 184 392 SURFACE PROPERTIES, 42 44
SHELF LIFE, 57 311 387 STAR-BRANCHED, 35 106 118 179 191 196 217 219
SHELLAC, 232 352 STARCH, 112 267 348 277 308 312 360 383
SHIFT FACTOR, 209 STARCH POLYMER, SURFACE TREATMENT, 61 62
SIDING, 385 STATIC HEAD SPACE GAS 81 168 176 178 182 197 205

© Copyright 2002 Rapra Technology Limited 143


Subject Index

223 230 262 277 298 343 371 133 134 144 147 149 154 155 THIN LAYER
SURFACTANT, 46 65 233 170 179 186 187 189 207 245 CHROMATOGRAPHY, 97 399
SURGICAL APPLICATION, 219 252 258 267 269 270 305 309 TIE LAYER, 168
393 313 324 325 367 377 383 386 TIME, 54 61 94 135 209 223 253
SWELLING, 15 237 250 326 360 394 261 268 277 289 317 338 354
SYNCHROTRON RADIATION, THERMAL CONDUCTIVITY, 80 394
291 179 309 324 377 TIME DEPENDENCE, 125 196
SYNTHETIC FIBRE- THERMAL DEGRADATION, 23 360
REINFORCED PLASTIC, 281 26 29 75 76 83 85 152 160 163 TIME OF FLIGHT, 103 127 137
189 192 194 196 244 258 266 158 159 166 178 202 204 229
273 318 325 380 381 310 312 322 335 356 376
T THERMAL DIFFUSIVITY, 179 TIME RESOLVED
TALC, 65 318 324 324 394 SPECTROSCOPY, 170
TAPE, 284 THERMAL FIELD-FLOW TITANIUM DIOXIDE, 40 65 217
TAPPING MODE ATOMIC FRACTIONATION, 35 237 325
FORCE MICROSCOPY, 58 THERMAL HISTORY, 57 135 136 TOLUENE, 56 185 241 261 319
TASTE, 57 207 245 254 262 287 309 TOTAL ORGANIC CARBON, 183
TEMPERATURE DEPENDENCE, THERMAL IMAGING, 67 TOXICITY, 173 195
49 99 135 146 147 170 196 259 THERMAL INSULATION, 80 276 TRACE ELEMENT, 177
269 308 336 354 364 382 THERMAL MECHANICAL TRANSITION PHENOMENA,
TEMPERATURE GRADIENT ANALYSIS, 196 377 254
INTERACTION THERMAL RELAXATION, 282 TRANSITION PROPERTIES, 203
CHROMATOGRAPHY, 304 290 269 340 354
375 THERMAL RESISTANCE, 196 TRANSITION TEMPERATURE,
TEMPERATURE MODULATED THERMAL STABILITY, 11 24 26 179
DIFFERENTIAL SCANNING 57 85 126 163 196 228 266 267 TRANSMISSION ELECTRON
CALORIMETRY, 54 78 136 269 295 317 377 MICROSCOPY, 2 5 13 59 63
252 253 280 287 290 309 336 THERMAL TRANSITION, 56 78 82 108 129 181 213 289 331
TEMPERATURE PROFILE, 67 220 282 290 309 358
324 THERMAL VOLATILISATION TRANSMISSION
TEMPERATURE ANALYSIS, 189 SPECTROSCOPY, 234 292 362
PROGRAMMED THERMALLY STIMULATED TRANSPARENCY, 57 236 323
ANALYTICAL PYROLYSIS, CURRENT, 323 377 TRANSPORT PROPERTIES, 56
273 THERMOANALYTICAL, 348 115
TEMPERATURE RANGE, 207 THERMODYNAMIC TRIAZINE, 40
317 364 380 382 PROPERTIES, 21 90 122 155 TRICHLOROBENZENE, 29
TEMPERATURE RISING 169 172 220 235 290 339 TRICHLOROMETHANE, 29
ELUTION FRACTIONATION, THERMOGRAM, 36 67 323 348 TRIETHYLAMINE, 298
370 396 370 TRIFLUOROACETIC ACID, 388
TENSILE PROPERTIES, 40 41 61 THERMOGRAVIMETRIC TROUBLESHOOTING, 30 181
63 65 86 114 115 231 277 315 ANALYSIS, 2 8 12 15 17 23 24 296 303
333 26 29 48 82 83 85 93 94 98 146 TWO-DIMENSIONAL, 55 58 209
TEREPHTHALIC ACID, 76 152 163 164 189 192 194 196 233 242 275 283 344 345 364
TERTIARY AMINE, 36 151 211 228 231 244 258 267 269 365
TEST SPECIMEN, 236 346 351 295 296 316 317 318 326 330
347 348 377 380 381 398
358
THERMOLYSIS, 189
U
TESTING, 19 43 58 59 62 71 79
96 108 112 120 123 124 134 THERMOMECHANICAL UHMWPE, 260 393
145 174 182 183 184 185 195 DEGRADATION, 266 ULTRA-HIGH RESOLUTION
206 208 254 255 270 288 293 THERMOMECHANICAL SPECTROSCOPY, 363
304 315 321 329 332 345 347 PROPERTIES, 179 269 ULTRASONIC, 112 126 272
357 363 365 379 382 398 THERMOOXIDATIVE ULTRAVIOLET ABSORPTION,
TETRAHYDROFURAN, 29 35 DEGRADATION, 41 94 152 229 274
240 241 319 395 269 348 ULTRAVIOLET CURING, 27 269
TEXTILE APPLICATION, 371 THERMORHEOLOGICAL 349
THERMAL AGEING, 88 152 PROPERTIES, 338 ULTRAVIOLET DEGRADATION,
THERMAL ANALYSIS, 7 20 26 THICKNESS, 27 56 62 67 168 179 16 19 196
36 54 56 67 78 83 92 95 110 236 255 257 263 ULTRAVIOLET IRRADIATION,

144 © Copyright 2002 Rapra Technology Limited


Subject Index

19 40 44 196 VINYL ESTER RESIN, 320 X


ULTRAVIOLET RESISTANCE, VINYL GROUP, 274
57 196 VINYL PYRROLIDONE X-RAY ANALYSIS, 6 108 129 212
ULTRAVIOLET SPECTRA, 3 41 COPOLYMER, 46 231 289 328 383
65 86 157 264 372 383 399 VISCOELASTICITY, 20 219 308 X-RAY DIFFRACTION, 13 41 57
ULTRAVIOLET VISCOMETRY, 29 200 203 355 83 92 95 117 213 260 277 291
SPECTROSCOPY, 1 3 41 46 65 VISCOSITY, 10 29 46 149 172 266 327 328 398 399
86 115 157 288 372 324 325 330 X-RAY FLUORESCENCE, 17 399
ULTRAVIOLET STABILISER, VISIBLE SPECTROSCOPY, 1 46 X-RAY FLUORESCENCE
225 288 399 115 288 SPECTROSCOPY, 108
UNIT CELL, 13 168 VITRIFICATION, 78 161 290 X-RAY NEAR EDGE
UNPLASTICISED POLYVINYL VOLATILE CONTENT, 72 185 ABSORPTION
CHLORIDE, 254 VOLATILE ORGANIC SPECTROSCOPY, 358
UNSATURATED POLYESTER, COMPOUND, 84 174 185 255 X-RAY PHOTOELECTRON
82 199 204 288 333 278 321 SPECTROSCOPY, 13 37 48
UV VIS SPECTROSCOPY, 1 46 VOLATILISATION, 72 97 100 121 145 167 175 176 196
115 288 VOLUME FRACTION, 13 227 197 202 277 279 298 308 312
231 324 332 367 316 320 333 343
X-RAY RESISTANCE, 104 279
V X-RAY SCATTERING, 13 24 41
W 57 83 92 95 117 213 260 277
VACUUM DISTILLATION, 97
185 WASTE, 87 122 128 211 212 266 291 327 328
VACUUM PYROLYSIS, 87 194 387 X-RAY SPECTROSCOPY, 13 37
VAPOUR PERMEABILITY, 56 WATER, 39 56 61 266 360 48 63 100 108 121 167 175 176
168 WATER ABSORPTION, 51 56 237 196 197 202 277 279 298 308
VAPOUR PHASE OSMOMETRY, 309 312 316 320 328 333 343 354
396 WATER CONTENT, 6 51 148 358
VAPOUR PRESSURE WATER PERMEABILITY, 56 237 XENON LIGHT, 274
OSMOMETRY, 29 200 378 WATER PIPE, 307 329
VARNISH, 174 WATER TREE GROWTH RATE, Y
VEHICLE BONNET, 329 148
VEHICLE MIRROR, 67 WATER VAPOUR YELLOWING, 288
VIBRATIONAL PERMEABILITY, 56 168 YOGHURT POT, 278
SPECTROSCOPY, 14 16 17 26 WAVE NUMBER, 168 YOUNG’S MODULUS, 40 114
27 30 33 36 39 42 43 47 51 69 WAVELENGTH, 44 207 288 168 231 256 269 309 365
70 85 108 109 129 140 142 150 WAX, 232
151 156 164 168 172 173 182 WEATHERING, 44 62 86 92 222
184 186 188 207 212 214 215 385 Z
216 225 226 230 244 256 257 WEIGHT AVERAGE ZEOLITE, 307
263 269 274 281 284 288 293 MOLECULAR WEIGHT, 375 ZIEGLER CATALYST, 102 129
297 300 318 342 345 346 353 WEIGHT CHANGE, 348 ZINC, 298
365 369 393 WEIGHT FRACTION, 176 394 ZINC BORATE, 359
VINYL ACETATE, 251 270 WEIGHT GAIN, 56 ZIRCONOCENE, 365
VINYL ACETATE COPOLYMER, WEIGHT LOSS, 56 94 164 267
209 359 389 296 347 380
VINYL ACETATE-ETHYLENE WETTABILITY, 37 343
COPOLYMER, 100 270 341 WIDE ANGLE, 117 213 260
359 WIDE ANGLE X-RAY
VINYL CHLORIDE, 199 392 SCATTERING, 24
VINYL CYANIDE, 119 WINDOW, 7
VINYL CYANIDE COPOLYMER, WOOD FIBRE-REINFORCED
57 PLASTIC, 9 82 141 258

© Copyright 2002 Rapra Technology Limited 145


Subject Index

146 © Copyright 2002 Rapra Technology Limited


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