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Tech Tip
Basis of Interactions in Gas Chromatography, Featured Applications
• Analysis of Butylated Hydroxytoluene in Food
Part 1 – Non-Polar Interactions with Headspace Trap-GC/MS
• Detecting Drugs of Abuse: Enhanced
Identification Using Benchtof-dx™ and
Associated Software
Click titles to learn more

Products
• GC Pressure and Flow Calculations
iPhone/iPod Application
• Separation of Drugs of Abuse
Click titles to learn more
To fully grasp the concepts of retention and selectivity of GC stationary phases,
one must first understand the fundamental intermolecular interactions that lead
to retention. This month we discuss the most dominant of those interactions –
dispersive, non-polar interactions.
Click here to read more...

www.sepscience.com Issue 8: October 2010

 Basis of Interactions in Gas Chromatography,
Part 1 – Non-Polar Interactions
Matthew Klee To fully grasp the concepts of retention and selectivity of GC stationary phases, one must first understand the
fundamental intermolecular interactions that lead to retention. This month we discuss the most dominant of those
interactions – dispersive, non-polar interactions.

There are fewer types of intermolecular interactions available for Table 1

interactions between solutes and stationary phases in gas chromatography Name Description Molecular traits Characteristic
compared to those possible in liquid chromatography. In addition, the Non-Polar
mobile phase in GC (the carrier gas) plays no role in adjusting or modifying
London2 (1930) induced dipole – in- All compounds, Transient polarization,
the nature of intermolecular interactions during the run. So, the range of dispersion duced dipole non-polar interaction scales with molecular size
possibilities in retention forces and selectivity is much more limited in GC
than in LC. Hydrogen bonding Extreme dipole–dipole Significant with
In gas chromatography, molecules can only interact with each other interaction: H acceptor compounds containing
interacts with H donor –OH or -NH groups
through intermolecular forces that fall under the umbrella of “van der
Waals” forces. They are listed in Table 1. Polar
Van der Waals forces can be overcome or disrupted by thermal motion, Keesom3 (1912) dipole–dipole Interaction between Electronegative groups
which increases as temperature increases. This is why liquids evaporate strong dipoles (e.g., halogens, -OR, -NOx,
faster when heated. and also why solutes are less retained (elute faster) in -SOx)
gas chromatography as the temperature is raised. Debye4 (1923) Dipole–induced dipole Interaction between More polarizable = easier
In gas chromatography, the dominant intermolecular attractive force is a strong dipole and a induction
dispersive interactions. Dispersive interactions are known also as temporary weak dipole
dipole interactions, because they result from transient random distortions Table 1: Van der Waals1 forces of interactions between molecules.
in the electronic clouds of molecules, London forces, after the scientist who
first described them. Dispersive interactions exist between all molecules.
 Figure 1

“The strength of dispersive interactions

track with the size of the molecule; the larger
δ- δ- δ- the molecule, the higher its mass, the more
electrons, the higher the strength of its
δ+ δ+ δ+
dispersive forces.
δ- δ- δ- Dispersive interactions are non-polar (also called apolar). Dispersive
interactions arise from random distortion of the electronic cloud of a
molecule, causing a slight electrostatic polarization – one side of the
δ+ δ+ δ+ molecule becomes more negative, the opposite more positive (Figure 1).
This spontaneous polarization then induces an opposite polarization
in neighbouring molecules. The opposite charges attract and draw the
molecules closer, further distorting the clouds.. A stabilizing oscillation
of the charge distortion results within the bulk liquid (in wall coated
open tubular columns, the stationary phase is considered a liquid).
The strength of dispersive interactions track with the size of the
molecule; the larger the molecule, the higher its mass, the more
electrons, the higher the strength of its dispersive forces. Larger
molecules have larger electron clouds which are more able to handle
δ+ δ+ δ+ electrostatic distortions. So, the distortions can be of higher magnitude
and of longer duration. For this reason, both boiling points and elution
temperatures of molecules track with the size of the molecule (Figure 2).
Although retention in GC is based on the sum of all possible
δ- δ- δ- interactions, polar + non-polar, some types of molecules such as
saturated hydrocarbons (alkanes) can only interact through dispersive
interactions. Even if a stationary phase were to have polar functional
δ+ δ+ δ+ groups and therefore a significant possibility for polar interactions,
saturated hydrocarbons would only interact with the non-polar,
δ- δ- δ- dispersive aspect.
The basic premise of retention in GC is illustrated in Figure 3. One
can see in Figure 3 that the solute represented by the blue triangles
has a higher proportion of molecules in the stationary phase than in
the gas phase. As such, it migrates slowly through the column (has a
high retention time). In contrast, the majority of the solute represented
by the green squares is in the gas phase, so it will migrate much faster
Figure 1: London dispersive (non-polar) forces dominate the intermolecular interactions in gas through the column (have a much lower retention time).
chromatography. They arise from spontaneous transient distortions, polarization, then coordinated Retention in gas chromatography is an exponential function of
oscillations in electronic molecular orbitals. The larger the molecule, the larger the dispersive forces, the temperature. As temperature is raised, there will be a temperature at
higher the strength of interaction, and therefore the higher the retention. which the more retained solute (blue triangles) will travel at the same
 Figure 2 Figure 3

80
70
60
Retention Time

50
40
30 A
20 carrier gas

10
0

250 µm i.d.
0 10 20 30 40 50

0.50 µm i.d.
Carbon number
stationary phase
600
column wall
500
Boiling Point ( C)

magnified 100X
o

400

300 B Column wall

200

100

0
0 10 20 30 40 50
Figure 3: Inner view of a capillary column. A film thickness 0.5 µm on a 250 µm i.d. column represents a
Carbon Number n-Alkane phase ratio of 125, which is typical of capillary columns. As it is almost impossible to see the
stationary phase when drawn to scale, the inset shows a representation of the surface magnified 100
times to better illustrated solute migration in/out of the phase. The solute with the weaker interactions
Figure 2: (A) Retention time trend of n-alkanes in a linear temperature programmed capillary GC run. (B) with the stationary phase (green squares) spends more time in the mobile phase and moves faster
Boiling point trend of n-alkanes. Retention of in gas chromatography tracks boiling point because of through the column, eluting first. The compound with stronger interaction with the stationary phase
dominance of non-polar (dispersive) forces. (blue triangles) spends less time in the gas phase and moves slower through the column.
 Figure 4
speed as the less retained one in Figure 3 did
1000 at the lower temperature. As illustrated in
900
Figure 4, retention decreases approximately
800
by ½ for each 23 oC change in temperature.
In Figure 5, example trends are plotted on a
Retention Factor (k) 700 log scale. One can see that all solutes follow
600 a similar pattern to a first approximation
500 because the dominant intermolecular force
400 of interaction is dispersive. There are slight
300 differences in slopes for homologs with
200 different functionalities. These arise from
100
polar interactions and will be discussed next
month.
0
0 25 50 75 100 125 150 175 200 225
References
Temperature (oC) 1. J. D. van der Waals, “The Thermodynamic Theory of Capillarity
Under the Hypothesis of a Continuous Variation of Density”,
Figure 4: Intermolecular interactions between a solute and a stationary phase lead to retention. originally published in Dutch in Verhandel. Konink. Akad. Weten.
Amsterdam, 1, 8, (1893)
Retention of solutes is an exponential function of temperature. Retention decreases by ½ for
2. Von R. Eisenschitz, F. London, “Über das Verhältnis der van der
approximately every 23 oC change in temperature (solute and stationary phase dependent).
Waalsschen Kräfte zu den Homöopolaren Bindungskräften” Z.
Physik, 60, 491-527, (1930)
Figure 5
3. W. H. Keesom, “On the Deduction of the Equation of State
From Boltzmann’s Entropy Principle”, Communications
1000 Physical Laboratory University of Leiden Supplement, Ed. By H.
Solute A
Kamerlingh Onnes, Eduard Ijdo Printer, Leiden, Supplement 24a
Solute B to No. 121-132, 3-2. 0, (1912)
Retention Factor (k)

100 Solute C 4. P. J. W. Debye, “Die van der Waalsschen Kohäsionskräfte”,

solute D Physik. Zeitschr., 21, 178-87, (1920)

Dr Matthew S. Klee is internationally recognized

10
for contributions to the theory and practice of gas
chromatography. His experience in chemical, pharmaceutical
and instrument companies spans over 30 years. During this
1 time, Dr Klee’s work has focused on elucidation and practical
0 50 100 150 200 250 300 demonstration of the many processes involved with GC
Temperature (oC) analysis, with the ultimate goal of improving the ease of use
of GC systems, ruggedness of methods and overall quality of
Figure 5: The exponential retention function of several solutes plotted on log scale. More volatile solutes results.
(e.g., solute B) will elute earlier and at lower temperatures in a temperature programmed run. To a first
approximation, for a polar stationary phases the dependence of retention on temperature follows the
same trend for all solutes because of dominance of dispersive (non-polar) forces of interaction,
differences in slopes arise from differences in solute polarities (e.g., solutes A and C). Homologs usually
have the the same retention vs temperature slope on a given stationary phase (e.g., solutes B and D).
Featured Applications
Automated Static and Dynamic Headspace Analysis with GC-MS for Determination of Abundant
Automated Static and Dynamic

and Trace Flavour Compounds in Alcoholic Beverages Containing Dry Extract

AppNote 3/2010
Headspace Analysis with GC-MS
for Determination of Abundant and

Company: Gerstel
Trace Flavour Compounds in Alcoholic
Beverages Containing Dry Extract
Kevin Mac Namara, Frank McGuigan
Irish Distillers-Pernod Ricard, Midleton Distillery, Midleton, Cork,
Ireland

Andreas Hoffmann
Gerstel GmbH & Co. KG, Eberhard-Gerstel-Platz 1,
D-45473 Mülheim an der Ruhr, Germany

KEYWORDS
PTV injection, Static headspace, Dynamic headspace,
Alcoholic beverages

ABSTRACT
Direct injection for gas chromatographic profiling of alcoholic
beverages is usually preferable, but where spirits and liquors
contain appreciable amounts of non-volatile material, some

In this application note a combination of static and dynamic headspace analysis is described for
mode of pre-treatment may be required to avoid both inlet
and column contamination. This consideration applies in
particular to products aged for extended periods in wooden
barrels and especially products containing added sugar,
as volatile artefacts from sugar decomposition in the hot
injection port can also complicate the chromatogram.
In this paper a combination of static and dynamic
headspace analysis is described for profiling both abundant
and trace compounds in these products. Static headspace is
used with a tenax packed injection port liner for the abundant

profiling both abundant and trace compounds in these products. Static headspace is used with
compounds. Dynamic headspace uses an additional purging
step to a second tenax liner which can then be desorbed
to the same injection port liner used for the simple static
headspace. In this case the previous abundant compounds
are overloaded in the chromatogram but many additional
trace compounds are now apparent. For both techniques the

a tenax packed injection port liner for the abundant compounds. Dynamic headspace uses an
additional purging step to a second tenax liner which can then be desorbed to the same injection port liner
used for the simple static headspace. In this case the previous abundant compounds are overloaded in the
chromatogram but many additional trace compounds are now apparent.
Download

Analysis of Butylated Hydroxytoluene in Food with Headspace Trap-GC/MS

a p p l i c at i o n n o t e

Gas Chromatography/
Mass Spectrometry

Company: PerkinElmer
Author

Meng Yuan

PerkinElmer, Inc.
Shelton, CT 06484 USA

Analysis of Butylated Introduction

This application note will demonstrate a fast and easy analytical technique to determine the
Butylated hydroxytoluene
Hydroxytoluene in (BHT, 2,6-di-tert-butyl-4-methylphenol)
is a common food additive. BHT is found
Food with Headspace in many types of food including butter,

Trap-GC/MS meats, cereals, chewing gum, baked

goods, snack foods, dehydrated potatoes
and beverages. It is used to preserve food
odor, color and flavor. BHT is oxidized
preferentially in fats or oils, protecting
the foods from spoilage.

amount of BHT in foods. Headspace sample introduction is used because it provides a means to
Concern exists that long-term human consumption of BHT may have potential
health risks. It has undergone the additive application and review process
required by the U.S. Food and Drug Administration (FDA); the committee concluded
that no evidence in the available information on BHT demonstrates a hazard to
the public when it is used at levels that are now current and in the manner now
practiced. However, uncertainties exist requiring that additional studies should
be conducted.1 The chemical properties which make BHT an excellent preservative
may also be implicated in health effects. The oxidative characteristics and
metabolites of BHT may contribute to carcinogenicity. Some people may have
difficulty metabolizing BHT, resulting in health and behavioral changes.

analyse food without any sample preparation. Headspace eliminates the need for solvents and
other sample preparation steps to reduce cost and complexity of extraction. In this method, an
adsorbent trap is used to concentrate the headspace sample and increase sensitivity, allowing for low-level
detection or small sample sizes.
Download

Application Note
Determination of 2,4,6 Trichloroanisole in Cork and Wine with HS-SPME/GCMS
Company: Shimadzu
Determination of 2,4,6 Trichloroanisole in cork
and wine with HS-SPME/GCMS
- standard
- fast

Cork stoppers used for wine bottles can effect For the method optimization in a first step a
the taste of the wine. The main contaminant is liquid standard was injected. In the second
the well known 2,4,6-Trichloroanisole. This is step the liquid extract prepared a stated
an off-flavor which is believed to be produced above was spiked with TCA. To have
by methylation of phenols of the cork tree and maximum intensity the MS was run in
final bleaching of the cork. Human nose and selected ion monitoring (SIM).
taste can trace back down to about 5-10 ng/L
(5-10 ppt). For the quality control of cork 10.0(x10,000)

stoppers therefore an enrichment technique 9.0

SIM trace 195
like solid phase microextraction (SPME) is
8.0

7.0
2,4,6 TCA
needed. Then the analysis with GC-ECD or 6.0

GCMS is performed. Here the result obtained

5.0

4.0

with GCMS are reported. 3.0

Cork stoppers used for wine bottles can affect the taste of the wine. The main contaminant is
Before the headspace SPME is done a liquid 2.0

1.0

extraction was performed with the corks. For 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0
this the cork stoppers were put into a 2 L
ethanol water solution (12 %) for 24 hours at Fig. 2: Top: SIM 1) data of mass trace 195 relative to an
room temperature. Then an aliquot of 10 ml extract spiked with 17 ppt TCA compared with an unspiked
were put into a 20 ml headspace vial extract.
saturated with 3 g NaCl. The latter increases
the effectivity of the adsorption of the TCA In figure 2 the SIM data of an extract spiked
onto the fiber. As an internal standard a with 17 ppt compared to the blank extract is
deuterized TCA is added (2H5-2,4,6-TCA). shown clearly indicating the 195 amu trace
With these vials the automatized headspace- relative to the 2,4,6, TCA which was used as

the well known 2,4,6-Trichloroanisole. This is an off-flavour which is believed to be produced by

SPME experiments were performed using a
polydimethylsiloxane fiber (PDMS, Supelco).
The instrument used was a GCMS-QP2010
with an AOC-5000 autosampler. In figure 1
the incubator of the AOC-5000 is shown
when the headspace vial is placed into it.
the quantifier ion. Qualifier ions used were
210 and 212.
The SPME parameters were: Extraction
temperature and time 50 °C 30 min,
desorption at 220 °C for 2 min.
The analysis conditions used for the GCMS
were: Injection splitless 2 min with high
pressure pulse at 200 Kpa, Column: TRB 5
25 m, 0.25 mm, 0.25 µm, 50 °C 2 min,
12 °C/min 138 °C 3 min 20 °C/min 260 ° 2
min linear velocity of the carrier gas 48.2

methylation of phenols of the cork tree and final bleaching of the cork. Human nose and taste can
cm/s, interface temperature: 270ºC.
As a quantifier ion for the D-TCA the mass
trace of 215 was used. Figure 3 shows the
zoomed mass trace of 195 and 215 relativ to
a standard of 0.7 ppt. The peak of the 2,4,6
Fig. 1: 20 ml Headspace vial placed into incubator of the TCA is still clearly visible. The calibration
AOC-5000 curve is also shown in that figure.

SCA_280_065 www.shimadzu.de

trace back down to about 5-10 ng/L (5-10 ppt). For the quality control of cork stoppers therefore an
enrichment technique such as solid phase microextraction (SPME) is needed. Then the analysis with GC-ECD or
GCMS is performed. Here the result obtained with GCMS are reported.
Download
 TDTS Automatic Detection of Trace Target Compounds in Complex Chemical Emission Profiles from
Products and Materials
Thermal Desorption Technical Support
Note 90: Automatic detection of trace target compounds in
complex chemical emission profiles from products and
materials

Company: Markes International

Keywords:
Chemical release, product emissions, plasterboard, mahogany, childrens’ toys, trace analysis,
target compounds

Background To operate TargetView, the GC/MS datafile is simply

imported into the software post-run and reprocessed.
Under new regulations, manufacturers of construction
The software can be configured to search for multiple
products and consumer goods are responsible for
target compounds within a library and is available pre-
identifying and measuring any dangerous chemicals
programmed with target libraries for emission testing
which could be emitted (released) by their products
(e.g. AgBB1/AFSSET2 ‘LCI’ [lowest concentrations of
under normal use. This is to make sure that they don’t
interest] compounds or California 013503 ‘CREL’ [chronic
pose a risk to consumers. The toxic and odorous
reference exposure levels] compounds). Ultimately, a
chemicals of interest are specified in standard protocols
simple report is produced for each sample, listing all
and include a wide range of volatile and semi-volatile
target components identified in the emission profile.
organic compounds ([S]VOCs).
TargetView is compatible with a variety of commercial
These new regulations are driving industry to implement
GC/MS file formats. It works by applying sophisticated
chemical emissions testing in-house, both for quality
chemometric processes to the data. Firstly, it selectively
control (QC) and for research and development (R&D).
eliminates any background, (water/air offset, column
Testing chemical emissions from products usually
bleed, etc.), from the TIC using ‘dynamic background
involves placing product samples in environmental
compensation’ (DBC). Figure 1 shows a comparison of
chambers, or micro-chambers, with subsequent vapour

Under new regulations, manufacturers of construction products and consumer goods are
the raw data and the DBC-reprocessed data. The process
sampling onto sorbent tubes and thermal desorption
of background compensation eliminates interfering
(TD)–GC/MS analysis. The emission profiles yielded from
background ions from the spectra of the
a product or material can be complex and contain many
chromatographic peaks. The enhanced spectral purity
target compounds at trace levels. This makes them time
and flatter baseline of the reprocessed data facilitate
consuming and difficult to interpret correctly, particularly
efficient data-mining and compound identification by the
in a busy industrial QC laboratory.
subsequent stages of TargetView.
An advanced software package (TargetView™; ALMSCO

www.markes.com
Note that TargetView creates a second reprocessed file
International, a division of Markes) has been developed
for each sample. The original data file is left intact
as an automated tool for interpretation of complex total
(without background compensation) and available for
ion chromatographic (TIC) data. Via sophisticated
calculations such as TVOC determination, if required.

responsible for identifying and measuring any dangerous chemicals which could be emitted
chemometrics, TargetView is able to identify target
compounds (e.g. those from a regulatory list) within
complex GC/MS chromatograms.
Introduction to TargetView
TargetView has been designed primarily for ease-of-use,
allowing non-experts to analyze emission profiles from
real-world samples. However, it can also be used to
enhance and speed-up detailed emission profile analysis
for research purposes.
The spectra of co-eluting peaks are then deconvoluted,
allowing each individual mass ion to be assigned to the
appropriate compound. ‘Principal component analysis’
(PCA; i.e. pattern recognition) is then applied to the
deconvoluted spectra to identify any compounds in the
sample which match target components in the library.
A match co-efficient is calculated (0–1), and compounds
with a co-efficient below a specified value (e.g. 0.9) can
be eliminated to enhance confidence in the results.
These ‘hits’ are then listed in a simple report format.

(released) by their products under normal use. Testing chemical emissions from products usually
Markes International Ltd. T: +44 (0) 1443 230935 F: +44 (0) 1443 231531 E: enquiries@markes.com

involves placing product samples in environmental chambers, or micro-chambers, with subsequent vapour
sampling onto sorbent tubes and thermal desorption (TD)–GC/MS analysis. An advanced software package has
been developed as an automated tool for interpretation of complex total ion chromatographic (TIC) data.
Download

Detecting Drugs of Abuse: Enhanced Identification Using Benchtof-dx™ and Associated Software
Company: ALMSCO
Application Note: ANBT12

Detecting drugs of abuse: Enhanced identification using

BenchTOF-dx™ and associated software

Introduction

When screening urine for drugs of abuse

(DOA), reliability is crucial. Detection of
compounds such as marijuana, cocaine,
heroin and amphetamines, as well as
their metabolites, is commonly carried
out by GC/MS, however the complexity
of a sample such as urine can present an
analytical challenge. High matrix effects
and frequent co-elution can signicantly
compromise reliability of identication,
particularly for DOA at trace level,

In this study, a urine sample was obtained for DOA analysis. Fast GC was performed with MS
therefore these factors need to be
addressed.

Traditionally used quadrupole MS Figure 1. The BenchTOF-dx time-of-ight mass spectrometer from ALMSCO International
systems are signicantly restricted in
terms of sensitivity when used for
Of late, increasing attention has been In this study, a urine sample was
screening (i.e. in scan mode) and spectra
drawn to modern time-of-ight (TOF) MS obtained for DOA analysis. Fast GC was
obtained are commonly affected by the
instruments as a potential solution to performed with MS detection using the
phenomenon of spectral skew, resulting
complex mixture screening. New systems BenchTOF-dx. The instrument’s
in false-positive or -negative results.
are able to acquire data over a very wide associated software incorporates
Increased sensitivity may be provided in
mass range at very fast scan rates. These background-compensation,
SIM mode, however whole sample

detection using the BenchTOF-dx. The instrument’s associated software incorporates background-
screening is not viable as the number of
compounds identiable is very limited.
Additionally, the identication of certain
polar drugs of abuse using GC/MS has
historically necessitated derivatisation.
It is these limitations that require a
screening technique that offers high
sensitivity and quality spectral data for all
compounds, including trace-level,
regardless of sample complexity.
robust instruments are achieving
popularity due to well-documented high
levels of sensitivity. However, a signicant
drawback of TOF MS systems to date has
been the generation of spectra that do
not resemble quadrupole-acquired
spectra. This means users’ existing or
commercially available (e.g. NIST)
libraries are not applicable for compound
identication, necessitating the laborious
and undesirable creation of bespoke,
TOF-specic spectral libraries.
deconvolution and data-mining which
enhance and automate the identication
of target compounds in very convoluted
data. In the software, a spectral library of
the compounds of interest is compiled
and the total ion chromatogram (TIC) of
the urine sample is searched for
matching spectra. The capabilities of this
software are enhanced by the high
quality spectra produced by the
BenchTOF-dx.

compensation, deconvolution and data-mining which enhance and automate the identification of
The recently-introduced BenchTOF-dx™
TOF MS (Figure 1), however,
demonstrates breakthrough capability to
provide exceptional sensitivity in
addition to spectra that exactly match
‘classical’, quadrupole-generated spectra,
resulting from very high data acquisition
speeds (up to 10,000 Hz; 560
spectra/second). Identication using
established or commercially available,
libraries is therefore possible, ensuring
Experimental
A urine sample was collected from a
methadone substitution programme.
Glucuronide separation was followed by
sorptive extraction (SPE) using SPEC DAU
cation exchangers to extract the organic
compounds from the urine. SPE is a
highly selective and sensitive technique
for sampling volatile compounds (such as
DOA) from aqueous matrices.

target compounds in very convoluted data. In the software, a spectral library of the compounds of
speed and accuracy of results.

WWW.ALMSCO.COM
Gwaun Elai Medi Science Campus | Llantrisant | RCT | CF72 8XL | United Kingdom
T: +44 (0)1443 233920 | F: +44 (0)1443 231531 | E: enquiries@almsco.com

interest is compiled and the total ion chromatogram (TIC) of the urine sample is searched for matching spectra.
The capabilities of this software are enhanced by the high quality spectra produced by the BenchTOF-dx.
Download

TDTS Food Decomposition Analysis Using the Micro-Chamber/Thermal Extractor and TD-GC/MS
Company: Markes International
Thermal Desorption Technical Support
Note 95: Food decomposition analysis using the
Micro-Chamber/Thermal Extractor and TD-GC/MS 

Keywords:
VOC, food, flavour, fragrance, dynamic headspace, shelf life

Introduction
The shelf life of food products is of huge interest to the
food industry. The main factor governing the period of
shelf life is the rate of decomposition. As food
decomposes, the emission profile changes such that the
desirable flavour compounds diminish while unfavourable

The shelf life of food products is of huge interest to the food industry. The main factor governing the
off-odours and hazardous compounds are emitted.
Valuable information regarding the rate of decomposition
and release of undesirable compounds can be obtained
by sampling and analysing the vapours emitted by a
product over time. Markes International’s Micro-
Chamber/Thermal Extractor™ (µ-CTE™) provides industry
with a compact dynamic headspace extraction Figure 1: The Micro-Chamber/Thermal Extractor (µ-CTE) units
instrument, which allows accurate control of an
atmosphere and extraction of emissions from multiple TD is a GC-specific sample concentration technique used
samples simultaneously. to significantly increase the sensitivity of organic
analysis. Markes’ leading-edge TD technology benefits
The µ-CTE has been designed for simplified dynamic from several key innovations pioneered by Markes

period of shelf life is the rate of decomposition. As food decomposes, the emission profile changes
headspace sampling of product emissions with minimal International over recent years. Examples relevant to this
sample preparation. Two versions of the µ-CTE are application include:
manufactured by Markes; one comprising four individual
chambers of 114 mL capacity and one comprising six • Compatibility with every TD application (including
chambers of 44 mL capacity (figure 1). All chambers are reactive species; amines, thiols, etc.) using a single
inert-coated stainless steel to minimise sink effects and valve/flowpath configuration.
www.markes.com

aid the recovery of very reactive species. Samples
including foods, drinks, ingredients, packaging, etc. may
be placed into the individual chambers within the unit,
incubated at a selected temperature and purged with a
constant flow of pure air or inert gas.
• The ability to quantitatively re-collect samples for
repeat analysis and method validation. Available on
manual and automated models.
• World’s most effective cryogen-free focusing offers

such that the desirable flavour compounds diminish while unfavourable off-odours and hazardous
Following an equilibration period, clean sorbent tubes are
connected to the outlet of each individual micro-chamber
to collect the organic vapours purged from the sample in
the flow of pure air or gas. Sorbents may be chosen to
retain all emitted headspace vapours or to selectively
retain key olfactory compounds while potential
interferences such as water, ethanol or acetic acid are
purged to vent. The sorbent tubes are subsequently
analysed by thermal desorption (TD) with GC(MS).
maximum uptime (no risk of ice blockage) without
compromising retention of ultra-volatiles.
• Efficient backflush desorption of the sorbent tube
and focusing trap offers simultaneous analysis of
compounds over a wide boiling range combined
with optimum sensitivity.
For further information see Markes’ Series 2 UNITY™ and
TD-100™ brochures.

compounds are emitted. Valuable information regarding the rate of decomposition and release of
Markes International Ltd T: +44 (0) 1443 230935 F: +44 (0) 1443 231531 E: enquiries@markes.com

undesirable compounds can be obtained by sampling and analysing the vapours emitted by a product over
time. This note describes the application of a Micro- Chamber/Thermal Extractor™ (μ-CTE™), compact dynamic
headspace extraction instrument, which allows accurate control of an atmosphere and extraction of emissions
from multiple samples simultaneously.
Download
Products

GC Pressure and Flow Calculations iPhone/ Separation of Drugs of Abuse

iPod Application Company: Phenomenex
Company: Agilent
Manufacturer’s description: Available from Phenomenex is an optimized
Manufacturer’s description: Agilent has developed phase for the separation of drugs of abuse. The Zebron™ ZB-Drug-1
a GC pressure and flow rate calculator app for the column provides at least 30% faster run times than existing technologies
iPhone/iPod to instantly and accurately determine and delivers improved resolution of target analytes, according to the
pressure and flow through open tubular capillary manufacturer. Zebron ZB-Drug-1 is a mid-polarity stationary phase that
columns. The Agilent GC Calculator app is based on separates target analytes from the common matrix interferences found in
the PC version that has been downloaded more than 10,000 times from the biological samples. Reported features of the column include:
Agilent website. The GC calculator enables you to:
• Fast analysis with good peak shape
• See how different GC conditions affect column flow and pressure before • Specially deactivated to improve quantification for drug compounds
setting up a system • Improved resolution of target analytes from matrix interferences
• Determine if your current column dimensions are appropriate and/or
what your inlet pressure should be when switching from GC (atmospheric For more information, visit www.phenomenex.com
pressure) to GC/MS (vacuum)
• Calculate new parameters when switching to a different carrier gas, such
as going from helium to hydrogen for faster chromatography
• Predict hold-up times during troubleshooting
• Check if your inlet can handle higher pressures associated with narrow
bore capillary columns

For more information, click here

For information on how to use the app, click here

Agilent GC Calculator works with iPhone 4®, iPhone 3G™, the original iPhone™, and iPod touch®.
Apple, the Apple logo, iPod, iPod touch, and iTunes are trademarks of Apple Inc., registered in the U.S. and other
countries. iPhone is a trademark of Apple Inc. App Store is a service mark of Apple Inc.
 Matthew Klee’s
GC Masterclass
2 day
Advanced Topics in Capillary Gas Chromatography – €695
Getting More from your GC
3-4 November, 2010

Venue: Park Inn Manchester, Victoria, UK

Day 1
1. Capillary GC tune-up
2. Large volume injection
3. Auxiliary sampling and focusing
4. Fast GC – how to painlessly and quickly migrate your current methods

Day 2
1. Multidimensional separations (instrumentation, practice)
2. Capillary column backflushing – BF with benefits
3. Automated sample preparation
4. Optimal mass spec.
5. Method development and troubleshooting - interactive discussion

CLICK HERE TO
REGISTER ONLINE

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