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SP 191-3

Determination of Water-Cement Ratio in Hardened


Concrete by Optical Fluorescence Microscopy

by U. H. Jakobsen, P. Laugesen, and N. Thaulow

SYNOPSIS
This paper describes a method for determining the water to cement ratio (w/c)
of hardened concrete using optical fluorescence microscopy. The method is well
established and has been used for many years. In Denmark the method is used for
quality control of hardened concrete. The method is based on vacuum impregnation
of concrete using a yellow fluorescent epoxy. During impregnation the capillary
porosity, cracks, voids, and defects in the concrete are filled with epoxy. The amount
of fluorescent dye entering the cement paste depends on the capillary porosity,
which is determined by the w/c and the degree of hydration. After impregnation
and hardening of the epoxy a thin section of concrete with a thickness of 0.020 mm
(20 J..lm) is prepared. The thin section is analyzed under an optical microscope using a
combination of a blue excitation filter and a yellow blocking filter. This is the
fluorescent light mode in which epoxy filling air voids and cracks appears
yellow, cement paste as shades of green, and aggregate black. The shade of green
of the cement paste depends on the capillary porosity. A sample with low w!c
appears dark green, i.e. has less fluorescence intensity due to a low amount of
epoxy within the paste. A sample with high w/c appears light green, i.e. has high
fluorescence intensity. These shades of green (fluorescence intensity) are used to
determine the wlc by comparing the fluorescence intensity of the cement paste
with the standards of known wlc. This paper describes the fluorescent impregnation
technique, the thin section preparation, the visual determination of w/c and discusses
the pitfalls in the w/c determination. Furthermore, the paper presents data from a
quality assurance project and damage analysis and data of Round Robin Testing.

Keywords: field tests; fluorescence; microscopy; vacuum forming; water-cement


ratio

27
28 Jakobsen et al.

U.H. Jakobsen is Chief Consultant at G.M. Idorn Consult, RAMBOLL. She has
10 years of experience in concrete petrography using optical and scanning electron
microscopy. She is involved in the forensic determination of deteriorated concrete.
Her work focuses on alkali silica reaction, delayed ettringite formation and external
sulfate attack.

P. Laugesen is senior geologist at Dansk Beton Teknik NS. He is an expert in


concrete microstructure, with 15 years of experience in concrete technology and
petrography. He works with quality assurance of concrete structures during
construction. damage analysis of older concrete structures and materials research.
He also participates in development of test methods and laboratory equipment.

ACI member N. Thaulow is the Principal of G.M. Idorn Consult, RAMBOLL.


He has more than 30 years experience in concrete petrography and concrete
materials technology. He frequently acts as an expert witness in concrete litigation
throughout the world. He is a member of ACI committee 201, Durability.

INTRODUCTION

The w/c is generally recognized as one of the most important mixture design
parameters for concrete. because the w/c effects the strength and durability of
concrete. It is easy to control the w/c in the concrete-making process. In hardened
concrete it is not possible to determine the w/c directly. There is a need for an
indirect, precise method for determination of the w/c in hardened concrete both for
quality control in young concrete and in the forensic determination of deteriorated
concrete. Optical microscopy of fluorescent impregnated thin sections has proven
to be such a method.
Optical microscopy offers a large field of view that facilitates an excellent
understanding of the microstructure and the possible causes of production faults or
deterioration mechanisms. Furthennore, it is fast and a fairly low cost type of
examination. The information obtained from the optical microscope is markedly
enhanced by adding a fluorescent facility to the two ordinary light modes namely
plane polarized and crossed polarized light. The fluorescent illumination gives
infonnation about the capillary porosity (w/c), transition zone porosity. cracks,
crack pattern, air void system, porosity of aggregates and paste defects,
information necessary for evaluating the quality and the condition of the concrete.
Optical fluorescence microscopy of concrete has been a principal tool in
examination of hardened concrete in Denmark for many years. The method is
accepted as a NORDTEST Standard since 1991 (1) and used for quality control as
well as for evaluating deteriorated concrete. The microscopic examination for
quality control follows a Danish Standard procedure, the TI-B 5 (2). and the
accredited laboratories performing analyses participate in an annual Round Robin
test. The microstructure of the concrete is examined according to the standard
procedures.
Water-Cement Ratio and Other Durability Parameters 29

For mature concrete the degree of hydration is high and there is a good
correlation between the capillary porosity of the cement paste and the w/c as
shown in Table 1. The yellow light generated in the fluorescent epoxy has a visual
intensity. which is proportional to the amount of fluorescent epoxy present in the
cement paste. The intensity can therefore be used as a direct measurement for the
capillary porosity and hence the w/c. The change in capillary porosity with w/c is
more pronounced at lower w/c than at higher w/c (Table 1). It is therefore much
easier to see the change in fluorescence intensity in going from w/c 0.40 to 0.45
than from 0.60 to 0.65. By comparing with standards of known w/c the w/c of an
unknown concrete sample can be determined visually quite accurately or measured
by automatic image analysis.
Visually determination of the w/c by optical fluorescent microscopy has been
described in several papers since 1980 (5, 6, 7. 8, 9, 10, 11, 12, 13). The method
has also been used in conjunction with image analyses in the !A-Project (14) and
by Elsen et a!. ( 15), Gran ( 16) and Jakobsen et a! ( 17).

METHODS

Fluorescence Impregnation Technique


The w/c determination of hardened concrete is performed microscopically using
fluorescent thin sections. To prepare fluorescent thin sections the concrete has to be
vacuum impregnated with a fluorescent epoxy (18, 19, 20, 21 ). An example of
components shown useful for fluorescent epoxy is given below:

Epoxy Resin: BY !58 from Ciba Geigy


Hardener: HY 2996 from Ciba Geigy
Fluorescent dye: Epo-dye from Struers

The procedure for mixing the fluorescent epoxy follows two steps:

• 1.28 grams of powdered fluorescent dye are mixed with 98.72 grams epoxy
resin to give a total of 100 gram. The solution is stirred for 24 hours. The
fluorescent resin shall be kept in a dark place until use.
• 100 grams of fluorescent resin is mixed with 28 grams of hardener
immediately before use. Following this procedure the final mixture contains
1% (w/w) fluorescent dye.

During preparation of the fluorescent epoxy, it is important always to use the


same concentration of fluorescent dye in the epoxy. Too much or too little of the
fluorescent dye will change the intensity of the green shade of the cement paste
when observed in the fluorescent light mode and make comparisons to standards
uncertain.
Depending on the condition of the concrete core. the first step of impregnation
30 Jakobsen et al.

may be a full size vacuum impregnation of the core with fluorescent epoxy (Fig.
1). A cracked or weak core should always be full size impregnated before any
cutting is performed to avoid further cracking during preparation. The vacuum
impregnation procedure is described below:
• The sample must be dry before impregnation but should not be exposed to
temperatures above 30-35 oc.
• The sample is wrapped in a strong plastic bag and placed in the desiccator and
evacuated for approximately 2 hours. A pump giving a specified maximum
vacuum corresponding to a pressure of3xl0-2mbar is suitable for evacuation.
• Fluorescent epoxy is sucked into the evacuated desiccator (through a tube to
the bottom of the sample) until the sample is completely covered. The vacuum
is released after 3-5 minutes.
• The sample in its plastic bag is removed from the vacuum chamber and placed
in a suitable beaker of water to cool, preventing excess heating from the
hardening of the epoxy. Care is taken not to mix any water into the epoxy.
• The epoxy is hardened after about 15 hours at 20-25 oc.
After hardening of the epoxy, the sample is cut and features such as cracks can be
studied macroscopically using UV-light (Fig. 1). Details ofthis method have been
discussed by Hemichsen & Laugesen (22) and Jakobsen (13). After this step. the
sample is ready for further cutting for thin sectioning.
Fluorescent Thin Section Preparation
The thin sectioning can be described in five steps as illustrated in Fig. 2:
Step 1 The concrete sample is cut into small blocks corresponding to the size of
the tina! thin section (e.g. 35 x 45 mm and a thickness of at least 20 mm).
Step 2 One side of the sample piece is glued onto a piece of window glass as
reference plane. The opposite side is ground and lapped until final thin
section quality before the next impregnation step. The following procedure
is used for impregnation:
0 The sample piece is placed in pure alcohol for approximately 15
seconds and dried in an oven for about 1 hour at a maximum
temperature of35 oc.
0 The sample is placed in a suitable beaker, placed in the desiccator and
evacuated for approximately 2 hours.
0 Fluorescent epoxy is added without vacuum release and the vacuum is
released after 3-5 minutes.
0 The sample is left for another 10 minutes and then removed from the
epoxy.
0 The impregnated sample is covered by a piece of strong plastic film in
order to minimize the amount of excess epoxy left on the surface.
0 The epoxy is generally hardened after 15 hours at 25 oc.
After hardening. the excess epoxy and further 0.005 mm of the ground concrete
surface is ground away. Plane parallel grinding is of utmost importance in this step.
The impregnation of the capillary porosity is checked by use of a stereo
Water-Cement Ratio and Other Durability Parameters 31

microscope with UV -light mode"


Step 3 The impregnated re-ground surface is glued onto an object glass using
UV-hardening glue.
Step 4 The concrete with the window glass attached is cut off leaving
approximately 0.5 mm attached to the object glass for thin sectioning. The
thin section is then ground and polished to a thickness of 0.020 mm (20
!lm).
Step 5 Finally a cover glass is glued onto the ground surface using UV -hardening
glue.
Minor refinements to the method described above may be necessary due to the
use of different lapping equipment.
The thickness of the finished thin section is checked by the interference colors of
quartz in crossed polarized light. With a thickness of 20 11m of the section, the
color of quartz is white to gray. A thickness of 25-30 11m can be accepted as long
as the reference samples are of the same thickness. However, for other
petrographic purposes (such as cement type determination and analysis of powder
dispersion) the standard thickness of20 11m has proved to be superior.
Importance of Proper Impregnation and Regrinding
The general impregnation depth of the fluorescent epoxy into the work piece is
dependent on the capillary porosity of the cement paste (23). Fig. 3 shows an
example of the impregnation depth of 2 samples, one with a w/c of 0.40 and one
with w/c 0.60. As seen from the sketch, the impregnation depth is rather restricted
and it is therefore important to place the thin section as close to the impregnated
surface as possible to get a fully impregnated thin section. However, it is likewise
important to regrind sufficiently to remove excess epoxy on the surface of the
sample to prevent ·false' porosity appearance.
The restricted impregnation depth calls for great accuracy in re-grinding the
impregnated sample. If the re-grinding depth is too large, the cement paste in the
finished thin section is not impregnated through its full thickness. Likewise, if the
re-grinding is not parallel to the impregnated surface, the ·deeper lying part' of the
thin section may not be well impregnated.
The impregnation depth has been measured in a series of impregnated and cross-
sectioned work pieces from concrete, ranging in w/c from 0.35 to 0.70. The
impregnation depths are given in Table 2. As seen from the table the process of
impregnation and re-grinding is of outmost importance for the quality of the thin
section especially when preparing thin sections of concrete with low w/c. The
impregnation depth of a sample with a w/c of 0.35 is only 0.020-0.050 mm. It is
worth mentioning when impregnating concrete that various highly permeable
features such as larger crack systems, aggregate de-bonding, interconnected
porosity, and agglomeration of air voids are readily impregnated. Hence, these act
as 'impregnation surfaces', causing the cement paste to be impregnated to larger
depths through them. Such causes of increased impregnation depth were not
present in the samples of Table 2.
32 Jakobsen et al.

W /C DETERMINATION USING FLUORESCENT LIGHT

The vacuum impregnation of the concrete samples with epoxy causes the
capillary porosity of the cement paste to be filled with the fluorescent epoxy. By
transmitting light, from a 25-100 W halogen light source and using a combination
of a blue excitation filter (BG 12) and a yellow blocking filter (K51 0 or K530),
through the optical, polarizing microscope the fluorescent epoxy transmits light.
The fluorescent set-up of the microscope is illustrated in Fig. 4.

Visual W/C Analyses


Before using the thin section for w/c detennination, it is checked for possible
preparation damages. This check is performed both in ordinary polarized, crossed
polarized and fluorescent light. Areas, which may give errors in the w/c
determination, are located and marked so that they can later be avoided during the
w/c determination. For example areas of carbonation or local Ca(OH) 2 depletion
should be avoided. Furthermore, only areas of correct thickness should be
measured.
When determining the w/c visually the green intensity of the cement paste is
compared to standards made with known w/c, in the range of 0.35 to 0. 70 varying
in increments of0.05. Two different operators can determine concrete with known
w/c by an accuracy of ±0.02 within the target value. Fig. 5 shows the appearance of
the cement pastes of varying w/c when viewed in fluorescent light.
W /C Determination on Field Concrete
The following examples show results of w/c determination by fluorescent
microscopy of samples from field concrete.
Petrographic analysis, including fluorescence impregnated thin sections, was
applied as QA/QC during the construction of concrete pavements, for aprons in
Copenhagen Airport in 1994. From 43 concrete cores a w/c average of 0.35 was
obtained. a number, which was only 0.02 lower than the value specified for the
mixture (Table 3). All procedures during hatching and mixing of the concrete
pavements were carefully controlled. The standard variation on the determination
was 0.006, which includes both the uncertainty in the visual w/c-determination and
the actual variations in the concrete. This shows that the fluorescence method is
very accurate with a small variation when an experienced petrographer performs
the analysis.
Determination of w/c of precast concrete railroad ties was performed on 522 thin
sections representing 127 ties (Fig. 6). The ties were in field service for a number
of years before determination of w/c. The average w/c of the ties was determined
to 0.42, a number which was only 0.02 lower than the average w/c used in the
production. The standard deviation was 0.026. Again a single experienced operator
did the determinations.
The precision of the method is regularly examined in laboratories with more than
one petrographer. Two experienced petrographers in the laboratory of G.M. Idom
Water-Cement Ratio and Other Durability Parameters 33

Consult, RAMBOLL, determined the w/c of 7 unknown mortar coatings from


prestressed lined cylinder concrete pipe in 1991. A total of 16 thin sections were
analyzed. The results are shown in Table 4. The standard deviation for each
petrographer includes both real variations in the mortar coatings and the
uncertainty of the w/c determination by fluorescence microscopy. It is seen that the
average for operator 1 is 0.350 with a standard deviation of0.014. For operator 2
the average is 0.356 with a standard deviation of0.023.

ROUND ROBIN TESTING

The Danish Accreditation Agency, DANAK. audits petrographic analysis of thin


sections of hardened concrete by Round Robin testing. These round robin tests
include the determination of capillary porosity, as equivalent w/c. Accredited
laboratories have to follow the requirements set out in the "Danish Agency for
Development of Trade and Industry Statutory Order No. 258 of 11 April 1994''.
DANAK circulates thin sections prepared by one laboratory to the participating
laboratories for w/c determinations. Table 5 shows some results of the Round
Robin testing. The results are given as equivalent w/c. The laboratory ID on the
results scheme is changed from year to year. The w/c from the mix designs given
at the bottom of Table 5 is unknown to the participants until the testing is closed. If
a laboratory one year obtains an unsatisfactory result the laboratory has to explain
their procedure to DANAK and possible improve their procedure to maintain their
accreditation. Examples of laboratories out of line are laboratory No. 4 in 1991 and
laboratory No. 2 in 1992 (Table 5). The Round Robin test is by itself a powerful
tool to keep up the standards of optical microscopy amongst the laboratories.
Modern specifications for concrete production often require a maximum
deviation of the amounts of the constituents of a mixture of 5% from the target
values. This corresponds in most concrete to an interval of ± 0.03 in w/c (25).
which is only possible to obtain by strict control during production of the fresh
concrete. As can be seen from Table 5, the detern1ination of the w/c is conducted
with accuracy at the same level as in concrete production. Hence, the thin section
teclmique is a prudent tool in QA/QC of concrete production and construction.

PITFALLS IN W/C DETERMINATION OF FLUORESCENT THIN


SECTIONS

To ensure correct detennination of the w/c in hardened concrete a series of


requirements to the thin section specimens are relevant:
• The concrete specimen should be reasonably well hydrated (preferably with a
maturity of28 days or higher)
• The thin section shall have a uniform thickness
• The thin section shall have the same thickness as the reference thin sections
(preferably 20 ~m)
• There should be no signs of damage from coring. cutting, grinding and lapping
34 Jakobsen et al.

• There should be limited leaching of mineral phases. Leaching may change the
capillary porosity
• Grinding sludge should not be present in pores, cracks etc.
• Same treatment (e.g. drying temperature and time, evacuation pressure and
time) should be applied as for the reference thin sections
• The concrete should be thoroughly impregnated by fluorescent epoxy
• The fluorescence intensity in the epoxy should be as the reference thin sections
• There should be no un-dissolved grains of fluorescent powder in the epoxy
• There should be no surplus fluorescent epoxy left over on the reground surface
of the thin section, giving 'false' fluorescence intensity
• There should be no fluorescence halos over dense areas such as aggregates -
note that porous aggregate such as opaline sand may exhibit a marked
fluorescence intensity
The impregnation and the preparation steps are very important and it is
fundamental that the technician is experienced in the procedure and in using the
microscope for quality control of the section. It is very important that the concrete
thin section is fully impregnated. Poor impregnation can be due to many factors
including incomplete drying, excessive re-grinding of the impregnated surface, or a
non-parallel grinding process. Other possible problems during preparation are poor
vacuum, old epoxy and insufficient mixing of the epoxy components. During thin
section production the use of a checklist may secure the needed quality.
It is well known that addition of pozzolans influence the capillary porosity. If
pozzolans, such as silica fume, fly ash and slag. is found in the hardened concrete
the w/c determined should be reported by the term 'equivalent w/c '. When
concrete contains pozzolans an activity factor could be used to calculate the actual
w/c (25. 26). The activity factor is the number of kg cement that gives the same
change in capillary porosity as one kg of pozzolan in the concrete. Activity factors
for the actual pozzolan could be determined experimentally or may be found in
tables.
Various parameters may influence the capillary porosity of hardened concrete.
some of which are not normally included in the computation of w/c of a mixture
design. These parameters include:
• Volume of cement paste in the concrete
• Specific surface of the sand
• Addition of pigments
• Addition of other binder systems, e.g. polymers
To deal with this a qualified operator is required. An untrained operator may get
false results if the w/c determination is perfom1ed on carbonated or severely
leached paste. On the other hand, a trained operator can make the w/c
determination very accurately.
The impregnated thin sections shall be kept in a dark drawer as the intensity of
the fluorescent dye decreases during time and during exposure to light. It is
Water-Cement Ratio and Other Durability Parameters 35

therefore important to prepare new standards relatively often (for instance


biannually).
It has been shown by Jakobsen et al. ( 17) that the light source in the microscope
fades. An old halogen bulb has lower intensity than a new one. This property,
however. is not so important when estimating the w/c visually in which
comparison to standards are performed regularly. When using automatic image
analysis for determining w/c new calibration curves have to be measured at regular
intervals to compensate for the fading.
As discussed the production of adequate thin section specimens for analysis is not
an easy task. However, available fully automated equipment may facilitate a
consistent and flawless production at a relatively low cost.

CONCLUSION

The water to cement ratio of hardened concrete can be determined by optical


fluorescence microscopy. To obtain reliable determinations an experienced
petrographer is needed. Moreover, the thin sections used have to be of a uniform.
high quality with full impregnation and well-defined thickness.
The method has been used extensively over 20 years especially in Northern
Europe and was accepted as a NORDTEST Standard, NT Build 361 in 1991.
Experience with field concrete and with Round Robin tests performed in Denmark
annually show that the expected accuracy of the method is about ±0.02.

REFERENCES

1. Nordtest Method, NT Build 361, 1991: Concrete, Hardened: Water-cement ratio


2. T1-B 5 1987: Petrographic Analysis in Connection with Quality Control (in Danish).
3. Jensen, A.D., Eriksen, K., Chatterji. S., Thaulow, N. and Brandt, I. 1985: Petrographic analysis
of concrete. Beton-Teknik, CtO, Aalborg Portland, 4/07
4. Powers, T.C. 1958: The physical structure and engineering properties of concrete. PCA
Research Dept. Bull. 90
5. Thaulow, Nand Jensen, A.D. 1980: Vakuumbeton. Struktur og Luftindhold (in Danish). Dansk
beton 4
6. "Concrete Durability. An investigation of recently constructed motorway bridges in Denmark",
Danish Ministry ofTmasport. The Road Directory. 1980
7. Thaulow, N .. Jensen, A.D., Chatterji, S., Christensen. P. and Gudmundsson, H., 1982:
Estimation of the compressive strength of concrete samples by means of fluorescence
microscopy. Nordisk Belong, 2-4
8. Mayfield, B. 1990: The quantitative evaluation of the water/cement ratio using fluorescence
microscopy. Magazine of Concrete Research, no. 150, pp. 45-49
9. Jomet, A., 1991: Optical and fluorescence microscopy: Potential and limitations. Proc. 3th
Euroseminar Microscopy Building Materials, Barcelona, Spain
10. Laugesen, P. 1993: Effective w/c ratio of cement paste in concrete. Proc. 4th Euroseminar on
Microscopy Applied to Building Materials, Wisby, Sweden.
11. Laugesen, P. 1995: The use of petrography in QA/QC of concrete. Proc. 5th Euroseminar on
Microscopy Applied to Building Materials, Leuven, Belgium,.
36 Jakobsen et al.

12. Jakobsen, U.I-1., Johansen, V. and Thaulow, N. 1997: Optical microscopy- A primary tool in
concrete examination! Proc. /9 'th JCMA, Cincinnati, pp 275-294
13. Jakobsen, U.I-1. 1998: Understanding the features observed in concrete using various
fluorescence impregnation techniques. Proc. 20'th ICMA, Mexico, pp. 28/-301
14. !A-Project, !990-1994: Image Analysis for Monitoring Building Materials: CSTB, DBT,
Kontron Elektronik, BBRI: Brite I Euram Project BE-4300, Contract BREU-CT-91-0490.
15. Elsen, J., Lens, N., Aarre, T., Quenard, D., Smolej, V. !995: Determination ofthe w/c ratio of
hardened cement paste and concrete samples on thin sections using automated image analysis
techniques. Cement and Concrete Research, Vol. 25, No.4, pp. 827-834, 1995.
16. Gran, H.C. 1995: Fluorescent liquid replacement technique. A means of crack detection and
water: binder ratio determination in high strength concretes. Cement and Concrete Research 25
(5) 1063-1074.
17. Jakobsen, U.I-1., Johansen, V. and Thaulow, N. I 995: Estimating the capillaty porosity of
cement paste by fluorescence microscopy and image analysis. Mat. Res. Soc. Symp. Proc. Vol.
370, pp. 227-236
18. Romer, B. and Dubrolubov, G. 1972: Angewandte Microskopie dei der Baustotfprlifung:
Beton, Martel, Zement, Kalk, Gips, Keramik. Betonstrassen
19. Walker, H.N. & Marshall, B.F., 1979: Methods and equipment used in preparing and
examining fluorescent ultrathin sections of Portland cement concrete. Am. Soc. Testing and
Materials, pp 3-9
20. Walker, H.N. 1981: Examination of Portland Cement concrete by fluorescent light microscopy.
Proc. 3th ICMA Conference, Houston, Texas
21. Andersen, K.T. and Thaulow, N. 1990: The study of alkali-silica reaction in concrete by the use
of fluorescent thin sections. ASTM STP 1061 Petrography Applied to Concrete and Concrete
Aggregates. Erlin I Stark, editor
22. Henrichsen, A. and Laugesen, P. 1995: Monitoring of concrete quality in high perfonnance
civil engineering constructions. Mat. Res. Soc. Symp. Proc. Vol. 370, pp. 49-56
23. Johansen, V. and Thaulow, N. 1994: At what scale do homogeneous Phenomena become
localized: The necessary and sufficient magnification. Rilem Workshop "The modelling of
microstructure and its potentia/for swdying transport properties and durability", Saint-Remy-
les-Chevreuse
24. Laugesen, P. 1994: Petrographic Analysis, unpublished Accredited Reports nos. 1373-73,
1384-1388, 1391 and 1393, Dansk Beton Teknik A/S.
25. Basic Concrete Specification for Building Structures, Publication No. !03, pp. 26. Published by
The National Building Agency, Denmark 1988, ISBN 87-503-7532-6
26. ASTM C311: Standard Test Methods for Sampling and Testing Fly Ash or Natural Pozzolans
for Use as a Mineral admixture in Portland-Cement Concrete, 1995, pp. !87-193
Water-Cement Ratio and Other Durability Parameters 37

TABLE 1-RELATION BETWEEN W/C AND CAPILLARY POROSITY.


w/c % Capillary porosity
of cement paste
0.40 8
0.45 14
0.50 19
0.55 24
0.60 28
0.65 32
0.70 35
0.75 38
0.80 41
*Data are from Jensen et al. (3), based on Powers (4)

TABLE 2-IMPREGNATION DEPTH AS MEASURED ON CROSS SECTIONS OF


BLOCKS OF CONCRETE WITH DIFFERENT W/C RATIOS.
w/c ratio Depth of epoxy
impregnation
mm
0.35 0.020-0.050
0.40 0.15
0.45 0.25
0.50 0.50
0.55 0.8
0.60 1.0
0.70 1.8
*samples are made avmlable by courtesy ofiA-Project (14)

TABLE 3-W/C DETERMINATION OF CONCRETE FROM COPENHAGEN AIRPORT.


Equivalent w/c ratio No. of Thin Sections
<0.35 0
0.35 77
0.36 4
0.37 2
0.38 3
>0.38 0
Average w/c 0.35
Standard deviation 0.006
Specified w/c 0.37
*results from (24), by courtesy ofP. Jeppesen, NCC Rasmussen & Schi0tz A/S
38 Jakobsen et al.

TABLE 4-VISUAL W!C DETERMINATION PERFORMED BY TWO DIFFERENT


OPERATORS.
Thin section Operator Operator Average Difference
No. 1 2 1-2
1.1 0.35 0.35 0.35 0.00
1.2 0.35 0.37 0.36 -0.02
1.3 0.38 0.37 0.38 0.01
2.1 0.33 0.32 0.33 0.01
2.2 0.34 0.35 0.35 -0.01
3.1 0.34 0.35 0.35 -0.01
3.2 0.32 0.32 0.32 0.00
4.1 0.35 0.35 0.35 0.00
4.2 0.35 0.35 0.35 0.00
4.3 0.36 0.35 0.36 0.01
5.1 0.35 0.33 0.34 0.02
5.2 0.35 0.35 0.35 0.00
6.1 0.37 0.40 0.39 -0.03
6.2 0.36 0.40 0.38 -0.04
7.1 0.35 0.37 0.36 -0.02
7.2 0.35 0.37 0.36 -0.02
Average 0.350 0.356 0.353 -0.006
Stdev 0.014 0.023 O.D18 0.016
AbbreviatiOn: (Stdev) standard deviatiOn

TABLE 5-ROUND ROBIN TEST RESULTS OF W/C DETERMINATION.


Concrete A B c D E F G
Year 1987- I 1987 -II 1990 1991 1992 1993 1994
Laboratory 1 0.40 0.35 0.40 0.38 0.49 0.40 0.40
Laboratory 2 0.40 0.35 0.35 0.40 0.55 0.38 0.40
Laboratory 3 0.45 0.40 0.35 0.40 0.45 0.40 0.40
Laboratory 4 0.40 0.35 0.40 0.50 0.45 0.35 0.47
Laboratory 5 - - 0.40 0.40 0.40 0.43 0.37
Laboratory 6 - - 0.40 - 0.50 - -
Laboratory 7 - - 0.35 - - - -
Mean 0.41 0.36 0.38 0.42 0.47 0.39 0.41
Stdev. 0.025 0.025 0.027 0.048 0.052 0.029 0.037
w/cfrommix - - 0.37 0.43 0.44 0.42 -
AbbreviatiOns: (Stdev) standard deviatiOn,(-) data not obtamed or not available.
Water-Cement Ratio and Other Durability Parameters 39

Fig. 1-Sketch showing full-scale impregnation of concrete core. When cut,


features that have been in contact with surface of core are seen to be impregnated
with fluorescent epoxy. Features, such as cracks, can then be studied by UV light.
Arrows illustrate epoxy impregnation.

concrete block

, . . - - - - - - - Cover glass
concrete specimen
object glass

3 window glass
concrete specimen
object glass

From Nordtest Method NT BUILD 361

Fig. 2-Sketch showing steps of thin sectioning. Arrows show epoxy impregnation
step.
40 Jakobsen et al.

+·-_;

Fig. 3-Sketch showing cross sections throught two epoxy impregnated work
pieces glued onto window glass. Arrows show direction of epoxy entering. Depth
of epoxy impregnation (dark grey in figure) into concrete depends on w/c. Sizes are
not to scale.

Yellow Blocking Filter

Fluorescent Thin Section

Blue Excitation Filter

Fig. 4-Sketch showing fluorescent setup of microscope with position of filters


and thin section.
Water-Cement Ratio and Other Durability Parameters 41

Fig. 5-Micrographs take in optical microscope in fluorescent light of samples with


w/c of 0.35, 0.45, and 0.60. Field of view: 1.6 mm x 2.4 mm.

Average= 0.42
Standard deviation = 0.026
Minimum= 0.36
Maximum= 0.54
Count = 522
., 1
1:
0

~.,
0
~
E
"
z

g :Jl
0 0
w/c ratio determined by fluorescence microscopy

Fig. 6-Distribution of w/c determined by fluorescence microscopy of concrete


railroad ties. W/c of mixture design was 0.44. Data from G. M. ldorn Consult,
RAMB0LL, 1992.

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