SHRP C 662

SHRP-C-662
Concrete Microscopy
D.M. Roy
M.W. Grutzeck
B.E. Scheetz
Materials Research Laboratory

The Pennsylvania State University
University Park, Pennsylvania
• G.M. Idom
Neils Thaulow
* K.T. Andersen
G.M. Idom Consult A/S

Blokken 44 Birkerod
Denmark
Strategic Highway Research Program

National Research Council
Washington, DC 1993
SHRP-C-662
Contract C-201
Program Manager: Don M. Harriott

Project Manager: Inam Jawed
Production Editor: Marsha Barrett .
Program Area Secretary: Ann Saccomano
June 1993
key words:
cement
concrete
fluorescence
microscopy
microstructure
sample preparation
thin section
Strategic Highway Research Program

National Academy of Sciences
2101 Constitution Avenue N.W.
Washington, DC 20418
(202) 334-3774
The publication of this report does not necessarily indicate approval or endorsement of the findings, opinions,
conclusions, or recommendations either inferred or specifically expressed herein by the National Academy of
Sciences, the United States Government, or the American Association of State Highway and Transportation
Officials or its member states.
© 1993 National Academy of Sciences
350/NAP/693
Acknowledgments
m
The research described herein was supported by the Strategic Highway Research Program
(SHRP). SHRP is a unit of the National Research Council that was authorized by section
128 of the Surface Transportation and Uniform Relocation Assistance Act of 1987.
iii
Contents
°o°
Acknowledgments ................................................. in
Abstract ........................................................ vii
1 Introduction ................................................... 1
Background ................................................. 1
2 Preparation of Fluorescent, Concrete Thin-Sections ......................... 3

Instrumentation ............................................... 5
Examination of Fluorescent Thin-Sections ............................ 8
References ................................................. 11
3 Examination of SHRP 1-19 Concrete Samples ........................... 13

Introduction ................................................ 13
Samples .................................................. 13
Microstructural Data .......................................... 14
Stereological Measurements ..................................... 15
General Examination .......................................... 16
Alternate Methods ............................................ 19
References ................................................. 20
4 Discussion .................................................. 21
References ................................................. 22
" Appendix A Figures ............................................... 23
Appendix B Tables ................................................ 77
Appendix C Nordtest 677-87 Concrete, Hardened; Water-Cement Ratio .......... 101
V
Abstract
Concrete microstructure can be evaluated using both thin and polished sections. Methods
described in this report were developed as a supplement to ASTM 856 procedures. The use
of an epoxy resin containing a fluorescent dye tended to enhance the ability to view
porosity and mechanical features such as interface porosity and cracking. Relationships of
formulation and microstructure for a series of nineteen concrete samples are presented
(SHRP $89-1 to $89-19). The proposed methods are useful to the highway engineer on a
variety of levels. A less skilled operator can use the epoxy impregnation technique for
developmental and forensic purposes, to more easily observe effects of making and
formulation on homogeneity, and the relationship of cracking and secondary hydration
products in deteriorated concrete, respectively. The determination of water/cement ratio is
more difficult inasmuch as it is done visually by comparing the fluorescence intensity of the
unknown with a series of known standards.
vii
Executive Summary
Optical and electron microscopy are valuable research tools for the study of concrete
microstructure. ASTM-C-856 already has a standard practice in place giving details of how
to use optical techniques for examination of hardened concrete. The supplemental methods
described in the accompanying report were also used to examine hardened concrete
specimens, $89-1 to $89-19. Although most of the report emphasizes data obtained using
epoxy impregnated thin sections, alternate methods have also been explored (polished
impregnated samples were examined in reflected fluorescent light and in the SEM).
Either thin sections dr polished sections of concrete impregnated with an epoxy dye reveal
enhanced inherent porosity of the paste, interface porosity and effects of cracking. In
addition, water/cement (w/c) ratio can be determined by comparing paste porosity with a
series of carefully prepared standard samples.
Impregnation is achieved using a combination of thin epoxy mixed with a fluorescent dye.
The sample is evacuated with a vacuum pump for -2 hours after which the epoxy is
allowed to wet the sample and fill the pores/cracks. After the epoxy hardens one can either
polish the sample for reflected light and SEM examination or prepare a -20/zm thick thin
section for transmitted light examination. Whereas the reflected light sample may be easier
to make, it transmits light through translucent grains in the sample. The thin section sample
is harder to make but it is more satisfactory for w/c determination because a uniform
thickness thin sectioning results in uniformity and reproducibility of the amount of
transmitted light.
Concrete microstructure is quite variable, and at least qualitatively, it can be correlated with
" the nature of the starting materials and the original formulation of the concrete. For
example, a formulation with a higher w/c ratio than a companion concrete revealed a higher
, porosity in thin section and higher relief in polished section (the higher w/c matrix was just
not as strong).
The examination of concrete microstructure, whether in thin section or reflected light/SEM,

is a powerful one, useful to the highway engineer on a number of levels. For forensic
purposes, it can be used to actually see why a concrete has deteriorated. In terms of
developing a new concrete formulation or mixing procedure, the method can give the
engineer information on homogeneity, relationship of porosity to interracial characteristics,
overall crack development, etc. These are easy to evaluate and do not require much more
ix
training than that currently described in ASTM-C-856. However, on a more sophisticated
level, the determination of w/c ratio is much more difficult. In this instance, the
investigator must compare the fluorescence of known standards with that of the unknown.
1
Introduction
ASTM C 856 details a standard practice for petrographic examination of hardened concrete.
It contains sections detailing microscopic methods to be used to examine polished sections
and thin sections. It is a useful technique but one which is learned over long periods of
time and examination of many specimens. ASTM states: "It is assumed that the
examination will be made by persons qualified to operate the equipment used and to record
and interpret the results obtained."
The methods and examples presented in the following report are a refinement of Romer's
original work on fluorescent impregnation microscopy, and a such are directly related to the
objectives of ASTM C 856. Fluorescent microscopy is a method by which the investigator
is aided in his examination procedure by the impregnation of pores and voids by a
fluorescent epoxy. When viewed under fluorescent light, features such as porosity and
cracks are enhanced by the fluorescence of the dye used to impregnate the sample.
Proponents of the method include Bert Romer (Switzerland), Hollis Walker (USA) and
Gunnar Idorn (Denmark). The following report was prepared with the cooperation of
GMIC. The report is divided into three sections. The first deals with the method itself,
i.e., the preparation of fluorescent thin sections, the equipment required, and some of the
basic principles needed to examine the thin section. The second section of the report
describes the results of using various methods to study a series of concrete specimens
prepared in this study (SHRP 1-19). The final section is a discussion section giving both
pros and cons of the method as a potential tool for the highway engineer.
Background
Thin sections have been used by petrographers and petrologists to study rocks for more
than 150 years. One of the major advantages of this method, is that it provides an
opportunity to both identify the individual mineral constituents and at the same time study
their mutual interrelationships (fabric), their morphology and their amounts.
Not surprisingly, the use of petrographic thin-sections has gained increasing recognition
within the field of concrete petrography. The first concrete thin-sections were hand-made
and generally quite large, having a uniform thickness falling between 0.02-0.03 man (20-30
microns). Thin-sectioning techniques have been improved, and several laboratories now
manufacture thin sections of the desired thickness on automatic lapping machines (Ahmed,
1983).
Another major step forward was the introduction of the fluorescent impregnation method
(Wilk et al., 1974) by which concrete is impregnated with a fluorescent epoxy prior to
grinding. By excitation of the fluorescent epoxy in the concrete with ultra-violet or blue
light, it became possible to observe even very small porosities and defects in the concrete
(Walker and Marshall, 1979; Walker, 1979; Gudmundson et al., 1981; Wilk and
Dubrolubov, 1984; Anderson and Thaulow, 1990).
The fluorescence method was further refined when it was demonstrated that it is possible to
obtain reasonably accurate figures for the water-cement ratio used in the concrete (Walker's
early work), by visual estimation of the brightness of the hardened cement paste when
viewed in fluorescent light. This method was refined and quantified by Thaulow et al.,
1982 and Damgaard Jensen, 1983. It is now a standard practice in several European
countries to determine the w/c ratio of hardened concrete using fluorescent thin-sections. In
addition, the preparation of fluorescent thin-sections has recently been approved as a Nordic
test method, by Denmark, Norway, Sweden, Finland and Iceland (Nordtest 677-87,
"Concrete, Hardened; Water-Cement Ratio," see Appendix C).
Today, about 6000-7000 fluorescent concrete thin-sections are prepared annually in

Denmark alone for use in quality control, damage analyses and research. Practically none
of these thin-sections are prepared solely for the determination of the water-cement ratio of
the cement paste since the determination of the w/c ratio only represents a small part of the
information which can be obtained from the study of fluorescent concrete thin-sections
(Damgaard Jensen, 1985; Soers, 1985; Thaulow et al., 1989). For detailed evaluations of
the method see Walker, 1979, and Mayfield, 1990. Both give statistics for fluorescent
microscopy examination of thin and reflected light samples, respectively.
2
2
Preparation of Fluorescent Concrete Thin-Sections
Most of the equipment required for the preparation of thin-sections from concrete, is similar
to the instrumentation used in the preparation of ordinary petrographic thin-sections. A
large variety of brands, including self-made machinery, are currently used in the USA and
Europe for the preparation of thin-sections. Consequently, a detailed description of these
items is beyond the scope of this report. Interested readers are referred to ASTM C 856 or
other publications dealing with thin-section preparation. However, these lists must be
supplemented with a few additional items in order to ensure the optimum quality of the
fluorescent thin-sections. These items include:
A desiccator with an attached vacuum pump,

A diamond grinding wheel (15-20 #m diamonds),
An epoxy resin, preferably low viscosity, and
Fluorescent dye.
Before preparation of the thin-section, it is important to select a proper volume of concrete

for the thin-sectioning.
This selection should depend both on the representativeness of the cores/samples, and on
the features which are being examined. If surface cracking and carbonation are to be
investigated, it would be logical to thin-section exposed surfaces of the concrete. The
identification of alkali-silica reactions and reacting aggregate particles usually requires that
the thin-section be located a couple of centimeters away from the exposed surface of the
. concrete as general experience shows that these reactions tend to be weaker at the
near-surface regions of the concrete.
The chosen area should be included in a rectangular piece of concrete, normally with the
size: 45x30x20 mm, which is cut from the specimen with a rock saw. The cutting should
be done with care in order to avoid the introduction of fine cracking and other flaws in the
specimen.
The cut concrete specimen is then immersed in pure ethanol and allowed to reside there for
approximately 12 hours. The ethanol replaces some of the water in the concrete which
reduces the tendency of cracking in the concrete during the subsequent drying procedure.
The concrete specimen is then placed in a vacuum chamber equipped with a hot plate for
final drying. It is important that this drying occurs at 30°-35°C (85°-95°F) as excessive
heating will introduce undesirable microcracking in the specimen.
The specimen should be allowed to dry for approximately 2 hours.
The specimen is then placed in a small vessel, with the side to be mounted on the glass
slide facing downwards, ready for the first vacuum impregnation with epoxy.
The epoxy should be of a low viscosity type in order to promote the penetration of the
epoxy into the concrete. Likewise, the epoxy must be intermixed with precisely 1.1% by
weight of a fluorescent dye. However, this may vary from epoxy to epoxy and dye to dye
depending on the combination chosen by the investigator.
It is very important that the dosage of dye per volume of epoxy is accurately measured as
even small variations in the concentration will seriously affect the determination of the w/c
ratios on the finished thin-sections.
For the same reasons, one should ensure that the epoxy/dye mixture is completely
homogenized. It is thus common practice to stir the mixture with a magnetic stirrer for at
least 24 hours before use.
Once ready for use, the epoxy is poured into the small vessel, containing the specimen.
The vessel is subsequently placed in a vacuum chamber and the specimen is allowed to
soak at < 0.1 mbar pressure for 1 hour while the samples are still submerged in epoxy, air
is then allowed to re-enter the chamber.
The penetration depth of the epoxy depends largely on the viscosity of the epoxy used and
on the permeability of the concrete. It is normally observed that the concrete will be
impregnated to a depth of approximately 1-2 ram. High strength concretes with a low w/c
ratio and concretes with mineral admixtures such as silica fume are normally more difficult
to impregnate adequately.
Following impregnation, the side opposite to the selected large face of the specimen is
glued to a glass plate with an ultraviolet (UV) hardening glue.
The glass plate should be of appropriate size so that it fits the clamping device of the
grinding equipment.
The next step is to prepare the selected face of the concrete specimen for mounting on the
object glass.
The epoxy covering the exposed large face of the concrete specimen is carefully removed
by mounting the glass plate which was glued to the specimen in the petrographic lapping
machine and subsequently grinding the opposite face carefully in order to obtain a
completely level surface. The finishing operation should be performed on a 15-20 #m
diamond disc.
4
It is important that loose abrasives are never used during these operations as the grit tend to
stick to the impregnating epoxy in the concrete. It must also be emphasized that the final
operations of the grinding procedure be performed as fast as possible as carbonation of the
freshly ground surface might otherwise occur.
The specimen is cleaned and allowed to dry before it is re-impregnated with fluorescent
epoxy. This impregnation should also include the recently ground surface. It is
- recommended that excess epoxy be scraped off the ground surface while it is still soft
leaving a layer approximately 1-2 mm thick, as this will facilitate the final polishing of this
face.
The excess epoxy on the ground face is carefully removed after it has hardened by
polishing on the diamond disc. Caution should be exercised during this grinding operation
as the removal of too much material will leave too little impregnated concrete for the
finishing operations. However, should this happen, one can recover the sample by
re-impregnating the concrete and repeating the grinding of the face.
After cleaning and drying of the ground surface, a glass slide is mounted to the surface
using an epoxy glue.
The specimen is now cut with a fine diamond saw parallel to the recently mounted slide
approximately 1 mm from the slide. Once cut, the piece containing the auxiliary glass plate
is saved/discarded.
The slide on the specimen is now mounted in a specimen holder on the lapping machine
and ground down to a thickness of approximately 100/zm. The final polishing of the
thin-section down to a thickness of 20 #m is performed by hand on the diamond disc. This
part of the preparation requires great skill as the thin-section might otherwise end up being
too thin, wedge shaped or feathered.
The polished face is covered with a cover glass by applying one drop of epoxy to the center
of the concrete and carefully pressing the cover glass down vertically on the drop. It is
important that no air bubbles are trapped underneath the cover glass as this would seriously
reduce the quality of the thin-section.
Many of the above procedures resemble the procedures followed during the preparation of
geological thin-sections. The major difficulties in preparing thin-sections from concrete are
normally associated with tearing out the cement paste, especially around voids in the
concrete and/or achieving an equal thickness over the entire thin-section. The latter
problem can be especially difficult to avoid when thin-sections are prepared from concretes
containing hard and dense aggregates.
Instrumentation
Evidently, the petrographic microscope plays a central role in the examination of the
concrete thin-section. A detailed treatment of the construction and function of the
petrographic microscope can be found in other textbooks and will only be treated briefly in
this report. The modifications of the standard petrographic microscope which are required
in order to use the fluorescent light illumination technique are rather few and uncostly and
will be treated during the description of the fluorescence technique.
Figure 1 is a schematic drawing of a "Leitz" petrographic microscope. The figure shows

the most basic features and the light path in the instrument. The thin-section is placed on
the rotating stage just below the objective. Light passes via a circular hole in the stage, up
through the semi-transparent thin-section and further through the magnifying lens, the
objective. Several objectives are mounted on a circular revolving nose which makes it
possible to shift between several magnifications. It is thus possible to examine the
thin-section in magnifications ranging from 25x to approximately 600x.
The light source needs to be more powerful than normally employed in petrographic
microscopes if examination in fluorescent light is desired. It normally suffices to use a
100-W halogen lamp.
Examination of the thin-sections can be performed in four different modes:
Ordinary light,
Polarized light,
Polarized light with compensator, and
Fluorescence.
Ordinary light examination as illustrated in Figure 2a, is achieved by allowing the light
from the light source to pass unhindered through the thin-section. Examination of the
concrete in this mode makes all of the constituents of the concrete appear in their natural
"transmitted light" color. Thus, quartz will appear white due to its lack of color, while
fly-ash can show various shades from almost colorless to deep brown. The hardened
cement paste normally has a buff colored appearance. Most minerals do, unfortunately,
appear colorless in transmitted light in thin-section which often makes their distinction
difficult. However, due to the crystalline characteristics of most minerals, it is possible to
make further identifications by the use of polarizing light microscopy. Polarized light
mode, shown in Figure 2b, is obtained by inserting a polarizing filter in the light ray before
it passes through the thin-section. This filter, normally called the "polarizer" causes light
from the lamp to oscillate in one direction, denoted "North-South" (N-S). Another -_
polarizing filter, the "analyzer", is inserted in the light ray after it has passed through the
thin-section only allowing light oscillating in the East-West (E-W) direction to pass through .3
to the observer.
Thus, if light is allowed to pass uninterrupted from the polarizer to the analyzer, that is, if
the thin-section is removed, the image seen in the eye pieces will be completely dark as all
light passing through from the polarizer is absorbed by the analyzer.
However, the image will not be dark when the thin-section is inserted in the light path
between the polarizer and the analyzer if birefringent material is present. When the light
which has been forced to oscillate in one direction by the polarizer, passes through a
6
crystalline solid in the thin-section, such as quartz, or calcite in a limestone aggregate, the
ray will be split into two oscillation directions. At the same time one of the rays will be
delayed with respect to the other due to differences in refractive index. The actual
mechanisms for this optical behavior of crystalline solids is rather complicated and the
reader who wants further knowledge about these topics is referred to the crystal optical
literature, for instance Phillips (1971). However, by treating the light emanating from the
crystalline materials in the thin-section with the analyzer, a distinct coloration of
birefringent minerals can be seen in the eyepiece. These colors assist the petrographer in
distinguishing between the different crystalline solids in the thin-section. Materials which
are either glassy, amorphous or belong to the cubic crystal system, do not alter the behavior
of the polarized ray during passage. These materials will appear completely dark when
viewed in polarized light; they are isotropic.
The difference between observation in polarized light and in polarized light with a
compensator is that the compensator adds or subtracts a well known "retardation" to the
rays emitted from the thin-section. This is seen in the microscope as a rather spectacular
coloration of the polarized image, Figure 2c. This method is only used as an aid in the
identification of minerals during examination in polarized light.
So far, only the examination devices available on the standard petrographic microscope,
have been described. Application of the fluorescence method for the determination of w/c
ratios and for the detection of flaws and inhomogeneities in the concrete requires a few
additional accessories.
First, a monochromatic light source is required which is able to induce fluorescence in the
epoxy in the thin-sections. The light should be monochromatic as excess light has to be
filtered away after passage through the thin-section. The monochromatic illumination is
obtained by inserting a filter designed to pass ultraviolet light (BG 12), in the light path
before it enters the thin-section. This UV filter allows the passage of light with a wave
length around 350 nm. Due to the large absorption of light during passage of the blue
filter, it is necessary to use a powerful light source with an intensity around 100 W.
The fluorescent dye in the epoxy is excited by the UV light and emits yellow light with a
peak intensity a little above 530 nrn. By insertion of a yellow filter (K510 or K530) in the
light path above the thin-section which absorbs all light with a wave length beyond 510 to
530 nm, the excessive UV light from the light source is filtered away. The resultant image
in the eyepieces thus comprises the light emitted from the fluorescent epoxy only. As
porous areas in the thin-section contain a higher portion of fluorescent epoxy, it follows that
porous areas in the concrete thin-section appear bright while dense areas appear dark. This
is shown in Figure 2d.
From the above principles it is evident that features such as microcracks, air voids, porous
paste-aggregate interfaces etc. will appear bright yellow when viewed in fluorescent light.
The coarse aggregates and the sand particles in the concrete are normally so dense that they
appear dark green in fluorescence. An aggregate with zero porosity should theoretically be
completely dark, but in practice it may appear dark green.
The hardened cement paste, however, displays varying "brightness" depending on the
amount of epoxy impregnated capillary voids in the cement paste.
As shown in Figure 3 the amount of capillary voids is closely related to the amount of
water used in the mix, i.e. the water-cement (w/c) ratio. The figure shows that assuming
that the water is capable of completely hydrating all the cement present, the only capillary
voids left in the cement paste will be those caused by the chemical shrinkage of the cement
- that is the volume reduction associated with the reaction: cement + water/E hydrated
paste. Complete hydration theoretically occurs at a water/cement ratio of 0.40. Increasing
the w/c ratio leads to the presence of an increasing surplus water which is located between
the hydration products in small capillary voids, i.e as capillary water.
Decreasing the w/c ratio below 0.40 leads to the presence of unhydrated relics of cement
grains as the amount of water was insufficient to cause complete hydration of the cement.
However, the assumption of complete hydration of the cement rarely holds true in real
concrete structures. Investigation of old concrete structures shows that between 20 and
25% of the cement grains still remain unhydrated after several years. Consequently, it is
still possi_ _ to observe capillary pores in concretes with a w/c ratio below 0.30.
These obsezvations suggest that a cement paste with a low w/c ratio would absorb less
epoxy than a cement paste with a higher w/c ratio. If the thin-sections of two such cement
pastes are compared in fluorescent illumination, it follows that the paste with the low w/c
ratio would appear darker than the paste with the high w/c ratio. Figures 4a and b which
show the appearance of mortars with w/c ratios of 0.40 and 0.60, respectively, confirms this
theory. By preparing thin-sections from mortar bars with known w/c ratios, a series of
standards can be obtained which vary in brightness as a function of w/c ratio. These
standards can then used to determine the w/c ratio of a sample of an unknown concrete
mix. Skilled operators which use these methods are capable of determining the w/c ratio of
an unknown concrete specimen with an accuracy of better than 0.1 often 0.03 (see
following report data). However, less skilled operators will have a harder time, but with
practice and proper standards should be able to determine the w/c ratio of hardened cement
paste to ::_ .1 or better.
Examination of Fluorescent Thin-Sections
The determination of the w/c ratio of an unknown concrete specimen should not be carried
out before the thin-section has been examined thoroughly in ordinary and polarized light.
There are several reasons for this warning. First, it is extremely important to check the
thin-section for flaws induced during the preparation which could affect the w/c
determinations. Second, one must ensure that the cement paste is suitable for w/c
determination with regards to both composition and potential secondary alteration of the
paste, e.g. carbonation.
Due to the large differences in hardness between the aggregates themselves and between the
aggregate and the cement paste, it is often difficult to achieve an equal thickness of 20 #m
over the entire face of the thin-section. The determination of the w/c ratio depends on
having an equal thickness of the thin-section. A reduction in thickness leads to a reduction
in the total amount of fluorescent epoxy and consequently a darker fluorescent image.
Figures 5a and b are micrographs of two concrete mixes with the same w/c, recorded in
fluorescent light. The thin-section in Figure 5b is only 10 microns thinner (but 50%
thinner) than the thin-section in Figure 5a. The apparent reduction in brightness when
going from a to b is seen to be quite significant. Hence, if the thin-section is too thick, this
would result in an apparent w/c ratio higher than the actual value and vice versa. It is
therefore important to check the thickness of the thin-section by observing the interference
colors of the minerals in the sand and in the coarse aggregates. The interference color of
"" quartz is a good indicator as this mineral is almost always present in the aggregates. The
interference color of quartz should be a first order white or grey (-20/_m thick). A yellow
color signifies too great a thickness (-30/_m thick) while dark grey signifies a too small
thickness (-10 #m thick) of the thin-section.
Another problem which is often encountered in fluorescent thin-section analyses is caused

by insufficient impregnation. This can either be due to the presence of a very dense paste
or poor impregnation procedure. One should therefore check especially the small voids in
the thin-section in ordinary light to see whether these are completely filled with the yellow
epoxy.
It is also a good idea to check the color and homogeneity of the impregnating epoxy in
larger voids in the thin-section. If the epoxy appears too pale or too yellow this could
indicate a wrong dosage of dye during the preparation of the fluorescent epoxy. Likewise,
inhomogeneities in the color distribution could indicate insufficient mixing of the epoxy.
Several other undesirable phenomena caused by the preparation procedure could be

mentioned but the items mentioned above appear to be the most common, and most
significant in their effect on the w/c determination.
Assuming the thin-section is adequate, one proceeds to the examination of the hardened
cement paste itself in order to verify whether it is suitable for w/c determination. This task
is especially important if the composition of the cement is unknown, as blended cements or
cements intermixed with a filler can yield misleading apparent w/c ratios when examined
by the fluorescence method.
Blended cements are cements intermixed with a mineral admixture such as silica fume,
fly-ash or slag. If the silica fume has been added to the concrete as a slurry it is often
difficult to determine its presence by thin-section microscopy.
The reason for this is that the silica fume particles are very small (-0.01 /_m). Close
examination of the hardened cement paste under high magnification (500-600x) in ordinary
light can, however, sometimes reveal the presence of small agglomerates of silica fume.
See Figure 6. It is also possible to get an indirect indication of the presence of silica fume
in an unknown concrete mix as the cement paste tends to be significantly darker than
normal, when viewed in polarized light. The reason for this is that a large part of the
disseminated calcium hydroxide in the hydrated paste has reacted with the silica fume.
Slag and fly-ash are easily discernible in thin-section. Slag occurs as angular, glassy
fragments with approximately the same size as the cement grains. See Figure 7. The slag
particles will appear completely dark in polarized light as they consist primarily of isotropic
glass.
Fly-ash is seen in the hydrated paste as massive and hollow spheres with colors varying
from colorless to yellow, brown and black.
The presence of a filler in the cement is normally quite easily recognized as the filler is
almost always calcium carbonate (CaCO3). The presence of such a filler provides the
cement paste with a brighter appearance than normal, when viewed in polarized light. The
same appearance of the cement paste can occur, however, if the polished surface of the
concrete was allowed to carbonate during preparation of the thin-section.
Carbonation due to the weathering of concrete structures is seen in polarized light as an

irregular, amber colored front which extends from the exposed surface and into the sample.
It is important to avoid carbonated cement paste when the w/c determinations are performed
as carbonated paste in some cases can be denser than the original paste and in some
instances, more porous.
Having checked the quality of the thin-section and the composition of the hardened cement
paste, the determination of the water - cement ratio can now proceed.
The microscope is equipped with a combination of objectives and oculars so that the total
magnification is somewhere around 65x. The UV filter (BG 12) and the yellow filter
(K510 or K30) are inserted into the light path and the intensity of the light is increased to
approximately 100 W. To ensure a sufficient intensity of light, it is recommended that the
iris diaphragm be open and that the polarizer be removed from the light path.
Having focussed the image, one randomly selects 10 areas in the thin-section and evaluates
in each case the w/c ratio of the paste. By selecting 10 sites in the thin-section the effects
of inhomogeneous mixing and dispersion of the cement paste is avoided. The average of
the 10 measurements is considered to be the w/c ratio of the concrete in question. It is
advisable to perform the measurements a few mm away from the edges of the thin-section
as light flare from the surrounding rim of epoxy, may increase the brightness of the paste -_
and hence the apparent w/c ratio.
By thoroughly practicing the technique, accurate w/c determinations can be carried out
without constant references to the standards. It is, however, recommended that reference to
the standards be made from time to time. Experience shows that the petrographer normally
does not have difficulty in distinguishing w/c ratios in steps of 0.02-0.03, but it is often
observed that the measured values generally tend to become too high or too low if regular
checks of the standards are not made.
10
References
W.U. Ahmed, Improvements in Sample Preparation Technique For Microscopic Analyses
of Clinker and related materials" Proceedings of The 5 International Conference on
Cement Microscopy, Nashville Tennessee, USA, 1983.
K.T. Andersen and N. Thaulow, "The study of Alkali-Silica reactions in Concrete by The
Use of Fluorescent Thin-Sections" Symposium on Petrography Applied to Concrete,
ASTM, St. Louis, June 1989.
A. Damgaard Jensen, "Investigation of Concrete by Analyses of Thin-sections" IABSE

Symposium on Strengthening of Building Structures, Venice, 1983.
A. Damgaard Jensen, "Strukturanalyse af Beton" (Structural Analyses of Concrete), Beton

Teknik, Cto, Denmark, 1985. (in Danish)
H. Gudmundsson, S. Chatterji, A. Damgaard Jensen, N. Thaulow and P. Christensen,

"Quantitative Microscopy as a Tool For The Quality Control of Concrete" Proceedings
of The 3 International Conference on Cement Microscopy, Nashville Tennessee, USA,
1981.
B. Mayfield (1990), "The Quantitative Evaluation of the Water/Cement Ratio Using

Fluorescence Microscopy," Magazine Concrete Research, 42, 45-49 (1990).
Nordtest 677-87, "Concrete, Hardened: Water-Cement Ratio," Nr. 677-87.
W.R. Phillips W. R., "Mineral Optics - Principles and Techniques," Freeman, 1971.
E. Soers, "Preliminary Results on a Petrographical Examination of Alkali-Silica Reactions

in Belgium" Proceedings of The 10 International Conference on Cement Microscopy,
San Antonio, Texas, USA, 1988.
N. Thaulow, A. Damgaard Jensen, S. Chatterji, P. Christensen and H. Gudmundsson,

"Estimation of The Compressive Strength of Concrete Samples by Means of
Fluorescence Microscopy" Nordisk Betong, No 2,4, 1982.
N. Thaulow, K.T. Andersen and J. Holm, "Petrographic Examination and Chemical

Analyses of The Lucinda Jetty Prestressed Concrete Roadway", 8 International
Conference on Alkali-Aggregate Reaction, Kyoto, Japan, 1989.
H.N. Walker and B.F. Marshall, "Methods and Equipment Used in Preparing and
Examining Fluorescent Ultrathin Sections of Portland Cement Concrete," Cement,
Concrete and Aggregates, CCAGDP 1 (1), 3-9, 1979.
H.N. Walker, "Evaluation and Adaptation of the Dubrulov and Romer Method of
Microscopic Examination of Hardened Concrete," VA Highway and Transportation
Research Council, Charlottesville, VA, April 1979, VHTRC 79-R42 (60 pp).
11
W. Wilk, G. Dubrolubov and B. Romer, "Development in Quality Control of Concrete",
TRR 504, Transportation Research Board, 1974.
W. Wilk and G. Dubrolubov, "Microscopic Quality Control of Concrete During

Construction" Proceedings of the 6th International Conference on cement Microscopy,
New Mexico, 1984.
12
3
.. Examination of SHRP 1-19 Concrete Samples
Introduction
The present examination of 19 concrete samples was carried out as part of the activities
under the SHRP-C-201 project, "Concrete Microstructure" which deals with the
microstructural characterization of hardened cement paste in concrete.
The objective of this examination was to assess and possibly quantify the porosity
variations occurring in the hardened cement paste. These porosity variations were
determined by the use of fluorescence microscopy of concrete thin sections as described in
Part One of this report. By stimulating a yellow fluorescence from a dye-impregnated
region by a deep blue U'V light through a thin section, porous areas will appear bright
yellow-green while the dense areas will appear dark green.
Samples
Nineteen concrete samples were received and identified as follows:
MRL No. GMIC No. T.S. No. Received
S89-1Ma 389-1 3113-1 24 April 89

$89-2Ma 389-2 3113-2 24 April 89
S89-3M28a 389-3 3114-1 24 April 89
S89-4M28a 389-4 3114.2 24 April 89
$89-5Mb 689-1 3171-1 29 May 89
$89-6Mb 689-2 3171-2 29 May 89
$89-7Mb 689-3 3171-3 29 May 89
$89-8 409-1 3278-2 27 June 89
$89-9 409-2 3278-1 27 June 89
$89-10 889-1 3171-4 27 July 89
$89-11 1289-1 3196-1 11 Sept. 89
$89-12 1289-3 3196-4 11 Sept. 89
$89-13 1289-2 3196-3 11 Sept. 89
$89-14 1689-1 3261-1 2 Oct. 89
$89-15 1689-3 3261-3 2 Oct. 89
13
$89-16 1689-2 3261-2 2 Oct. 89
$89-17 0690-1 3284-1 5 Feb. 90
$89-18 0690-2 3284-2 5 Feb. 90
$89-19 0690-3 3284-3 5 Feb. 90
One thin section was prepared from each sample.
The heading "T.S." refers to the number assigned to the thin section prepared from the ..
concrete samples. Specifics regarding the mix design, water-cement ratio, etc., for the
concrete samples are presented, together with the quantified results from the microscopic
examination and illustrative micrographs in a series of tables and figures. The data
regarding mix designs were obtained from the Second Quarterly Report, Year Two,
presented to SHRP July 17, 1989 and the Third Quarterly Report, Year Two, presented to
SHRP October 17, 1989.
Specifics regarding the mix design, w/c ratio, etc., for the concrete samples are presented in
the following pages together with the quantified results from the microscopic examination.
Microstructural Data
As the work proceeded, so did the quantitative nature of the results. The microstructural
features found in SHRP 89-1 to 7 thin sections were evaluated using a numerical scale
ranging from 0 to 3. The following (qualitative) terms are used to describe the individual
grades:
0: Not present, insignificant.

1: A little, of minor importance.
2" Clearly present, significant.
3: Dominant, severe.
In addition, due to the potential significance of porous zones around the coarse aggregates
(Figures 9, 11, 12 and 14) and their effect on permeability, an attempt was made to
determine the fractional percentage of porous zones around these aggregates. An average
value was obtained by estimating the percentage of porous zones at the interface of the
individual coarse aggregates in the entire thin section.
Two other parameters were determined in order to quantify the microstructure:
(1) The surface area of the coarse aggregates per unit volume of concrete (cm2/cm3) was
determined by combining line intercept and point counting data for the coarse
aggregates in cross sections of the concrete cores, and
(2) The intersection per unit length of test line with the microcracks in the thin sections.
From the microcrack line intercept, the average line intercept in cm and the surface of the
crack planes per unit volume can be estimated. Similarly the specific surface of the coarse
14
aggregates and the mean free distance between them can be determined (see Underwood,
1970).
As work progressed, the use of quantitative stereology was emphasized and in the cases
where microstructural features are now described by stereological methods, earlier
semi-quantitative terms ($89-1 to 7) have been omitted. The following section explains the
measurement and meaning of the stereological parameters presented during the microscopic
examination of samples $89-1 to 19 (summarized in Table 1).
Stereological Measurements
Measurements have been performed on cut slices of concrete and on thin sections. Point
counting and the linear traverse method have been used on the cut slices to obtain
information about the amount and surface area of the coarse aggregates. Fluorescent thin
section studies combined with linear traverse method have provided information about the
amount of microcracking in the concrete.
Referring to Table 1, features listed under the heading "MICROSCOPY" have been
measured using stereological methods. A short description of each of these features is
presented below:
Vv, Volume, coarse aggregate: The volume of coarse aggregate is determined by simple
point counting on the cut slices of concrete. This value is used in the calculation of lambda
which is defined later in the text.
Pll, line intercept coarse aggregates: Represents the number of paste/aggregate intercepts
per unit length of testing line. Also see ASTM C457. Several lines are drawn on the cut
concrete slices and the number of intercepts with paste/aggregate boundaries are registered.
This number is divided with the total line length and the result is presented as P1.
Sv, surface of coarse aggregates per test volume: According to the rules of stereology, the
surface to volume ratio, Sv, can be calculated as 2P1. The surface to volume ratio
expresses the surface area of the coarse aggregates per unit volume of concrete. This value
will increase with a decreasing aggregate size and an increasing amount of aggregates.
Lambda, mean free distance between coarse aggregates: This value expresses the average
distance between the coarse aggregates and is calculated as
2x(1 -Vv)
P1
P12, line intercept cracks: This value is measured in the thin section in fluorescent
illumination and expresses the number of intercepts of microcracks per unit length test line.
It is here important to realize that although cracks are seen as lines in the thin section, they
are in fact planar structures.
15
L, mean free distance between cracks: Expresses the average distance between cracks per
unit volume of mortar; that is, exclusive of coarse aggregates. The value is calculated as:
(1-Vv aggregates)
P1
The value is normalized per volume mortar as this operation makes the L values from
different concrete mixes straightforward comparable.
Epsilon, cracks: This value represents the fraction of the paste/aggregate interface which
appears porous or cracked when viewed in thin section in fluorescent light. This value has
been established by measuring the length of the periphery of the individual coarse aggregate
particles in thin section and subsequently by measuring the length of the porous or cracked
paste/aggregate interface.
General Examination
Samples $89: 1Ma, 2Ma, 3M28a and 4M28a
These four concrete samples are treated together as they represent concrete mixes with
similar cement-aggregate ratios, slumps and w/c ratios See Tables 1-5 and Figures 8-11.
Figure 8(a) shows sample S89-1Ma in normal transrr: :1 fluorescent light, while 8(b)
shows the same concrete in reflected fluorescent lig_ i_he other figures are all thin
sections in transmitted light.
The four concrete samples have a coarse aggregate content consisting of a crushed
limestone while the sand primarily consists of single- and polycrystalline fragmenz_ of
quartz.
A narrow zone of cement paste with a high porosity and/or cracks is occasionally seen at
the interface between the coarse aggregate particles and the surrounding hardened cement
paste. The same zone is seen around a few schistose aggregates. Furthermore these
particles also exhibit signs of internal cracking which is probably due to drying shrinkage
of the particles.
The cement paste is homogeneous both in macro- and micro-scale.
The concrete contains some microcracks which are seen to interconnect several of the sand
particles in the cement paste. It is not clear why these cracks have formed.
Samples $89: 5Mb, 6Mb and 7Mb
The compositional difference between these three concrete mixes and the four mixes
mentioned above is that these samples contain a higher amount of aggregate and have been
made with the addition of a superplasticizer. The specific mix compositions are presented
in Tables 6-8 and data are presented in Tables 1, 6-8 and Figures 12-14.
16
Examination of the hardened cement paste in fluorescent light shows that sample No. 5Mb
in particular possesses a rather inhomogeneous microstructure. Also, the w/c ratio for this
sample was measured as 0.42 although the accompanying mix specifications states a w/c of
0.47. Concrete $89-6Mb in transmitted fluorescent light (Fig. 13a) as well as in reflected
fluorescent light (Fig. 13b) both show a homogeneous microstructure.
Samples $89: 8 and 9 (Tables 1, 9, 10, Figures 15, 16)
These two samples represent concrete mixes with differing water-cement ratios, 0.42 and
" 0.53, respectively. It should be noted that a superplasticizer has been added to sample
$89-8 (Figure 15). These two concrete samples are generally quite homogeneous as viewed
in thin section (Figures 15, 16) but it is noted that sample $89-9 (see Figure 16) contains
significantly fewer microcracks and porous paste/aggregate interfaces than the rest of the
concrete samples examined, despite its higher w/c ratio.
Samples $89: 10, 11, 12 and 13 (Tables 1, 11-14, Figures 17-20)
These concrete samples are treated together as they represent concretes with a fixed binder
to aggregate ratio and a fixed aggregate size. The difference between the concrete samples
is comprised by the substitution of a part of the cement with slag, two types of fly ash and
silica fume, respectively.
Sample $89-10 has, according to the mix formulation, a slag content of 40% by weight of
binder. The slag particles are clearly seen in thin-section as small, transparent glass shards
in the hardened cement paste. See Figure 17a. They are also easily distinguishable in
polarized light as their glassy nature causes them to appear completely dark.
The porosity of the paste is very low when viewed in fluorescent light. As Figure 17b
shows, most of the paste appears very dark which indicates an "equivalent" water-cement
ratio below 0.35. These observations tend to be in conflict with the calculated
water-(cement+slag) ratio which is reportedly 0.47.
Figure 17 also shows that the amount of microcracking in the paste is quite significant.
Likewise, porous paste/aggregate interfaces appear to be quite common in this thin-section.
Sample $89-11 comprises a concrete mix with a substitution of 20% by weight of the
cement with a Class F fly ash. As shown in Figure 18a this fly ash often contains rather
large hollow spheres of glass. The amount of microstructural inhomogeneities is rather low
in this concrete mix. The fluorescence images (Figure 18b) show that the dispersion of the
cement and fly ash is good and that the number of microcracks and paste/aggregate
porosities is rather low.
Sample $89-12 represents another concrete mix with fly ash addition. The percentage of
cement replaced by fly ash is the same as for Sample S 89-11 but the fly ash is a Class C
fly ash. This type of fly ash is seen in thin-section to be smaller in average grain size than
17
the Class F fly ash, previously examined. Likewise, a larger portion of this fly ash is
constituted by massive spheres of glass as seen in Figure 19a. Under fluorescent light, the
microstructure of this concrete mix resembles the microstructure of Sample S 89-11, that is,
a rather homogeneous dispersion of the binder and a low amount of microcracks and
paste/aggregate porosities, see Figure 19b.
Sample $89-13 has been prepared with silica fume constituting 7.5% by weight of the
binder material (silica fume+cement). During examination of concrete with silica fume
added, it is normally observed that the cement paste achieves a hazy appearance when
examined in thin-section in polarized light. Likewise, the hardened cement paste normally
appears dark due to the removal of the disseminated calcium hydroxide in the paste. In
fact, in this way the slag and silica fume pastes bear a greater resemblance to each other
than to the other materials. A certain lack of Ca(OH)2 in the paste is observed in the
thin-section prepared from Sample $89-13. See Figure 20a. However, as the paste did not
appear particularly hazy and as it was not possible to detect any agglomerations of silica
fume in the paste, even at high magnifications, it was not possible to obtain a positive
identification of silica fume by the thin-section technique. The fluorescent examination
revealed a fair amount of micro cracks in the paste and porosities at the paste aggregate
interface. See Figure 20b.
Samples $89: 14, 15 & 16 (Tables 15-17, Figures 21-23)
These samples represent concrete mixes where the normal coarse, #67 limestone aggregate
has been substituted with #8 limestone aggregate, #67 siliceous gravel and #8 siliceous
gravel, respectively.
The differences between the microstructure of the hardened cement paste in the three
samples are generally very small (Figures 21-23). They all exhibit a minor amount of
microcracking and porosities at the paste-aggregate interface and the light variations in the
dispersion of the cementitious particles in the paste do in all three incidents classify them as
"grade 1" in terms of micro-inhomogeneity.
Hence, it does not appear that the reduction of the aggregate size and/or the change to
siliceous gravel has any noticeable effect on the microstructure of the concrete samples.
Samples S 89: 17, 18 & 19 (Tables 1, 15-17, Figures 24-26)
Although the exact mix compositions were not present at the time of preparation of this
report, it clearly appears from the stereological measurements (Figures 24a, 25a, 26a) that
these three concrete samples have a decreasing content of quartzite coarse aggregate in the
order $89-17, 18 to 19. It also appears that the decrease in the coarse aggregate content
has been counteracted by an increase in the content of fine aggregate.
18
The fluorescence studies (Figures 24b, 25b, 26b) show that the samples have been prepared
with different water-cement ratios as sample $89-17 has a w/c of 0.40-0.45, 18 has a w/c
around 0.35 and 19 has a w/c of approximately 0.35-0.40.
The frequency of microcracking and porous zones along the paste/aggregate interfaces
appear within the normal range when compared to the samples earlier examined.
Alternate Methods
• As an alternate, one can examine polished sections rather than thin sections. Figure 27
illustrates differences in surface relief resulting from a decreasing w/c ratio. The upper
sample is SHRP $89-9 (w/c = 0.53), and the lower sample is SHRP $89-8 (w/c = 0.42).
Other than this difference, formulations are identical. Photos are -50x. Much more relief
in $89-9 is present, as a result of polishing. This is probably due to lower matrix strength
of $89-9 compared to $89-8, the paste has been eroded. Upper photo also suggests more
cracking and more porosity at interfaces. The crack in the lower figure is most probably an
artifact caused by cutting of the sample.
Figure 28 demonstrates the effects of packing on density. The upper sample is SHRP
$89-5 (w/c = 0.47) and the lower is SHRP $89-4 (w/c = 0.47). $89-4 has a higher cement
content (8 bags/cubic yard) than $89-5 (6.25 bags/cubic yard).
In addition $89-5 has a lower sand/aggregate ratio than $89-4. Even though Sg9-5 has
higher strength than $89-4, $89-5 still appears rougher. The matrix is not as strong and
polishing relief is higher. Particles from the paste have been plucked during polishing.
The increased strength is apparently the result of improved packing ($89-5) not the matrix
strength itself ($89-4).
19
References
E.E. Underwood, Quantitative Stereology, Addison-Wesley Publishing Company, Reading,

MA (1970), 274 pp.
2o
4
. Discussion
The investigation of concrete in thin section is a powerful tool both for development and
forensic applications. But, because it is a "learned" technique, at present it cannot be fully
implemented by an unskilled operator.
Standards are necessary and difficult to make. Thin sections must always be exactly the
same thickness over the entire section and from sample to sample. The preparation and
polishing is an art in itself. Great care must be exercised to prevent the inadvertent
introduction of microcracks (see for example, Struble's papers NBS IR 88-3702 and NBS
87-3504).
However, once these hurdles are overcome, the technique can be very useful. It can be
used to evaluate homogeneity of mixing, dispersion of aggregates, effectiveness of
superplasticizers, etc. The ability to better observe alkali silicates, carbonation, sulfate
attack, microcracking, etc., is self evident. Our recommendation is to implement the
technique, but develop automated computer-assisted data interpretation as much as possible.
Preliminary observations were made on some of the fluorescent epoxy impregnated

specimens in reflected light. Although some features show up well, the amount of
information does not appear to be equal to that in the thin sections. However, the
concurrent examination of the polished sections can provide some important information on
relative matrix strength related to variations in w/c and packing.
21
References
L. Struble and E. Byrd, "Epoxy Impregnation of Hardened Cement Pastes for

Characterization of Microstructure," NBSIR 87-3504 (1986).
L. Struble and P. Stutzrnan, "Epoxy Impregnation Procedure for Hardened Cement

Samples," N-BSIR 88-3702 (1988).
22
Appendix A
o
- Figures
Figure 1. Schematic draw_g of a "Leltz" petrographic microscope. Pathway of llght and
the location of the thin-section and auditory filters are shown.
1: Slot for compensator or yellow filter

2: Location of thin-section
3: Location of polarlzLng filter
4: Location of blue filter, BG-12
2S
o
Figure 2. Micrograph of concrete recorded in: (a) Ordinary light, (b) Polarized light, (c)
Polarlzed light with compensator and (d) Fluorescence. Field of view: 2.5 x 2.5
ITIm.
27
100
vol
• °/o
0
0 .2 .4 .e .8 1.0 1.2 1.4
wit ratio
Figure 3. Diagrnm depicting the distribution of unhydrated cement, C-S-H gel, gel water,
capillary water and chemical shrlvkage voids as a function of the w/c ratio.
?9
Figure 4. Micrographs of thin-sections prepared from mortars with a w/c ratio of 0.40
(top) and 0.60 (bottom), respectively. The images show that the paste with a w/c
of 0.40 appears significantly darker in fluorescence than the paste with w/c
0.60. Field of view: 3.9 x 2.7 ram.
31
Figure 5. Fluorescent images of two thin-sections with similar w/c ratio but 10 !_m
difference in thickness. Note the apparent change in w/c ratio on going from 20
!Jrn (top) to 10 !Jrn (bottom). Field of view 1 x 1.5 mm
35
Figure 6. Micrograph of the hardened cement paste of a concrete intermixed with
approximately 7% silica fume. The presence of silica fiJme is revealed by the
presence of small globules of agglomerated silica particles. Ordinary light. Field
of view 0.12 x 0.16 ram.
Figure 7. Micrograph of slag cement. The slag particles arc easily discerned as small
angular shards of transparent glass. Ordinary light. Field of vie_. 0.27 ×
0.16 ram.
3S
(a)
Figu_-e 8. Micrographs cf sm_pie $89- IMa. Fluorescence 2.7 x 3.£ rnn-_. (a] The
section shows +._heappearance of the hardened cement paste in fluorescent light.
The paste is homogeneous with a water-cement ratio of 0.48. [5] Image of same
specimen in reflected fluorescent light. Note ira_.slucence cf sand graf_.nso and
_5ne sha_-C can_ast in the crack in the aggregate.
37
(a)
Figure 9. Micrograp__ cf sample $89-2Ma depicting a homogeneous ce_._ent paste.

Fluorescence 2.7 x 3.9 rp_.. (a] A weakly deveIoped porous zo:._e cm_..be seen
gong the coarse aggregaLe interface at the lower right of the !_icture. (5) Viev¢
shows i'iw,e cracking which appears to ra¢liate out from tke cv._tr_ aggregate
particle. Tb.e cracks may be shrinkage cracks.
39
(a)
(b)
Figure 10. Micrograph of sample S89-3M28a. Fluorescence. 2.7 x 3.9 Emil. View (a) suggests
that the hardened cement paste appears rather homogeneous. View (b) depicts
the presence of a spherical air void in the sample. Fine cracks are seen radiating
from the void. It is not clear which mechanisms have caused the microcracks.
41
(a)
(b)
Figure i I. Micrograph of sample S89-4M28a. Fluorescence. 2.7 x 3.9 ram. View (a) shows
that the interface between the coarse aggregate particle to the lower left and the
bulk cement paste is dominated by a porous zone. View B suggests that the
cement paste, which has an average w/c ratio around 0.46, is homogeneous.
43
Figure 12. Micrograph of sample $89-5Mb. A coarse aggregate particle (lower left]. Note
the porous zone between the aggregate and the bulk cement paste. Also note the
varying porosity of the cement paste. Fluorescence. 2.7 x 3.9 mm.
Figure 13. Micrograph of sample $89-6Mb. This thin section illustrates a concrete with
practically no paste-aggregate porosity. Fluorescence. 2.7 x 3.9 ram.
45
(a)
(b)
Figure 14. Micrograph of s_mple $89-7Mb. Fluorescence. 2.7 x 3.9 turn_ View (a) shows a
weakly developed porous zone at the interface between the cement paste and the
coarse aggregate particle at the lower right. Also note the varying porosity of
the hardened cement paste. View (b) depicts the distribution of microcracks
radiating from the air voids. It is not clear which mechanism has caused the
microcracks.
47
Ca3
Figure 15. Micrograph of sample $89-8. Field of view: 3.9 x 2.7 ram. View (a) represents
image in ordinary light. View (5) represents a micrograph of the same area
recorded in fluorescent light. Note the general absence of microcracks and
paste/aggregate porosity.
49
(a)
(b)
Figure 16. Micrograph ofs_mple $89-9. Field of view: 3.9 x 2.7 n_,u. View (a) represents
the appearance of the sample in ordinary light. View (b) represents a
micrograph of the s_me area recorded in fluorescent light.
51
(a)
tbJ
Figure 17. Micrograph of sample $89-10. Field of view: 3.9 x 2.7 ram. View (a) is seen in
thin section and ordinary light. View (5) is recorded in fluorescent light,
depicting the same image as in View (a). Note the grainy appearance of the paste
caused by the presence of slag in the cement.
$3
(a)
(b)
Figure 18. Micrograph ofs_mple $89-11. Field of view: 3.9 x 2.7 ram. View (a) depicts the
sample in thin section and ordinary light. View (b) gives a micrograph for the
same image area recorded in fluorescent light.
55
Ca)
Figure 19. Micrograph of s_mple $89-12. Field of view:. 3.9 x 2.7 turn View (a) gives data
as seen in thin section and ordinary light. View Co)is a micrograph for the s_rne
image area recorded in fluorescent light.
$7
!
(a)
Co)
Figure 20. Micrograph of sample $89-13. Field of view: 3.9 x 2.7 ram. View (a) is seen in
thin section and ordinary light. View (b) is a micrograph of the same image
area recorded in fluorescent light.
59
Ca)
Figure 21. Micrograph of sample $89-14. Field of view. 3.9 x 2.7 rnrn. View (a) depicts its
appearance in ordinary light. View (b) represents the same image as View (a),
but is recorded in fluorescent light.
61
(a)
I,
_b)
Figure 22. Microgrraph ofssmple S 89-15. Field of view: 3.9 x 2.7 rrrm View (a) gives
details of the sample as seen in ordinary light. View [b) depicts the s_me image
as recorded in fluorescent light.
63
+"++ Ca)
(b)
Figure 23. Micrograph of smmple $89-16. Field of view:. 3.9 x 2.7 ram. View (a) represents
the sample as seen in thin section recorded in ordinary light. View (b)
represents the s_me s_mple recorded in fluorescent light.
65
Ca)
Figure 24. Micrograph of sample $89-17. Field of view: 3.9 x 2.7 mm View (a) represents
the sample as seen in thin section and ordinary light. View (b) represents a
micrograph of the s_me area recorded in fluorescent light.
67
Ca)
_b)
Figure 25. Micrograph of sample $89-18. Field of view: 3.9 x 2.7 rr_m. View (a) depicts the
sample as seen in thin section and ordinary light. View (b) represents a
micrograph of the same area recorded in fluorescent light.
69
i (a)
(b)
Figure 26. Micrograph of sample S89-19. Field of view: 3.9 x 2.7 mm. View (a) represents
the sample as seen in thin section and ordinary light. View (b) represents the
same sample recorded in fluorescent light.
71
Figure 27. SEM electron backscatter photographs of polished sections of $89-9 (upper) and
$89-8 flower) samples. The higher relief observed in the upper photo is
attributed to lower matrix strength.
75
o
Figure 28. SEM electron backscatter photographs of polished sections of $89-5 (upper) and
$89-4 (lower) samples. Once again, higher relief observed in the upper photo
occurred during polishing, reflecting relative matrix weakness.
75
Appendix B
Tables
q
"_'a,l_e I,
79
T'_:_le 1 ct.d.
80
Table I ct4.
! I 'I
i II. i,
I iIII
III,I ,L
lliil!l
II
lJ !,l
Li IL!ii'i'Ii!
l!j llIll
Ii!IIIibil1I;iL l IIIIIi!ll
*I 'w_, , * ,0 O'O
°°°- I I I'"
81
Table 2. Concrete Mix No. $89-1Ma.
Cement (Keystone) 32.20 Pounds

Lycornlrlg Sand (PTM 616) 51.77 Pounds
Limestone Aggregate 93.40 Pounds
Water 15.13 Pounds
Water/Cement Ratio (calc) 0.47
Mleromractm_ Scale
Cracks > 0.1 mm 0

Cracks < 0.1 mm 1 A few microcracks in paste.
Average intercept: 1.45 cm

Specific surface of crack planes: 1.38 cm2/_c_n3
Paste/aggregate cracks 1-2 Occaslon_l]y porous zones and cracking

around several llmestone coarse aggregate
particles.
Mean free distance: 0.72 em

Specific aggr. surface: 5.60 cm2/cm 3
Interface with porosity. 20% or I. 11 cm2/c yn3
Coarse agg. distribution 1
Fine agg. distribution 0-1
Cement paste distribution

macro 1
1
Entrapped air 0
w/c measured 0.46 measured as an average over entire thin

section
8?.
Table 3. Concrete Mix No. $89-2Ma.
i

Lycom|ng Sand (PTM 616) 37.05 Pounds
T,Iroestone Aggl_gate 106.25 Pounds
Water 17.01 Pounds
Mleroo_arQetm_ Scale
"- Cracks > 0.1 mm 0

Cracks < 0. I mm I A few microcracks in paste.

Specific surface of crack planes: 2.72 cm2/cm 3
Paste/aggregate cracks 1-2 Porous zones and cracking around several

limestone coarse aggregate particles
Mean free distance: 0.56 em

Specific aggr. surface: 7.18 cm2/c_13
Interface with porosity. 50% or 3.59 cm 2/cm 3
Fine agg, distribution 0-1

macro 2
rmcm 1
Entrapped air 0
w/c measured 0.46 measur_ as an average over entire thin

section
83
Table 4. Concrete Mix No. S89-3M28a.
Recipe
C_ent (Keystone) 36.21 Pounds
Lycoming Sand (FrM 616) 57.10 Pounds
Water 17.02 Pounds
Mlerc_x_'tm_ Scale
Cracks > 0.1 mm 0 - "


Sper_flc surface of crack planes: 1.44 cm2/cm 3

limestone coarse aggregate particles.
Mean free distance: 0.73 cm

Interface with porosity:. 5% or 0.27 cm2/cm 3
Coarse agg. distribution I

macro I
mtero 1-1
Entrapped air 0

section
84
Table 5. Concrete Mix No. S89-4M28a.
Rpe
Lycomi_g Sand (FIM 616) 75.70 Pounds
Water 17.02 Pounds
Mi_ Scale
Cracks > 0.1 mm 0

Average intercept: 1.43

Speolflc area of crack planes: 1.40 cm2/rm 3

limestone coarse aggregate particles.
Mesnfree distance: 1.12 cm

Interface with porosity=. 30% or 1.07 cm2/cm 3
Fine agg. distribution 0-I

macro 1
micro 0-1
Entrapped air 0

section
8S
Table 6. Concrete Mix No. $89-5Mb.
Rec
Lycoming Sand _ 616) 48.56 Pounds
Water 13.30 Pounds
Mlcrostructure Scale
Cracks > 0.1 mm 0 "

Cracks < 0.1 mm 2 Several microcracks in paste.
Average intercept: 0.45

Specific area of crack planes: 4.55 em2/cm3

]_nestone coarse aggregate particles.

Specific aggr. surface: 10.10 cm2/c_3
Interface with porosiW. 30% or 3.03 cm2/cwn3
Coarse agg. distribution 0-1

rrm<wo 2 Area with more dense paste in one side of
thin section.
micro 2 Some clotting in paste.
Entrapped air 0

section
i
86
P.ec
Cement {Keystone) 28.29 Pounds
Lycoming Sand (PTM 616) 73.32 Pounds
Water 13.29 Pounds
Mighty 150 SPL 0.42
_ Water/Cement Ratio (calc) 0.47
Microstraetu_ Scale
° .
Cracks > 0.1 mm 0

Cracks < 0.I mm 1 A few micro_-acks in paste.
Average intercept: 1.18 c_n

Specific area of crack planes: 1.70 cm2/_cwn3
Paste/aggregate cracks 2-3 Occasionally cracking around limestone

coarse aggregate particles but practically
no porosities.

Interface with porosity= 0% or 0 cm 2/cm 3
Fine agg. distribution 0-I

macro 1 Area with more dense paste in one side of
thin section.
micro 1-2 Some clotting in paste.
Entrapped air 0

section
87

Lycomlng Sand (PTIVI616) 89.20 Pounds
Water 13.30 Pounds
Mighty 150 SPL 0.63
Mlcrostruet_e Scale
Cracks > 0.1 rnrn 0

Cracks < 0.1 rnrn 1 A few microcracks in paste.

Specific area of crack planes: 2.70 cm2/e_rn 3
Paste/aggregate cracks 1 Occasion_11y porous zones and cracking

around limestone coarse aggregate particles.

Specific aggr. surface: 2.93 _2/cm3
Interface with porosity. 20% or 0.59 _c_rn2/_
c_n3
Cement paste tlJ-qtrlt_ution

1 Area with more dense paste in one side of
thin section.
micro 1-2 Some dotting in paste.
Entrapped air 0

section
88
Table 9. Concrete Mix No. $89-8.

Lycomlng Sand (FI"M616) 57.02 Pounds
Water 13.54 Pounds
Mighty 150 SPL. 0.32 Pounds
Water/Cement Ratio (ca)c) 0.42
Inhomogeneity

Fine agg. distribution 0/1
Cement paste
macro 1
micro 1
Entrapped air 0
w/c measured 0.45
Coarse Aggregate
P1 mm "I 0.21
Sv= 2x_ mm-I 0.42
T_ml_:]a rnrn-1 5.26
Microcracb
Pj ram- I 0.18
L mm 3.07
Epsflon 0.30
89
Recipe
Cement (Keystone} 24.81 Pounds
Lycornlng Sand WTM 616) 36.57 Pounds
Water 13.15 Pounds
Inhomogeneity

Fine agg. distribution 0/I
Cement paste
macro 1
micro 1
Entrapped air 0
w/c measured 0.45
Coarse Aggregate
PI mm'l 0.338
Sv= 2xPl ram-1 0.676
T_rn'l"_da rnm "I 3.04
Microcracks
PI ram- 1 0.04
L u_ 12.85
Epsflon 0.10
i
9O
P.ece
Cement (Keystone)2 2.32 Pounds
Lycoming Sand (PTM 616) 60.12 Pounds
Newcem Slag 14.88 Pounds
Water 17.49 Pounds
Water/Binder Ratio (calc) 0.47
Inhomogeneity

Cement paste
macro 1
micro 1
Entrapped air 0
w/c measured 0.35
Coarse _gregate
I_ mm "I 0.214
Sv= 2xPI mm "I 0.428
Lambda ram-1 4.80
Microcracks
PI mm-I 0.251
L mm 2.05
Epsflon 0.51
91
i i
P.ec
LycornJng Sand (PTM 616) 59.62 Pounds
Fly Ash Class F 6.33 Pounds
Water 17.08 Pounds
Tnhomogeneity
Coarse agg. dtctribution 1

Cement paste
macro 1
micro 1
Entrapped air 0
wlc measured 0.45
Coarse Aggregate
Pl ram-1 0.172
Sv= 2xPI ram-1 0.344
I_rnhda mm -I 4.37
/_icrocracks
PI rrrm-1 0.06
L mm 6.27
Epsflon 0.20
92
Table 13. Concrete MixNo. $89-12.
Ree
Lycomlng Sand (PTIVl616) 60.45 Pounds
Ltmestone Aggregate 107.78 Pounds
Fly Ash Class C 6.33 Pounds
Water 15.94 Pounds
Inhomogeneity
w .

Cement paste
macro 1
micro 1
Entrapped air 0
w/c measured 0.45
PI ram- 1 0.14
Sv= 2xPI ram-1 0.28
T_mhda m "I 6.69
M/crocracks
PI ram-1 0.12
L mm 3.90
Epsflon 0.32
95
Table 14. Concrete Mix. No. $89-13
Rec_
Lycomtng Sand {FI1VI616) 59.93 Pounds
!.Imestone Aggregate 107.78 Pounds
Silica Fume 2.79 Pounds
Water 15.13 Pounds
Mighty 150 SPL 0.2 Pounds .
Inhomogenelty

Cement paste
macro 1
micro 1
Entrapped air 0
w/c measured 0.45
Coarse ._gregate
PI mm-1 0.168
Sv= 2xPI rnm'l 0.336
!-qrnhda ram" 1 4.92
Microcraeks
PI ram-1 0.455
L mm 0.91
Epsflon 0.30
94
Table 15. Concrete MixNo. $89-14.

Lycomlng Sand (PTM 616) 19.91 Pounds
Limestone Aggregate#8 35.40 Pounds
Water 5.82 Pounds
Water/C_ment Ratio (calc) 0.47
Inhomogeneity
" Coarse agg. distribution 1

Cement paste
macro 1
micro 1
Entrapped air 0
w/c measured 0.45
Coarse Aggregates
Pl mm-1 0.333
Sv= 2xPI mm-I 0.666
T-_mhda ram- I 2.70
Microcracks
PI ram- 1 0.105
L mm 4.28
Epsflon 0.13
95
Recipe

Lycomiz_ Sand [FI3Vl 616) 59.73 Pounds
Siliceous Aggregate#67 105.78 Pounds
Water 17.46 Pounds
Tnhomogeneity
Coarse agg. di_hlbution 1

Cement paste
macro 1
micro 1
Entrapped air 0
w/c measured 0.45
Coarse Aggregate
PL rrm1-1 0.177
Sv= 2xPI mm -I 0.354
t_s"n_ rm'n-1 4.77
Microcracks
PI mm -1 0.08
L mm 5.28
Epsflon 0.15
95
Zed
Water 5.82 Pounds
Inhomogeneity
" Coarse agg. distribution I

Flne agg. distribution 0/1
Cement paste
macro I
micro 1
Entrapped air 0
w/c measured 0.45
coarse egate
PI mm "1 0.43
Sv= 2xPl mm -1 , 0.86
T_rrthda mm-I 2.18
Microcracb
PI mm -i 0.13
L mm 3.60
Epsflon 0.18
97
Table 18. Concrete M/x No. $89-17.
Re.pc
Cement (Keystone} 20.90 Pounds
Towson Siliceous Aggregate 60.18 Pounds
Water 9.82 Pounds
Inhomogeneity

Fine agg. distribution 1 .-
Cement paste
macro I
micro 1
Entrapped air 0/I
w/c measured 0.40 - 0.45
Coarse sggregate
Pi rm_-I 0.191
Sv= 2xPl mm "1 0.382
I_mhda mm -1 5.03
Microcracks
PI mm-I 0.11
L mm 4.36
Epsflon 0.35
98
P.ec
Lycomlng Sand (IrrM 616) 32.94 Pounds
Towson Siliceous Aggregate 45.53 Pounds
Water 9.83 Pounds
Water/Cement Ratio (ca]c) 0.47
. Tnhomogeneity

Cement paste
macro 1
micro 1
Entrapped air 0
w/c measured 0.35
coarse
turn-1 O.191
2xPI mm -I 0.382
T_mtx:]a Into" 1 5.76
Microcracks
PI ,_In-I 0.11
L mm 5.00
Epsflon 0.33
99

Towson Slllceous Aggregate 34.70 Pounds
Water 9.83 Pounds
Water / Cement Ratio (calc) 0.47
Tnhomogeneity
Coarse agg. distribution 1 .-

Cement paste
macro 1
micro 1
Entrapped air 0
w/c measured 0.35 - 0.40
Coarse sggregate
PI ram-1 0.159
Sv= 2xP1 ram-1 0.318
Lambda ram-1 9.31
Microeracks
PI mm "I 0.11
L mm 6.73
Epsilon 0.20
IO0
Appendix C
Nordtest 677-87
Concrete, Hardened; Water-Cement Ratio
1 (4)
.. CONCRETE, HARDENED: WATER-CEMENT RATIO UDC691.32
Key words: test method, concrete, hardened
1 SCOPE 4 DEFINITIONS
(_ This NORDTEST method can be applied to estimate the Water-Cement Ratio: W/C ratio. The ratio by weight
water-cement ratio (W/C ratio) in hardened concrete, using between water and cement in concrete.
microscopic investigationof thin sections.
Capillary porosity: The number of submicroscopic pores
(greater than 50 nm) which can possibly be filled with epoxy
2 FIELD OF APPLICATION resin.
The method is applicable for well-hydrated Ordinary Portland
Cement (OPC) concrete with or without admixtures such as Degree of hydration: The ratio byweight of hydrated cement
plasticizers and air-void entraining agents, to the total cement.
The degree of hydration of the tested concrete and the Equivalent W/C ratio: The apparent W/C ratio of concrete
references shouldbe of the same order, containing fly ash, silica fume or slag.
The method is not applicable when fly ash, silica fume and 5 SAMPLING
slag are present. In these cases the "equivalent water-cement
If no sampling procedure is described in the test report,
ratio" is estimated in the same manner as for OPC. It is not
possible to estimate the W/C of Polymer Cement Concrete sampling is as stated in NT BUILD 191 or NT BUILD 202.
(PCC) or of coloured concrete. The number of specimens is not stipulated.
_- 6 METHOD OF TESTING
6.1 Principle
3 REFERENCES The capillary pores in the cement paste are filled with
Sandstr6m Matz: Mikroskopisk bed6mning av vct i betong, fluorescent epoxy by impregnating the specimen in vacuum.
_" SP-AR 1988:43, Statens provningsanstalt, Bor&s 1988. A thin section isthen prepared and analyzed in a microscope.
The intensity of fluorescence of the cement paste is afunction
Kdstensen J A, Brandt I, Damg_d Jensen A: Betons of the capillary porosity. The capillary porosity is a function of
mikrostruktur. Projektrapport, Teknologisk Institut, Taastrup the W/C ratio and the degree of hydration. The W/C ratio can
1988. therefore be estimated by comparing the thin section of the
test sample with a thin section of a reference sample under a
NORDTEST: NT BUILD 191, NT BUILD 192, NT BUILD 202 microscope.
_, Published by NORDTEST Postbox 111 SF-02101 ESBO FINLAND Tel + 358 0 455 4600 Fax + 358 0 455 4272
103
ISSN 0283-7153 Proj. 677-87
NORDTEST METHOD NTBUILD361 2
6.2 Apparatus 6.2.2 For examination of thin section
6.2.1 For preparation of thin sections Standard polarizing microscope for examination in
transmitted light with
Diamond saw
Barrier filter 510 - 530 nm
Drying chamber
Lenses 2 - 10x
Vacuum chamber
Oculars 10x
Face grinding machine with diamond impregnated disc for
coarse surface grinding. Exciter filter BG12, 3 mm or equivalent
. r
Face grinding disc impregnated with diamonds, of grain size

25 - 30 microns, for final surface grinding.
6.3 Preparation of samples
Epoxy Resin CIBA CEIGY BY 158 or equivalent 6.3.1 Preparation of thin sections
The following procedure is an example of the method of
Hardener CIBA CEIGY HY 2996 or
equivalent preparation. Other methods can be used as long as a thin
section with the same thickness and quality is obtained. -
Fluorescent dye DAYGLO HUDSON YELLOW or

equivalent, (1% by weight of the
epoxy) Cutting of the specimen
Alcohol A specimen of minimum size 40 x 20 x 10 mm, see figure 1, is

cut with a diamond saw and glued with epoxy on a
Microscope slide minimum 28 x 48 mm microscope slide (working glass). The specimen is then face
ground, see figure 1.
Cover glass
Canada Balsam or equivalent Dryingthe specimen

The specimen is dried in alcohol or in a drying chamber
Epoxy Low molecular weight overnight at 30 - 40 °C.
A B
• • ,. -
ql=
Concrete block Polished
Figure I Test sample (A) of concrete, glued on a microscope slide (working glass) and face ground (B).
104
A B
Working glass"
Concrete specimen
..
(
• Object glass
t_'i, Figure 2 The impregnated sample mounted on a microscope slide (object glass) (A) and cut approximately 1 mm above
the object glass (B)
Impregnation Finishingthe thin section

The specimen is evacuated in a vacuum chamber at The cover glass is mounted on the specimen with Canada
maximum 0.05 Bar for approximately 10 rain. The epoxy, balsam, seefigure 3.
prepared in advance, is added and the vacuum is maintained
for another 10 minutes. The specimen is then stored in a Cover gloss
plastic bag at normal atmosphere until the hardening of the
epoxy is complete. Concrete specimen
Grinding of the lower surface of the thin section
The specimen is ground until the edges of the air voids are
sharp. The paste should, however, still be fully impregnated
with epoxy. To ensure that the surface issatisfactory, grinding
should be carried out in two steps. Firstthere should be face
i grinding to achieve an absolutely plane surface, followed by j/,-;t' ,(,'..-._,.'_
v final grinding on the gnndmg disc to achieve a smooth
surface. (" k
\Object glass
Mounting on microscope slloes
The specimen is glued to a m_croscopeobject glass slide with Figure 3 The concrete slice on the object glass is ground to
,_ the ground face towards the slide, see figure 2. a thickness of 25 microns and protected with a
cover glass.
_ Grinding of the upper surface of the thin section
The specimen is cut approximately 1 mm above the glass
slide, see figure 2. 6.3.2 Thin section of the reference concrete
Six different batches of concrete are made.
The upper surface of the thin section is face ground on the
face grinding machine until the thickness of the specimen is Concrete for making reference samples should have the
about 0.05 mm. Grinding is then continued on the grinding following composition
disc until the thickness is 0.025 ram. The thickness is checked
by use of birefringent colours of common minerals such as W/C ratio 0.35; 0.40; 0.45; 0.5; 0.6; 0.7
quartz and feldspar.
Maximum size of aggregate 8 mm
It is very important that the thickness is the same in all parts of
the thin section. Paste content _ 30 % by volume
105
Slump 60 - 80 mm 6.5 Results
Aircontent - 3 % The W/C ratio is determined as the mean value of the W/C
ratio in 10 fields of images.
Plasticizer if necessary The W/C ratio isstated as a non-dimensional number with two
decimals where the second decimal is rounded to 0 or 5.
From each batch of concrete a sample is prepared according
to NT BUILD 201. Thin sections from each reference sample The variation of the W/C ratio is stated as homogeneous,
are then prepared according to section 6.3.1. The thin
sections used as references should always be stored in a dark inhomogeneous or very inhomogeneous, according to . °
table 1.
place,
New references should be prepared when the method for

sample preparation is changed. Table I Homogeneity of cement paste
Once a year the intensity fluorescence of the reference Homogeneity Range of variationof W/C in
samples should be checked. If there have been any changes 10 fields of images
new reference samples must be made. Homogeneous < 0,1
Inhomogeneous 0.1 - 0.2
6.3.3 Thin section of test samples Very inhomogeneous -> 0.2
A thin section of the test sample is made according to section
6.3.1 and in the same way as the reference samples are
prepared.
The following should be noted:
- The paste content and air void content must be of the 6.6 Test report
same order as in the reference samples The test report shall include the following information,when
relevant:
- The thickness of the thinsections of the test sample and
of the reference samples must be 25 microns, a) Name and address of the testing laboratory
b) Identification number of the test report
6.4 Procedure c) Name and address of the organization or the person
6.4.1 Examination of test samples ordering the test
The exciter filter and the barrierfilter are placed in the ray path d) Purpose of the test
of the microscope. The test sample is placed on the e) Method of sampling and otherfactua! information (date
microscope stage. The reference samples are then placed on and person responsible for sampling)
the stage by turn. The W/C ratio is determined to the nearest
0.05 by comparing the fluorescent intensity of the samples, f) Name and address of manufa_urer or supplier of the
tested object
The W/C ratio is determined in 10 different fields of images, g) Name or other identification marks of the tested object
h) Description of the tested object
The range of variation between the fields is calculated.
i) Date of supply of the tested object
During the examination the following must be considered: D Date of test ,i, ._
k) Test method
- The air void content and the cement paste content in the
field of image of the test sample and the reference m) Any deviations from the test method
sample must be of the same order, n) Test results
- Each field of image must be in uncarbonated cement o) Inaccuracy or uncertainty of the test results
paste and at least 5 mm from the original surface of the p) Date and signature
concrete.
106
Concrete and Structures Advisory Committee
Chairman Liaisons
James J. Murphy
New York State Department of Transportation (retired) Theodore R. Ferragut
Federal Highway Administration
Vice Chairman
Howard H. Newlon, Jr. Crawford F. Jencks
Virginia Transportation Research Council (retired) Transportation Research Board
Members Bryant Mather

"_ _, USAE Waterways Experiment Station
Charles J. Arnold
Michigan Department of Transportation Thomas J. Pasko, Jr.
", Federal Highway Administration
Donald E. Beuerlein
Koss Construction Co. John L. Rice
Federal Aviation Administration
Bernard C. Brown
lowa Department of Transportation Suneel Vanikar
Richard D. Gaynor
National Aggregates Association Ready Mixed 11/19/92
Concrete Association
Expert Task Group
Robert J. Girard
Missouri Highway and Transportation Department Amir Hanna
Transportation Research Board
David L. Gress
University of New Hampshire Richard H. Howe
Pennsylvania Department of Transportation (retired)
Gary Lee Hoffman
Pennsylvania Department of Transportation Stephen Forster
Brian B. Hope
Queens University Rebecca S. McDaniel
Indiana Department of Transportation
Carl E. Locke, Jr.
University of Kansas Howard H. Newlon, Jr.
Virginia Transportation Research Council (retired)
Clellon L. Loveall
Tennessee Department of Transportation Celik H. Ozyildirim

Virginia Transportation Research Council
David G. Manning
Ontario Ministry of Transportation Jan P. Skalny

W.R_ Grace and Company (retired)
Robert G. Packard
Portland Cement Association A. Haleem Tahir
American Association of State Highway and Transportation
James E. Roberts Officials
t California Department of Transportation
Lillian Wakeley
John M. Scanlon, Jr. USAE Waterways Experiment Station
Wiss danney Elstner Associates
_ Charles F. Scholer
Purdue University
Lawrence L. Smith
Florida Department of Transportation
John R. Strada
Washington Department of Transportation (retired)

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SHRP-C-662

Materials Research Laboratory

G.M. Idom Consult A/S

Strategic Highway Research Program

Program Manager: Don M. Harriott

Strategic Highway Research Program

© 1993 National Academy of Sciences

Abstract ........................................................ vii

2 Preparation of Fluorescent, Concrete Thin-Sections ......................... 3

3 Examination of SHRP 1-19 Concrete Samples ........................... 13

" Appendix A Figures ............................................... 23

Appendix B Tables ................................................ 77

Appendix C Nordtest 677-87 Concrete, Hardened; Water-Cement Ratio .......... 101

The examination of concrete microstructure, whether in thin section or reflected light/SEM,

Today, about 6000-7000 fluorescent concrete thin-sections are prepared annually in

A desiccator with an attached vacuum pump,

Before preparation of the thin-section, it is important to select a proper volume of concrete

The specimen should be allowed to dry for approximately 2 hours.

Figure 1 is a schematic drawing of a "Leitz" petrographic microscope. The figure shows

Examination of the thin-sections can be performed in four different modes:

Examination of Fluorescent Thin-Sections

Another problem which is often encountered in fluorescent thin-section analyses is caused

Several other undesirable phenomena caused by the preparation procedure could be

Carbonation due to the weathering of concrete structures is seen in polarized light as an

A. Damgaard Jensen, "Investigation of Concrete by Analyses of Thin-sections" IABSE

A. Damgaard Jensen, "Strukturanalyse af Beton" (Structural Analyses of Concrete), Beton

H. Gudmundsson, S. Chatterji, A. Damgaard Jensen, N. Thaulow and P. Christensen,

B. Mayfield (1990), "The Quantitative Evaluation of the Water/Cement Ratio Using

Nordtest 677-87, "Concrete, Hardened: Water-Cement Ratio," Nr. 677-87.

E. Soers, "Preliminary Results on a Petrographical Examination of Alkali-Silica Reactions

N. Thaulow, A. Damgaard Jensen, S. Chatterji, P. Christensen and H. Gudmundsson,

N. Thaulow, K.T. Andersen and J. Holm, "Petrographic Examination and Chemical

W. Wilk and G. Dubrolubov, "Microscopic Quality Control of Concrete During

Nineteen concrete samples were received and identified as follows:

MRL No. GMIC No. T.S. No. Received

S89-1Ma 389-1 3113-1 24 April 89

One thin section was prepared from each sample.

0: Not present, insignificant.

Two other parameters were determined in order to quantify the microstructure:

Samples $89: 1Ma, 2Ma, 3M28a and 4M28a

The cement paste is homogeneous both in macro- and micro-scale.

Samples $89: 5Mb, 6Mb and 7Mb

Samples $89: 8 and 9 (Tables 1, 9, 10, Figures 15, 16)

Samples $89: 10, 11, 12 and 13 (Tables 1, 11-14, Figures 17-20)

Samples $89: 14, 15 & 16 (Tables 15-17, Figures 21-23)

Samples S 89: 17, 18 & 19 (Tables 1, 15-17, Figures 24-26)

E.E. Underwood, Quantitative Stereology, Addison-Wesley Publishing Company, Reading,

Preliminary observations were made on some of the fluorescent epoxy impregnated

L. Struble and E. Byrd, "Epoxy Impregnation of Hardened Cement Pastes for

L. Struble and P. Stutzrnan, "Epoxy Impregnation Procedure for Hardened Cement

1: Slot for compensator or yellow filter

Figure 9. Micrograp__ cf sample $89-2Ma depicting a homogeneous ce_._ent paste.

Cement (Keystone) 32.20 Pounds

Cracks > 0.1 mm 0

Average intercept: 1.45 cm

Paste/aggregate cracks 1-2 Occaslon_l]y porous zones and cracking

Mean free distance: 0.72 em

Coarse agg. distribution 1

Fine agg. distribution 0-1