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CEMENT and CONCRETE RESEARCH. Vol. 9, pp. 653-654, 1979. Printed in the U.S.A.

0008-8846/79/050653-02S02.00/0 Copyright (c) 1979 Pergamon Press, Ltd.

HOW TO PREPARE POLISHED CEMENT PRODUCT SURFACES FOR


OPTICAL MICROSCOPYWITHOUT INTRODUCING VISIBLE CRACKS
Dirch H. Bager and Erik J. Sellevold
Technical University of Denmark
Building Materials Laboratory
Building 118, 2800 Lyngby
Denmark
(Communicated by P. J. Sereda)
(Received May 2; in f i n a l form May 29, 1979)
ABSTRACT
I t is shown that preparation procedures may introduce cracks
in epoxy impregnated hardened cement paste specimens. This
is of v i t a l importance for optical microscopic examination.
A method which gives no v i s i b l e cracks due to preparation is
described.
Introduction
Microscopic examinations of hardened concrete have been carried out for a
long time in order to assess the degree of deterioration of old concrete, and,
more recently, to predict the d u r a b i l i t y of new concrete. Depending on the
purpose of the i n v e s t i g a t i o n e i t h e r thin sections or polished surfaces are examined. Thin sections generally allow more detailed examinations to be made,
p a r t i c u l a r l y in conjunction with polarized l i g h t and/or flourescent epoxy impregnation. Essential features to observe when assessing concrete q u a l i t y are
the crack pattern and the crack density. I t is consequently of v i t a l importance that no v i s i b l e cracks are introduced when the specimens are prepared.
Using cement paste specimens we w i l l show that preparation procedures in general use do introduce v i s i b l e cracks. A procedure which avoids the problem
w i l l be outlined.
Specimen preparation commonly includes the following main steps: a) sawing
and preliminary polishing under water; b) drying; c) epoxy impregnation and
hardening; and, d) final polishing. Based on our experience with the extreme
s e n s i t i v i t y cement paste displays towards even mild drying, we believe the ini t i a l drying to be the crucial step in the preparation procedure. Two procedures are therefore compared here: I) a "conventional" procedure involving drying, and, 2) a "new" procedure in which epoxy impregnation takes place via step.
wise l i q u i d replacement. Direct drying from a wet state is thus avoided.
Preparation Procedures
"Conventional" procedure
A procedure using a r e l a t i v e l y mild drying step was chosen. Specimens in
the form of disks (thickness = 1 cm, diameter = I0 cm) were cut from cylinders
and polished under water. The disks were dried in a dessicator over s i l i c a gel
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D.H. Bager, E.J. Sellevold

at atmospheric pressure for two days, followed by evacuation for one hour using
a mechanical pump. The dessicator was then opened and epoxy poured on the polished surface. A b r i e f period of evacuation followed.
A f t e r the epoxy had hardened the surface was again polished and was now ready for microscopic examination.
More severe drying steps are commonly used, for instance, d i r e c t pumping
on a specimen for one or two days at temperatures up to 40C. We expect increased s e v e r i t y of the drying procedure to r e s u l t in increased damage to the
specimen.
"New" procedure
A f t e r the i n i t i a l p o l i s h i n g of the specimen in water i t was submerged in
ethanol f o r about 24 hours. The surface to be impregnated was then quickly wiped
o f f and epoxy was poured over i t .
When the epoxy had hardened the f i n a l p o l i s h ing was performed.
Materials
The cement paste (w/c = 0.40) was mixed with Danish "Rapid" type cement.
Curing took place in water for about one month. The epoxy used is soluble in
ethanol, has a v i s c o s i t y of 550 cp. at room temperature and a p o t l i f e of 30 minutes.

FIG. 1
Polished sections of cement paste prepared by a ) " n e w " procedure,
and, b ) " c o n v e n t i o n a l " procedure.
Results
Figure 1 shows photographs of polished sections of hardened cement paste
prepared by the "new" (a), and the "conventional" (b) procedures. S i m i l a r , but
less d r a s t i c differences in crack d e n s i t i e s were observed in mortar specimens
prepared by the two procedures.
I t appears t h a t the "new" procedure with i t s replacement process rather
than a drying-impregnation process has been successful in not introducing v i s i b l e
cracks. This in s p i t e of the short time used, which probably has allowed only
shallow impregnation of the epoxy. We therefore believe t h a t the "new" procedure
is quite s u i t a b l e f o r routine work.
The ethanol treatment does not, however, prevent v i s i b l e
oping during drying. Cement paste disks soaked in ethanol f o r
dried in room conditions did show v i s i b l e cracks; although the
extensive than those developed in control specimens dried from

cracks from devel24 hours and then


cracks were less
a wet state.

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