CEMENT and CONCRETE RESEARCH. Vol. 23, pp. 329-334, 1993. Printed in the USA.

0008-8846/93. $6.00+00. Copyright © 1993 Pergamon Press Ltd.

THE POLARIZING MICROSCOPE :

A TOOL OF INTEREST FOR INVESTIGATION ON CONCRETE ;
APPLICATION TO CARBONATION.

s 8
L. CURTIL , J. GIELLY , M. MURAT**
* LGCHE, IUT Genie Civil,
69622 VILLEURBANNE CEDEX, FRANCE.
** GEMPPM (U.A. CNRS 341), INSA de LYON,
69621 VILLEURBANNE CEDEX, FRANCE.

(Communicated by M. MoranviUe-Regourd)
(Received March 7, 1992)

ABSTRACT
Polarizing microscope is the technique the more commonly used by geologists
whereas it is not so much used in concrete or mortar studies.
But nevertheless this technique can be very interesting in petrographic field for the
determination of aggregates (mineralogy, state of alt6ration, regularity of
composition, size of grains...) and for cement paste investigation.
This paper treats the study of the carbonation of concrete by polarizing
microscope.

RESUME
Le microscope polarisant est l'outil le plus utilis6 par les g6ologues alors qu'il ne
l'est ~u6re dans l'6tude des b6tons et mortiers. Or son utilisation peut se r6v61er
fort instructive quant ~ la nature des granulats (min6ralogie, 6tat d'alt6ration,
r6gularit6 de composition ...) mais 6galement des renseignements peuvent 6tre
obtenus sur la pate de ciment. L'objet de cet article est l'6tude de la carbonatation
de la pgtte de ciment d'un b6ton au microscope polarisant.

Introduction
The study of hardened concrete requires the use of some instrumental techniques
(1) : optic microscope in reflected light, scanning electron microscope, energy-dispersive X-
ray analysis, X-ray diffraction, infra-red spectroscopy...
Polarizing microscope (2,3) is not much used in concrete study although it is an excellent
and less expensive analysis technique.
This work shows the interest of investigation on the behaviour of concrete towards
carbonation by use of a polarizing microscope.

329
 330 L. Curtil et al. Vol. 23, No. 2

Polarizing microscope
The favourite technique of geologists, polarizing microscope is very useful in petrographic
study for the determination of mineralogy and structure (4).
During the microscopic examination, the light must pass through the samples that is why it
is necessary to make a thin section of sample. This section must be thirty microns thick.
Study by polarizin~ microscope is composed of two parts :
- First an observation of the form, the colour, the breaks, the cleavages of minerals is made
under plane-polarized light.
-Then with crossed polars, we determine the birefringence and the extinction angle of
minerals.
A third phase can be necessary sometimes with the use of Bertrand lens to know the optic
sign of minerals.
Use of the polarizing microscope is very interesting to determine the mineralogy of
concrete aggregates, their state of alteration, their size, their regularity of composition ....
Moreover with a greater magnification, some interesting information about components of
cement paste can be collected and more particularly about calcite and also about the
carbonation depth of cement paste.
Carbonation
Carbonation is a natural phenomenon of concrete : action of carbon dioxide in air
0.03% in air) (5). The CO 2 acts on components of concrete in gaseous phase or in water
the dissolved CO~ has an action more efficacious).
In fact, from the-thermodynamic viewpoint (equilibrium state at infinite time), all the
hydrated or anhydrous compounds with calcium must undergo carbonation. The ultimate
formed phases are calcium carbonate, hydrated silica, alumina and ferric oxide (6).
The CO 2 acts progressively on hydrates of cement (7). The portlandite (CH) is the faster
converted to CaCO 3 (8), hut calcium aluminates and silicates also react at short range with
carbon dioxide to form transitional carbohydrates (carboaluminates and carbosilicates) (9).
Carbonation modifies progressively the structure of the material and therefore its
behaviour.
It can be beneficial (diminution of porosity) or harmful (decrease in alkalinity and also
possible destruction of the protective p assivation zone around steel reinforcement).
This phenomenon modifies the durability of the structure. That is why a good knowledge of
this phenomenon is very necessary.
In order to clarify the expression of this phenomenon, we used the polarizing microscope to
visualize the depth of carbonation in cement paste and to compare this with the depth
obtained by the phenolphtalein test. Moreover we obtained information about the nature
of carbonation reaction products.
Study of the carbonation by polarizing microscone
1 Samples investigated
We have made thin sections of a twenty years old concrete. This concrete had a good
general appearance and was weakly carbonated : the depth of the carbonation was only 15
mm.
2 Use of the analyser and its particular interests
Observations made with a polarizing microscope under plane-polarized light are the same
as ones with an ordinary microscope. In figure 1A, we observe aggregates and cement paste
of concrete with the polarizing microscope using plane-polarized light. The magnification is
too low t o distinguish minerals of paste. The same figure can be obtained with an optic
microscope.
On the other hand with crossed polars (original aspect of polarizing microscope), minerals
are coloured depending on their birefringence, their thickness and their orientation. That is
why we can distinguish very clearly in figure 1B the carbonated paste (in light) from the
uncarbonated paste (in black).
Vol. 23, No. 2 CARBONATION, CONCRETE, PETOGRAPHY, MICROSCOPY 331

FIG 1 :Polarizing Microscope micrograph showing a concrete, the surface of which is

above the top of the micrograph (depth = 15mm)A. under plane-polarized
light. B. with crossed polars. We can observe quartz, quartz with undulatory
extinction, feldspar, carbonated paste (in light) and uncarbonated paste (in black).

3 Phenolphtalein test and its particular interests

A rapid test method exists for determining the depth of carbonation by using
phenolphtalein solution (7): uncarbonated cement paste is defined by a pink colour
because of the presence of portlandite whereas carbonated cement paste is colourless.
Change in colour of phenolphtalein occurs between pH 8,2 and pH 10.
a) Study with a low magnification.
- Uncarbonated zone (depth > 15ram).
Figures 2A and 2B show a zone before the use of phenolphtalein test. Figures 2C and 2D
show the results. In these figures we have a representation of an uncarbonated paste after
reaction with phenolphtalein (pink colour on micrograph ; figure 2E).
- Transition between carbonated zone and uncarbonated zone (10mm < depth < 15ram).
In figures 3A and 3B, we have the same experiment (after the use of phenolphtalein). We
can see that the exact boundary of carbonation is not revealed by the test (table 1). In fact
the latter gives a greater value of the depth of carbonation :

TABLE 1 : Phenolphtalein test and carbonation.

Depth Carbonation Staining by

phenolphtalein

0-10mm calcite Colourless

10-15mm no calcite Colourless

> 15mm no calcite Pink Colour

b) Study of an uncarbonated zone with a bigger magnification (depth > 15mm).

Figures 4A and 4C show an uncarbonated zone at different magnifications. When we use
phenolphtalein on thin section of a concrete, the uncarbonated zones are coloured
uniformly in pink. But with a microscope, we can see that the pink colour is not uniform
(figures 4B and 4D) : only portlandite (CH) and lime (C) reacted to phenolphtalein by a
332 L. Curtilet al. Vol.23, No.2

..... 0,s o ' s m~

FIG 2 : Polarizing Microscope micrograph showing a concrete (depth = 25ram)A. under

plane-polarized light. B. with crossed polars. C. under plane-polarized light with
phenolphtalein. D. with crossed polars with phenolphtalein. E. schema of 2C or 2D
showing the uncarbonated paste after reaction with phenolphtalein (pink colour on
micrograph). We can observe quartz and microcrystalline quartz.

colour Portlandite comes from the hydration of 3CaO.SiO-) (CaS) or 2CaO.SiO-)

P c 2 i n k
( S) of ar~ydrous cement. Lime is a clinker residue. Lime is coloTared-by phenolphtalei~
because it is hydrated superficially by the aqueous solution of phenolphtalein.
In these figures, we probably have lime twenty years old. Pink aureoles correspond to the
presence of OH'. In fact, these are isotropic grains scattered in cement paste. Therefore
Vol. 23, No. 2 CARBONATION, CONCRETE, PETROGRAPHY, MICROSCOPY 333

FIG 3 : Polarizing Microscope micrograph showing a concrete (depth = 15ram) A. under

plane-polarized light with phenolphtalein. B. with crossed polars with
phenolphtalein. We can observe quartz, microcrystalline quartz and conglomerate
of fine particules cemented by micrite. The uncarbonated paste does not react with
phenolphtalein.

0.5 I

1 ~iilll
/
FIG 4 : Polarizing Microscope micrograph showing a concrete (depth = 25ram) A. under
plane-polarized light with phenolphtalein. B. schema of 4A showing the pink
colour. C. enlarged portion of the uncarbonated cement paste showing probably
lime. D. schema of 4C showing the pink colour.

they could not become hydrated (2). They do not surround aggregates like amorphous
Ca(OH)7. Besides this is a thin section of a concrete with some signs of alkali-ae_j~re~ate
reaction-and we know that there is more lime in clinkers rich in alkali oxides. -- -
334 L. Curtil et al. Vol. 23, No. 2

Conclusion

The three findings of this study by polarizing microscope are :

- First, we should use the polarizing microscope which is a technique of analysis offering
many possibilities in the study of hardened concrete. In fact, the polarizing microscope
gives clear pictures of the carbonation of concrete or mortar and the mineralogical
components can be identified.
- Phenolphtalein test is an excellent indicator of pH and therefore an excellent detector of
the vulnerability of the framework. But it is not accurate for determining the depth of
carbonation because it overestimates the depth of carbonation.
- The only way to distinguish portlandite (CH) to lime (C) which reacted to phenolphtalein
by a pink colouration is their different forms.
References

1. F.X. DELOYE. "L'analyse du b6ton durci", Le b6ton hydraulique , Presses de

l'Ecole Nationale des Ponts et Chauss6es (Paris, 1982), p531-541.
2. P. TERRIER & H. HORNAIN. " Sur l'application des m6thodes min6ralogiques
rindustrie des liants hydrauliques, Publication technique n ° 180, Revue des
Mat6riaux de Construction "ciments et b6tons" (1967), n ° 618 ~ 621, p60.
3. E. KOELLIKER. "Skins of calciumcarbonate and their significance for the corrosion
of concrete", 8tla International Congress on the Chemistry of Cement, Rio, 1986, Vol
V, p159-164.
4. J. JUNG. Pr6cis de p6trographle, • Edition
'' Masson et C l e , Paris 1969.
5. H.G. SMOLCZYK. "Physical and chemical phenomena of carbonation",
Carbonation of Concrete, RILEM, London, 5-6 april 1976, pl-10.
6. J. CALLEJA. "Durabilit6", Pricipal Report, 7tn International Congress on the
Chemistry of Cement, Paris, 1980, Vol I, pVII 2/1-VII 2/50.
7. M. VENUAT. La carbonatation des b6tons hydrauliques, La pratique des ciments et
des b6tons, Edition du Moniteur des travaux publics et du b~timent (Paris, 1976),
p305-316.
8. M. REGOURD. "La r6sistance du b6tons aux alt6rations physiques et chimiques",
Le b6ton hydraulique, Presses de l'Ecole Nationale des Ponts et Chauss6es (Paris,
1982), p513-530.
9. R. LACHAUX & M. SALOMON. "Les alt6rations des b6tons", Annales de
I'I.T.B.T.P, s6rie B224, n°458 (1984), p21-61.