-
Nuclear Engineering and Design 237 (2007) 20832089
Chemo-mechanical coupling behavioPart I: Experimental r
d,,
ole Naarnea-DeParisson, 9ry 20
Abstract
This pape adatieffects of th re hicement paste cs ofbeen chosen
by using an ammonium nitrate solution instead. The specimens are
immersed into a 6 mol/l ammonium nitrate solution with a
controlledpH disposal. To quantify the leaching evolution, the
degradation depth is then measured at certain time intervals by
means of a phenolphthaleinsolution. The experimental results show
the chemical degradation of the cement-based material and the
important role of aggregate in the calciumleaching process of
concrete. Compression tests of concrete samples are also performed.
We observe that there is a strong coupling between thecalcium
leaching and the mechanical behaviour; as leaching grows, a loss of
stiffness and of strength are observed and a smoother
post-peakbehaviour is 2007 Else
1. Introdu
Durabilcrete in londurabilityinduced bymay also dconcrete isand
concrethe load-bethe level oscenario ofsite water.modificatioother
thing
DOI of or Correspon
Cedex 15, FraE-mail ad
0029-5493/$doi:10.1016/jnoted.vier B.V. All rights reserved.
ction
ity will certainly be the key in future use of con-g-term
structural applications. In the long term, the
of concrete is not exclusively affected by damagemechanical
loads. The lifetime of such a materialepend on the environment. As
a typical example,commonly employed in radioactive waste
disposal
te containment structures that must therefore ensurearing
capacity over extended periods depending onf radioactivity. In the
lifetime of nuclear waste, theconcrete degradation is calcium
leaching due to on-This leaching implies an increase in porosity,
andn of the microstructure of concrete which, amongsts, influences
the mechanical behaviour.
iginal article:10.1016/j.nucengdes.2007.02.012.ding author at:
LCPC Paris, 58, Boulevard Lefebvre 75732 Parisnce. Tel.: +33 1 40
43 54 40; fax: +33 1 40 43 65 20.dress:
[email protected] (J.M. Torrenti).
The calcium leaching of the cementitious material is con-trolled
by the chemical equilibrium of the hydration production.It depends
on two main consecutive phenomena with differentkinetics (see
Torrenti et al., 1999):
material transport by diffusion, resulting from
concentrationgradients between the solid interstitial solution and
the aggres-sive environment outside the cement samples;
dissolutionprecipitation chemical reactions induced by
theconcentration variations brought about by diffusion.
The leaching process begins with a total dissolution
ofportlandite, then ettringite and followed by a progressive
decal-cification of C-S-H phase. Several authors have researchedthe
chemical degradation on cement paste and mortar also(Adenot, 1992;
Bourdette, 1994; Carde et al., 1996; Gerard,1996; Tognazzi, 1998;
Le Bellego, 2001; Ulm et al., 2003)among many other references.
Experimental data reveal that theleaching process timescale is
governed by the diffusion process,as the dissolution is much
faster, i.e. the leaching fluxes are
see front matter 2007 Elsevier B.V. All rights
reserved..nucengdes.2007.02.013V.H. Nguyen a, H. Colina b, J.M.
Torrenti c,a Laboratoire dAnalyse des Materiaux et Identication,
Ec
Institut Navier, 6 et 8, Avenue Blaise Pascal, 77455 Mb ATILH,
7, Place de la Defense, 92974 Paris-L
c LCPC Paris, 58, Boulevard Lefebvre 75732d LMT, ENS Cachan, 61,
Avenue du President Wil
Received 10 April 2006; received in revised form 5 Februa
r deals with concrete behaviour under chemical and mechanical
degre calcium leaching process of concrete on its mechanical
properties a, mortar and concrete samples are presented. Because of
the slow kinetiur of leached concreteesultsC. Boulay c, B. Nedjar
ationale des Ponts et Chaussees,la Vallee Cedex 2, Francefense
Cedex, FranceCedex 15, France4235 Cachan, France07; accepted 14
February 2007
ons. Experimental investigations are described where
theghlighted. The calcium leaching and mechanical tests onleaching
under deionised water, an accelerated method has
-
2084 V.H. Nguyen et al. / Nuclear Engineering and Design 237
(2007) 20832089
imposed by diffusion. In the solid phase assemblage, a
sharpleaching frzones whements alsothe degrada(Carde et aagrees
with2000).
Naturalhundred yewater is noseveral cenessary to leprincipal
wture (KamaGerard, 19ent solutiothe interstimajority otious
materThe deionammoniumCarde et aTognazzi,2003).
The inflbehaviour oby severalBellego etof the expestiffness
ofthe total dition of C-Sa linear vain porositysound crosductility
ofthe microsdegradationrelation bethe elastici(Torrenti etBellego
(20ties of mortequal to 48mens is abof cement sdependencdue to the
ials frictionsee (Heukafor calciumconcrete leferences becontent,
sizprocess anin the pre a
The paper is organised as follows. In Section 2, we
outlineerimental setup and results on cement paste, mortar andte
specimens. In Section 3, the mechanical properties ofte are
investigated on cylindrical concrete samples sub-to uniaxial
compression tests after accelerated leaching.ean stressmean strain
diagrams at different degradationare presented. Finally, the
conclusions and perspectiveswn in Section 4.
ign and setup of the accelerated leachingure
aimlea
(cemuenhisg de
ater
con
C cepre
ompcemcemnentur e
entm hilindeers w
etes war tot at t
ealis
his sen used w
expgradhe p
ition
ents
s sands sands sandiliceoCEMont is observed experimentally. These
fronts separatere mineralogy is constant (Adenot, 1992).
Experi-show that the leaching fluxes and the position oftion front
are proportional to the square root of time
l., 1996; Tognazzi, 1998; Torrenti et al., 1998),
whichtheoretical considerations (Mainguy and Coussy,
leaching is a very slow process (a few centimetres perars). For
laboratory experiments, the use of deionisedt an optimum choice for
concrete for which we needtimetres of degradation. Accelerated
leaching is nec-ach the samples in a reasonable time. There are
threeays to accelerate calcium leaching: using tempera-li, 2003),
using an electrical field (Saito et al., 1992;96) and by replacing
deionised water with a differ-n agent to increase concentration
gradients betweential solution and the aggressive environment. Thef
the experiments on calcium leaching of cementi-ial samples are
performed by using the last method.ised water is replaced by a
strongly concentrated
nitrate solution (Goncalves and Rodrigues, 1991;l., 1996; Carde
and Francois, 1997; Gerard, 1996;1998; Le Bellego, 2001; Ulm et
al., 2003; Kamali,
uence of calcium leaching on the mechanicalf the cement paste
and mortar has been investigatedauthors (Carde et al., 1996; Ulm et
al., 1999; Leal., 2001; Heukamp et al., 2001). In their
analysisrimental results, Carde et al. (1996) show that thethe
material specimens is significantly reduced afterssolution of
portlandite and the progressive dissolu--H. Both mechanical and
water porosity tests showriation between the loss of strength and
the growthin relation to the ratio between the degraded and
thes-sections. Compared with the sound material, thethe chemically
degraded material is larger because
tructure is modified. The influence of the chemicalon mechanical
behaviour has been presented by a
tween the calcium concentration in solid phase andty modulus, as
in (Gerard, 1996) or the strength as inal., 1998) by using
micro-hardness experiments. Le01) has shown recently that the
mechanical proper-ar decrease as leaching grows. For degradation
ratios, 59 and 74%, the loss of stiffness of mortar speci-
out 23, 36 and 53%, respectively. From triaxial testspecimens
subjected to accelerated leaching, a strong
e of the mechanical properties on the pore pressurencreased pore
space and the reduction of the materi-al performance of the leached
cement paste is noted,mp et al., 2001, 2003). However, experimental
result
leaching of concrete and post-peak behaviour ofached are not yet
available in literature data. The dif-tween cement paste or mortar
and concrete (cemente of aggregates, . . .) should influence the
leaching
d the mechanical behaviour of the leached concretend post-peak
regimes.
the expconcre
concre
jectedThe mlevelsare dra
2. Desproced
Thecalciumscalesthe inflcrete. Tleachin
2.1. M
Thean OPused iscrete cwaterwatercompo
In oof cem100 mfull cycylindof diamsamplein ordeand no
2.2. R
In thas bedeionilightedThe deusing t
Table 1Compos
Compon
SiliceouSiliceouSiliceouCrotoy sCementWaterof the experimental
campaign is to determine theching kinetic of the cementitious phase
at differentent paste, mortar and concrete). It allows to
observe
ce of the aggregate on the calcium leaching of con-section
presents design considerations for the calciumvice and its
practical application and results.
ials and samples
crete was composed of siliceous aggregates andment (CEM 1 52,5).
The composition of concretesented in Table 1, where the ratio
between the con-onents is: cement:sand:gravel = 1:1.82:2.8, with
a
ent ratio of 0.6. The cement paste has the sameent ratio equal
to 0.6 and the ratio between the mortars is: water:cement:sand =
0.6:1:1.82.xperimental program, the samples used for the casepaste
and mortar are cylinders 32 mm diameter andgh. Two types of
specimens are used for concrete:rs with dimensions 110 mm 220 mm
and hollowith the same external dimensions and a centred hole
r = 27 mm. The top and the bottom of the concretes protected
from leaching by means of a silicon resinhave only leaching in the
central part of the sampleshe level of loaded surfaces.
ation of the calcium leaching process
tudy, a degradation under ammonium nitrate solutionsed. The
equivalence of the leaching process underater and under ammonium
nitrate solution is high-
erimentally by Carde et al. (1996), Tognazzi (1998).ed state of
specimens may be determined easily byH indicators.
of a 1 m3 of concrete
Quantity (kg)S28 (0.20.5 mm) 281S30 (0.41.0 mm) 193S36 (1.03.15
mm) 210
us gravel (4.012.5 mm) 1050I 375
225
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V.H. Nguyen et al. / Nuclear Engineering and Design 237 (2007)
20832089 2085
Fig. 1. Schemnitrate solutio
After 5 mimmersed iequal to 6 mcalcium leaare recordewas
chosenavoid renewcalcium thaammoniuming procesbetween thsive
solutioinduce a dsolution towof time (36of concretethe chemic
2.3. Result
To avoidplaned to bage. But limwe presentstone. Thisleaching
prnique used
Table 2Experimental results of chemical degradation of
limestone
Length (cm) Diameter (cm) Weight (g) PorositySound state
0.79 2.85 2.70 28.6After 142 days of degradation
0.60 2.70 1.40 32.3
degradation, we show that the specimens of limestone have
alimited increase in porosity and mainly a significant reductionin
volume and mass (see Table 2 and Fig. 2).
This result shows that limestone is unstable in the ammo-nium
nitrate solution. This explains the choice to use
siliceousaggregates for our tests. For real storage structures
limestone
stabcalcof sdegon s
entinviroH vnt. Wuishhaleiic soer, tuese exer, b
haleihaset ca
mea
.17 e
cros
erveenolpoloure of the calcium leaching test of concrete under 6
M ammoniumn.
onths of curing (water storage), the specimens weren an ammonium
nitrate solution with a concentration
ol/l (6 M). The experimental setup for acceleratedching is
presented in Fig. 1. The pH and temperatured by an acquisition
system. The volume of solutionto avoid renewal: while pH is lower
than 8.2 we caning (Le Bellego, 2001). Knowing the quantity of
t would be leached we can estimate the quantity ofnitrate we
need to respect this condition. The leach-
s results from the high gradients of concentrationse pore
solution in the cement paste and the aggres-n that surrounds the
samples. These gradients then
iffusion process of the calcium present in the poreards the
environment. Subsequently, at each period
, 57, 105, 152, 163, 197, 274 and 547 days for the case),
specimens were extracted to measure the depth ofal degradation and
test their mechanical behaviour.
s
alkali-aggregate reaction, limestone aggregates aree used for
concrete in the case of nuclear waste stor-estone could be leached
in our solution. That is why
firstly the result of the chemical degradation of lime-
will beties ofinstead
Thethaleinof cembasic ewith pronme
distingnolphtin basHowevpH valgive
thHowevnolpht2001)depthephenol
et = 1In thebe obsthe phgrey cexperiment has been performed to
characterise theoperties of limestone as well as to check the
tech-and precautions for the later test. After 142 days of
The thicthe measurdegraded d
Fig. 2. Photo of the limestone sample on the sound state and
ale, because on-site water contains sufficient quanti-ium.
Calcareous aggregates could therefore be usediliceous ones for
nuclear waste storage.raded depth is determined by using the
phenolph-ectioned samples. The pH value in the pore solutiontious
materials is higher than 12.5, creating a verynment. Consequently,
an ammonium nitrate solution
alues below this level characterises the acid envi-e can use the
pH indicator like phenolphthalein tobetween the sound zone and the
degraded zone. Phe-n turns from colourless in acidic solutions to
pinklutions with the transition occurring around pH 9.he
dissolution of portlandite occurs as long as thedrop below 12.
Therefore, phenolphthalein does notact position of the dissolution
front of portlandite.y comparison between the measurement by phe-n
and by SIMS microprobe analysis (Le Bellego,shown that for the
cement paste the total degradedn be determined by correcting the
degraded depthsured by phenolphthalein with the formula:
phenol (1)s-section of the specimens, two distinct zones mayd: a
sound zone, i.e. with the pink colour caused byhthalein solution,
and a degraded zone, i.e. with the(see Figs. 39).
kness of this degraded zone can be measured by usingements at 16
points around the specimen. The totalepth is the mean of these
measurements.fter 142 days of degradation.
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2086 V.H. Nguyen et al. / Nuclear Engineering and Design 237
(2007) 20832089
Fig. 3. Degradation state of the cement cylinder after 14 days.
The pH indicatoris phenolphthalein (pink when pH > 12.5). (For
interpretation of the referencesto colour in this figure legend,
the reader is referred to the web version of thearticle.)
The relaof time
t
paste, mortthat the kinmaterial isusing Fick
Compartar, it is intealmost theand the expdifference.ence
betwe15% (see Fof the aggrlogical geo
Fig. 4
Fig. 5. Degradation state of the concrete hollow cylinder after
36 days.
g. 6. Degradation state of the concrete full cylinder after 36
days.tion between the degraded depth and the square rootshows a
linear evolution for the three cases (cementar and concrete) (see
Figs. 10 and 11). This meansetics of the chemical degradation of
the cementitiousgoverned by a diffusion process and can be
describeds law.ing the results obtained with cement paste and
mor-resting to note that the degraded depth evolutions are
same for the two cases. A comparison of these resultserimental
results of concrete highlights a significantFor example, after 25
days of degradation, the differ-en the degraded depth in concrete
and mortar is aboutigs. 10 and 11). These results highlight the
influenceegates in concrete. Its volume fraction and morpho-metries
obviously play an important role. This effect Fi. Degradation state
of the mortar cylinder after 14 days. Fig. 7. Degradation state of
the concrete hollow cylinder after 197 days.
-
V.H. Nguyen et al. / Nuclear Engineering and Design 237 (2007)
20832089 2087
Fig. 8. D
is accounteet al., 2006
Comparwe note thinternal degexternal. Tin the holenot
possibl
3. Mechan
3.1. Exper
At eachspecimensthe compleand strengtimum capaplaced betwsometer
isdisplacemebase lengththree LVDTthis displac
Fig. 9. De
Degrd mor
fnescurve
esult
mean strain is the relative variation of the base length l0
ofensometer (110 mm). This is only a mean strain
becauselocalisation process in the softening range (Torrenti et
al.,
mean compressive stress is evaluated by dividing theby the area
of the cross-section of specimen S. It is a meanbecause, due to the
heterogeneity of the chemical degra-egradation state of the
concrete full cylinder after 197 days.
d for by using the homogenisation method (Nguyen).ing the
results obtained with full and hollow cylinder,at the external
degraded depth is the same. But theraded depth of the hollow
cylinder is lower than the
his seems to be due to a different boundary condition: the
calcium concentration should be higher (it wase to check this
assumption).
ical behaviour of leached concrete
imental setup
time interval of the chemical degradation, concreteare subjected
to compression tests in order to measurete mean stressmean strain
curve, the mean stiffnessh. The device used is a MFL-5000 press
with a max-city of 5000 kN. An extensometer and three LVDTeen the
platens are used (see Fig. 12). The exten-
clamped directly on the specimen and measures the
Fig. 10.paste an
the stifstrain
3.2. R
Thethe extof the1993).
Theload Fstressnt of the central part of the sample on a 110
mm(Boulay and Colson, 1981). The mean value of theis used to
control the test. Loading is controlled by
ement between the platens with cycles to determine
gradation state of the concrete hollow cylinder after 163
days.Fig. 11. Degrspecimens.aded depth evolution vs. the square
root of time for the cementtar specimens.
s, the mean strength, the complete mean stressmeans and
irreversible deformations.
saded depth evolution vs. the square root of time for the
concrete
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2088 V.H. Nguyen et al. / Nuclear Engineering and Design 237
(2007) 20832089
Fig. 12. Experimental setup for the compressive test of
concrete.
dation, we have different local mechanical properties
(Youngsmodulus for instance) conducting to different local stresses
inthe samples.
We obsestrength desponding toby (Ulm etmodulus. F
In additipression tetimes are shbetween thThe soundleaching
grimportant stimes highwere obtain
In the cathe existenThese defoan evolutiomaterial. T
Fig. 13. Evolhollow cylind
Fig. 14. Evolution of the strength vs. the degradation time for
full and hollowcylinders.
Mean stress vs. mean strain curves at different degradation
times (hol-nders).
that leached C-S-H is a cohesive incompressible mate-d that the
pores created by the calcium leaching providesfor the
incompressible solid during compressive loadingamp et al.,
2003).ntually, one should note that in only two cases ourould be
considered homogeneous: for plain concreter totally leached
concrete. In these cases, the constitu-rve that the mean stiffness
and the mean compressivecrease with the degradation time until
values corre-a totally degraded concrete are stabilised. As
found
al., 2002), we observe residual strength and Youngsigs. 13 and
14 illustrate these evolutions.on, and by way of illustration, the
results of the com-sts for the hollow cylinders at different
degradationown in Fig. 15. We note that there is a strong couplinge
calcium leaching and the mechanical behaviour.concrete has an
almost brittle behaviour, while as theows, concrete becomes more
and more ductile withtrains: the mean strain at peak stress is
almost threeer when concrete is totally leached. Similar resultsed
by (Le Bellego, 2001) with mortar.se of cyclic loading, the
experimental results reveal
ce of inelastic deformations (see Figs. 16 and 17).rmations are
larger with the leaching time. There isn when concrete is leached
towards a more plastichis is coherent with Heukamps results who
have
Fig. 15.low cyli
shownrial anspace(Heuk
Evetests cand foution of the mean stiffness vs. the degradation
time for full anders.
Fig. 16. Meanof degradationstress vs. mean strain curves under
cyclic loading after 197 days(hollow cylinders).
-
V.H. Nguyen et al. / Nuclear Engineering and Design 237 (2007)
20832089 2089
Fig. 17. Meadays of degra
tive behaviintermedianon-homog
4. Conclu
We havemechanicatest on cemics of calcshown cleaprocess
ofmechanicacoupling bbehaviour.is observeding irreversa
plastic-likconcrete.
Acknowled
FinanciaENPC-IRSThis suppo
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Chemo-mechanical coupling behaviour of leached
concreteIntroductionDesign and setup of the accelerated leaching
procedureMaterials and samplesRealisation of the calcium leaching
processResults
Mechanical behaviour of leached concreteExperimental
setupResults
ConclusionsAcknowledgementReferences