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A concrete performance test for delayed ettringite formation:
Part I optimisation
⁎
Alexandre Pavoine , Loïc Divet, Stéphane Fenouillet
LaboratoireCentraldesPontsetChassées.58BdLefebvre,75732ParisCedex15—France
Received25November2004;accepted18September2006
Abstract
Delayed ettringite formation (DEF) is a rare internal swelling reaction of concrete that, in a wet environment, may considerably reduce the
durability of a structure or amember that has been prefabricated in afactory.As a result of alargenumber of studies, the main causesof this
problem have been established and this paper proposes a test method to predict the susceptibility of a concrete to DEF and provide long-term
protectionagainstthishazard.Afteranexaminationofthefeasibilityofatestbasedonwettinganddryingcycles,theresultsofanoptimisation
studybasedonafactorialexperimentalplanarepresented.Thetestisinfourstages:concretemanufacture,aheattreatmentthatsimulatessteam
curing in a factory or the heating that occurs in mass cast in-situ concrete, wetting and drying cycles and the monitoring of the longitudinal
expansionofspecimensthatareimmersedinwater.Optimisationessentiallyconcernsthelasttwostagesandresultedinthedecisiontoapplytwo
dryingcycles(38°Catarelativehumidityofapproximately30%)andwettingcycles(inwaterat20°C)followedbypermanentimmersionin
water(at20°C).Thistestisappliedtoconcretethathasundergoneearlyageheating.Itprovidesameansofevaluatingthepotentialreactivityof
“mix design–heating cycle”pairs as realistically as possible withinareasonable period of time.
©2006Elsevier Ltd.All rights reserved.
Keywords:Delayedettringiteformation;Expansion;Sulfateattack
1. Introduction mation. For this reason, the problem can only occur in mass
concrete due to self heating or in concrete that has undergone
Delayed ettringite formation (DEF) is the term used to de- heat treatment. The normally stated critical temperature is
scribeaphysicochemicalprocessthatmayleadtothepremature around 70 °C. To limit risks in the long term, current recom-
deteriorationofaconcretemember.DEFisaninternalswelling mendations propose, among other things, a maximum temper-
reaction of the concrete that occurs merely in the presence of ature of 60–70 °C for heat curing [4–9].
water without any external ingress of sulfate from the envi- Water. In situ, appraisals have shown that the presence of
ronment in contact with the concrete. This concrete swelling water in contact with the concrete is a necessary condition for
reaction is influenced by a large number of factors that play a delayedettringiteformation.Theroleofhighrelativehumidity
roleinitsdevelopment.ThemainparametersinvolvedinDEF around the concrete has also been confirmed by laboratory
are asfollows: studies [10–13].
Temperature. A temperature rise considerably modifies the Alkaliintheconcrete.Thisisknowntoaffectthesolubility
chemical equilibrium during cement hydration as well as the ofettringite[14].Asthesolubilityofettringitealsovarieswith
texture of the material [1–3]. It is recognized that a high temperature, there is a strong interaction between these two
temperature is a necessary condition for delayed ettringite for- parameters during theDEF process [15–17].
Initial cracking ofthe concrete. This probably hasan effect
on the kinetics and extent of expansion. However, the topic is
controversial and the available theoretical investigations [18]
⁎ and experimental studies [19] do not allow us to reach a con-
Correspondingauthor.
E-mailaddress:[email protected](A.Pavoine). clusion with regard tothe importance ofthis parameter.
0008-8846/$-seefrontmatter©2006ElsevierLtd.Allrightsreserved.
doi:10.1016/j.cemconres.2006.09.009
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Sulfate in the clinker. Recent changes in cement manufac- wouldthreateneitherthesafetyofusersorthedurabilityofthe
turing processes have changed the amount and nature of the structure [26].
sulfates in the clinker. A considerable number of kinetic and Theliteratureproposesseveralteststoevaluatethereactivity
thermodynamic studies have been conducted to evaluate the ofconcreteinrelationtoDEF[12,27,28].Untilnow,thesetests
roleofthesesulfatesintheswellingprocess.Laboratorytests have been performed on small specimens (of cement paste or
have shown that these sulfates only account for a small pro- mortar) and have not been shown to be generally applicable
portion of the totalamount of sulfate in the cement, that their because very high temperatures are applied on one or more
proportion in relation to aluminates favours the formation of occasions. More recently, Petrov [25] has shown that a
monosulphoaluminate and that their solubility kinetics are discriminant test can be achieved by varying the temperature
suchthattheymaybedissolvedduringbinderhydration[20]. and the relative humidity during a performance test. However,
It is accepted that these sulfates cannot be responsible for when these tests were conducted on mortar, a large difference
long-term expansion without heating of the material. How- was noted between the amplitude of expansion of the control
ever, expansion tests have demonstrated that the sulfates pre- specimens (without cycles)and thetest specimens.
sentintheclinker,asalkalisulfates,modifytheamplitudeand Aperformancetestmustbearepresentativeofthereality.It
the kinetics of expansion of the material in the event of must also be possible to carry out the test within a reasonable
considerable early age heating [19]. Nevertheless, there is no length of time. To meet these constraints, we have applied a
evidencethatthesulfatesintheclinkerhaveadifferenteffect three-stageapproach:
from those added.
Sulfates and aluminates in the cement. Ettringite (Ca Al 1. Verificationofthefeasibilityofaconcretetestinvolvingthe
6 2
(SO ) (OH) 26H O) is a trisulfo calcium aluminate hydrate. application of wetting and drying cycles and expansion
4 3 12 2
Sulfates and aluminates therefore play an important role in measurement[29].
the reaction mechanism. Studies have been concerned with 2. Optimisation of the test based on the application of a
theequilibriabetweensulfatesinsolution,hydratedsulfatesand factorial experimental plan describedin Table 1.
C–S–H during hydration and over a period of time. During 3. Validationofthetestbyapplyingittoconcretewithknown
hydration,theseequilibriaareconsiderablymodifiedbyheating behaviour with regard to DEF[30].
asaresultoftheeffectofthetemperatureonthetextureofthe
C–S–H,changesinthedomainsofthermodynamicsstabilityof 2. Experimental description
hydrates and variations in the products of solubility. This
subject has been widely discussed in the literature that deals 2.1. The proposed test
with the reaction mechanisms [1,2,15,20–22]. The role of the
aluminates in thecement has frequently been studied and C A During the feasibility study, it was observed that internal
3
limits or criteria which relate to both aluminates and sulfates sulfate reaction may cause damage to concrete [29]. The
havebeenputforward.Nevertheless,inviewofthecomplexity similarity between the results obtained on specimens stored in
of the phenomenon, these criteria taken individually are not water, known as control specimens (without cycles), and
always relevant. specimenssubjectedtowettinganddryingcycleswaschecked.
Additives. Adding substances that modify the physical cha- When concretes were susceptible to DEF, expansion was
racteristicsthatinfluencethedurabilityofconcrete(pozzolanic measuredonbothspecimenswithoutcyclesandthosesubjected
reactions,porosity)seemstoreducethepotentialriskofagiven to drying and wetting cycles. Non-reactive concretes did not
concrete expansion [23]. However, few studies have explored expandwhenthedryingcycleswerecarriedoutat38°C.These
this topic. Recent results with regard to air-entraining agents
describe the impact of included air bubbles which can act as Table1
expansionvesselswithout,inprinciple,reducingthematerial's Scopeofstudyforoptimizingtheperformancetest
frost susceptibility [24,25]. Reference Parameter Levels
Although progress has been considerable, controversial letter
points, or areas where data is lacking, exist and these limit A Concretecuringtimebefore 5h;3days;14days
our overall understanding of DEF. However, it is of great applicationofdryingand
interest to try to develop performance tests [16] to meet the wettingcycles
B Timekeptinawater-saturated 0day;3days;7days
requirements of project owners and contractors.
enclosure(relativehumidity
Some countries have already introduced restrictions to re-
closeto100%)
duce the risk of DEF [4–9]. In the case of France, the official C Durationofawettingand 7days;14days;28days;
recommendationistoassessthereactivityofaconcreteusinga dryingcycle
performance test when certain temperature (from 65 °C to D Numberofcyclesbefore 1cycle;2cycles;3cycles
permanentimmersionof
85 °C) and concrete composition criteria (low C A, SO and
3 3 concretespecimen
Na O ) cannot be met. With regard to the management of
2 equi E Dryingtemperature 38°C;60°C
existing structures, a technical guide has recently been pub- F Solutionspecimensarekeptin Tapwater;tapwatersaturated
lished in France in which the use of this type of test is also duringwettingandpermanent withlime(leveldoubledto
recommended for structures or members in which the reaction immersion obtainanorthogonalplane)
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Table2 1 and 2. This plan was repeated two times on concretes made
Concretemixdesign(kg/m3) withPortlandcementCEMIandsiliceousaggregate(Tables2
Material Siliceousaggregate Siliceoussand CEMI Water and 3). After mixing and placing in cylindrical moulds (110×
(5/12) (0/5) cement 220mm)thedifferentconcretesweresubjectedtothefollowing
Amount(Kg/m3) 1050 700 410 196.8 heat treatment:
▪ The temperaturewas increased by 35°C/hfor 2 h;
firstresultsledtotheproposalofafour-phaseperformancetest. ▪ The temperaturewas maintainedat 90°C for 10 h;
The first phase consists of the manufacture of concrete spe- ▪ Thetemperaturewasgraduallyreducedfrom90°Cto20°C
cimens,thesecondsimulatesheattreatmentinafactoryorheat overa periodof 10 h.
generation within a massive member. The third consists of
imposing wetting and drying cycles and the last is permanent Thisaggressivetemperaturecyclewaschosentoensurethat
immersion, during which length change of the specimens is DEF would be provoked in susceptible concretes in order to
measured. In some case the effect of the cycles was limited, bestevaluatethepostcuringconditionsofthetest.Asdescribed
especially when specimens are very reactive. In such cases, in part II of this study [30], the actual mix design and tem-
drying and wetting cycles may not be necessary to accelerate peraturecycleoftheconcreteareintendedtobeusedinthetest
expansion in comparison with specimens which have not inpractice.
undergonethosecycles.But,thesecyclesdonotalterthelong- The duration of curing in the wet enclosure (with a relative
termperformanceoftheconcreteandinsomecasessavetime. humidity of almost 100%) at 20 °C varied according to the
Theproposedtestisconductedonconcretespecimens.This factorial experimental plan.
allows realistic experimental conditions to be used and limits Expansionwasmonitoredusingthelowstiffness-freevibrat-
alkali leaching. ing wire sensors developed by the LCPC [32]. These sensors
were connected to an automatic data collection system. The
2.2. Optimisation study error in the expansion measurements due to the apparatus is
0.0016% at a maximum frequency of 2000 Hz. The measure-
The objective was to estimate the impact of the various mentrangeofthisapparatusisoftheorderof0.6%expansion.
parameters involved in the test procedure, and then to specify
experimentalconditionswhichwillallowthedurationofthetest 2.3. Repeatability study
to be minimized. The study was based on the application of a
factorial experimental plan. The parameters studied are sum- The repeatability of the test was quantified by applying the
marized in Table 1. optimized test procedure to 10 concrete nominally identical
For curing time, drying temperature and the type of storage specimens (Table 2) which had undergonethesame heat treat-
solution, the scope of the study was defined on the basis of ment.Forthisstudy,thetemperatureplateauappliedduringthe
knowledgederivedfrompreviousstudies[12,27,28].Thetem- heattreatmentwasreducedfrom90°Cto80°C.Theexpansion
peraturesof38°Cand60°Cwerechosensoasnottoprovoke measurements were conducted using a Pfender ball extensom-
thedissolutionoftheettringiteduringthetestinviewofthefact eter distributed by Mohr and Federhaff [32]. The expansion
that the threshold values for the risk of DEF found in the curves given in Fig. 1 show the average expansion of the
literatureare near 70°C. specimensobtainedbymonitoringthreestraingaugesforeach
Lastly,thenumberofcycles,theirdurationandthelengthof specimen.
timethespecimenswerekeptinawetenclosurewerespecified
inordertocoverasufficientlylargedomainbeyondwhichthe 3. Results
time taken by the wetting and drying cycles is considered to
exceed a reasonabledurationfor atest. 3.1. Optimisation
A “REX” strategy model proposed by Tagushi [31] was
applied to the experimental plan, which had 18 combinations. Optimisationof thetest was mainlyconcerned with the last
ThecorrespondingtableisreferredtoasL (21×37)RNO-REX twostagesasphases1and2(mixdesignandheatingcycle)are
18
Table3
BoguecomputationsofchemicalandmineralogicalcompositionoftheCEMIPortlandcementused(%)
SiO AlO TiO FeO CaO MgO NaO KO SO Cl− S2
2 2 3 2 2 3 2 2 3
19.58 4.32 0.22 3.16 63.10 1.19 0.10 0.61 3.94 b0.01 Néant
Insolubleresidue Loss on heating to MnO NaO a C3S C2S C3A C4AF
2 equi
975°C
1.21 1.33 0.06 0.5 55.2 14.3 6.1 9.6
a NaO =NaO+0.658∗K O.
2 equi 2 2
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Fig. 1. Average longitudinal expansion — 10 concrete specimens (110× Fig.2.Relativeuncertaintyaccordingtoaverageexpansion.
220mm).
meant to represent the real conditions of concrete use and be system.Thisphasewasthereforenotincludedintheoptimized
adapted according to the concrete considered, as discussed in test procedure adopted. The previous study [29] indicated that
part II ofthis study [30]. non-reactiveconcretesmaybereactivewhenthedryingphaseis
The variance of the results was analyzed so that the role of conducted at 60 °C. Therefore a temperature of 38 °C and a
each of the parameters could be studied. After immersion for relativehumidityofabout30%forthetwodryingphaseswere
100 days, the various concrete specimens had expanded suf- selected for the optimizedtest.
ficiently for the impact of the parameters to be studied. The The optimized test procedure thus consists of two drying
results aregiven inTable 4. cycles(at38°Cwitharelativehumidityofabout30%)andtwo
The experimental plan shows that the nature of the im- wetting cycles (water at 20 °C) followed by monitoring the
mersionsolution(tapwaterortapwatersaturatedwithlime)has longitudinal expansion of the concrete specimens immersed in
no impact. This is probably due to the large size of our waterat20°C.Thetestisdesignedtobeusedwithagivenmix
specimens.Theplanalsoshowsthatincreasingthedurationof designandtemperaturecuringcyclerepresentativeofrealcon-
thecuringphasewhichprecedesthefirstdryingcyclefrom5h crete to allow investigation of “concrete mix design/heat treat-
to 28 days has no impact. The duration of a cycle and the ment”pairs [33].
numberofcyclesarethesecondandthirdorderparameters.The
largest effect on expansion was obtained for two cycles with a 3.2. Repeatability
duration of 14 days. Inclusion of a period of storage at high
relative humidity before the cycles was not considered to be After 1000 days of testing, it was observed that the expan-
significantasitseffectwasclosetothenaturalvariabilityofthe sion of the 10 concrete specimens was quite variable (Fig. 1).
The population of specimens has an average expansion of
0.75%±0.12%.
Table4
Optimisationofperformancetest
Action DoFa Sof Experimental F c F d %Contribution
exp crit
squaresb variance
A 2 0.0027 0.0013 0.33 3.23 0
B 2 0.0278 0.0139 3.48 3.23 2
C 2 0.1509 0.0755 18.90 3.23 13
D 1 0.6628 0.6628 166.01 4.08 58
E 2 0.0624 0.0312 7.81 3.23 5
F 2 0.0006 0.0003 0.08 3.23 0
CD 2 0.1628 0.0814 20.38 3.23 14
Residue 32 0.0798 0.0040 7
Y 45 1.1498 0.0434 100
Analysisofvariance.Resultsobtainedafterimmersionfor100days.
a DoF:Degreesoffreedom;
b Sofsquares:sumofthesquaresofthedifferencewiththeoverallaverage
ofthemeaneffectofeachlevelofaction;
c F :ratiobetweentheexperimentalvarianceoftheactionandthevariance
exp
oftheresidues;
d F :tabulatedvalues(Fischer–Snedecor)ofFbelowwhichthevalueof
crit
theactionisnotsignificant. Fig.3.Modelexpansioncurve[32].
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Table5 subjected to two heating cycles, which has an impact on the
Orderofmagnitudeofthecharacteristicparametersoftheaverageexpansion kinetics of expansion.
plots for seven specimens that have undergone the performance test and a
controlspecimenthathasnotbeensubjectedtothewettinganddryingcycles
5. Conclusions and perspectives
Latencyperiod Characteristictime Finalexpansion
(days) (days) (%)
Theapplicationoffactorialexperimentalplantechniqueshas
Performancetest 436 116 0.76
resultedintheoptimisationofparametersinaperformancetest
Specimenconserved 603 125 0.79
forevaluatingthepotentialreactivityof“concretemixdesign–
inwaterat20°C
heatingcycle”pairswithregardtoDEF.Thesetestswereapplied
ononespecificmixdesign.Theresultsarevalidatedwithother
Fig. 2 shows the variation of confidence interval with a mixdesignsandheatingcyclesinthesecondpartofthispaper.
degree of expansion. At low expansions during the latency The performance test proposed as a result of this research
period, when the average expansion is less than 0.04%, the comprises four stages:
confidence interval is larger than the average expansion. As
expansionstartstheconfidenceintervalislow,butincreasedue 1. Concretemix design and manufacture;
todifferentkineticsofexpansion.Athighlevelsofexpansion,it 2. Aheattreatmentthatsimulatesheattreatmentinafactoryor
falls with the level of expansion and reaches a value of 33% theheatingthattakesplaceinamassivecastin-situconcrete
witha95%confidencelevel(Fig.2).Thesevaluesareobtained member;
for one heat cured concrete. A large study of the fidelity is 3. Two cycles of wetting and drying. Each cycle lasting for
actually conducted byseveral laboratories. 14daysandconsistofthetwophases:dryingfor7daysinan
On the basis of these results, we were able to evaluate the enclosureat38°Cwitharelativehumidityof30%followed
impactofwettinganddryingcyclesontheexpansioncurvesin byimmersion for 7 days intapwaterat 20 °C.
comparison with the control specimens that have not been 4. Monitoring longitudinal expansion of the specimens im-
subjected to wetting and drying cycles. For this, three charac- mersed inwaterat 20°C.
teristic parameters (ϵ∞, τ and τ ) are determined to
charac latency
describe the expansion curves (Fig. 3) using the equation put The nature of the immersion solution (water or saturated-
forward by Larive [32], given below: lime solution) plays a secondary role. The concrete specimens
shouldbesufficientsizetoavoidalkalileaching.Theexpansion
eðtÞ¼el 1−e−schatrac mechanismsarenotacceleratedbyimposingalargenumberof
1þe−t−ssclhaateranccy cycles or increasing the duration of the periods of wetting and
drying.Likewise,raisingthedryingtemperaturefrom38°Cto
where: 60°C does notlead toa marked accelerationin expansion.
Our statistical analysis has shown that the repeatability of
ϵ∞ isthemaximum amplitude ofexpansion, this test is of the order of 33% with a 95% confidence. Addi-
τcharac isthecharacteristictimerepresentativeofhalftimeof tionaltestsareinprogresstoconfirmthesepreliminaryfindings.
the period between the end of the latency period and Theperformancetestmustbevalidatedbeforeitcanbeusedin
the time when maximum amplitude of expansion is the framework of a rigorous preventive approach. For this
reach. purpose,astudyhasbeenconductedonconcretethathasbeen
τlatency isthelatencytimerepresentativeoftheperiodwhenno subjected toheat treatmentrepresentative offactory processor
expansion ismeasured. concrete heated within a massive cast in-situ member whose
long-term performance in a wet environment is known from
TheresultsaresetoutinTable5.Itisapparentthatapplying experience.Theresultsofthisstudyarepresentedinthesecond
two wetting and drying cycles reduces the latency period by part of this paper [30].
5 months without significantly reducing or increasing the am-
plitude of expansion. Acknowledgments
4. Discussion The authors would like to thank the Association Technique
de l'Industrie des Liants Hydrauliques (Technical Association
The application of cycles after the heat treatment can forHydraulicBinders)andtheCentred'EtudeetdeRecherche
reduce the latency period and consequently reduce the test del'IndustrieduBéton(ManufacturedConcreteIndustryStudy,
duration. The impact of these cycles is probably twofold: on Design and Research Centre) for their financial and technical
the one hand they may favour localized oversaturation of support.
ettringite and on the other create and/or increase the size of
microcracksintheconcrete.Theunstablepropagationofpre-
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Research(2006),doi:10.1016/j.cemconres.2006.09.009
