‘The Use of Gamma-Ray Spectrometry for Dynamic Determination of Moisture Fields in a High Performance Concrete Subjected to Elevated Temperatures. by. P. Kalifa’, FD. Menneteau’, H. Sallée’,D. Quenard” High performance concretes (HPC) may be subject to spalling when exposed to elevated temperatures, as in fies, which may jeopardise the integrity of the lement The European projet HITECO BE-1158, within which the present work was caried out, aims at modelling the behaviour of HPC at elevated temperatures and at studying solutions to reduce the risk of spalling, Spalling isin particular due to the build-up of high vapour pressure: the low permeability of HPC strongly inhibits vapour transfer Gamma-ray spectrometry wes used for dynamic monitoring of the water content fields in HPC specimens heated on one end and thermally insulated and sealed on their sides. The penetration of the drying-dchydration front was studied and characterisedin terms of velocity and slope. These preliminary results show that this technique is very promising for this purpose. ‘The results will be used 0 validate the numerical simulation of the behaviour of concrete at high temperatures. Keywords: high performance concrete, fire, high temperature, spalling, gamma- ry spectrometry, moisture distribution. “are“Research engineer at Centre Scientifique et Technique du Batiment, St Martin @'Hetes, France. NOMENCLATURE 4 Thickness ofthe absorber (diameter ofthe specimen) Na Number of incident photons Nj [Number of tansmitted photons through the reference specimen in nial state iy Namber of transmitted photons trough the reference specimen in : dry tate be Mass attenuation coefficient of water Ms Mass attenuation coefficient of solid ® Volume water content ° “Mass water content measured by spectrometry ‘plop Homogensed mass water content ofthe test specimen deduced from set spectrometry measurements 7 Average of © Zit Average intl mass water content ofthe reference specimen be ‘Water density Pw ‘Apparent concrete density INTRODUCTION ‘The present work was performed within the framework of the European Brite EuRam project HITECO (BE-1158). This project aims at modelling the behaviour of high and ultrahigh performance concrete under fire conditions and at studying the effect of organic fibres on the spalling behaviour of ultra high-strength coneretes. This study focuses on the dynamic measurement of temperature and ‘moisture fields in a cylindrical specimen heated on one face and thermally insulated and sealed on its side. This configuration simulates a quasi one- dimensional situation, asin a wall heated on one face. ‘As observed by several authors [I-11], high performance concrete (HPC) may exhibit spalling (sudden and sometimes explosive removal of concrete layers with @ thickness up 10 5 em) [1] when subjected to high temperatures as in fire. This Page 1990process may be repeated several times, then rebars are directly exposed to fire and the integrity of the element may be jeopardised. Spalling occurs mainly between 250 and 400°C, even under low heating rates [2]. However the results published in the literature are contradictory : some works report a very good behaviour of HPC at high temperatures [12-14]. These apparent discrepancies exist because many parameters are involved in the spalling process, among them + At the macroscopic scale: Heating conditions (heating rate and maximum temperature), size and shape of the element, reinforcement, pre-stessing, external loading. * At the meso and microscopic scales: parameters controlling heat and mass transfer (thermal conductivity, sensible heat, permeability to water and vapour) and ‘mechanical properties (compressive and tensile strength, elastic modulus, transient creep), in correlation with the microstructure characteristics (porosity, pore size distribution, connectivity, mirocracking, ete.) and inital moisture state. Besides permeability, external loading and moisture state seem to be critical parameters, however their influence is strongly correlated to the other parameters Thus, spalling involves four main coupled processes: thermal (heat transfer), chemical (dehydration of cement paste and transformation of other mineral species), hydral and hygral (transfer of liquid and vapour water), and mechanical processes. If the constitutive laws of those processes are fairly well known, complexity stems from the fact they depend upon the microstructure, which changes during heating. These processes can be grouped into two main coexistent ‘mechanisms that lead to spalling = Thermo-mechanical mechanism: thermal stresses are induced both by temperature gradients and by local gradients of thermal expansion (16) (aggregates ‘expand as tong as they are not chemically altered, whereas cement paste shrinks ‘with dehydration that starts at 180°C) ‘+ Thermohygral mechanism, which was described by Harmathy [15]; as {temperature rises in the element, pore water is vapotised and chemically bound Water is freed during dehydration of the cement paste and tums into vapour. This vapour migrates towards both the heated face and the inside of the element. As a result the element contains schematically, from outside to inside, a rather dry zone, followed by a semi-saturated or drying zone and the remainder of the element in the initial state (figure 1). Between the drying zone and the remainder of the clement, there is a layer where the migrating vapour condenses (since temperature is lower) which may result in an almost saturated material through which vapour cannot migrate readily. Water transfer is controlled by permeability which depends ‘upon microstructure and moisture state. Low permeability results in bulding-up of vapour pressure in the porous network. The peak pore pressure is located at that layer. Which mechanism is dominant depends in particular upon heating conditions Explosive spalling indicates thatthe thermohygral process is dominant. ‘A numerical code called HITECOSP has been designed by the Italian partners within HITECO [17]. This code simulates the thermo-hygro-mechanical processes that lead to spalling. The main outputs of the simulation are temperature field m2(thermal process), moisture and pore pressure fields (hygral process) and stress fields (mechanical process). The code also provides a damage field and a spalling indicator. ‘The present work deals with the thermohygral process, more particularly with the drying-dehydration front penetration into the concrete element as itis heated on one face. The use of gamma-ray spectrometry enables dynamic measurement of moisture fields in a specimen while being heated. Since water movement in ‘concrete is the most critical phenomenon for spalling, this experiment is of prime importance to validate the code and to understand the ongoing physical process, although the capabilities ofthe set-up do not allow reproducing fire conditions, as in an 10-834 fi EXPERIMENTAL PROCEDURE Gamma-ray speetrometry, the physics and the spectrometer Gamma-ray spectrometry has been used extensively for determining moisture content in soils, and is now adapted to various materials. Matter absorbs gamma rays emitted by a radioactive material, either parilly or totaly, depending upon the energy of the photons, and the nature and thickness ofthe absorber. It is generally accepted thatthe absorption of a mono-energetic gamma ray passing through a two-component absorber (water and solid in the present case) Follows an exponential law: N (x)= Ng exp CaP ttaoa dt a where N and Np = number of transmitted and incident (subscript 0) gamma photons {d= thickness ofthe absorber = mass attenuation coefficient of the component (w for water, s for solid) lensty of the component (w for water, s for solid) 8 = volumetric water content ‘The volumetric water content @ ofa specimen is determined using equation (2) and ‘reference measurement on a dry specimen made of the same material oS ox 1a : io NB 2 where Nit and Nf are the number of photons transmitted through the specimen ints inal sate and the number ansmited through the dry reference specimen, 1 cerespectively. The mass water content « is then deduced using the bulk density of the specimen (p) and the density of water (py = 1) o= 0h @ ° Several factors such as collimation, background radiation, resolution of the analyser, acquisition frequency of the detector, nature of the radioactive source, intensity of the radiation, may influence the accuracy of the result, However the errors induced by those factors have been analysed and appropriate corrections suggested [18-21]. The most important factor affecting accuracy stems from the random nature of photon emission, which can be compensated for by increasing the counting time: accuracy increases with the square root af counting time. However, the latter should not be too long in order to get a dynamic picture of the drying, process. The counting time used inthe present work is 6 min, ‘The major hypothesis made is that any change in the transmitted beam intensity is, interpreted asa loss or a gain of water (free ot bound water). As a consequence, the physical effects of changes in the microstructure (cracking, cement paste hydration, ct.) are neglected ‘The spectrometer is made of two main parts: 1. The gamma-ray source made of Caesium 137, with an energy of 660 keV. This source is embedded in a block of lead. The gamma-ray beam is collimated through a © 4-mm slot. Therefore a 4-mm thick slice is monitored. 2. The detector/analyser, which analyses the transmitted beam. ‘The spectrometer is interfaced with a computer for data acquisition and processing, and for controlling the positioning of the specimen with respect tothe spectrometer. ‘The specimens and the experimental set-up ‘This experiment was designed to provide quasi one-dimensional heat and mass transfer in a specimen. A heater is placed at one end of the specimen that is thermally insulated and sealed on its side (figures 2 and 3). The other end is fee. ‘Temperature and moisture distribution at various positions (distance from heated surface) inthe specimen are measured during heating, The results presented in this paper relate to test performed on a high performance concrete with silica fume, C90, designed and fabricated by the company ADDTEK, 4 partner of the HITECO consortium. The specimens are cylinders with a length of 100 mm and a diameter of 60 mm. They were kept for 3 months in a sealed beg. They were instrumented with 7 thermocouples (with a fibre glass jacket) installed at the time of easting at 2, 10, 20, 30, 40, 50 and 75 mm from the heated surface Their ends were placed above the centre line ofthe specimen so that thermocouples ‘would not interfere with spectrometry measurements, The concrete mix and specimen characteristics are given in table 1 s31The lateral water tightness was achieved by coating the specimen side with a 2-mm thick layer of high-temperature resistant silicone sealant and wrapping. the specimen with a very thin metal jacket that ensured the mechanical resistance of the sealant (figure 2). The lateral heat insulation was provided by ceramic wool Gigue3). Heating was supplied by a flat radiant heater (12 em x12 cm) with a maximum power of 51 kW/m reached at 800°C. By controlling the temperature ofthe heater, 4 heat flux is imposed at the end of the specimen. The heater was placed in a ‘vertical position at about {em from the surface of the specimen and a metal cover was installed on the top of i, so that heat would nat escape by convection (Figure 3) ‘The whole set-up (specimen, insulation and heater) was placed on a cariage free to rove along the axis ofthe specimen, that is perpendicular tothe gamma-ray bear, Moisture was measured at various positions : the moisture state ofa given slice is considered as that measured inthe gamma-ray beam with a diameter of 4 mm. The ‘water content was determined at 4 locations: 15,25, 35 and 45 mm from the heated surface. This gives a sampling interval of 24 min. This rate is rather slow, however itis consistent withthe drying rate involved in the present experiment. Dat processing. At each location, the variation inthe spectrometer output is due to water loss, Since the initial water content is unknown, i is not possible to directly deduce the current absolute water content of the specimen. Furthermore, the amount of water removable in a given volume of conerete at a given temperature, depends upon both the amount of cement paste (Where almost all the water is) and the water content of the cement paste (including pore water, water at the matrix-aggregate interface and chemically bound water). Due to the size of the aggregates (up 10 16 mm), conerete is heterogeneous at the scale ofthe Volume of the studied specimens (@ 60 mm): the amount of paste may vary from slice to slice in which the measurements are performed. Henee, the same change in moisture state in two different locations may result in different water losses in the corresponding slices However, it was demonstrated experimentally that the spatial variation due to specimen heterogeneity is at most about 25 % of the variation due to dehydration during heating. ‘Therefore data processing was carried out in order to make those data easier to use ‘The aitm ofthis processing is to: + Obiain absolute values of water content, not only relative water loss. ‘© Calibrate the spectrometer output in the initial conditions: the actual initial water content was defined as that deduced from measuring the water content by weighing ofa reference specimen dried at 105°C. ‘+ Homogenise spatially the output.This data processing uses a reference specimen along with the test specimen and. assumes that both specimens are in a homogeneous moisture state. Its performed. in steps 1. Reference specimen: scanning and weighing before and after drying. The reference specimen is scanned each S mm by the spectrometer, before and after drying to constant mass at 105°C. After drying the specimen is placed back in the exact same position. This yields for each position an output inthe form of a ‘number of counts (photons) in the intial state N'S}(x) and inthe dry state NE{C«). The water coment of the reference specimen u(x) was calculated using eqs. 2 and3 andthe average valu is Lore (x) Bret 5 @) In addition, alnear relationship Nad = FOND 6 is derived from the data through linear regression (Figure 4), that will be wed instep 2 Atlas weighing the reference specimen before and afer dying also ives the average initial water content ofthe reference specimen OTe Inter is considered as the true initial water content andthe spectrometer output ae {is multiplied by the calibration factor an 2. Test specimen: scanning in initial sate, Measurement is performed atthe target locations on the test specimen and provides Nik(x). N&{(x) is obtained from og. 5, then the inital water content at the target positions «lt (x) is erived using gs. 2and 3 3. Performance ofthe real test. Counting atthe target positions during heating Yields Nog (st). Using eqs. 2 and 3 and N32), the curent water content at ‘each postion ojgu(x,) is ealeulated 4. Homogenisation and calibration of the output, The homogenised and calibrated water content at each target position is calculated as follows on Ont OPO) = OC) 6 01509) xt ‘The first ratio in eq. 6 expresses the fact that of2%"(x,t) is the water content ofa fictitious slice of concrete with an initial water content equal to the average value . In other words, o227(%,1) isthe water content of a fittious slice of conerete with an amount of paste equal to the average value. The second ratio is the calibration factor mentioned earlier. ‘The experimental results should be compared with predictions of the numerical codes. The latter consider a homogeneous material with an average content of ‘cement paste, Therefore the numerical results should be compared with ‘ofS? (x1) calculated ftom moisture measurements by spectrometry RESULTS AND ANALYSIS Before testing, the initial water content of the test specimen, measured by drying the reference specimen at 105°C until steady mass state and using the procedure described above, was equal to @ = 9.8% in terms of volume. The total water porosity (e) and the apparent density (pay) of the concrete after drying at 108°C Were measured using a usual saturation under vacuum method: © = 14.0 + 0.9 % and Papp = 2.46. The degree of saturation ratio u and the mass water content > were then calculated: «o = 4.0 % (mass) and w= 70 % (volume). Results are summarised in Table 2. ‘The results of the test are presented with the help of 4 graphs (figures 5 t0 8). Figures 5 and 6 give, respectively, water content and temperature as a function of time, whereas figures 7 and 8 show water content and temperature versus distance from the heated face. The absolute uncertainty of the w data due to the random nature of the photon emission was estimated to be 1 % (mass). With a plateau temperature of S00°C imposed to the heater, the maximum temperature achieved in the specimen was 347°C at 2 mm and 245°C at 50 mm (Figure 6). An important part of the cement paste is dehydrated within this temperature range (22-25). The highest temperature gradient (close to the heated surface) is around 4°C/mm (figure 8). The initial mass water content is 4% at all locations (figures 5 and 7). The 0% value corresponds to the state where all the so-called free water (that is the water removed at 105°C) was withdrawn. The negative values correspond to. the withdrawal of physically (adsorbed) and chemically bound water. In figure 5 the specimen clearly exhibits a rapid drop in water content down to = ~ 6.8 % at 15. ‘mm, This means that more than 40% of the water removable at the temperature at 15 mm (© 310°C) is bound water. In other words, bound water may play a very important role in the build-up of vapour pressure, partly responsible for spalling ‘The 15-mm and the 25-mm curves reach a plateau directly after the drop. This is not the case for the 35-mm and 45mm curves: the removal of bound water is slower and the curves exhibit a second slope before reaching a plateau. This phenomenon may be due to the presence of higher vapour pressure that would slow own the dehydration of the paste. waaFigure 5 as well as figure 7 clearly show the penetration of the drying and dehydration front. The main characteristics of this front are its velocity and its slope. Those characteristics are strikingly dependent upon the material properties ‘and characteristics: intial water content, porosity, permeability and diffusivity to liquid water and vapour. However, other parameters, such as heating conditions and specimen size, are of significant influence. The denser the material (the less porous and the less permeable), the lower velocity of the drying front and the steeper the slope of the front, The slope of the front expresses the water content gradient in the material. A steep front induces, in turn, a high pressure gradient, ‘which increases propensity to spall. ‘The penetration velocity was estimated by considering the time of intersection of the 1S-mm and the 45-mm curves with the x-axis on figure 5. This yielded a velocity of = 13 mm/h. The slope cf the front was estimated from figure 7. It is equal to = 0.37 %imm. The results are gathered in Table 3. The characteristics of the drying front cannot be interpreted by themselves. Their interest resides in the fact that they can be compared to those of other concretes(ordinary and high- performance). This work is currently being performed. The results are also of most ‘importance for comparison with results of the numerical simulations. In figure 7, the curves exhibit a minimum water content for t> 5.2h: the difference in water content between 15mm and 25mm is equal to 1.8% at most. This feature appears on al the curves with t 52h (some of them were removed from the graph for the sake of readability), Therefore, although this minimum is close to the accuracy of the procedure (1%), it seems to correspond to a real phenomenon, Furthermore, this minimum almost disappears at t= 8.5b, when the drying front is further inthe specimen, CONCLUSIONS ‘As shown in the preliminary results presented here, gamma-ray spectrometry appears to be a promising method to make dynamic measurements of moisture ‘movement in a heated specimen. The experimental set-up provided a quasi one- imensional configuration, asa simulation of apiece of wall heated on one face. ‘The penetration of the drying-dehydration front could be easily monitored and characterised in terms of slope and velocity. These data are essential for modelling the behaviour of concrete at high temperatures and for predicting spalling. The results are currently being used to verify the thermo-hygro-mechanical code for the simulation of the behaviour of high and ultra high performance concrete under fire conditions. Moreover several other mixes, including concrete with polypropylene fibres are currently being studied, “135REFERENCES Copier L.W.J. 1979. The spalling of normalweight and lightweight concrete on exposure to fire. Heron, Vol.24, No. Noumowé A., Clastres P,, Debicki G., Bolvin M. 1994. Effects of high temperature on high performance concrete (70°C-600°C) - Strength and porosity. 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Espoo 1989. Helsinki University of Technology, Department of Structural Engineering, Report 92. p. 72 Jensen J-J., Hansen E A., Danielsen U., Seglem $. 1987, Offshore concrete ‘structures exposed to hydrocarbon fire. The first international conference on ‘concrete for hazard protection, Edinbourg Meyer-Ottens, C. 1975. On the question of speiling of fire exposed concrete constructions (In German). Deutscher Ausschus fur Stahlbeton, Heft 248. Wilh. Emst & Sohn KG. Berlin Hertz K. 1984, Heat-induced explosion of dense coneretes. Technical University of Denmark, Institute of Building Design, Report No 166, Shirley $.7., Burg R.G. and Fiorato A.E. 1988. Fire endurance of high-strength concrete slabs. ACI Materials Joumal, March-April 1988, pp 102-108, Williamson R.B. and Rashed A.J. 1987. A comparison of ASTM E-119 Fire Endurance Exposure of Two EMSAC Concretes With Similar Conventional Coneretes. Fire Research Lab,, University of California, Berkeley, CA, Rep. No. UCB FRG 87-1, July 22-87, p. 20. Maage M, and Rueslaten H. 1985. Trykkfasthet og blaeredannelse pe anpakjent hoyfast betong. FCB. Research Institute for Cement and Concrete STF F 8505015. Harmathy. T.Z. 1965. Effect of moisture on the fire endurance of building element. National Research Council, Research paper No 270 of the division of building research, Ottawa, Canada 16. Jumppanen U-M. 1989. Effect of strength on fire behaviour of concrete. Nordic ‘Conerete Research, No 8, pp 116-127. 17. Majorana C., Gawin D., Pesavento F. and Schrefler B. 1996. A multiphase ‘model for behaviour of concrete at high temperature. Joint Conf. Of ltalian Group on Comput. Mech, And Ibero-latin Amer. Ass. Of Comput. Mech. In Eng. Sept. 25-27, 1996, Padova, pp 209-212. 18, Thony J.P. 1970. Ph-D Thesis. Grenoble University, France. 19, Belleudy P. 1981. Ph-D Thesis. Grenbole University, France, 20, Kumaran M.K. and Bomberg M. 1985. Int. Symposium on moisture and humidity, Washington D.C. (USA), pp 485-490. ‘Nielsen A.P. 1983. Autoclaved aerated concrete, Moisture and properties, Ed EH, Wittman, Elsevier, pp 43-53, 22, Harmathy T.Z, 1970, Thermal properties of concrete at elevated temperatures, ASTM Journal of Materials, Vol. 5 (1), pp 47-74. 23. Lachaud R. 1968, Le comportement du ciment la chaleur étude de Pévolution d'une alite hydratée dans la gamme 20 ~ 400°C. Matériaux et Constructions, Vol.I (4). 24, Bazant Z.P. and Kaplan M.F. 1996, Concrete at high temperatures. Material properties and mathematical models. Longman house, Burnt Mill, England. 25. Diederichs U., Jumppanen U.M. and Penttala V. 1989, Behaviour of high strength concrete at high temperatures. Espoo: Helsinki University of technology report 92: 15.26. 2 ACKNOWLEDGEMENTS This work was performed within the framework of the EC project HITECO BE- 1158, Funding of the project by the European Commission under Brite EuRam Programme is gratefully acknowledged,‘Table 1. Mix composition and specimen characteristics. Denominations Cone CEMMTA SERPS sok Siliea fame Sky? Miron Brkwn Sand 62 mn TTkpa| Aaareunes (Gabba ani) 74 3a kg Aggreenes (Gabbro granite) 28 ma Bakar | Aggregates (Gabbro granite) 8-16 mm_ ‘950.9 kg/m | [Fasicize Soper Parmix kg Water Toi Wate Binder a aa TMs oi TOP Specimen mensions DamAXL mn] Table 2. Density and ierostuctre character often specimen a nil ste Foal water poraiy Taos 09% Apparent densi 26 Volume water conent@) Tava [Mass water content () “4.0 (mass %)| Degre of saturation () 7034 ‘Table 3. Estimated characteristics of the drying-dehydration front Front penetration velocity 13 mm] Front slope 0.37 96/mm|Fig. 1. Simplified representation ofthe various zones and their moisture state in a concrete element heated on one face. <— thermocouple ‘metal plate |+— metal jacket sealant Fig. 2. Set-up for sealing specimen. The specimen is coated with a layer of silicone sealant and wrapped witha thin metal jacket aeFig. 3. Experimental set-up for in-situ gamma-ray spectrometry (the thermocouples are not shown),0.000 2000 02000 Number contin dy ate ‘sso00 s8n00 90000 92000 94000 9400098000 0HEND| Nombe f Couns inna sare N40) Fig. 4. Reference specimen. Correlation between counting inthe dry state and the initial state on the same specimen. A linear regression line is plotted and its ‘equation is given,3 3 2 3 Howogenized water conten (mass 4 2 bad Tine (hous) Fig, 5. Homogenised water content versus time forthe various depths Tene (hows) Fig. 6. Temperature of the heater and within the specimen as a function of time, for various depthsRRR F 7 Homogenizd water content (nase # isan fo he etd ice nen) Homogenised water content as a function of distance for various times : *reance om te Rated atce (an? a Fig. 8. Temperature profiles inthe specimen for various times.