International Journal of Engineering Trends and Technology (IJETT) – Volume 33 Number 6- March 2016 Assessing the Freezing and Melting Point of GGBS Concrete Adama Lami Kawu1, Mahmud Abba Tahir2, Mohammad Balteh3, Yusuf Mohammed Nuruddeen4, Raji Mohammed Mudashir5 1 Department of Building Technology, Abubakar Tafawa Balewa University, Bauchi. Nigeria 2,3&4 Department of Building Technology, Federal Polytechnic, Bauchi. Nigeria 5 Department of Quantity Surveying, Federal Polytechnic, Bauchi. Nigeria Abstract-The pore structure of a concrete material is made up pores of various sizes. This study is aimed at assessing the freezing and melting point of concrete within the cover zone by monitoring the formation of ice and melting at different temperatures using electrical measurement technique. A multi-electrode array system was used to obtain the temperature of ice formation and melting at discrete depths within the cover zone of the concrete. A total number of four concrete specimen (250mm x 250mm x 150mm) made of ordinary Portland cement concrete and ordinary Portland cement replaced by 65% ground granulated blast furnace slag (GGBS) with water/binder ratios of 0.35 and 0.65 were produced and ponded with water to ensure full saturation and then subjected to freezing and melting process in a refrigerator within a temperature range of -300C and 200C over a period of time 24 hours each. The data was collected and analysed. Results obtained shows that the freezing and melting behavior of all specimens differs. It was also observed that at a much lower depth of 75mm which is close to the rebar, the pores freezes at a much lower temperature of about -290C but melts at different temperatures irrespective of w/b ratio and GGBS additive. Keywords—GGBS, Concrete, durability, Freezing, Melting I. INTRODUCTION Concrete durability to freezing and thawing is closely related to its pore structure. The freezing point depression of the pore solution and the volume of ice formed in the pores are greatly influenced by the volume, radius and pores size distribution. Commonly, within a particular temperature interval, more frozen concrete pore solution induces greater internal hydraulic pressure and therefore, further serious damages. Once ice is formed within the pore system, ice cannot propagate instantaneously through the whole material because of its porous microstructure features such as the pore size distribution and geometry. The temperature at which ice is formed or solidification of water in a particular pore depends on the size and shape of the throat which connects the pores within the pore network. The pore neck usually freezes at a lower temperature ISSN: 2231-5381 and once that happens, the pores will freeze at a higher temperature due to the hydraulic pressure developed. According to [3], the larger pores freezes at low temperature and any further drop in temperature leads to further freezing of the water in the pores due to the different pore sizes. Studies conducted by [2] suggest that freezing takes place at about -100C and that the pore solution freezes more quickly beyond -100C than below -100C. Freezing is a function of temperature. The rate at which pore water in concrete freezes depend on the temperature, pore connectivity, pore size and the pore neck. The pore water freezes due to the percolation of the ice front through the connected pore network because the pores, whether frozen or unfrozen, depends on the state of their neighbours. According to [5], pores are larger than their neck and pores with radius bigger than the breakthrough radius may freeze at a particular temperature. However, the freezing of the pores highly depends on the pore system connectivity. Because, freezing is a gradual percolation process of an ice front through the connected network, some pores with pores bigger than the breakthrough radius will not freeze at that particular temperature but rather at a much lower temperature. Freezing requires the ice front to be able to reach the pores and for those pores which are far away from the ice front, there is likely going to be constraints along the way that may slow the ice front from reaching them and hence, they will remain unfrozen until temperatures lower than the exposed temperature is applied. Therefore, freezing of pores is solely dependent on the direction of the ice front as well as the position of the pores [4]. Unlike freezing, thawing is independent of the surrounding pores. Pores of the same radius and shape will thaw at a particular temperature. Small crystals of a liquid in the concrete pores melt at a temperature below that for the bulk liquid. The melting point depression is inversely proportional to the size of the pores. However, ice expands faster than the surrounding pore space and as a result expansive forces are generated into the matrix and subsequent cracking. Equally, the difference in entropy of the gel and capillary water causes the diffusion of the gel to the capillary cavities. During freezing and thawing, the pore system pressure can be calculated based on the theory of thermodynamics. In this theory which is solely based http://www.ijettjournal.org Page 295 International Journal of Engineering Trends and Technology (IJETT) – Volume 33 Number 6- March 2016 on thermodynamic relationship, the pore structure of a material is considered partly filled with water and air. During freezing or ice formation, under pressure takes place in the pore system because of the fast contraction of ice than in the surrounding cement matrix. [1] Stated that, the shape of the pores upon freezing and thawing varies. Upon freezing (cooling), the ice/water interface is assumed or considered to be hemispherical (f=1) and therefore, the relationship for the freezing point depression can be expressed as: ΔTcool = - 64.67/rp-0.57 ……………… Equation 1 Upon melting (heating), the interface is considered to be cylindrical (f=2) and the ice fills the cylindrical pores and hence, the hydraulic radius of the melting point is different and therefore, the relationship for the melting point depression can be expressed as: ΔTheat = -32.33/rp-0.68 ……………… Equation 2 II. MATERIAL, SAMPLE AND CURING The sample comprised of OPC clinker combined with ground granulated blast furnace slag as Supplementary Cementitious Materials (SCM) used in blending was combined in accordance with BS EN 197-1:2000. A water binder ratio of 0.35 and 0.65 were used. The sand used was concreting sand with a maximum particle size of 4mm along with two grades of crushed granite (10mm and 20mm) of low porosity (~0.7%-0.9%). Plasticizer polycarboxylate SikaPlast, conforming to BS EN 934-2 was used. Specimens were 250×250×150mm (thick) slabs, the upper surface of each slab had a 20mm high ponding area which held water, hence, allowing water to be ponded on the surface of the slab III. EXPERIMENTAL AND TEST PROCEDURE A. Two-point multi-electrode array set-up This experiment used a two point embedded multielectrode array system. The set-up of the inverted T shaped PVC which holds the electrode in place is illustrated in Figure 1. Each electrode was made up of stainless steel pins of 1.6mm diameter. A stainless steel of 10mm diameter was exposed on the end of each electrode. The electrodes were spaced horizontally at 10mm interval, and then vertically spaced at depths of 10mm, 20mm, 30mm, 40mm, 50mm, and 75mm respectively from the surface of the specimen. In order to ensure better distribution around the probes when pouring, the electrodes were overlapped against each other in a vertical plane. The tip of each probe exposed was placed at a distance of 45mm from the face of the T shaped PVC so as to reduce the aggregate-wall-effect. In order to take temperature readings during the experiment, thermistors were integrated into the face of the PVC former at varying depths of 10mm, 30mm, 50mm and 75mm. the data collected were ISSN: 2231-5381 then corrected to temperature. The thermistor resistances were then converted to temperature readings in (0C) and kelvin (K) using the Stein-Hart equation: T = [A + BlnR + C (lnR) 3]-1- 273.15 … Equation 3 T = [A + BlnR + C (lnR) 3]-1 ………….. Equation 4 Where, R = the measured resistance of the thermistor (ohms) T = temperature (ºC) and K; A, B, C = coefficients which depend on the type of thermistor, were calculated from manufacturer data, respectively, to be: 1.287600011×10-3 K-1; 2.357183092×10-4 K-1 and 9.509464377×10-8 K-1. Ln = natural logarithm. Fig 1: Multi Electrode sensor array B. Freezing and thawing procedure The samples were ponded using pure tap water which has been allowed to cool at room temperature to ensure that the specimens are fully saturated before subjecting them to the freezing and thawing process. The ponding process lasted for 7 days. Before subjecting the specimens into the freezing and thawing chamber, the surface of the specimens were de- ponded by the use of clean dry sponges and also covered with a thick plastic lid to prevent any further moisture loss. After attaining full saturation, each of the four specimens X1(65% GGBS and 0.35 w/b ratio), X3(65% GGBS and 0.65 w/b ratio), C1 (100% OPC and 0.35 w/b ratio) and C3 (100% OPC and 0.65 w/b ratio) was separately put in a freezing and thawing chamber for 24 hours for the freezing cycle. The freezer temperature was dropped to -300C from the room temperature of 20 0C. After 24 hours, the freezing and thawing chamber was then switched off and the specimen was allowed to melt for 24 hours at room temperature for the thawing cycle to take place. The same procedure was repeated for specimen C3, X1 and X3. The set up can be seen in figure 2. http://www.ijettjournal.org Page 296 International Journal of Engineering Trends and Technology (IJETT) – Volume 33 Number 6- March 2016 readings were used to analyse both the resistivity data and conductivity data. Equally all the data recorded by the logger was in resistance, and therefore it was decided to use resistance for the analysis. The temperatures after correction in the region of approximately 230C and -290C during the experimental programme which is quite okay as the laboratory temperature is supposed to be controlled at 200C and the refrigerator temperature ranges was set at -300C for the freezing cycle and then possibly down to the laboratory temperature of 20 0C. Figure 2: Freezing and thawing chamber setup C. Electrical Measurement System An automated measurement system was used to gather two-point resistance data from the electrode embedded array system in the concrete slabs. The system consists of a concrete resistance logger linked to a multiplexing unit, which allows up to seventy two 2-point channels to be monitored via six 37-way D-type connector and cable assemblies. Measurements are obtained using a 1000 mV peak to peak ac voltage signal (350 mV rms) at 1000 Hz. The logger stores measured resistance data in an operator pre-programmed format to a non-volatile memory. As-measured data is uploaded in 39 Microsoft Excel csv format for subsequent processing to a personal computer (PC) via an RS232 port connector. The logger was set to record a cycle reading at every 5minutes interval for a period of 24 hours. Figure 4: Natural logarithm of conductance vs 1000/T for specimen C1 Figure 5: Natural logarithm of conductance vs 1000/T for specimen C3 Figure 3: Measurement system IV. RESULT AND DISCUSSION The freezing and melting points and pore sizes of each specimen at different depths were obtainedfrom the plots of natural logarithm of conductance (s/m) versus 1000/T(k) and Equation 1 and Equation 2 respectively, presented and discussed. A. Temperature Correction The logger record or measures thermistor resistance and therefore they were converted to temperature readings (0C) and kelvin (K) using equation 3 and equation 4 respectively. These corrected temperature ISSN: 2231-5381 Figure 6: Natural logarithm of conductance vs 1000/T for specimen X1 http://www.ijettjournal.org Page 297 International Journal of Engineering Trends and Technology (IJETT) – Volume 33 Number 6- March 2016 takes place at different temperature. At depths 10mm and 30mm, temperature at which the pores freezes is approximately 00C, but at depths 50mm and 30mm, the freezing point temperature is observed to be approximately -10C. This could be that there is no much change in the pore structure as the pores are of same sizes However, it is quite interesting to see that the pores at all depths melts at the same temperature at approximately 20C. Also, there is not any change in the pore structure at all the depths because the pores are of same sizes. Figure 7: Natural logarithm of conductance vs 1000/T for specimen X3 Figure 8: Natural logarithm of conductance vs 1000/T for specimen C110mm 3 cycles subjected to 3 cycles of freezing and thawing TABLE I: Freezing and melting point for Specimen C1, C3, X1 and X3 In analysing specimen C1, it can be observed that at depth 10mm, the concrete pores freezes at approximately -30C, but was different at lower depths. At depths 30mm, 50mm and 75mm, the temperature at which ice is formed in the pores is much lower than that at depth 10mm at approximately -290C. This could also be attributed to the change in the pore structure at lower depths with pores at the surface 10mm depth larger in size than at lower depths. However, the temperature at which the pores melt does not coincide with that of ice formation. At depth 10mm, the pores melting point temperature is observed to be approximately -10C, but is much higher at lower depths of 30mm, 50mm and 75mm with a temperature of approximately 140C. This again could be due to change in the pore structure at lower depths. In analysing specimen C3, it can be seen that the freezing and melting of the pores at various depths ISSN: 2231-5381 In analysing specimen X1, it can be observed that at depth 10mm, the concrete pores freezes at approximately -190C, but was different at lower depths. At depths 30mm, 50mm and 75mm, the temperature at which ice is formed in the pores is much lower than that at depth 10mm at approximately -290C. This could be attributed to the change in the pore structure at lower depths with pores at the surface 10mm depth larger in size than at other depths. However, the temperature at which the pore melts does not coincide with that of ice formation. At depth 10mm, the pores melting point temperature is observed to be approximately 2 0C, but is much higher at lower depths of 30mm, 50mm and 75mm with a temperature of approximately 130C. This again could be due to changing pore structure at various depths. In analysing specimen X3, it can be seen from Table 5.4 that at depth 10mm, the concrete pores freezes at approximately 00C, but was different at lower depths. At depths 30mm, 50mm and 75mm, the temperature at which the pores freezes is observed to be much lower than that at depth 10mm at approximately -290C. This could also be attributed to the change in the pore structure at lower depths with pores at the surface 10mm depth larger in size than at other depths. However, it can be observed that the pore does not melt at the same temperature with ice formation. At depth 10mm, the pores melt above at approximately 40C, but melts at a much lower temperature below freezing point at approximately 30C at depths 30mm, 50mm, and 75mm respectively. This again could be due to changing pore structure at various depths. TABLE II:Freezing and melting point for Specimen C1 Subjected to 3 freezing and thawing cycles Specimen C1 was subjected to 3 repeated cycles of freezing and thawing. It can be observed from that the analysis was done at only depth 10mm and http://www.ijettjournal.org Page 298 International Journal of Engineering Trends and Technology (IJETT) – Volume 33 Number 6- March 2016 75mm because they are the depths at the surface and close to the rebars. At depth 10mm for all the 3 cycles, the pores freezes at the same temperature of approximately -30C and melts at the same temperature of approximately -10C for all cycles but at a different temperature with the temperature of ice formation. At depth 75mm, the pores freezes at a much lower temperature than that at depth 10mm with a temperature of approximately -290C. Also, the pores melt at the same temperature of approximately 140C for all the cycles. This could also be due to change in the pore structure at lower depths with pores at the surface 10mm larger than that at lower depths V. CONCLUSION In conclusion, it can be observed that the freezing and melting behavior of all specimens differs. Specimen C3 was observed to perform poorly by freezing at between 00C to -10C at all depths and melts at about 20C. However, because the depth 75mm is the depth close to the rebar, it can be seen that irrespective of w/b ratio and additive, the pores freezes at a much lower temperature of about -290C but melts at different temperatures. This could be that the pore structure changed at much lower depths possibly with much larger pores. For specimen C1 was subjected to 3 repeated cycles of freezing and thawing, the number of cycles did not change its behaviour as the freezing and melting points remain the same in all the 3 cycles. REFERENCES [1] [2] [3] [4] [5] Brun, M., Lallemand, A., Quinson, J.F. and Eyraud, C. 1977. ‘A new method for the simultaneous determination of the size and shape of pores’: The thermoporometry, Thermochimica Acta 21, 59–88. Cai, H. & Liu, X. 1998. Freeze-thaw durability of concrete: ice formation process in pores. Cement and Concrete Research, 28, 1281-1287. Kaufmann, J. P. 2004. Experimental identification of ice formation in small concrete pores. Cement and Concrete Research, 34, 1421-1427. Schulson, E. M., Swainson, I., P, Holden, T. M. & Korhonen, C. J. 2000. Hexagonal ice in hardened cement. Cement and Concrete Research, 30, 191-196. Swainson, I. P. & Schulson, E. M. 2001. A neutron diffraction study of ice and water within a hardened cement paste during freeze–thaw. Cement and Concrete Research, 31, 1821-1830. ISSN: 2231-5381 http://www.ijettjournal.org Page 299