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Effect of relative humidity and air permeability on prediction of the rate of carbonation of concrete D. Russell, P. A. M. Basheer, G. I. B. Rankin and A. E. Long The effect of relative humidity on both air permeability and rate of carbonation is investigated.Descriptivemodels, based on data from an accelerated carbonation test, were developed to quantify the effects of the relative humidity and the air permeability on the rate of carbonation. The relationships between the rate of carbonation and physical properties, such as the permeation properties and compressive strength were established. It was found that the permeation measurements should only be used to estimate the likely rate of carbonation when the relative humidity of the concrete specimen is known. 1. INTRODUCTION The moisture content of concrete in service can be decisive in determining the life span of a concrete structure. This is due, not only to its effect on the permeation properties of the con- crete, but also to its effect on various deterioration processes acting in concrete. Carbonation is one of the mechanisms that is influenced by both the permeation properties and the moisture content of the concrete. The moisture conditions of the cover concrete are most often expressed in terms of relative humidity (RH). This varies with variations in the ambient conditions. Therefore, a cyclic wetting and drying exposure could lead to fluctuations in RH in the cover concrete.1 In this situation, carbonation effectively stops when the concrete is saturated and only proceeds when the concrete dries out enough to allow the ingress of carbon dioxide. Another possibility is when the concrete is dry enough to allow the ingress of CO2, but still contains sufficient amounts of moisture to allow the chemical reactions, necessary for carbonation, to occur. In this situation carbonation reaches a maximum level at relative humidities between 50 and 70%.2–4 At relative humidity values above 70% the carbonation slows down due to the slower rate of diffusion of CO2 through water filled pores. At relative humidity values below 50% there is insufficient moisture to allow carbonation reactions to take place. The influence of moisture on permeation properties is well documented.5–9 Nagataki et al.10 proposed that the air permeability is related to the water evaporated from the concrete. Parrott11 has related the internal relative humidity to the air permeability; it has been shown that an increase in relative humidity caused a decrease in the air permeability of the concrete. Parrott5 also presented the effect of relative humidity on air permeability in concrete from different researchers. The influence of the different concretes on this relationship is most pronounced at high relative humidities. 1.1. The effect of air permeability on carbonation of concrete Dhir et al.12 have related permeability to carbonation and it has been shown that concrete with low permeability carbonates at a lower rate in comparison to one with high permeability. They have also found that there is a close relationship between intrinsic permeability of cover concrete and its resistance to carbonation, irrespective of mix proportions and curing. The relationship between permeability and carbonation is very much an interactive one, with the permeation controlling the ingress of carbon dioxide and the carbonation altering the permeation properties. Dewaele et al.13 report permeability reductions of between three and five orders of magnitude in fully carbonated cement paste compared to uncarbonated cement paste. This is not the only interactive process involved in carbonation, but it is significant. It is further complicated by the fact that both the permeability and the process of carbonation are affected by the relative humidity, as discussed previously. This paper discusses the quantitative influence of the moisture content on both the air permeability and the rate of carbonation, in an accelerated carbonation test. Furthermore, the combined effect of air permeability and relative humidity on carbonation is presented. 2. EXPERIMENTAL PROGRAMME 2.1. Test variables The test specimens consisted of eight different concrete mixes, with variables of four water/cement ratios, (w/c) and two cement contents (CC). Three batches of these eight mixes were cast for testing at three RH conditions: 55, 65 and 75% RH. The curing, conditioning and exposure to the CO2 environment were held constant for all mixes and RH conditions that are discussed in subsequent sections. 2.2. Mix constituents Details of the eight mixes used in the test programme are given in Table 1. Class 42.5N Portland cement (OPC) conforming to Proceedings of the Institution of Civil Engineers Structures & Buildings 146 August 2001 Issue 3 Pages 319^326 Paper 11814 Received 09/09/1998 Accepted 24/01/2001 Keywords: code of practice & standards/ concrete technology & manu- facture/field testing & monitoring Derek Russell Structural Engineer, Kirk McClure Morton Consulting Engineers, Belfast, Northern Ireland P. A. Muhammed Basheer Professor of Structural Materials, School of Civil Engineering, The Queen’s University of Belfast, Northern Ireland G. I. Barry Rankin ManagerofConstructionDivision, Northern Ireland Technology Centre, TheQueen’s University of Belfast, Northern Ireland Adrian E. Long Dean, Faculty of Engineering, The Queen’s University of Belfast, Northern Ireland Structures & Buildings 146 Issue 3 Effect of relative humidity and air permeability Russell et al. 319 BS12: 199114 was used in the manufacture of all mixes. The coarse aggregate used was 10 mm maximum size basalt and the fine aggregate was medium size natural sand.15 All the aggregates were oven dried at 408C for at least 24 h and cooled to 208C prior to casting in order to remove moisture from aggregates so that it did not affect the effective water/cement ratio of the mixes. However, in order to remove any effect of water absorption by aggregates during the mixing, a pre- determined quantity of water, based on the one-hour water absorption of the aggregates, was added to the mixing water. The concrete mixes were designed in accordance with a procedure given in ‘Design of Concrete Mixes’ by the Building Research Establishment.16 2.3. Preparation of test specimens Six 2506 2506 80 mm slabs were cast for each mix for each of the relative humidity sets. Three slabs from these were used for the measurements of both the air permeability and the relative humidity. From the remaining three slabs, 27 cores of 50 mm diameter were removed, which were used for the determination of the rate of carbonation. Along with the slabs, 100 mm cubes were cast to determine the compressive strength of the concrete. The concrete was manufactured in accordance with BS 1881: Part 12517 using a 0?085 m3 capacity pan mixer. The moulds were filled in two equal layers and each layer was compacted using a vibrating table until no air bubbles appeared at the surface. The concrete in the moulds was then covered with a polythene sheet and left for 24 h in the laboratory at 208C (+28C). After 24 h the specimens were removed from the moulds and placed in a curing tank at 208C (+18C). After three days the specimens were removed from the tank and wrapped and sealed in polythene sheets. The specimens were then placed in a conditioning room at 208C (+28C) and 55% (+2%) RH for 25 days. At 28 days the cubes were crushed and cores taken from the three slabs. The curved sides of the cores and the four sides of the slabs received three coats of Sikaguard, 680 ICOSIT concrete cosmetic acrylic paint that had in previous tests been shown to provide good resistance to both CO2 and moisture penetration. Initial air permeability and relative humidity readings were taken at this stage before the specimens were subjected to drying. 2.4. Drying After initial testing for air permeability and relativehumidity at the age of 28 days, both the slabs and the cores were placed in a drying cabinet at 408C (+28C). The drying period depended on the target moisture conditions required and was selected based on previous experience with the selected mixes. The target uniform relative humidities of 55, 65 and 75% after conditioning resulted in drying periods of 4, 2 and 1 week respectively. 2.5. Conditioning After drying, the specimens were conditioned at 408C (+28C) for 6 weeks to establish a uniform moisture profile in the cover concrete in which carbonation could occur. In order to achieve this the specimens were wrapped in 300-gauge polythene sheets and the joints sealed with heavy-duty parcel tape. This was based on a method used by Parrott16 wherein it was shown that the increased temperature allowed the redistribution of moisture within the concrete to proceed more freely than at lower temperatures. After the conditioning period, the trowel- finished face of both the cores and the slabs was treated with three coats of paint in order to leave only the face cast against the mould exposed to the environment. 2.6. Accelerated carbonation test The carbonation test was carried out in a specially built carbonation chamber, manufactured by LEEC, England. This chamber was capable of maintaining a constant environment with respect to temperature, relative humidity and carbon dioxide concentration. The chamber was set to maintain a 5% CO2 (+0?5%) concentration at 208C (+18C) during the testing. The relative humidity was programmed to each of the three target RH levels when each set of specimens were tested, the accuracy of the relative humidity control was +1%. The specimens were exposed to this environment for 6 weeks. 2.7. Measurement of carbonation The depth of carbonation was measured after each week of the 6-week exposure to carbon dioxide in the chamber. At these times three cores from each mix were removed from the chamber, split open longitudinally and the freshly fractured Mix no. w/c ratio Cement content: kg/m3 Water content: kg/m3 Fine aggregate content: kg/m3 Course aggregate: content: kg/m3 Achieved a/c ratio 1 0?50 375 192 685 1243 5?14 2 0?57 375 215 664 1207 4?99 3 0?63 375 234 647 1174 4?86 4 0?70 375 256 625 1140 4?71 5 0?50 315 164 732 1329 6?54 6 0?57 315 184 711 1296 6?37 7 0?63 315 201 696 1296 6?23 8 0?70 315 220 679 1233 6?07 Note: Fine aggregae/course aggregate ratio held constant at 0?55. Table 1. Details of mixes used in investigation 320 Structures & Buildings 146 Issue 3 Effect of relative humidity and air permeability Russell et al. surfaces were sprayed with a 1% phenolphthalein solution to determine the depth of carbonation. After 24 h the depth of carbonation was measured at three locations at right angles to the exposed surface to an accuracy of 0?5 mm in accordance with the RILEM recommendations CPC-18.18 An average of three readings from the three cores was reported as the depth of carbonation after each week’s exposure in the chamber. 2.8. Measurement of air permeability The air permeability was measured before the specimens were exposed to CO2 and at weekly intervals to coincide with measurement of the carbonation depth. The air permeability was measured using the Autoclam permeation system7 and the result reported as an air permeability index (API). The test was carried out on a total of three 2506 2506 80 mm slabs for each mix and relative humidity condition. An average air permeability index was determined from the three results. 2.9. Measurement of relative humidity The internal relative humidity of the concrete was monitored at the same time as the air permeability and the depth of carbonation. It was measured at 0, 10, 20, 30 and 40 mm depths from the exposed surface. A chilled mirror dew point probe purchased from Protimeter plc, England was used to measure the relative humidity in preformed cavities of 22 mm diameter. The probe was used in conjunction with a shield device to ensure a constant and sealed volume of air was used in each test.18 3. EXPERIMENTAL RESULTS ANDDISCUSSION The 28-day compressive strength values for the eight mixes are presented in Table 2. The results show that mixes with an adequate range of quality control were produced. In addition, there was sufficient repeatability between the three sets of mixes which were cast several months apart. 3.1. Effect of relative humidity on air permeability of concrete The relative humidity profiles were determined to a depth of 40 mm from the concrete surface and the variation over the depth was found to be within a narrow band of 5% deviation from the target RH. The relative humidity at 10 mm (RH10) was, chosen to determine the effect of RH on air permeability. It was considered that the RH at 10 mm was less likely to be affected by short term fluctuations in the ambient RH, whilst still reflecting the RH of the near surface concrete, as the RH profiles in the specimens were stable. The API values obtained at both prior to and after the 6 weeks of carbonation are reported in Table 3. The changes in API over the carbonation period were erratic, with the API of some mixes increasing whilst some others decreased due to the carbonation. However, as can be seen in Table 3, there was a general trend of slightly increasing API due to carbonation and this was most pronounced for the 0?7 w/c ratio mixes, particularly the 375 kg/m3 mixes. The API of the mixes varied differently at the three RH levels. However, no clear patterns were established. Parrott16 reported that air permeability remained constant between 40–70% RH, with API decreasing above 70%. These results were supported by Nolan.19 The results presented in Table 3 support these findings, with the exception of the high w/c ratio mixes, whose API decreased marginally from 55 to 65% RH, particularly in uncarbonated concrete. In addition, the results show that the lower the RH of the concrete at the time of carrying out the API test the easier it becomes to distinguish between the various mixes. This finding is in agreement with that reported by Nolan. The results also demonstrate the importance of using the API measured at the same RH for comparing the relative performance of concretes. 3.2. Effect of relative humidity on carbonation of concrete The rates of carbonation (RoC) of all mixes given in Table 4 are calculated from the results of depth of carbonation over the 6-week period plotted against the square root of the exposure period. The overall trend in Table 4 is that of decreasing RoC with increasing RH. However, the RoC does not appear to change at a constant rate over the range of RH studied. For the lower w/c ratio mixes the greatest change in RoC occurred between 55 and 65% target RH. This is the range for which the change in API was not constant, as highlighted in the previous section. Maximum carbonation occurred at 55–65% RH. However, the API, while not consistent, did not alter significantly within this range. This would mean other factors might have influenced the RoC between these RH values. From 65 to 75% RH there was a decrease in both the carbonation and API. Hence, the lack of carbon dioxide may be the factor controlling the RoC in this range of RH values. The results show that while the RH affects the RoC, the effect is not the same for all the mixes investigated. The effect of w/c ratio on API and RoC is the largest at 55% RH and is the least at 75% RH. This can be attributed to the fact that the pores are free of moisture at low RH, i.e. the open porosity effect is obtained at the low RH. Overall the trend of decreasing RoC with increasing RH within this range is similar to that which could be expected. However, what the results show is that there is a wide range of variability depending on the mix proportions and the quality of the concrete. Target relative humidity Cement 55% 65% 75% content: w/c ratiokg/m3 Compressive strength: N/mm2 0?50 375 58?8 61?5 61?7 0?57 375 48?4 51?8 50?4 0?63 375 41?1 42?2 41?1 0?70 375 26?5 33?7 35?5 0?50 315 55?7 63?0 59?7 0?57 315 42?9 50?0 57?8 0?63 315 35?7 44?6 49?5 0?70 315 29?3 35?3 39?5 Table 2. The 28-day compressive strength of mixes used in investigation Structures & Buildings 146 Issue 3 Effect of relative humidity and air permeability Russell et al. 321 3.3. Combined influence of API and RH on rate of carbonation The previous sections discussed the effect of the RH on both API and RoC. This section firstly tries to relate the API to the RoC first and then discusses the combined effect of API and RH on RoC. The RoC was plotted against the initial and the final API in Figs 1 and 2 respectively. In these figures the effect of changing the RH is clear (55% at top to 75% target RH at bottom). The graphs show that a good relationship can be determined for individual sets of mixes. The trend lines in both Figs 1 and 2 for the two cement contents (CC) are separated. A close examination of Fig. 1, by comparing the RoC of mixes with the same w/c ratio but different CC, would reveal that the RoC did not differ much between the two cement contents. That is, the separation of the two trend lines is primarily due to the effect of the CC on the API. A similar observation can be made in Fig. 2 as well. The two figures also demonstrate the necessity of carrying out RH measurements when measuring the API. The results presented in this section show that the API can be related to the RoC. However, it depends on both the internal RH and the cement content. That is, the many factors influencing the RoC of concrete make assess- ment of concrete’s carbonation resistance difficult to deter- mine on the basis of API measurements alone. Then it should be borne in mind that API measurements should be taken in conjunction with RH measurements. Furthermore, any additional information about a concrete, for example, its w/c ratio or CC, or another material property such as strength, can improve the accuracy of the prediction. 3.4. Prediction of the rate of carbonation based on relative humidity and air permeability In this section, the development of prediction models to describe the relationship between the rate of carbonation, the relative humidity and the air permeability of concrete is discussed. In order to do this multiple linear regression (MLR) models were employed. The first stage in developing the MLR models was to ensure that the data was normally distributed and to transform any data that was not normally distributed. All of the data used in developing the models were normally distributed, with the exception of the API data, which required a logarithmic transformation to provide the normality. The next stage was to determine the coefficient of correlation between the various factors under consideration, namely, the air permeability and the relative humidity and the rate of carbonation, Table 5. MLR models were developed with the variable with the highest coefficient included first. Altogether three models were developed from this study and these are presented in Table 6. Two of the models relate the air permeability to the rate of carbonation whilst the final model also includes the compressive strength. All of the models in this section should be considered as descriptive as they relate to accelerated carbonation tests, not real time exposure. The intercepts and multipliers for the models are presented in Table 7. The results obtained from the three models within this Target relative humidity Cement 55% 65% 75% content: w/c ratio kg/m3 API at start of carbonation: (ln mbar)/min>100 0?50 375 7?28 8?95 2?81 0?57 375 20?90 16?25 7?61 0?63 375 15?64 13?65 5?01 0?70 375 54?63 24?68 13?59 0?50 315 11?35 7?76 4?87 0?57 315 13?81 13?51 5?05 0?63 315 12?40 12?57 4?04 0?70 315 18?53 21?07 13?48 Target relative humidity Cement 55% 65% 75% content: w/c ratio kg/m3 API at end of carbonation: (ln mbar)/min>100 0?50 375 7?71 12?01 2?52 0?57 375 13?79 21?21 7?60 0?63 375 18?62 18?57 9?58 0?70 375 75?52 46?33 22?46 0?50 315 11?16 7?57 4?61 0?57 315 13?15 12?82 4?65 0?63 315 15?75 16?62 5?20 0?70 315 23?69 31?39 14?36 Table 3. Measured API for all mixes before and after 6 weeks of accelerated carbonation Target relative humidity Cement 55% 65% 75% content: w/c ratio kg/m3 Carbonation rate: mm/(week0?5) 0?50 375 3?32 1?43 1?97 0?57 375 5?56 2?90 2?39 0?63 375 5?49 6?08 3?06 0?70 375 9?84 7?94 2?74 0?50 315 4?40 1?71 1?32 0?57 315 4?48 4?20 2?42 0?63 315 8?72 6?34 2?82 0?70 315 10?96 7?62 4?18 Table 4. Rate of carbonation for all mixes 322 Structures & Buildings 146 Issue 3 Effect of relative humidity and air permeability Russell et al. section are compared to the actual data in graphical form in Figs 3, 4 and 5. 3.5. Model based on log (initial air permeability) and relative humidity This model combines the logarithm of the initial measurement of the air permeability (APIi) with the relative humidity at 10 mm depth from the surface (RH10). The APIi was used to represent the property of the concrete’s structure at an early age and the RH to indicate the service condi- tions. The model is presented below: RoC = b0 + b1[ln(APIi)] + b2(RH10) + eI 1 This model produced a coeffi- cient of multiple deter- mination (R2) of 0?595. This result was disappointing given the high initial correlation coefficients. However, it must be remembered that there was a wide scatter of API values for the mixes investigated. This is evident in Fig. 3, which presents the model’s effectiveness graphically. A close examination of Fig. 3 would indicate that another possible reason for the low R2 value is due to the nature of the data itself. A curve rather than a straight line better represents the trend in Fig. 3. 3.6. Model based on log (final air permeability) and relative humidity In this model the final air permeability (APIf) data is used to provide a more mature representation of the concrete’s condition, while the RH indicates the service conditions. The model is presented below: RoC = b0 + b1[log(APIf)] + b2(RH10) + eI2 This model proved slightly better than the previous model producing a coefficient of multiple determination of 0?644. As can be seen in Fig. 4 there is less scatter of the data points with this model. Once again, a curvilinear relationship could better express the relationship in Fig. 4. 3.7. Model based on log (initial air permeability), compressive strength and relative humidity The final model combined the first model with the fcu data for the mixes. In this model it is considered that both the strength and permeation measurements would be used in the assessment of a structure’s carbonation resistance. The model is shown below: RoC = b0 +b1[log(APIi)] + b2( fcu) + b3(RH10) + eI3 The fcu is well established as an indicator of concrete quality and is related to the rate of carbonation of concrete. The addition of the fcu to the model dramatically improves the coefficient of 12 10 8 6 4 2 0 12 10 8 6 4 2 0 12 10 8 6 4 2 0 0 20 40 60 80 100 Initial air permeability index, API: Ln mBar/min × 100 (c) (b) (a) R at e of c ar bo na tio n, R oC : m m /w ee k0 ·5 R at e of c ar bo na tio n, R oC : m m /w ee k0 ·5 R at e of c ar bo na tio n, R oC : m m /w ee k0 ·5 0·50/375 0·57/375 0·63/375 0·70/375 0·50/315 0·57/315 0·63/315 0·70/315 (w/c)/CC 315 kg/m3 CC, R 2 = 0·51 375 kg/m3 CC, R 2 = 0·96 315 kg/m3 CC, R 2 = 0·83 375 kg/m3 CC, R 2 = 0·66 315 kg/m3 CC, R 2 = 0·60 375 kg/m3 CC, R 2 = 0·71 Fig. 1. Rate of carbonation versus initial permeability index Correlation coefficient: R Response variable Rate of carbonation: RoC Measured properties Compressive strength ”0.694 Relative humidity, at 10 mm depth ”0?583 Air permeability index Initial 0?708 Final 0.708 log (air permeabilityindex) Initial 0?754 Final 0.753 Table 5. Correlation between rate of carbonation and experimental variables Structures & Buildings 146 Issue 3 Effect of relative humidity and air permeability Russell et al. 323 correlation to 0?781. This is presented graphically in Fig. 5. The results from this model indicate that the addi- tion of fcu to the model in equation (1) provides a better representation of the likely rate of carbonation. This is presumably due to fcu’s non- dependence on RH while the API is dependent on the RH. 3.8. Discussion on the models for describing the rate of carbonation All of the models developed in this study are of the descriptive type. The models incorporate both the relative humidity at 10 mm depth from the surface and a measure of the air permeability of the concrete. The relative humidity is meant to give some indication of the service conditions and the API an indication of the concrete quality. In summary, on the basis of the results obtained, the API and RH do not provide a good indication of the likely rate of carbonation. However, the 12 10 8 6 4 2 0 12 10 8 6 4 2 0 12 10 8 6 4 2 0 0 20 40 60 80 100 Initial air permeability index, API: Ln mBar/min × 100 (c) (b) (a) R at e of c ar bo na tio n, R oC : m m /w ee k0 ·5 R at e of c ar bo na tio n, R oC : m m /w ee k0 ·5 R at e of c ar bo na tio n, R oC : m m /w ee k0 ·5 0·50/375 0·57/375 0·63/375 0·70/375 0·50/315 0·57/315 0·63/315 0·70/315 (w/c)/CC CC = 315 kg/m3, R 2 = 1·00 CC = 375 kg/m3, R 2 = 0·95 CC = 315 kg/m3, R 2 = 0·98 CC = 375 kg/m3, R 2 = 0·74 CC = 315 kg/m3, R 2 = 0·77 CC = 375 kg/m3, R 2 = 0·88 Fig. 2. Rate of carbonation versus final air permeability index Variablity: % Coefficient Response Variables included of multiple variable in model Explained Improvement Unexplained determination, R2 Rate of carbonation (RoC) log APIi log APIi+RH10 56?85 59?52 +2?67 43?15 40?48 0?595 Rate of carbonation (RoC) log APIf log APIf+RH10 56?70 64?43 +7?73 43?30 35?57 0?644 Rate of carbonation (RoC) log APIi log APIf+ fcu log APIf+ fcu+RH10 56?85 63?58 78?11 +6?73 +14?53 43?15 36?42 21?89 0?781 Table 6. Development of MLR descriptive models for the rate of carbonation Response variable Explanatory variable Intercept Multiplier R2 Rate of carbonation (RoC) log APIi RH10 2?377 6?041 70?062 0?592 Rate of carbonation (RoC) log APIf RH10 4?264 4?864 70?080 0?644 Rate of carbonation (RoC) log APIi fcu RH10 26?735 70?916 70?183 70?194 0?781 Table 7. Intercepts and multipliers for MLR models developed 324 Structures & Buildings 146 Issue 3 Effect of relative humidity and air permeability Russell et al. inclusion of the API and RH parameters into a model based on the compressive strength improves the accuracy of the model. 4. CONCLUSIONS On the basis of the results obtained from this investigation the following conclusions were reached: (a) The air permeability of the specimens fluctuated during the course of exposure to carbon dioxide. This contradicts the generally held belief that carbonation reduces the permeation properties of the concrete. Further investigation to assess the effects of pore refinement and shrinkage cracking during carbonation is required in order to establish the reasons for the fluctuation in air permeability. (b) The dependence of both air permeability index and rate of carbonation on relative humidity was as expected based on published work. That is, an increase in API with a decrease in RH and RoC reaches a peak between 55 and 65% RH. (c) The difficulty in using API in combination with RH measurements in order to estimate the rate of carbonation was attributed to the susceptibility of API measurements to changes in RH. A test that describes the pore structure or gives an indication of its quality (strength) in combination with RH measurements may be of more use. Furthermore, the results may have been influenced by the fact that an accelerated test was used. (d ) The models based on permeation properties were found to be inadequate to describe the rate of carbonation. On the basis of the results from this investigation air permeability could not be used to represent accurately the rate of carbonation. Age and exposure related inputs might be required to improve these models. REFERENCES 1. BAKKERAKKER R. F. M. The significance of carbonation measure- ments to the corrision risk of reinforcement. 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