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each image analysed by the evaluator was given a score of zero, one or two based on the strength of the optical images. all sub-specimens were evaluated by each evaluator. these scores were recorded and then used by the evaluator to calculate an aggregate rank for each lab. a maximum of five labs from each group were considered, with the top performing lab receiving 5 points and the fifth lab receiving one point. finally, the aggregate ranks for the six labs were combined to give an aggregate score for each evaluation method within the groups. the weightings for each score were derived from the original discussion of the method’s reliability (as in figs. 4 and 5 ): five points for lab performance, a score of 0.5 for repeatability, 0.3 for reproducibility, and a score of 0.2 for the availability of an external standard. the overall aggregate score for each method was calculated by combining the lab performance scores and the aggregate scores (average of each lab’s five laboratory aggregate scores).
two wet-set concretes were used for calibration of fluorescence intensity against w/c ratio. these calibration mixes were composed of 70% cement and 30% sand by weight (table 3) and were hydrated at a range of w/c ratios (0.3, 0.36, 0.42).
one wet-set concrete was used for calibration of apparent optical features against w/c ratio. it was composed of (by mass) 71% cement and 29% sand by weight (table 4) and was hydrated at a range of w/c ratios (0.3, 0.36, 0.42, 0.45) the other wet-set concrete was used to validate the methodology for the concrete samples. it was composed of (by mass) 70% cement, 10% limestone and 20% aggregate and was hydrated at a range of w/c ratios (0.45).
the results of the current study suggest that scanning electron microscopy (sem) using backscattered electron (bse) imaging and energy dispersive spectroscopy (eds) are both non-destructive and suitable for quantifying the w/c ratio in cementitious pastes. the use of backscattered electron imaging (bse) allows the acquisition of highly magnified and three-dimensional images that can be used to quantitatively describe the cement paste microstructure, in particular the distribution of fine carbonate grains. identification of individual grains and their spatial distribution can also be used to evaluate and quantify the cement phase microstructure in concrete mixes. although the resolution is relatively poor compared with electron microscopy, the ability to quantify the distribution of individual cementitious particles using sem-bse has the potential to deliver a semi-quantitative estimate of the w/c ratio, at least at lower w/c ratios. further work is needed to evaluate the viability of using bse-eds for quantitative measurements, and certainly sem-bse can be considered as an alternative non-destructive technique for estimating the w/c ratio in concrete, however, the results are at least as accurate as the physicochemical technique. the mip measurements were only applied to the flexure results and not, for example, the uniaxial or biaxial compressive or shrinkage results as these measures are only sensitive to the outer surface of the specimen, that is, the cement paste above the surface of the hardened cement paste. the investigation presented in this paper highlights that morphological analysis of core specimens recovered from concretes can be a reliable method of estimating w/c ratio. the examination of the pits and channels formed on the outer surface of concrete, which is generally considered to be more representative of the bulk material, shows that it does not provide any significant additional information over that which is measured in the bulk. in addition, mip analysis of pit and channel dimensions is an equally effective method for estimating w/c ratios in concrete, and is an additional technique that can be used during the observation of fresh concretes, alongside the traditional methods of visual inspection and penetration testing, to ensure the quality of concrete in cases of alleged deficiency (fig. 4). because the present investigation focused on the inner core of concrete, it is evident that this technique may have limitations with respect to the assessment of surface-water-vapour systems where secondary effects such as w/c bleeding are prevalent. however, the investigation of concrete to a depth of at least 3mm (from this study, for example) and studying a subsample of that core material will form an accurate estimate of the w/c ratio. it is generally accepted that when core samples of cement paste are taken from a concrete mix during its immersion in water, it is very difficult to obtain an accurate estimate of the w/c ratio, either from visual inspection or the measurements of porosity. this is because, particularly as the w/c ratio increases, the difference between the inside of the concrete and the outside becomes very small, and it becomes more difficult to assign a material sample to either the immersed or non-immersed portion of the mixture. 5ec8ef588b
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