Development of an accurate pH measurement methodology for the pore fluids of low pH cementitious materials

Abstract

The main objective of this project has been the development of an agreed set of protocols for the pH measurement of the pore fluid of a low pH cementitious material. Three protocols have been developed (Chapter 2), a reference method, based on pore fluid expression (PFE), and two routine methods with and without filtering, based on Ex Situ Leaching (ESL) procedures. Templates have been designed on which to record details of the pH measurement for the reference (PFE) method (Appendix C) and the routine (ESL) methods without and with filtering (Appendix D). Preliminary protocols were based on a broad review of the literature (Appendix A) and refined through a series of test experiments of the more critical parameters (Appendix B). After definition of the preliminary protocols, two phases of interlaboratory tests were performed. The first phase (Chapter 3) used the same low pH cement paste and enabled the nine participating laboratories to use, become familiar with and to identify any problems/uncertainties in the preliminary protocols. The reported pH values were subjected to a statistical analysis of the (within laboratory) repeatability and (between-laboratory) reproducibility and so provided a reliability test of the preliminary protocols. The second phase (Chapter 4) of interlaboratory tests used four different candidate low pH cementitious materials in the same nine laboratories, which allowed testing, validation and comparison of the reported pH values, which were obtained using the final protocols for the reference (PFE) and routine (ESL) methods by statistical analysis. The proposed final protocols (Chapter 2) have resulted in the reported pH values having low deviation and high reproducibility and repeatability. This will allow confidence in the pH value when selecting a candidate low pH cementitious material to be used in the engineered component of a high-level nuclear waste repository.