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An iterative Rietveld–PONKCS (partial or no known crystal structure) technique has been developed for precise and accurate determination of the weight percentages of predominantly amorphous supplementary cementitious materials (SCMs) contained in Portland cement–SCM blends. This technique involves the iterative refinement of the SCM amorphous phase (SCMAP) content, with the separation of the refinement of the SCMAP shape parameters from background refinement. The technique also includes an internal and external standard refinement of both the calibration SCM and the cement–SCM blend. This approach enables the separation of the contributions of the SCMs and the cement to the amorphous content of the cement–SCM blend. The technique has been successfully applied to binary systems of cement–slag and cement–fly ash, and ternary blends of cement–fly ash–slag, over a wide range of cement replacement levels. In the ternary systems, the proposed technique was successfully able to separate the individual amorphous contributions of slag and fly ash to the total amorphous content of the system. The approach was also implemented on a pair of commercially available binary blended cements containing 30% slag and 30% fly ash, respectively.

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