A simple complexometric method, with ethylenediaminetetraacetic acid as titrant, was developed for the determination of calcium and magnesium in a single aliquot of solution at pH =lo. The method involves determination of calcium at pH =lo, with use of a mixed indicator, after masking magnesium with acetylacetone at room temperature, followed by de-masking of magnesium at 90°C and direct titration of magnesium at the same pH. The method was standardized against synthetic solutions and applied t o various calcareous materials, and the results were compared with those obtained by a standard method.
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