Evaluation of Procedures for Urinary Calcium.

In a comparative study of urinary calcium methods, many of the recently proposed procedures proved either impractical or invalidin our hands. A preliminary isolation of the calcium as the oxalate, followed by perchloric acid oxidation of the oxalate seemed to be the simplest procedure whereby urinary calcium could be put in a state suitable for chelometric titration. The isolated calcium could also be titrated with considerable precision and accuracy by a modified procedure with a derivative automatic titrator which is available commercially. It was suggested from our observations that too little attention has been directed towards the problems imposed by the occurrence of calcium precipitates in urine. An untreated 24-hr. urine specimen is not suitable for direct analysis of calcium by chelometric titration, by colorimetric analysis, by emission flame photometry, or by atomic absorption flame photometry because these methods do not give a true measure of the calcium in the precipitate. Boiling for 5 mm. with 1 part concentrated nitric acid to 25 parts urine proved a suitable means for completely dissolving the calcium precipitate.