Using a gas-chromatographic method, we examined the effects of phosphate concentration, added calcium chloride, and pH on precipitation of oxalate from urine. All three factors are important, but the pH of precipitation is particularly so, especially in the presence of even normal concentrations of ascorbic acid. At pH 8, increases in measured oxalate ranged from 20% at an ascorbic acid concentration of 1 mmol/L to more than 300% at 15 mmol/L. Ascorbic acid is rapidly converted to oxalate at alkaline pH. We also investigated the stability of both untreated and acidified urine containing ascorbic acid during storage for up to one month at -70, -20, and 4 degrees C, and room temperature. After one month, untreated collections were stable at -70 degrees C and acidified collections at -20 and -70 degrees C. We recommend conditions for assay and storage of urine specimens that are to be assayed for oxalate under which positive interference by ascorbic acid is minimized.