The chloric acid method is most commonly used to obtain accurate and reproducible measurements of iodine and remove interfering substances. Unfortunately chloric acid is a potential hazard, requiring an explosion-proof hood, among other precautions. We have developed a simple, convenient, and economic method for measuring urinary iodine by using 1 mol/L ammonium persulfate, a nonexplosive, nonhazardous chemical, as the oxidizing reagent. The oxidation procedure can be completed in 30 min at a temperature of 91-95 degrees C. The iodine in the urine is then measured by a modification of the traditional colorimetric method of Sandell and Kolthoff. Urine samples (110) collected from a mixed population of healthy males and females, ranging in age from 6 to 79 years and living in the US, were analyzed for urine iodine content by two methods: the proposed ammonium persulfate method and the chloric acid method. The ammonium persulfate method has an intraassay CV of 9.1% at 0.42 +/- 0.04 micromol/L (mean +/- SD), 7.8% at 1.46 +/- 0.11 micromol/L, and 4.0% at 3.54 +/- 0.14 micromol/L. The interassay CV is 10.2% at 0.46 +/- 0.05 micromol/L, and 7.9% at 3.27 +/- 0.26 micromol/L. Recovery of iodine added to urine in vitro was 107%, 94%, and 97% for 0.42 micromol/L, 0.77 micromol/L and 3.64 micromol/L, respectively. The lower limit of detectability was 0.0034 microgram of iodine. Values for iodine in 110 urines measured by the reference chloric acid method ranged from 0.06 to 8.03 micromol/L and by the ammonium persulfate method from 0.05 to 7.4 micromol/L. The persulfate method (y) correlated extremely closely with the reference chloric acid method (x) by the Pearson correlation (y = 0.923x + 0.810 micromol/L, and r = 0.994, Sy/x = 1.841).