A procedure is described for the determination of51Cr(III) in51Cr(VI) samples having a51Cr(VI) to51Cr(III) ratio of 105, by means of a single zinc hydroxide coprecipitation at apH of ca. 13. Acceptable precision (standard deviation of 10–15%) is possible with solid51Cr(VI) samples containing 10 ppm of51Cr as51Cr(III).