An analytical method for the determination of 1251 and lZsI in environmental samples is described. Samples are treated to convert all iodine to a common oxidation state prior to chemical separation and purification. The iodine is reduced to I,; then the elemental iodine is extracted into CC14, back extracted into water and precipitated as PdI,. The chemical recovery is determined gravimetrically. The PdI, precipitate is counted on an intrinsicgermanium detector, and the intensities of the K, X-rays from l%I and 12gI are measured.A matrix solution is used to correct for the interference of one spectral region to the other. If 1311 is present, as indicated by an independent measurement, a correction for l3lI interference is also made.