A method for the determination of Bidrin and Azodrin, a major metabolite, and eight other metabolites of these two insecticides is described. The organophosphorus compounds are analyzed by a modified version of thin-layer chromatography in which the chromatogram is scraped to make narrow straight strips. Two adsorbents, silica gel G and silica gel H, are employed for preparing the chromatographic plates. Twenty-seven solvent systems are tested, and two chromogenic reagents are employed Good separations are obtained for most compounds; however, no single solvent system can separate all of the organophosphorus compounds. The practical minimum detectable amount is 2 μg. when the chromatogram is treated with bromine vapor and silver nitrate solution; this is lowered to 1 μg. or less when the chromatogram is treated with 4-(p-nitrobenzyl)-pyridine and tetraethylenepentamine solutions. Thirty-eight dyes are included in this study. © 1969, American Chemical Society. All rights reserved.