A method is described for the routine, semiquantitative determination of several nonvolatile degradation products of thetriazine herbicides atrazine, cyanazine, and cyprazine in soil samples. The procedure involves the extraction of soil samples with aqueous methanol and with a methanol-hydrochloric acid mixture and the partition of the chloro-s-triazines into ethyl acetate. The aqueous extract which contained the hydroxy-s-triazines was cleaned up by use of a column of cationic exchange resin; the hydroxys-triazines were converted to their methoxy derivatives by methylation with diazomethane. Gas chromatographic analysis was carried out by use of a Hall electrolytic conductivity detector (nitrogen mode). Recovery studies indicated that hydroxy-atrazine [2-hydroxy-4-(ethylamino)-6-(isopropylamino)-s-triazine], hydroxy-cyprazine [2-hydroxy-4-(cyclopropylamino)-6-(isopropylamino)-s-triazine] , and cyanazine I11 [2-chloro-4-(l-carboxy-l-methylethylamino)-6-(ethylamino)-s-triazine] could be extracted relatively more efficiently from fortified (37.8-790.0 pg/kg) soil samples than could N-dealkylated hydroxy-s-triazines. Overall recoveries of the hydroxy-s-triazines from soil were reduced by the poor efficiency of methylation to the corresponding methoxy-s-triazines.The hydroxy-s-triazines are the major degradation products of the chloro-s-triazine herbicides in soil. The determination of the hydroxy degradation products is made difficult by their low solubility in nonacid or nonalkaline solvent systems (Ward and Weber, 1968), strong adsorption to organic matter and clay surfaces of soils (Weber, 1972), and low efficiency of derivatization for gas chromatographic analysis (Cochrane, 1975).