A gas-liquid chromatographic (GLC) method for determining Bolstar insecticide in liquid technical material and emulsifiable concentrate formulations was collaboratively studied using Youden’s matched pair scheme. Three matched sample pairs were analyzed by 21 laboratories using integrator area measurements and/or peak height measurements. Samples of a technical material containing about 78% active ingredient, a commercial 6 lb/ gal. emulsifiable concentrate containing about 64% active ingredient, and a synthetic emulsifiable concentrate containing about 64% active ingredient were dissolved in a measured amount of internal standard solution, tetracosane in toluene, and were subjected to gas-liquid chromatography on a column of 1.5% SE-30 + 1.5% OV-210. Bolstar was detected using flame ionization. The mean coefficient of variation by integrator area measurement for the 6 samples was 1.22%, and the mean coefficient of variation by peak height measurement for the 6 samples was 1.65%. The method was adopted as official first action.
The determination of ethyl parathion in Penncap-E insecticide was studied collaboratively by 14 laboratories. The assay of methyl parathion in Penncap-M insecticide was studied by 8 laboratories. The original method which was adopted official first action for methyl parathion specified dimethoate, which is currently classified as a suspected carcinogen, as the internal standard. The current collaborative efforts were conducted as a supplemental study to evaluate the performance of the new internal standard, bis-2-methoxyethyl phthalate, and to test the gas-liquid chromatographic method for microencapsulated ethyl parathion (internal standard, dibutyl phthalate). The method uses essentially the same grinding and extraction with acetonitrile as the original study. At the 20% methyl parathion level, the standard deviation within laboratories was 0.186%, and among laboratories, 0.737%. Two formulations of ethyl parathion at approximately 16 and 24% were analyzed in replicate on 2 days by the same analyst, and provided excellent agreement within laboratories as well as among laboratories. The standard deviation (pooled) within laboratories was 0.284% and among laboratories, 0.518%. The method has been adopted as official first action.
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