Interlaboratory study of toxaphene analysis in ambient air

An interlaboratory study was conducted for total toxaphene and selected congeners in an extract of ambient air from the southern United States. All participating labs were experienced in toxaphene analysis and used GC-MS techniques. Ten labs reported the concentration of total toxaphene in a technical toxaphene solution, with a 113% average recovery of the target value and 40% relative standard deviation (RSD). Only six of the 10 labs fell within ±30% of the target value, a criterion recommended by good laboratory practice standards. The interlaboratory RSD was 65% for total toxaphene in the air sample extract (lowered to 43% when one outlying lab was omitted). Nine labs reported the concentrations of five toxaphene components (B8-1413, B8-1414+B8-1945, B8-806+B8-809, B8-2229 and B9-1679) with 33–47% RSD for the technical toxaphene unknown and 34–62% for the air sample. The precision was poorer for a sixth component, congener B9-1025, which has a very low response by electron capture negative ion mass spectrometry (ECNI): 59% RSD for the technical toxaphene unknown and 196% for the air sample. Factors contributing to the interlaboratory variability for total toxaphene and single components are discussed, and follow-up studies are required to identify and minimize the causes of variability. Based on the average analysis, B8-1413 was enriched and B8-806+B8-809 was depleted in the air sample relative to the technical toxaphene standard.