Determination of terphenyls in water and sediment by mass fragmentography

Abstract

Trace analyses of terphenyl isomers in water and sediment by mass fragmentography were studied. The isomers in water samples were extracted with n-hexane and the average recovery was approximately 95%. For sediment samples, a continuous extractor was used and the extraction for 4 h was enough to get a good recovery. Silica-gel column chromatography was applied to remove interferences. In this procedure the first n-hexane fraction (16 ml) was discarded and then terphenyls were eluted in a fraction of n-hexane: benzene mixture (20% benzene in n-hexane, 20 ml). Nano grams of terphenyl isomers were sufficiently separated on 3% OV-17 as a liquid phase in GC-FID system. For determination of pico grams of terphenyls by mass fragmentography, mixed columns of 1% OV-101/0.1% Bentone 34 and 2% OV-101/1% BMBT were used. Detection limits of terphenyls in a water sample were 0.007, 0.025 and 0.05 ppb for o-, m- and p-isomer, respectively. Those for a sediment sample were 0.14, 0.5 and 1.0 ppb, respectively. Water and sediment samples taken in the Kitakyushu district were analyzed. No terphenyl isomers were detected in water samples, while, 0.8 to 390 of o-isomer, 1.1 to 210 of m-isomer, and 1.7 to 180 ppb of p-isomer were found in sediment samples.