炎光光度検出器付きガスクロマトグラフィーによる水,底質中のN-シクロヘキシル-2-ベンゾチアゾールスルフェンアミドと2-(4-モルフォリノチオ)ベンゾチアゾールの微量定量法

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Microdetermination of N-cyclohexyl-2-benzothiazole sulfenamide (CHBSA) and 2-(4-morpholinothio)benzothiazole (MTBT) were developed. One litre of a water sample was extracted with 50 ml each of hexane twice. The extract was dried through an anhydrous sodium sulfate column and concentrated to 1 ml with a Kuderna-Danish (KD) evaporator at reduced pressure. The concentrate was analyzed by gas chromatography with a flame photometric detector (FPDGC). In case of sediment samples, 50 ml of acetonitrile was added to a sample (20 g). The mixture was filtered after vigorous shaking for 10min. The sediment residued on the filter was shaked with 50 ml of acetonitrile again. After filtration of the mixture, all the filtrate were combined. The filtrate was washed with 50 ml of hexane 3 times to remove the interferences. The acetonitrile layer was extracted with 50 ml each of hexane twice after 400 ml of water had been added to the acetonitrile layer. Then hexane layer was treated in the similar way as water samples. When the removal of interferences was inadequate, alumina column chromatography was required. The alumina (neutral, W 200, 1 % water added) column (1cmφ×10cm) was prepared with benzene. The concentrate was placed on the top of the alumina column. CHBSA and MTBT were eluted with benzene/ethyl acetate/triethylamine (16/4/1) after the column had been washed with 20 ml of benzene. The first 7 ml was discarded. The next 20 ml was collected and concentrated to 1 ml with a KD evaporator at reduced pressure. Recoveries of CHBSA and MTBT for a water sample were 92 % and 82 %, and these for a sediment sample were 68 % and 93 %, respectively. Detection limits of CHSBA and MTBT for a water sample (11) were 0.04 ppb and 0.02 ppb, and these for a sediment sample (20 g) were 2 ppb and 1 ppb, respectively. This method was applied to some environmental samples. MTBT was detected at 8 ppb in one river sediment sample, while not detected in other environmental samples. No CHBSA was detected in the all samples examined.
社団法人日本分析化学会の論文
1980-03-05

炎光光度検出器付きガスクロマトグラフィーによる水,底質中のN-シクロヘキシル-2-ベンゾチアゾールスルフェンアミドと2-(4-モルフォリノチオ)ベンゾチアゾールの微量定量法

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