2,4-dichlorophenyl 4-nitrophenyl ether および 2,4,6-trichlorophenyl 4-nitrophenyl etherの微量定量法 : 乾式薄層クロマトグラフィーとアゾ色素生成反応による除草剤の微量定量法(第2報)

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A spectrophotometric method for determination of 2, 4-dichlorophenyl-4-nitrophenyl ether (NIP) and 2, 4, 6-trichlorophenyl-4-nitrophenyl ether (CNP) was investigated and the recommended procedure for the analysis of soil sample was presented. A test sample containing 10100 μg of NIP or CNP was extracted with methylene chloride by batch procedure. One ml of n-hexane was added to the extract and the solution was concentrated to 1 ml on a water bath at about 50°C. The condensed solution was applied to a loose-layer plate with 1 mm thickness of alumina powder. The plate was developed using n-hexane-acetone (9 : 1) as a solvent. After drying for 15 minutes the band of NIP or CNP was scraped out, collected into a glass filter and eluted with ether. After evaporation of ether, NIP or CNP obtained was dissolved in acidic ethanol and reduced with zinc dust by refluxing for 10 minutes. The resulting amino compound was diazotized with sodium nitrite solution containing potassium bromide, and the excess of nitrite was decomposed with ammonium sulfamate. The diazonium compound formed. was coupled with N-(1-naphthyl) ethylenediamine dihydrochloride and the resulting magenta color was subjected to the spectrophotometric determination. The results of recovery test were shown in Tables IIIIV.
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