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A method for the detection of trace amounts of nucleophilic functions in aqueous media

机译:检测水性介质中痕量亲核功能的方法

摘要

A new process for the detection of trace amounts of pollutants with nucleophilic properties such as thiols, phenols, oximes and amines using isocyanate reactants. Isocyanates are used to react with the nucleophilic functions in aqueous solution to form carbamates, thiocarbamates or urea derivatives which can then be analyzed by HPLC. The procedure comprises three stages:- -addition of the isocyanate, or precursor, to a basic aqueous solution containing the nucleophilic agent(s); - maintenance of the solution, for a few mins. to 2 hs, at a temperature less than 100 deg C; -analysis of the carbamate, thiocarbamate or urea obtained. The isocyanate can be formed in situ from a nitrosourea of general formula R1NHCON(NO)R2 (I). An Independent claim is also included for a test kit which comprises: (1) A quantity of N-2,4 dintrobenzoyl N1(N-2-chloroethyl)-N-nitroso)carbamoyl-1,4-diamonobutane, as a pure 99% powder; (2) A solution of 99% triethylamine; (3) A standard pure histamine derivative with NMR and UV spectra; and (4) solutions of the histamine standard in acetonitrile for calibration of the system.
机译:一种使用异氰酸酯反应物检测痕量具有亲核性质的污染物的新方法,例如硫醇,酚,肟和胺。异氰酸酯用于与水溶液中的亲核功能反应形成氨基甲酸酯,硫代氨基甲酸酯或脲衍生物,然后可以通过HPLC分析。该过程包括三个阶段:-将异氰酸酯或前体加到含有亲核试剂的碱性水溶液中; -维持解决方案几分钟。在小于100摄氏度的温度下持续2个小时; -分析所获得的氨基甲酸酯,硫代氨基甲酸酯或尿素。异氰酸酯可以由通式R1NHCON(NO)R2(I)的亚硝基脲原位形成。一个测试套件还包括一个独立的权利要求,该套件包括:(1)一定量的N-2,4二硝基苯甲酰基N 1(N-2-氯乙基)-N-亚硝基)氨基甲酰基-1,4-二单丁烷纯度为99%的粉末; (2)99%三乙胺溶液; (3)具有NMR和UV光谱的标准纯组胺衍生物; (4)组胺标准品在乙腈中的溶液,用于系统校准。

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