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本文应用自行设计的JTY—lA型流动注射多功能溶液自动处理系统,研究了流动注射在线液—液萃取及在线氢化物发生与原子荧光光谱法的联用技术,设计了流动注射在线液—液萃取及在线氢化物发生的流路和操作程序,选择了最佳的仪器工作条件和流路参数,改进了气液分相器。本文选用KI+KNO_3(稀)+(NH_2)_2CS/TBP(少量MIBK)为萃取体系,把Hg萃取到有机相中,用冰乙酸调节酸度,用NaBH_4—DMF溶液还原汞,最后进行AFS测定。实验结果表明,该法流路及程序设计合理,具有操作简单、快速,试剂用量少,环境污染小,分析成本低,基本上无干扰等特点。通过对国家一级标样GSD—4和GSD—6的分析验证,结果令人满意。
In this paper, a self-designed JTY-1A flow injection multi-purpose solution automatic processing system was designed. The combination of flow-injection on-line liquid-liquid extraction and on-line hydride generation with atomic fluorescence spectrometry was studied. Extraction and on-line hydride flow path and operating procedures, the choice of the best instrument operating conditions and flow parameters, improved gas-liquid phase separator. In this paper, Hg was extracted into organic phase using KI + KNO 3 (dilute) + (NH 2) 2CS / TBP (a few MIBK) as extraction system, acidity was adjusted by glacial acetic acid, mercury was reduced by NaBH 4-DMF solution, and finally AFS was performed. The experimental results show that the method has the advantages of simple operation, fast operation, less reagent consumption, less environmental pollution, lower analysis cost and basically no interference. Through the analysis and verification of the national standard GSD-4 and GSD-6, the results are satisfactory.