检测有机汞的标准物质氯化甲基汞的合成条件

The synthetic condition of methylmercuric chloride.

选择两步法合成ＣＨ３ＨｇＣｌ，即ＣＨ３Ｉ与Ｈｇ通过光化学反应制得ＣＨ３ＨｇＩ，再使用ＡｇＣｌ将ＣＨ３ＨｇＩ转化为ＣＨ３ＨｇＣｌ。以白炽灯作为光反应的光源；选用无水乙醇或丙酮或乙醚作为转化反应的溶剂，在进行转化反应操作时，必须加以搅拌；同时，确定在相应的溶剂中重结晶３次及操作条件。揭示了ＡｇＣｌ转化ＣＨ３ＨｇＩ的反应为固液异相反应，并确定了相应的溶剂。合成ＣＨ３ＨｇＣｌ的熔点为１６９～１７０℃，元素分析的结果为Ｃ：４．８９％、Ｈ：１．１１％，与文献值一致。使用合成的ＣＨ３ＨｇＣｌ配成标准溶液。

The two steps method was chosen as a convenient way to synthesize methylmercuric chloride.First,methylmercuric iodide was prepared by photochemical reaction of iodomethane with mercury;then,the methylmercuric iodide was transformed to methylmercuric chloride by reacting with silver chloride.Under the circumstance that incandescent burner is used as light source,absolute ehtyl alcohol,or acetone,or ether is used as solvent in the transforming reaction,adopting the new conditions such as stirring and recrystallizing for 3 times,the super pure methylmercuric chloride is prepared through solid liquid heterogeneous reaction.The melting point of product is 169～170℃.The results of element analysis are C:4.89% and H:1.11%.The mercury content of standard sample determined accords with the standard value using the home made methylmercuric chloride to make up the standard solution.