气相色谱—质谱法测定蒸馏出的混合物中硼酸三甲酯

Determination of Trimethyl Borate in Mixture after Distillation by Gas Chromatography-Mass Spectrometry

中文关键词:  气相色谱-质谱法  硼酸三甲酯  混合物

英文关键词:Gas chromatography-mass spectrometry（GC-MS）  Trimethyl borate  Mixture

中文摘要:

      硼酸三甲酯是合成储氢材料硼氢化钠的重要原料,以硼酸、甲醇为原料合成硼酸三甲酯是目前硼酸三甲酯合成的重要方法之一。提供了一种测定硼酸、甲醇合成硼酸三甲酯蒸馏混合物中硼酸三甲酯成分、含量的测定方法,即气相色谱一质谱法（GC-MS）。该方法简单、快捷、准确。确定了优化的GC-MS测定条件,适合不同合成条件下蒸馏后混合物中硼酸三甲酯的定性、定量。测定结果表明,该方法对同一条件下合成混合物中硼酸三甲酯做测定分析,加标回收率在91.8%-100.5%,相对标准偏差1.9%-4.1%,检出限3.64 mg/mL。通过对16组不同工艺合成条件下混合物中硼酸三甲酯的测定分析,该方法重复性较好,较为稳定,对硼酸三甲酯检测分析具有重要意义。

英文摘要:

      Trimethyl borate is an important raw material for the synthesis of sodium borohydride.The method of synthesis of trimethyl borate by boric acid and methanol as raw material is currently one of the important methods for the production of trimethyl borate.A simple and accurate method was developed for the determination of the content of trimethyl borate of the synthesis distillation mixture by boric acid and methanol,the method is Gas Chromatography- Mass Spectrometry（GC- MS）.This method was suitable for qualitative and quantitative determination of the trimethyl borate of the trimethyl borate distillation mixture in different synthesis conditions.The recovery rate of this method was in the range of 91.8%-100.5%.The relative standard deviation was 1.9%-4.1%.The lowest detective content（S/N 〉10） was3.64 mg/mL.With the results of 16 group determination test of trimethyl borate under content in different synthesis conditions,the determination method repeatability is good and relatively stable.This method for trimethyl borate analysis is of great significance.