GC方法快速分析N-甲基二乙醇胺脱碳剂

Rapid Analysis of Methyldiethanolamine Decarburizing Agent by Gas Chromatography

建立了一种同时测定N-甲基二乙醇胺(MDEA)脱碳剂中MDEA和哌嗪(PIP)含量的毛细管气相色谱法,并采用GC-MS对实验结果进行了验证,同时考察了不同色谱柱、溶剂、脱水剂对测定结果的影响。实验结果表明,使用Rtx-5毛细管色谱柱、氢火焰离子化检测器,以甲醇为溶剂,试样不经脱水处理,采用外标法定量,即可同时测定MDEA脱碳剂中MDEA和PIP的含量。测定结果为:MDEA脱碳剂原液中MDEA含量99.0%～99.3%(w),PIP含量10.1%～10.4%(w);MDEA脱碳剂工作液中MDEA含量为41.4%～42.9%(w),PIP含量为7.3%～8.2%(w);MDEA回收率为96.43%～99.98%,PIP回收率为96.64%～102.02%;MDEA检出限为0.21μg/L,PIP检出限为0.29μg/L。该方法具有操作简便、分析速度快、准确、分离效果好、精密度高等特点,能满足工厂生产质检过程中的分析要求。

A rapid analysis method for the determination of methyldiethanolamine（MDEA） and piperazine（PIP） in MDEA decarburizing solution was established based on capillary gas chromatography. The experimental results were verified by GC-MS. The effects of capillary columns, solvents and dehydrating agents on the analysis were investigated. The optimized chromatographic conditions were gotten as follows Rtx-5 as chromatographic column, FID as detector, methanol as solvent and no dehydrating agent. The results show that the contents of MDEA and PIP are between 99.0%-99.3%（w） and between 10.1%- 10.4%（w） in original MDEA solution respectively, and that the contents of MDEA and PIP are between 41.4%-42.9%（w） and between 7.3%-8.2%（w） in MDEA working solution respectively. The recoveries and detection limits are 96.43%-99.98% and 0.21 gg/L for MDEA, 96.64%-102.02% and 0.29μg/L for PIP, respectively.