工业甲醇中微量三甲胺的气相色谱测定  

Determination of the Trace Trimethylamine in Industrial Methanol by Gas Chromatography

作　　者：姜新其 赵建斌[2] 

机构地区：[1]大唐内蒙古多伦煤化工有限责任公司,内蒙古多伦027300 [2]国家煤及煤化工产品质量监督检验中心,山西太原030012

出　　处：《煤化工》2015年第2期56-59,共4页Coal Chemical Industry

摘　　要：介绍了一种分析甲醇中微量三甲胺的方法,通过试验,确定出色谱操作条件：柱温120℃,检测器温度250℃,进样口温度150℃,载气（氦气）流量4.0 mL/min,尾吹气（氮气）流量10 mL/min,氢气流量2.0mL/min,空气流量140mL/min,热离子源加热电流1 pA,进样量2μL,分流比1∶20.在选定的色谱操作条件下,最低检出限为10×10^-9,线性范围为0～375×10^-9,相对标准偏差在5.3％～9.2％,回收率在95.2％～104.0％.生产运行表明,采用该法对生产的甲醇中三甲胺进行监控分析,MTP催化剂未发生失活,所生产的丙烯产品质量稳定.A method for analyzing trace trimethylamine in methanol was introduced and the operation condition of the gas chromatography was determined through the experiment, i.e. the column temperature was 120 ~C, the detector temperature was 250 ~C, the inlet temperature was 150 ~C, the carrier gas flow rate was 4.0 mUmin, the make-up gas flow rate was 10 mL/ min, the hydrogen flow rate was 2.0 mL/min, the air flow rate was 140 mL/min, the hot ion source heating current was 1 pA, the injection sample amount was 2 μL and the split ratio was 1：20. According to the selected gas chromatographic conditions, the lowest detection limit was 10×10^-9, the linear range was between 0-375×10^-9, the precision was between 5.3%-9.2% and the recovery rate was between 95.2%-104.0%. Production operation indicated that through monitoring and analyzing the TMA in the methanol produced, the MTP catalyst did not lose its activity, and the propylene produced was stable in its quality.

关 键 词：工业甲醇 三甲胺 气相色谱法 催化剂 失活 

分 类 号：O657.71[理学—分析化学] TQ223.121[理学—化学]