离子排斥-脉冲安培法检测水相中的痕量甲醇  

Determination of Trace Methanol in Water Phase by Ion Exclusion Chromatography with Pulsed Aerometric

作　　者：徐雪萍[1] 尹雪梅[1] 马浩[1] 姚宝龙[1] 施超欧[1] 

机构地区：[1]华东理工大学分析测试中心,上海200237

出　　处：《实验室研究与探索》2015年第7期40-43,共4页Research and Exploration In Laboratory

摘　　要：针对水相中痕量甲醇的检测,建立了离子排斥-脉冲安培法检测水相中痕量甲醇的方法。实验中比较了TOSOH TSK-GEL Oapak-A和SHODEX Rspak KC-811两种排斥柱检测甲醇的效果,考察了3种不同酸（H2SO4、HCl O4、H3PO4）在不同浓度下作为淋洗液时对甲醇的分离效果,同时进行了杂质分离度测试。结果表明,色谱条件的选择对分析结果的优劣具有显著影响,尤其是色谱柱和流动相的影响最为明显;使用TOSOH TSK-GEL Oapak-A色谱柱,20 mmol/L H2SO4流动相（检出限：3.30 mg/L,加标回收率：97%-107%）或30 mmol/LHCl O4为流动相（检出限0.791 mg/L,加标回收率：99%-102%）具有最佳的分离效果,能满足一般分析检测的要求;离子色谱法还能够有效地避开乙醇的干扰,做到甲醇和乙醇等其他醇类的同步分析检测。该方法简便、准确,有良好重现性,可用于水相中痕量甲醇检测。Determination of traces of methanol in water phase is always a difficult problem. And a new method,named ion exclusion chromatography with pulsed aerometric detection,was developed to determine the traces. Two different Ion exclusion columns（ TOSOH TSK-GEL Oapak-A SHODEX Rspak KC-811） were compared; three different acids（ i.e. H2SO4,HCl O4 and H3PO4） were compared while used as the mobile phase; in addition,tests of resolution between methanol and the other alcohols were made. Results showed that chromatographic condition has a significant impact on the analysis results. Influence of the column and the mobile phase was the most obvious. The optimal result was achieved while using the column of TOSOH TSK-GEL Oapak-A with mobile phase of 20 mmol / L H2SO4 or 30 mmol /LHCl O4,these could meet the requirement of general analysis. Ion exclusion chromatography with pulsed aerometric can also avoid the interference of ethanol effectively. With the advantage of accessibility, high sensitivity and good reproducibility,this method can be used in the determination of traces of methanol in water phase.

关 键 词：离子排斥 脉冲安培 痕量甲醇 

分 类 号：O657.7[理学—分析化学]