离子排斥-脉冲安培法检测水相中的痕量甲醇

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...

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Published in实验室研究与探索 Vol. 34; no. 7; pp. 40 - 43
Main Author 徐雪萍 尹雪梅 马浩 姚宝龙 施超欧
Format Journal Article
LanguageChinese
Published 华东理工大学分析测试中心,上海,200237 2015
Subjects
痕量甲醇
离子排斥
脉冲安培
离子排斥
ion exclusion
pulsed aerometric
痕量甲醇
trace methanol
脉冲安培
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ISSN1006-7167

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Summary: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。
Bibliography:ion exclusion; pulsed aerometric; trace methanol
XU Xue-ping,YIN Xue-mei,MA Hao,YAO Bao-long,SHI Chao-ou （Instrument Analysis Center, East China University of Science and Technology, Shanghai 200237, China）
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
ISSN:1006-7167