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脂肪酸乙氧基化物在超临界甲醇中进行酯交换反应,然后采用气相色谱 - 质谱联用仪测定衍生的甲酯,以鉴定引发剂。

Transesterification of fatty acid ethoxylates in supercritical methanol, then gas chromatography-mass spectrometric determination of the derived methyl esters, for identification of the initiators.

作者信息

Socher G, Nussbaum R, Rissler K, Lankmayr E

机构信息

CarboGen Laboratories (Neuland) AG, Hunzenschwil, Switzerland.

出版信息

Fresenius J Anal Chem. 2001 Oct;371(3):369-75. doi: 10.1007/s002160100985.

DOI:10.1007/s002160100985
PMID:11688652
Abstract

Unknown fatty acid ethoxylate samples have been transesterified in supercritical methanol, using a loop made of a stainless-steel tubing as the reactor vessel. The initiator acids, now present as the corresponding methyl esters, were determined by gas chromatography-mass spectrometry (GC-MS). Quantitative transesterification is achieved by heating a solution of the ethoxylate sample in methanol at 280 degrees C for 10 min under pressure. The influence of reaction time, temperature, and presence of a Lewis acid catalyst has been investigated. The method of transesterification was optimized in respect of low cost, short reaction time, and availability to laboratories with standard analytical equipment.

摘要

未知的脂肪酸乙氧基化物样品在超临界甲醇中进行了酯交换反应,使用不锈钢管制成的回路作为反应容器。引发剂酸现在以相应的甲酯形式存在,通过气相色谱-质谱联用仪(GC-MS)进行测定。通过在280℃下于压力下将乙氧基化物样品在甲醇中的溶液加热10分钟来实现定量酯交换反应。研究了反应时间、温度和路易斯酸催化剂的存在的影响。在低成本、短反应时间以及具有标准分析设备的实验室可操作性方面对酯交换方法进行了优化。

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