使用基于N-甲基甲酰胺的卡尔费休试剂对双（草酸根）硼酸锂中的水进行无干扰库仑滴定。

Interference-free coulometric titration of water in lithium bis(oxalato)borate using Karl Fischer reagents based on N-methylformamide.

作者信息

Larsson William, Panitz Jan-Christoph, Cedergren Anders

机构信息

Department of Chemistry, Analytical Chemistry, Umeå University, Umeå, Sweden.

出版信息

Talanta. 2006 Mar 15;69(1):276-80. doi: 10.1016/j.talanta.2005.10.004. Epub 2005 Nov 9.

DOI:10.1016/j.talanta.2005.10.004

PMID:18970565

Abstract

A non-alcoholic coulometric reagent based on N-methylformamide (NMF) was shown to eliminate the severe interference effect caused by the alcohol component of the conventional Karl Fischer (KF) reagent on the battery electrolyte lithium bis(oxalato)borate (LiBOB). For sample amounts up to 240 microg of water, the stoichiometry of the KF reaction deviated only slightly from the ideal 1:1 ratio for the best reagent composition. Both solid and dissolved (in acetonitrile, tetrahydrofuran (THF), and ethylene carbonate/ethyl methyl carbonate) LiBOB were titrated successfully using a Metrohm 756 KF Coulometer with a diaphragm cell. The detection limit was estimated to be 0.5-1 microg of water using 100ml of reagent in this system.

摘要

一种基于N-甲基甲酰胺（NMF）的非酒精库仑试剂被证明可以消除传统卡尔费休（KF）试剂中的酒精成分对电池电解质双草酸硼酸锂（LiBOB）造成的严重干扰效应。对于高达240微克水的样品量，在最佳试剂组成下，KF反应的化学计量比仅略微偏离理想的1:1比例。使用配备隔膜池的万通756 KF库仑仪成功滴定了固态和溶解态（在乙腈、四氢呋喃（THF）以及碳酸亚乙酯/碳酸甲乙酯中）的LiBOB。在该系统中，使用100毫升试剂时，检测限估计为0.5 - 1微克水。