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气相色谱-质谱选择离子监测法测定有机溶剂中的痕量水分。

Determination of trace water contents of organic solvents by gas chromatography-mass spectrometry-selected ion monitoring.

机构信息

School of Applied Chemistry and Biotechnology, Shenzhen Polytechnic, Shenzhen 518055, China.

Shenzhen Consumer Testing Technology Co., Ltd., Shenzhen 518055, China.

出版信息

J Chromatogr A. 2018 Oct 5;1570:109-115. doi: 10.1016/j.chroma.2018.07.068. Epub 2018 Jul 27.

DOI:10.1016/j.chroma.2018.07.068
PMID:30098730
Abstract

This paper describes the development of a novel gas chromatography-mass spectrometry-selected ion monitoring (GC/MS-SIM) method for the determination of trace water contents of organic solvents, using the characteristic m/z 18, m/z 17, and m/z 16 ions of HO as the qualitative ion and the m/z 18 ion as the quantifier ion. The accuracy and precision of this method were validated. An excellent linear correlation was obtained for trace water contents between 0 and 0.5217 wt%, with a correlation coefficient (R) of 0.9999, in addition to spike recoveries of 82.6-112.6%, and relative standard deviations (n = 6) of 0.4-7.2%. The limit of detection (S/N = 3) and limit of quantitation (S/N = 10) for the trace water contents of organic solvents were 0.0005% wt% and 0.0016% wt%, respectively.The analytical results confirmed that this method was useful for determining the trace water contents of organic solvents, because it has a low detection limit and wide linear range. It requires only small amounts of the samples and enables sample batch analysis. It is very environmentally friendly and saves reagents.

摘要

本文描述了一种新型的气相色谱-质谱选择离子监测(GC/MS-SIM)方法,用于测定有机溶剂中痕量水分,以 HO 的特征 m/z 18、m/z 17 和 m/z 16 离子作为定性离子,m/z 18 离子作为定量离子。该方法的准确性和精密度得到了验证。在痕量水含量为 0 至 0.5217wt%的范围内,得到了极好的线性相关性,相关系数(R)为 0.9999,加标回收率为 82.6-112.6%,相对标准偏差(n=6)为 0.4-7.2%。该方法对有机溶剂痕量水分的检测限(S/N=3)和定量限(S/N=10)分别为 0.0005wt%和 0.0016wt%。分析结果证实,该方法对于测定有机溶剂中的痕量水分非常有用,因为它具有较低的检测限和较宽的线性范围。它只需要少量的样品,并且能够进行样品批量分析。它非常环保,节省试剂。

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