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无氘质子(No-D)核磁共振作为一种分析有机溶剂的便捷方法。

No-Deuterium Proton (No-D) NMR as a Convenient Method for Analysis of Organic Solvents.

作者信息

Creary Xavier

机构信息

Department of Chemistry and Biochemistry, University of Notre Dame, Notre Dame, Indiana 46556, United States.

出版信息

J Org Chem. 2023 Aug 18;88(16):11545-11551. doi: 10.1021/acs.joc.3c00807. Epub 2023 Jul 31.

Abstract

NMR spectra of 25 neat solvents have been recorded using No-D (no-deuterium proton) NMR, and water signals are visible in all spectra. Larger amounts of water can be measured by integration. Water can easily be detected at 0.01% (100 ppm), and amounts can be estimated by comparison with solvent C satellite peaks. Molecular sieves efficiently remove water from most solvents such that it cannot be detected by this NMR method. Additives in halogenated solvents and peroxides in ether and THF are also easily detected by No-D NMR.

摘要

已使用无氘质子(No-D)核磁共振记录了25种纯溶剂的核磁共振谱,并且在所有谱图中均可见水信号。通过积分可测量更多量的水。水在0.01%(100 ppm)时即可轻松检测到,其含量可通过与溶剂C卫星峰比较来估算。分子筛可有效去除大多数溶剂中的水,以至于用这种核磁共振方法无法检测到水。卤代溶剂中的添加剂以及醚和四氢呋喃中的过氧化物也可通过无氘质子核磁共振轻松检测到。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/389c/10442915/019ac316655b/jo3c00807_0002.jpg

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