Preprint Article Version 1 Preserved in Portico This version is not peer-reviewed

Defanging Chloroform – Mitigation of Deuterated Chloroform Decomposition to Stabilise Susceptible NMR Samples

Jan Teipel
* ,
Vera Gottstein
ORCID logo ,
Eva Hölzle
,
Katja Kaltenbach
,
Dirk W. Lachenmeier
ORCID logo ,
Thomas Kuballa
Version 1 : Received: 30 June 2022 / Approved: 5 July 2022 / Online: 5 July 2022 (03:53:09 CEST)

A peer-reviewed article of this Preprint also exists.

Teipel, J.; Gottstein, V.; Hölzle, E.; Kaltenbach, K.; Lachenmeier, D.W.; Kuballa, T. An Easy and Reliable Method for the Mitigation of Deuterated Chloroform Decomposition to Stabilise Susceptible NMR Samples. Chemistry 2022, 4, 776-785. Teipel, J.; Gottstein, V.; Hölzle, E.; Kaltenbach, K.; Lachenmeier, D.W.; Kuballa, T. An Easy and Reliable Method for the Mitigation of Deuterated Chloroform Decomposition to Stabilise Susceptible NMR Samples. Chemistry 2022, 4, 776-785.

Abstract

Highly reactive decomposition products of (deuterated) chloroform can deteriorate samples dissolved in this commonly used NMR solvent. For sensitive samples (such as peptides, unsaturated fatty acids, vitamins), this can lead to abnormal NMR spectra (e.g. signal shifts depending on pH, attenuation of signals over time due to chemical changes of analytes, new signals from reaction products). Such irreproducibly influenced spectra are especially problematic for non-targeted analysis methods. To prevent these artefacts, chlorine, phosgene and hydrochloric acid need to be eliminated from deuterated chloroform prior to its use. Since the common stabilization methods have proven insufficient for sensitive NMR samples, another purging method has been tested: Mitigation is easily and reliably achieved by washing the deuterated chloroform with concentrated Na2CO3-solution and subsequent desiccation with oven-dried Na2CO3.

Keywords

NMR; chemometrics; chloroform; phosgene; hydrochloric acid; sample degradation; pH-shift; protonation

Subject

Chemistry and Materials Science, Analytical Chemistry

Copyright: This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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