Analysis of the Alcohol Amine Mixtures by 1D Selective COSY

Zhang He; Huang Guilan; Yang Hongyu

doi:doi:10.11648/j.mc.20221001.12

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Analysis of the Alcohol Amine Mixtures by 1D Selective COSY

Zhang He, Huang Guilan, Yang Hongyu

Published in Modern Chemistry (Volume 10, Issue 1)

Received: 18 March 2022 Accepted: Published: 23 March 2022

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Abstract

Proton nuclear magnetic resonance (¹H-NMR) is one of the most commonly used techniques for structure identification in the field of chemical warfare convention (CWC) because of its strong ability in aiding structure assignment of chemicals. However, due to the lack of separation function coupled with chromatograph, the greatest disadvantage of ¹H-NMR in the analysis of environmental and biological samples is that the resonances can be easily covered or interfered. One-dimensional NMR selective excitation technology can effectively remove background interference and reveal the hidden spectral peak information. In this paper, three schedule chemicals of Chemical Weapons Convention (CWC), triethanolamine, N-methyldiethanolamine and 2-diisopropylaminoethanol, were selected as model chemicals. Homonuclear 1D COSY NMR selective excitation analysis method was established with these chemicals to solve the problem of resonances covered in ¹H-NMR. Key experiment parameters of 1D COSY were optimized. The optimized experimental conditions of 1D COSY are as follows: pulse sequence is selcogp, shaped pulse is G3, relaxation delay of d1 is 4 s, the excitation width of d_H 0.91 (a), 2.51 (g), 2.62 (e) and 3.44 (d) is 39.16, 35.34, 20.00 and 26.03 Hz respectively. The established 1D COSY method was used to analyze 1~10 μg/mL alcohol amine mixtures with 2 mg/mL quinuclidinol as the background interference and the LOD was 5 μg/mL. This method is simple, fast and can wipe off the interference effectively in the ¹H NMR spectrum without proceeding complex sample pretreatment. 1D selective COSY reflects the more accurate position of hydrogen atom, and can be used as a reliable auxiliary technology for structural identification.

Published in	Modern Chemistry (Volume 10, Issue 1)
DOI	10.11648/j.mc.20221001.12
Page(s)	5-11
Creative Commons	This is an Open Access article, distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution and reproduction in any medium or format, provided the original work is properly cited.
Copyright	Copyright © The Author(s), 2024. Published by Science Publishing Group

Keywords

Precursors of Chemical Weapon, Selective Excitation, 1D COSY, Mixture, Alcohol Amine

References

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APA Style

Zhang He, Huang Guilan, Yang Hongyu. (2022). Analysis of the Alcohol Amine Mixtures by 1D Selective COSY. Modern Chemistry, 10(1), 5-11. https://doi.org/10.11648/j.mc.20221001.12

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ACS Style

Zhang He; Huang Guilan; Yang Hongyu. Analysis of the Alcohol Amine Mixtures by 1D Selective COSY. Mod. Chem. 2022, 10(1), 5-11. doi: 10.11648/j.mc.20221001.12

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AMA Style

Zhang He, Huang Guilan, Yang Hongyu. Analysis of the Alcohol Amine Mixtures by 1D Selective COSY. Mod Chem. 2022;10(1):5-11. doi: 10.11648/j.mc.20221001.12

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@article{10.11648/j.mc.20221001.12,
  author = {Zhang He and Huang Guilan and Yang Hongyu},
  title = {Analysis of the Alcohol Amine Mixtures by 1D Selective COSY},
  journal = {Modern Chemistry},
  volume = {10},
  number = {1},
  pages = {5-11},
  doi = {10.11648/j.mc.20221001.12},
  url = {https://doi.org/10.11648/j.mc.20221001.12},
  eprint = {https://article.sciencepublishinggroup.com/pdf/10.11648.j.mc.20221001.12},
  abstract = {Proton nuclear magnetic resonance (1H-NMR) is one of the most commonly used techniques for structure identification in the field of chemical warfare convention (CWC) because of its strong ability in aiding structure assignment of chemicals. However, due to the lack of separation function coupled with chromatograph, the greatest disadvantage of 1H-NMR in the analysis of environmental and biological samples is that the resonances can be easily covered or interfered. One-dimensional NMR selective excitation technology can effectively remove background interference and reveal the hidden spectral peak information. In this paper, three schedule chemicals of Chemical Weapons Convention (CWC), triethanolamine, N-methyldiethanolamine and 2-diisopropylaminoethanol, were selected as model chemicals. Homonuclear 1D COSY NMR selective excitation analysis method was established with these chemicals to solve the problem of resonances covered in 1H-NMR. Key experiment parameters of 1D COSY were optimized. The optimized experimental conditions of 1D COSY are as follows: pulse sequence is selcogp, shaped pulse is G3, relaxation delay of d1 is 4 s, the excitation width of dH 0.91 (a), 2.51 (g), 2.62 (e) and 3.44 (d) is 39.16, 35.34, 20.00 and 26.03 Hz respectively. The established 1D COSY method was used to analyze 1~10 μg/mL alcohol amine mixtures with 2 mg/mL quinuclidinol as the background interference and the LOD was 5 μg/mL. This method is simple, fast and can wipe off the interference effectively in the 1H NMR spectrum without proceeding complex sample pretreatment. 1D selective COSY reflects the more accurate position of hydrogen atom, and can be used as a reliable auxiliary technology for structural identification.},
 year = {2022}
}

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TY  - JOUR
T1  - Analysis of the Alcohol Amine Mixtures by 1D Selective COSY
AU  - Zhang He
AU  - Huang Guilan
AU  - Yang Hongyu
Y1  - 2022/03/23
PY  - 2022
N1  - https://doi.org/10.11648/j.mc.20221001.12
DO  - 10.11648/j.mc.20221001.12
T2  - Modern Chemistry
JF  - Modern Chemistry
JO  - Modern Chemistry
SP  - 5
EP  - 11
PB  - Science Publishing Group
SN  - 2329-180X
UR  - https://doi.org/10.11648/j.mc.20221001.12
AB  - Proton nuclear magnetic resonance (1H-NMR) is one of the most commonly used techniques for structure identification in the field of chemical warfare convention (CWC) because of its strong ability in aiding structure assignment of chemicals. However, due to the lack of separation function coupled with chromatograph, the greatest disadvantage of 1H-NMR in the analysis of environmental and biological samples is that the resonances can be easily covered or interfered. One-dimensional NMR selective excitation technology can effectively remove background interference and reveal the hidden spectral peak information. In this paper, three schedule chemicals of Chemical Weapons Convention (CWC), triethanolamine, N-methyldiethanolamine and 2-diisopropylaminoethanol, were selected as model chemicals. Homonuclear 1D COSY NMR selective excitation analysis method was established with these chemicals to solve the problem of resonances covered in 1H-NMR. Key experiment parameters of 1D COSY were optimized. The optimized experimental conditions of 1D COSY are as follows: pulse sequence is selcogp, shaped pulse is G3, relaxation delay of d1 is 4 s, the excitation width of dH 0.91 (a), 2.51 (g), 2.62 (e) and 3.44 (d) is 39.16, 35.34, 20.00 and 26.03 Hz respectively. The established 1D COSY method was used to analyze 1~10 μg/mL alcohol amine mixtures with 2 mg/mL quinuclidinol as the background interference and the LOD was 5 μg/mL. This method is simple, fast and can wipe off the interference effectively in the 1H NMR spectrum without proceeding complex sample pretreatment. 1D selective COSY reflects the more accurate position of hydrogen atom, and can be used as a reliable auxiliary technology for structural identification.
VL  - 10
IS  - 1
ER  -

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Author Information

Zhang He

Department of Underwater Weaponry and Chemical Defense, Dalian Naval Academy, Dalian, China
Huang Guilan

State Key Laboratory of NBC Protection for Civilian, Institute of Chemical Defense, AMS, PLS, Beijing, China
Yang Hongyu

Department of Underwater Weaponry and Chemical Defense, Dalian Naval Academy, Dalian, China

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APA Style

Zhang He, Huang Guilan, Yang Hongyu. (2022). Analysis of the Alcohol Amine Mixtures by 1D Selective COSY. Modern Chemistry, 10(1), 5-11. https://doi.org/10.11648/j.mc.20221001.12

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ACS Style

Zhang He; Huang Guilan; Yang Hongyu. Analysis of the Alcohol Amine Mixtures by 1D Selective COSY. Mod. Chem. 2022, 10(1), 5-11. doi: 10.11648/j.mc.20221001.12

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AMA Style

Zhang He, Huang Guilan, Yang Hongyu. Analysis of the Alcohol Amine Mixtures by 1D Selective COSY. Mod Chem. 2022;10(1):5-11. doi: 10.11648/j.mc.20221001.12

Copy | Download

@article{10.11648/j.mc.20221001.12,
  author = {Zhang He and Huang Guilan and Yang Hongyu},
  title = {Analysis of the Alcohol Amine Mixtures by 1D Selective COSY},
  journal = {Modern Chemistry},
  volume = {10},
  number = {1},
  pages = {5-11},
  doi = {10.11648/j.mc.20221001.12},
  url = {https://doi.org/10.11648/j.mc.20221001.12},
  eprint = {https://article.sciencepublishinggroup.com/pdf/10.11648.j.mc.20221001.12},
  abstract = {Proton nuclear magnetic resonance (1H-NMR) is one of the most commonly used techniques for structure identification in the field of chemical warfare convention (CWC) because of its strong ability in aiding structure assignment of chemicals. However, due to the lack of separation function coupled with chromatograph, the greatest disadvantage of 1H-NMR in the analysis of environmental and biological samples is that the resonances can be easily covered or interfered. One-dimensional NMR selective excitation technology can effectively remove background interference and reveal the hidden spectral peak information. In this paper, three schedule chemicals of Chemical Weapons Convention (CWC), triethanolamine, N-methyldiethanolamine and 2-diisopropylaminoethanol, were selected as model chemicals. Homonuclear 1D COSY NMR selective excitation analysis method was established with these chemicals to solve the problem of resonances covered in 1H-NMR. Key experiment parameters of 1D COSY were optimized. The optimized experimental conditions of 1D COSY are as follows: pulse sequence is selcogp, shaped pulse is G3, relaxation delay of d1 is 4 s, the excitation width of dH 0.91 (a), 2.51 (g), 2.62 (e) and 3.44 (d) is 39.16, 35.34, 20.00 and 26.03 Hz respectively. The established 1D COSY method was used to analyze 1~10 μg/mL alcohol amine mixtures with 2 mg/mL quinuclidinol as the background interference and the LOD was 5 μg/mL. This method is simple, fast and can wipe off the interference effectively in the 1H NMR spectrum without proceeding complex sample pretreatment. 1D selective COSY reflects the more accurate position of hydrogen atom, and can be used as a reliable auxiliary technology for structural identification.},
 year = {2022}
}

Copy | Download

TY  - JOUR
T1  - Analysis of the Alcohol Amine Mixtures by 1D Selective COSY
AU  - Zhang He
AU  - Huang Guilan
AU  - Yang Hongyu
Y1  - 2022/03/23
PY  - 2022
N1  - https://doi.org/10.11648/j.mc.20221001.12
DO  - 10.11648/j.mc.20221001.12
T2  - Modern Chemistry
JF  - Modern Chemistry
JO  - Modern Chemistry
SP  - 5
EP  - 11
PB  - Science Publishing Group
SN  - 2329-180X
UR  - https://doi.org/10.11648/j.mc.20221001.12
AB  - Proton nuclear magnetic resonance (1H-NMR) is one of the most commonly used techniques for structure identification in the field of chemical warfare convention (CWC) because of its strong ability in aiding structure assignment of chemicals. However, due to the lack of separation function coupled with chromatograph, the greatest disadvantage of 1H-NMR in the analysis of environmental and biological samples is that the resonances can be easily covered or interfered. One-dimensional NMR selective excitation technology can effectively remove background interference and reveal the hidden spectral peak information. In this paper, three schedule chemicals of Chemical Weapons Convention (CWC), triethanolamine, N-methyldiethanolamine and 2-diisopropylaminoethanol, were selected as model chemicals. Homonuclear 1D COSY NMR selective excitation analysis method was established with these chemicals to solve the problem of resonances covered in 1H-NMR. Key experiment parameters of 1D COSY were optimized. The optimized experimental conditions of 1D COSY are as follows: pulse sequence is selcogp, shaped pulse is G3, relaxation delay of d1 is 4 s, the excitation width of dH 0.91 (a), 2.51 (g), 2.62 (e) and 3.44 (d) is 39.16, 35.34, 20.00 and 26.03 Hz respectively. The established 1D COSY method was used to analyze 1~10 μg/mL alcohol amine mixtures with 2 mg/mL quinuclidinol as the background interference and the LOD was 5 μg/mL. This method is simple, fast and can wipe off the interference effectively in the 1H NMR spectrum without proceeding complex sample pretreatment. 1D selective COSY reflects the more accurate position of hydrogen atom, and can be used as a reliable auxiliary technology for structural identification.
VL  - 10
IS  - 1
ER  -

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