Combination of DOSY and 1D selective gradient TOCSY: Versatile NMR tools for identify the mixtures from glycerol hydrogenolysis reaction

Zexiang Lyu; Fen Yue; Xiuyin Yan; Jianfeng Shan; Danlei Xiang; Christian Marcus Pedersen; Chunju Li; Yingxiong Wang; Yan Qiao

doi:10.1016/j.fuproc.2017.11.011

Combination of DOSY and 1D selective gradient TOCSY: Versatile NMR tools for identify the mixtures from glycerol hydrogenolysis reaction

Zexiang Lyu, Fen Yue, Xiuyin Yan, Jianfeng Shan, Danlei Xiang, Christian Marcus Pedersen, Chunju Li^*, Yingxiong Wang, Yan Qiao

^*Corresponding author for this work

Department of Chemistry

4 Citations (Scopus)

Abstract

Hydrogenolysis is necessary for preparing various value-added chemicals from glycerol. Routine methods like GC and HPLC are not sufficient for analysis the reaction mixtures because the products usually have high boiling or similar polarity, especially when new chromatographic peaks are found which requires other technologies such as NMR. Although they were developed for years, but either DOSY or 1D selective TOCSY NMR has nature limitations. Herein we took their advantages and combined them to analyse glycerol hydrogenolysis mixtures for the first time. A model reaction mixture was first pseudo separated in DOSY spectrum, and 1D selective gradient TOCSY was further applied to assign the overlapped signal which could not be confirmed just by DOSY. A genuine reaction mixture was tried afterwards, and main signals could be assigned well in DOSY diffusion dimension. Notably, n-propanol was found as by-product by 1D selective gradient TOCSY, which is not visible in DOSY spectrum. The experimental results demonstrate that the combination of these two NMR methods could provide a fast, effective, feasible and reliable way for the identification of glycerol hydrogenolysis mixtures and is expected to apply in other research areas.

Original language	English
Journal	Fuel Processing Technology
Volume	171
Pages (from-to)	117-123
Number of pages	7
ISSN	0378-3820
DOIs	https://doi.org/10.1016/j.fuproc.2017.11.011
Publication status	Published - 2018

Keywords

1D selective TOCSY
DOSY
Glycerol hydrogenolysis
Mixture analysis
NMR

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10.1016/j.fuproc.2017.11.011

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@article{a9709b2390ff45839efb0acd5401eccd,

title = "Combination of DOSY and 1D selective gradient TOCSY: Versatile NMR tools for identify the mixtures from glycerol hydrogenolysis reaction",

abstract = "Hydrogenolysis is necessary for preparing various value-added chemicals from glycerol. Routine methods like GC and HPLC are not sufficient for analysis the reaction mixtures because the products usually have high boiling or similar polarity, especially when new chromatographic peaks are found which requires other technologies such as NMR. Although they were developed for years, but either DOSY or 1D selective TOCSY NMR has nature limitations. Herein we took their advantages and combined them to analyse glycerol hydrogenolysis mixtures for the first time. A model reaction mixture was first pseudo separated in DOSY spectrum, and 1D selective gradient TOCSY was further applied to assign the overlapped signal which could not be confirmed just by DOSY. A genuine reaction mixture was tried afterwards, and main signals could be assigned well in DOSY diffusion dimension. Notably, n-propanol was found as by-product by 1D selective gradient TOCSY, which is not visible in DOSY spectrum. The experimental results demonstrate that the combination of these two NMR methods could provide a fast, effective, feasible and reliable way for the identification of glycerol hydrogenolysis mixtures and is expected to apply in other research areas.",

keywords = "1D selective TOCSY, DOSY, Glycerol hydrogenolysis, Mixture analysis, NMR",

author = "Zexiang Lyu and Fen Yue and Xiuyin Yan and Jianfeng Shan and Danlei Xiang and Pedersen, {Christian Marcus} and Chunju Li and Yingxiong Wang and Yan Qiao",

year = "2018",

doi = "10.1016/j.fuproc.2017.11.011",

language = "English",

volume = "171",

pages = "117--123",

journal = "Fuel Processing Technology",

issn = "0378-3820",

publisher = "Elsevier",

}

TY - JOUR

T1 - Combination of DOSY and 1D selective gradient TOCSY

T2 - Versatile NMR tools for identify the mixtures from glycerol hydrogenolysis reaction

AU - Lyu, Zexiang

AU - Yue, Fen

AU - Yan, Xiuyin

AU - Shan, Jianfeng

AU - Xiang, Danlei

AU - Pedersen, Christian Marcus

AU - Li, Chunju

AU - Wang, Yingxiong

AU - Qiao, Yan

PY - 2018

Y1 - 2018

N2 - Hydrogenolysis is necessary for preparing various value-added chemicals from glycerol. Routine methods like GC and HPLC are not sufficient for analysis the reaction mixtures because the products usually have high boiling or similar polarity, especially when new chromatographic peaks are found which requires other technologies such as NMR. Although they were developed for years, but either DOSY or 1D selective TOCSY NMR has nature limitations. Herein we took their advantages and combined them to analyse glycerol hydrogenolysis mixtures for the first time. A model reaction mixture was first pseudo separated in DOSY spectrum, and 1D selective gradient TOCSY was further applied to assign the overlapped signal which could not be confirmed just by DOSY. A genuine reaction mixture was tried afterwards, and main signals could be assigned well in DOSY diffusion dimension. Notably, n-propanol was found as by-product by 1D selective gradient TOCSY, which is not visible in DOSY spectrum. The experimental results demonstrate that the combination of these two NMR methods could provide a fast, effective, feasible and reliable way for the identification of glycerol hydrogenolysis mixtures and is expected to apply in other research areas.

AB - Hydrogenolysis is necessary for preparing various value-added chemicals from glycerol. Routine methods like GC and HPLC are not sufficient for analysis the reaction mixtures because the products usually have high boiling or similar polarity, especially when new chromatographic peaks are found which requires other technologies such as NMR. Although they were developed for years, but either DOSY or 1D selective TOCSY NMR has nature limitations. Herein we took their advantages and combined them to analyse glycerol hydrogenolysis mixtures for the first time. A model reaction mixture was first pseudo separated in DOSY spectrum, and 1D selective gradient TOCSY was further applied to assign the overlapped signal which could not be confirmed just by DOSY. A genuine reaction mixture was tried afterwards, and main signals could be assigned well in DOSY diffusion dimension. Notably, n-propanol was found as by-product by 1D selective gradient TOCSY, which is not visible in DOSY spectrum. The experimental results demonstrate that the combination of these two NMR methods could provide a fast, effective, feasible and reliable way for the identification of glycerol hydrogenolysis mixtures and is expected to apply in other research areas.

KW - 1D selective TOCSY

KW - DOSY

KW - Glycerol hydrogenolysis

KW - Mixture analysis

KW - NMR

U2 - 10.1016/j.fuproc.2017.11.011

DO - 10.1016/j.fuproc.2017.11.011

M3 - Journal article

AN - SCOPUS:85034576834

SN - 0378-3820

VL - 171

SP - 117

EP - 123

JO - Fuel Processing Technology

JF - Fuel Processing Technology

ER -

Combination of DOSY and 1D selective gradient TOCSY: Versatile NMR tools for identify the mixtures from glycerol hydrogenolysis reaction

Abstract

Keywords

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