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 -