Citation: CHEN Li-shi, WANG Lan-lan, PAN Tie-ying, ZHOU Yang, ZHANG Yuan-yuan, ZHANG De-xiang. Calibration of solid state NMR carbon structural parameters and application in coal structure analysis[J]. Journal of Fuel Chemistry and Technology, ;2017, 45(10): 1153-1163. shu

Calibration of solid state NMR carbon structural parameters and application in coal structure analysis

1.
Department of Chemical Engineering for Energy Resources, East China University of Science & Technology, Key Laboratory of Coal Gasification and Energy Chemical Engineering of Ministry of Education, Shanghai 200237, China
2.
Analysis and Research Center, East China University of Science and Technology, Shanghai 200237, China

Corresponding author: ZHANG De-xiang, zdx@ecust.edu.cn
Received Date: 5 April 2017
Revised Date: 20 June 2017

Fund Project: the National Key Research and Development Program of China 2016YFB0600303The project was supported by the National Key Research and Development Program of China(2016YFB0600303)

Figures(5)

Carbon structure parameters were obtained accurately, if the NOE effect of carbon nucleus has been eliminated in¹³C CP/MAS/TOSS NMR test. This study has investigated different model compounds NOE effect intensity. And the results show that there is an obvious carbon structure error between the fitting test value and theoretical value in the different model compounds. The aliphatic carbon error is 25%-125%, and the aromatic carbon is 4%-50%, the NOE effect has great influence in solid state NMR. Therefore, the nonlinear regression equation was obtained by regression analysis of the measured and theoretical values of the model compound aliphatic and aromatic carbon. And this equation was used to calibrate the carbon structure of 9, 10-dimethylanthracene. It is found that after calibration the error between the measured value and the theoretical value of the modified aliphatic is reduced from 119.60% to 7.84%. The error of the aromatic carbon is reduced from -17.10% to 1.11%. And the error is within 10%. Then, the carbon structural parameters of different coal are calibrated by the regression equation. It is found that the H/C error of different coal is 45%-53% compared with elements analysis, and the calibration error is only 4%-13%, which is consistent with the results of elemental analysis. It indicated that the nonlinear regression equation could easily and precisely correct the solid state NMR carbon nuclear NOE effects and also provides new technical support for analysis of carbon structure in coal.
- coal structure,
- model compounds,
- NOE,
- NMR,
- carbon structural parameters
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沈阳化工大学材料科学与工程学院沈阳 110142