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Correction of sideband effects of nuclear magnetic resonance carbon spectrum in coal and its application in coal structure analysis
被引:3
作者:
Chang, Tianyi
[1
]
Zhou, Xingyu
[1
]
Deng, Xiaopeng
[2
]
Xiang, Jianhua
[1
,3
]
机构:
[1] Taiyuan Univ Technol, Dept Earth Sci & Engn, Key Lab Coal Sci & Technol, Minist Educ & Shanxi Prov, Taiyuan, Shanxi, Peoples R China
[2] Shanxi Inst Energy, Dept Geol & Surveying & Mapping, Jinzhong, Shanxi, Peoples R China
[3] Taiyuan Univ Technol, Dept Earth Sci & Engn, Key Lab Coal Sci & Technol, Minist Educ & Shanxi Prov, Taiyuan 030024, Shanxi, Peoples R China
基金:
中国国家自然科学基金;
关键词:
C-13;
NMR;
carbon structure parameter;
coal structure;
sideband effect;
total suppression of sidebands;
STATE C-13 NMR;
QUANTITATIVE CHARACTERIZATION;
CROSS-POLARIZATION;
SPECTROSCOPY;
FTIR;
AROMATICITY;
PYROLYSIS;
INSIGHTS;
FRACTION;
RAMAN;
D O I:
10.1002/ese3.1490
中图分类号:
TE [石油、天然气工业];
TK [能源与动力工程];
学科分类号:
0807 ;
0820 ;
摘要:
In the nuclear magnetic resonance (NMR) test of coal, when the spinning frequency of magic-angle spinning (MAS) is less than the frequency range of chemical shift anisotropy, serious aromatic carbon spinning sidebands will appear. Existing solutions to the sideband effect, such as changing the MAS frequency, inserting total suppression of sidebands (TOSS) pulse sequences, or simply defining the peak after chemical shift of 200 ppm as the sideband peaks generated by aromatic carbon peak, multipling the identified sideband integral by 2 and adding to the main peaks of protonated aromatic carbon and aromatic bridgehead carbon. None of these methods can reasonably correct for the sideband effect and cause errors to accurately quantifying the carbon structure parameters. Compared with C-13 nuclear magnetic resonance (C-13 NMR) spectrum without sideband suppression (C-13 CP-MAS NMR) and C-13 NMR spectrum under sideband suppression conditions (C-13 CP-MAS/TOSS NMR), according to the chemical shifts of the main peaks of four aromatic carbons, namely protonated aromatic carbon, aromatic bridgehead carbon, alkylated aromatic carbon and oxygen-linked aromatic carbon, combined with the MAS frequency, the first- and second-level sideband peaks generated by four types of aromatic carbons were accurately located and quantified, and they were added to the corresponding aromatic carbon main peaks in C-13 CP-MAS/TOSS NMR spectrum, thus realizing the accurate correction of sideband effect of the solid-state C-13 NMR spectrum of coal samples. The relative area of corrected aliphatic carbon, carbonyl (carboxyl) carbon, and various aromatic carbons were recalculated, and more accurate carbon structure parameters were obtained, which is significant for studying the coal structure from a microscopic perspective.
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页码:2763 / 2774
页数:12
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