Correction of sideband effects of nuclear magnetic resonance carbon spectrum in coal and its application in coal structure analysis
Abstract 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...
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| Format: | Article |
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Wiley
2023-08-01
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| Series: | Energy Science & Engineering |
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| Online Access: | https://doi.org/10.1002/ese3.1490 |
| _version_ | 1827577716072775680 |
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| author | Tianyi Chang Xingyu Zhou Xiaopeng Deng Jianhua Xiang |
| author_facet | Tianyi Chang Xingyu Zhou Xiaopeng Deng Jianhua Xiang |
| author_sort | Tianyi Chang |
| collection | DOAJ |
| description | Abstract 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 13C nuclear magnetic resonance (13C NMR) spectrum without sideband suppression (13C CP‐MAS NMR) and 13C NMR spectrum under sideband suppression conditions (13C 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 13C CP‐MAS/TOSS NMR spectrum, thus realizing the accurate correction of sideband effect of the solid‐state 13C 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. |
| first_indexed | 2024-03-08T21:31:49Z |
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| id | doaj.art-04a42717628748c585af908a3e4959c8 |
| institution | Directory Open Access Journal |
| issn | 2050-0505 |
| language | English |
| last_indexed | 2024-03-08T21:31:49Z |
| publishDate | 2023-08-01 |
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| series | Energy Science & Engineering |
| spelling | doaj.art-04a42717628748c585af908a3e4959c82023-12-21T06:55:47ZengWileyEnergy Science & Engineering2050-05052023-08-011182763277410.1002/ese3.1490Correction of sideband effects of nuclear magnetic resonance carbon spectrum in coal and its application in coal structure analysisTianyi Chang0Xingyu Zhou1Xiaopeng Deng2Jianhua Xiang3Key Laboratory of Coal Science & Technology, Ministry of Education & Shanxi Province, Department of Earth Science & Engineering Taiyuan University of Technology Taiyuan Shanxi ChinaKey Laboratory of Coal Science & Technology, Ministry of Education & Shanxi Province, Department of Earth Science & Engineering Taiyuan University of Technology Taiyuan Shanxi ChinaDepartment of Geology And Surveying And Mapping Shanxi Institute of Energy Jinzhong Shanxi ChinaKey Laboratory of Coal Science & Technology, Ministry of Education & Shanxi Province, Department of Earth Science & Engineering Taiyuan University of Technology Taiyuan Shanxi ChinaAbstract 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 13C nuclear magnetic resonance (13C NMR) spectrum without sideband suppression (13C CP‐MAS NMR) and 13C NMR spectrum under sideband suppression conditions (13C 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 13C CP‐MAS/TOSS NMR spectrum, thus realizing the accurate correction of sideband effect of the solid‐state 13C 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.https://doi.org/10.1002/ese3.149013C NMRcarbon structure parametercoal structuresideband effecttotal suppression of sidebands |
| spellingShingle | Tianyi Chang Xingyu Zhou Xiaopeng Deng Jianhua Xiang Correction of sideband effects of nuclear magnetic resonance carbon spectrum in coal and its application in coal structure analysis Energy Science & Engineering 13C NMR carbon structure parameter coal structure sideband effect total suppression of sidebands |
| title | Correction of sideband effects of nuclear magnetic resonance carbon spectrum in coal and its application in coal structure analysis |
| title_full | Correction of sideband effects of nuclear magnetic resonance carbon spectrum in coal and its application in coal structure analysis |
| title_fullStr | Correction of sideband effects of nuclear magnetic resonance carbon spectrum in coal and its application in coal structure analysis |
| title_full_unstemmed | Correction of sideband effects of nuclear magnetic resonance carbon spectrum in coal and its application in coal structure analysis |
| title_short | Correction of sideband effects of nuclear magnetic resonance carbon spectrum in coal and its application in coal structure analysis |
| title_sort | correction of sideband effects of nuclear magnetic resonance carbon spectrum in coal and its application in coal structure analysis |
| topic | 13C NMR carbon structure parameter coal structure sideband effect total suppression of sidebands |
| url | https://doi.org/10.1002/ese3.1490 |
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