煤有机硫分析中XPS分峰拟合方法及参数设置

马玲玲; 秦志宏; 张露; 刘旭; 陈航

煤有机硫分析中XPS分峰拟合方法及参数设置

中国矿业大学化工学院, 江苏徐州 221116

基金项目: 国家重点基础研究发展规划（973 计划，2012CB214900）；国家自然科学基金（51274201）；中央高校基本科研业务费专项资金（2010LKHX01）。

详细信息

通讯作者:
秦志宏（1963-），Tel：0516-83591059; E-mail：qinzh1210@163.com

中图分类号: TQ533.6
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出版历程
- 收稿日期: 2013-06-18
- 修回日期: 2013-09-03
- 刊出日期: 2014-03-31

Peak fitting methods and parameter settings in XPS analysis for organic sulfur in coal

School of Chemical Engineering and Technology, China University of Mining and Technology, Xuzhou 221116, China

摘要

摘要: 通过对含硫模型化合物和新峪焦精煤中的有机硫含量的分析，对XPS谱图的分峰拟合方法和参数设置进行了探讨。结果表明，用XPS解析煤中不同形态硫含量时，应按2p_3/2和2p_1/2劈裂峰分峰方法进行，并设置劈裂峰的面积比约为2：1，裂距为1.18 eV，L-G%相同，FWHM值也相同；限定各有机硫2p_3/2峰峰位分别为：硫醇硫醚类硫162.1~163.6 eV；噻吩类硫164.0~164.4 eV；亚砜类硫165.0~166.0 eV，同时对分峰拟合参数在一定范围内进行动态微调，可实现良好的数据重现性和较佳的拟合度。
- 煤 /
- 有机硫 /
- XPS /
- 劈裂峰 /
- 分峰拟合方法 /
- 参数设置
Abstract: By analyzing the organic sulfur content in the model compounds and the Xinyu refined coking coal, the curve fitting methods and setting parameters of XPS spectra were discussed. The results indicate that when analyzing the content of different sulfur forms in coal with XPS, the curve fitting methods of 2p_3/2 and 2p_1/2 splitting peaks and some other parameters are set as follows: an approximate 2:1 relative area separated by 1.18 eV with equal L-G% and FWHM level. In addition, the 2p_3/2 peak of each organic sulfur is fixed as: mercaptan/thioether 162.1~163.6 eV, thiophene 164.0~164.4 eV, and sulfoxide 165.0~166.0 eV. Good reproducibility and fitting level are achieved when the curve fitting parameters are adjusted finely and dynamically within a certain range.
- coal /
- organic sulfur /
- XPS /
- splitting peak /
- peak fitting method /
- parameter setting

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参考文献(20)

KOZLOWSKI M. XPS study of reductively and non-reductively modified coal[J]. Fuel, 2004, 83(3): 259-265.

PIETRZAK R, WACHOWSKA H. The influence of oxidation with HNO₃ on the surface composition of high sulphur coals XPS study[J]. Fuel Process Technol, 2006, 87(11): 1021-1029.

MAES L I, MITCHEL S C, YPERMAN J. Sulphur functionalities and physical characteristics of the maritza iztok basin lignites[J]. Fuel, 1996, 75(11): 1286-1293.

MARINOV S P, TYULIEV G, STEFANOVA M, CARLEER R, YPERMAN J. Low rank coals sulphur functionality study by AP-TPR/TPO coupled with MS and potentiometric detection and by XPS[J]. Fuel Process Technol, 2004, 85(4): 267-277.

刘艳华, 车得福, 徐通模. 利用X射线光电子能谱确定煤及其残焦中硫的形态[J]. 西安交通大学学报, 2004, 38(1): 101-104. (LIU Yan-hua, CHE De-fu, XU Tong-mo. X-ray photoelectron spectroscopy determination of the forms of sulfur in coal and its chars[J]. Journal of Xi'an Jiaotong University, 2004, 38(1): 101-104.)

URBAN N R, ERNST K, BERNASCONI S. Addition of sulfur to organic matter during early diagenesis of lake sediments[J]. Geochimica et Cosmochimica Acta, 1999, 63(6): 837-853.

WILDE L, POLCIK M, HAASE J, BRENA B, COCCO D, COMELLI G, PAOLUCC G. Adsorption and temperature-dependent decomposition of SO₂ on Ni(110): An XPS and XAFS study[J]. Surf Sci, 1998, 405(2/3): 215-227.

MOULDER H F, STICKLE W F, SOBOL P E, BNNXBEN K D. Handbook of X-ray photoelectron spectroscopy[M]. USA: Perkin-Elmer Corporation, 1992.

陈鹏. 鉴定煤中有机硫类型的方法研究[J]. 煤炭学报, 2000, 25(S1): 174-181. (CHEN Peng. Study on determination of the forms of organic sulfur in coals[J]. Journal of China Coal Society, 2000, 25(S1): 174-181.

陈鹏. 煤中有机硫的脱除[J]. 煤炭分析及利用, 1994, 9(4): 7-18. (CHEN Peng. The removal of organic sulfur in coal[J]. Coal Analysis and Utilization, 1994, 9(4): 7-18.)

代世峰, 任德贻, 宋建芳, 秦胜飞. 应用XPS研究镜煤中有机硫的存在形态[J]. 中国矿业大学学报, 2002, 31(3): 12-15. (DAI Shi-feng, REN De-yi, SONG Jian-fang, QIN Sheng-fei. Application of XPS in research on occurrence of organic sulfur in vitrain[J]. Journal of China University of Mining & Technology, 2002, 31(3): 12-15.)

张蓬洲, 赵秀荣. 用XPS研究我国一些煤中有机硫的存在形态[J]. 燃料化学学报, 1993, 21(2): 205-210. (ZHANG Peng-zhou, ZHAO Xiu-rong. An XPS study of the forms of oaganic sulfur in some chinese coals[J]. Journal of Fuel Chemistry and Technology, 1993, 21(2): 205-210.)

陈鹏. 用XPS研究兖州煤各显微组分中有机硫存在形态[J]. 燃料化学学报, 1997, 25(3): 238-241. (CHEN Peng. Application of XPS in study forms of organic sulfur in macerals of Yanzhou coal[J]. Journal of Fuel Chemistry and Technology, 1997, 25(3): 238-241.)

KELEMEN S R, GEORGE G N, GORBATY M L. Direct determination and quantification of sulfur forms in heavy petroleum and coals: 1. The X-ray photoelectron spectroscopy(XPS) approach[J]. Fuel, 1990, 69(8): 939-944.

YAGI S, NAMBU M, TSUKADA C, OGAMAA S, KUTLUKB G, NAMATAMEB H, TANIGUCHIB M. Spectral studies on sulfur poisoning of Pd/Mg 6 Ni by NEXAFS and XPS[J]. Surf Sci, 2013, 267: 45-47.

GRZYBEK T, PIETRZAK R, WACHOWSKA H. X-ray photoelectron spectroscopy study of oxidized coals with different sulphur content[J]. Fuel Process Technol, 2002, 77-78: 1-7.

ARONNIEMI M, SAINIO J, LAHTINEN J. Chemical state quantification of iron and chromium oxides using XPS the effect of the background subtraction method[J]. Surf Sci, 2005, 578(1/3): 108-123.

OLIVELLA M A, PALACIOS J M, VAIRAVAMURTHY A DEL RIO J C, De LAS HERAS, F X C. A study of sulfur functionalities in fossil fuels using destructive-(ASTM and Py-GC-MS) and non-destructive-(SEM-EDX, XANES and XPS) techniques[J]. Fuel, 2002, 81(4): 405-411.

朱应军, 郑明东. 炼焦用精煤中硫形态的XPS分析方法研究[J]. 选煤技术, 2010, (3): 55-57. (ZHU Ying-jun, ZHENG Ming-dong. The study of methods for analysize the forms of sulfur in coking refined coal[J]. Coal Preparation Technology, 2010, (3): 55-57.)

戴冬瑾. 新峪焦煤中有机硫赋存规律的研究[D]. 徐州: 中国矿业大学, 2013. (DAI Dong-jin. Research on the occurrence law of the organic sulfur in Xinyu coking coal[D]. Xuzhou: China University of Mining and Technolgy, 2013.)

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