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煤基富勒烯烟灰萃取产物的质谱分析
引用本文:李永峰,邱介山,周颖,三重野哲.煤基富勒烯烟灰萃取产物的质谱分析[J].分析化学,2002,30(7):769-773.
作者姓名:李永峰  邱介山  周颖  三重野哲
作者单位:1. 大连理工大学材料化工系炭素材料研究室,大连,116012
2. 日本静冈大学理学部物理学科, 静冈市大谷,422-8529
基金项目:国家自然科学基金 (No .2 95 0 6 0 41和No .2 9976 0 0 6 ),辽宁省科学基金 (No .95 0 31和No .9810 30 0 70 1),教育部留学归国人员基金,教育部骨干教师培训计划资助项目
摘    要:用甲苯等有机溶剂对由煤制得烟灰(soot)进行索氏萃取,用时间飞行质谱及气相色谱-质谱联用(GCMS)技术对所得的萃取产物进行了分析,结果发现,煤基粗富勒烯中除含有大量的C60和C70外,高碳富勒烯(如C74、C78,C82、C84、C100及C106等)的丰度也较高。在煤基粗富勒烯的伴生副产物中存在一些含有苯环结构的芳香性碳氢化合物和少量的长烷烃化合物,由此推测煤基富勒烯的形成过程可能遵循着一条与以石墨为原料时的机制完全不同的途径。

关 键 词:煤基富勒烯  烟灰  萃取产物  质谱分析  高碳富勒烯  气相色谱  孛氏抽提  制备  分离

Laser Desorption Time-of-flight Mass Spectrometry and Gas Chromatography-Mass Spectrometry Analysis of Extracts from Coal-derived Fullerene Containing Soots
Li Yongfeng ,Qiu Jieshan ,Zhou Ying ,Testsu Mieno.Laser Desorption Time-of-flight Mass Spectrometry and Gas Chromatography-Mass Spectrometry Analysis of Extracts from Coal-derived Fullerene Containing Soots[J].Chinese Journal of Analytical Chemistry,2002,30(7):769-773.
Authors:Li Yongfeng  Qiu Jieshan  Zhou Ying  Testsu Mieno
Institution:Li Yongfeng 1,Qiu Jieshan *1,Zhou Ying 1,Testsu Mieno 2 1
Abstract:The direct current arc discharge method was adopted to evaporate the coal-derived carbon electrodes to produce soot that contains fullerenes. Organic solvents such as toluene, o-xylene and 1,2,4-trichlorobenzene were used to extract crude fullerenes from the soot obtained from the arcing process. The crude fullerenes and its by-products were analyzed using laser desorption time-of-flight mass spectrometry and gas chromatographtry-mass spectrometry (GC-MS). It is found that in addition to C 60 and C 70 fullerenes, higher fullerenes such as C 74, C 78, C 82, C 84, C 100 and C 106 exists in the coal-derived crude fullerenes in relatively high content. The GC-MS analysis results indicate that the oil-like yellow by-products mainly consists of aromatic hydrocarbons, which may directly come from the recombination of small fragments formed during the arcing process of coal-based carbon. It implies that the formation mechanism of fullerenes from coal may be different from that when graphite is used as the starting material. In the case of coal, fullerenes could be directly formed from larger units rather than from C 1 and C 2 units, in other words, the large polycyclic aromatic carbons ions may act as the precursors in the formation of coal-based fullerenes.
Keywords:Coal  higher fullerenes  laser desorption time-of-flight mass spectrometry  gas chromatographtry-mass spectrometry
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