| 5A分子筛吸附混合溶剂洗脱-气相色谱-同位素质谱分析土壤中正构烷烃单体碳同位素 |
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| 引用本文： | 张逐月,刘美美,谢曼曼,王道聪,凌媛,尚文郁,刘舒波,岑况,孙青.5A分子筛吸附混合溶剂洗脱-气相色谱-同位素质谱分析土壤中正构烷烃单体碳同位素[J].岩矿测试,2012,31(1):178-183. |
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| 作者姓名： | 张逐月 刘美美 谢曼曼 王道聪 凌媛 尚文郁 刘舒波 岑况 孙青 |
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| 作者单位： | 天津市地质调查研究院, 天津 300191; 国家地质实验测试中心, 北京 100037; 中国地质大学(北京)地球科学与资源学院, 北京 100083;国家地质实验测试中心, 北京 100037;中国科学院地质与地球物理研究所, 北京 100029;中国地质大学(北京)地球科学与资源学院, 北京 100083;国家地质实验测试中心, 北京 100037;中国地质大学(北京)地球科学与资源学院, 北京 100083;中国地质大学(北京)地球科学与资源学院, 北京 100083;中国地质大学(北京)地球科学与资源学院, 北京 100083;国家地质实验测试中心, 北京 100037 |
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| 基金项目： | 国家自然科学基金项目(40972121); 国土资源地质大调查项目(121010816028,1212011120281); 国土资源部公益性行业科研专项经费项目(200911043-29) |
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| 摘 要： | 利用5A分子筛吸附,环己烷-正戊烷混合溶剂洗脱分离富集正构烷烃,用气相色谱法测定正构烷烃含量,气相色谱-气体同位素质谱(GC-C-IRMS)测定土壤样品中正构烷烃单体碳同位素。实验优化了5A分子筛用量和洗脱剂的比例,需要络合的正构烷烃的量与分子筛加入量呈线性关系,络合x mg的正构烷烃,需加入2.75x g分子筛,络合环己烷-正戊烷最佳比例为9∶91。探讨了络合过程中5A分子筛对不同链长正构烷烃的络合规律,短链正构烷烃被5A分子筛优先吸附,长链正构烷烃的络合相对滞后。正构烷烃的络合洗脱回收率为44%～72%,精密度(RSD,n=6)为4%～8%;正构烷烃单体碳同位素分析精度为0.04‰～0.38‰(1σ)。采用5A分子筛净化混合溶剂洗脱方法,分析加油站附近的实际土壤样品,未分峰基本消除,获得良好的净化效果,满足正构烷烃单体碳同位素分析的要求。
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| 关 键 词： | 正构烷烃 单体碳同位素 气相色谱法 5A分子筛 |
| 收稿时间： | 2010/11/27 0:00:00 |
Specific Carbon Isotopic Analysis of n-Alkanes in Soils by Gas Chromatography-Isotope Ratio Mass Spectrometry with 5A Molecular Sieve Adsorption and Mixed Solvent Elution |
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| ZHANG Zhu-yue,LIU Mei-mei,XIE Man-man,WANG Dao-cong,LING Yuan,SHANG Wen-yu,LIU Shu-bo,CEN Kuang and SUN Qing.Specific Carbon Isotopic Analysis of n-Alkanes in Soils by Gas Chromatography-Isotope Ratio Mass Spectrometry with 5A Molecular Sieve Adsorption and Mixed Solvent Elution[J].Rock and Mineral Analysis,2012,31(1):178-183. |
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| Authors: | ZHANG Zhu-yue LIU Mei-mei XIE Man-man WANG Dao-cong LING Yuan SHANG Wen-yu LIU Shu-bo CEN Kuang and SUN Qing |
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| Institution: | Tianjin Institute of Geological Survey, Tianjin 300191, China; National Research Center for Geoanalysis, Beijing 100037, China; School of the Earth Sciences and Resources, China University of Geoscience, Beijing 100083, China;National Research Center for Geoanalysis, Beijing 100037, China;Institute of Geology and Geophysics, Chinese Academy of Sciences, Beijing 100029, China;School of the Earth Sciences and Resources, China University of Geoscience, Beijing 100083, China;National Research Center for Geoanalysis, Beijing 100037, China;School of the Earth Sciences and Resources, China University of Geoscience, Beijing 100083, China;School of the Earth Sciences and Resources, China University of Geoscience, Beijing 100083, China;School of the Earth Sciences and Resources, China University of Geoscience, Beijing 100083, China;National Research Center for Geoanalysis, Beijing 100037, China |
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| Abstract: | n-alkanes were concentrated after separating by a 5A molecular sieve and extracted by a mixture solvent of cyclohexane and n-pentane.In this study,the amount of 5A molecular sieve and the ratios of cyclohexane and n-pentane were optimized as 2.76 g and 9∶91,respectively.It was discovered that short carbon chain n-alkanes were readily absorbed by a 5A molecular sieve,compared to the long carbon chain n-alkanes.The complexation efficiency is higher for long carbon chain n-alkanes than that of short carbon chain n-alkanes with enough 5A molecular material at higher temperature.In this study,n-alkanes contents were determined by Gas Chromatography(GC) and compound specific carbon isotope ratios of individual n-alkanes in soil were measured by Gas Chromatography-Isotope Ratio Mass Spectrometry(GC-IRMS).The recoveries of n-alkanes ranged from 44% to 72‰ with a precision of 4%-8%.The accuracies of compound specific carbon isotopes of n-alkanes ranged from 0.04‰ to 0.38‰(1σ).The 5A molecular sieve procedure was used to analyse soil samples around a gas station.The results indicate that almost all of the unseparated and interference peaks were eliminated and the purification of n-alkanes met the requirements of stable carbon isotope analysis. |
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| Keywords: | n-alkanes specific carbon isotope gas chromatography 5A molecular sieve |
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