岩矿测试

文章摘要

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

ZHANG Zhu-yue,LIU Mei-mei,XIE Man-man,WANG Dao-cong,LING Yuan,SHANG Wen-yu,LIU Shu-bo,CEN Kuang,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.DOI:

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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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

投稿时间：2010-11-27

DOI：

中文关键词: 正构烷烃单体碳同位素气相色谱法 5A分子筛

英文关键词: n-alkanes specific carbon isotope gas chromatography 5A molecular sieve

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)

作者	单位
张逐月	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
刘美美	国家地质实验测试中心, 北京 100037
谢曼曼	中国科学院地质与地球物理研究所, 北京 100029
王道聪	中国地质大学(北京)地球科学与资源学院, 北京 100083
凌媛	国家地质实验测试中心, 北京 100037
尚文郁	中国地质大学(北京)地球科学与资源学院, 北京 100083
刘舒波	中国地质大学(北京)地球科学与资源学院, 北京 100083
岑况	中国地质大学(北京)地球科学与资源学院, 北京 100083
孙青	国家地质实验测试中心, 北京 100037

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中文摘要:

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。

英文摘要:

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.

主管单位：	中国科学技术协会
主办单位：	中国地质学会岩矿测试技术专业委员会国家地质实验测试中心