FID/TCD并联气相色谱法测定天然气水合物的气体组成  

Compositional Analysis of Gases in Natural Gas Hydrates by GC-FID/TCD

作　　者：贺行良[1,2,3] 夏宁[1,2] 刘昌岭[1,2] 王江涛[3] 孟庆国[1,2] 

机构地区：[1]国土资源部海洋油气资源与环境地质重点实验室,山东青岛266071 [2]青岛海洋地质研究所,山东青岛266071 [3]中国海洋大学海洋化学理论与工程技术教育部重点实验室,山东青岛266100

出　　处：《分析测试学报》2012年第2期206-210,共5页Journal of Instrumental Analysis

基　　金：国土资源部公益性行业科研专项资助(201111026);中国地质调查局地质调查项目资助(1212011120271);国家自然科学基金资助项目(41072037)

摘　　要：建立了一种氢火焰离子化检测器(FID)与热导检测器(TCD)并联检测的气相色谱分析技术。该方法一次进样,即可实现天然气水合物中C1～C6、CO2、H2S、O2+N2 16种气体成分的同时测定。实验优化了色谱柱、升温程序、柱流速、进样口温度、检测器温度、TCD参考气和尾吹气流速等仪器分析参数。在优化条件下,16种气体分子在实验浓度范围内线性关系良好,r2为0.999 03～0.999 98,方法检出限为0.000 3～0.046 mol/mol,相对标准偏差(n=6)为1.6%～5.0%。对祁连山冻土区、南海神狐海域、人工合成水合物样品的分析表明,该方法简便实用、灵敏可靠,可满足天然气水合物气体组成的分析要求。A gas chromatographic analysis technique with parallel detectors of flame ionization detector and thermal conductivity detector（GC-FID/TCD） was established.The method can be used to determine 16 gases（C1-C6 alkanes,CO2,H2S,O2＋N2） of natural gas hydrates simultaneously by one injection.The analysis parameters,such as capillary column,temperature program,column flow,inlet temperature,detector temperature,the reference and makeup flow of TCD were optimized.Under the optimal conditions,good linearities were obtained in the experimental concentration range for the 16 gases with correlation coefficients（r2） of 0.999 03-0.999 98.The limits of detection ranged from 0.000 3 mol/mol to 0.046 mol/mol with relative standard deviations（RSDs,n=6） of 1.6%-5.0%.The method was successfully applied in the determinations of gas compositions in the natural gas hydrates from Qilian Mountain Permafrost,South China Sea and laboratory synthetic samples.The result showed that the method was simple,practical,sensitive and reliable,and was suitable for the determination of gases in natural gas hydrates.

关 键 词：天然气水合物 气体组成 GC-FID/TCD 毛细管分流器 

分 类 号：O657.71[理学—分析化学] O659[理学—化学]