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作 者:陈卫明[1] 肖细炼[1] 李庆霞[1] 薄玮[1] 张勤[1]
机构地区:[1]中国地质科学院地球物理地球化学勘查研究所,河北廊坊065000
出 处:《岩矿测试》2015年第6期698-703,共6页Rock and Mineral Analysis
基 金:中国地质调查局地质调查项目(12120114004101;12120113015400);中央级公益性科研院所基本科研业务费资助项目(AS2010J03)
摘 要:本文通过改进传统制备酸解烃样品的单套脱气装置,采用多套酸解烃脱气装置,建立了自动进样一毛细管柱气相色谱法测定油气化探样品中酸解烃的分析方法,并对主要仪器分析条件及质量监控方法进行了讨论。结果表明,样品在真空40℃水浴条件下酸解反应10min,酸解烃脱出气储存于密封瓶中供气相色谱检测,方法检出限为0.007~0.057μL/kg,精密度(RSD,n=12)为0.8%~1.1%。对105件样品2次独立测试结果的相对偏差为0.01%~19.66%,平均值为7.81%(以甲烷计算)。该方法能够满足油气化探酸解烃样品分析的质量要求,并在天然气水合物勘查中取得了较好的应用效果。A method for the determination of acidolysis hydrocarbons in oil/gas geochemical exploration samples by autosampler-GC-FID using multiple acidolysis devices was developed based on the improvement of traditional single set acidolysis equipment. The optimization of the main analytical conditions and quality control are also discussed in detail in this paper. The acidolysis of samples was carried out in vacuum in a 40℃ water bath for 10 min. The emitted gases of acidolysis hydrocarbons were stored in sealed bottles for gas chromatography determination. The detection limit of this developed method was 0. 007 - 0. 057 μL/kg with relative standard deviation (RSD) of 0.8% -1. 1%. The relative deviation (RD) of two independent tests for 105 samples varied from 0.01% to 19.66% with an average of 7. 81% (calculated by methane). This proposed method is suitable for the determination of acidolysis hydrocarbons in oil/gas geochemical exploration samples and has been successfully used in natural gas hydrate prospecting.
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