气相色谱法同时测定10种卤代烃石油示踪剂的方法研究  

Study on the Determination Method of 10 Petroleum Tracers by Gas Chromatography

作　　者：李博文 徐静[1] 李伯平[1] 闫峻[1] LI Bowen;XU Jing;LI Boping;YAN Jun(Beijing ResearchInstitute of Uranium Geology,Beijing 100029 China)

机构地区：[1]核工业北京地质研究院,北京100029

出　　处：《世界核地质科学》2022年第4期757-765,共9页World Nuclear Geoscience

摘　　要：建立了一种中性氧化铝固相萃取(Al2O3)-负压溶剂蒸发(NPSE)-气相色谱(GC)-电子捕获检测(ECD)同时测定10种卤代烃石油示踪剂(对氟溴苯、溴苯、溴代环己烷、间二氯苯、对二氯苯、邻二氯苯、对二溴氯苯、对二溴苯、1,2,3-三氯苯、溴代十二烷)的方法。方法前处理:准确称取1.00 g原油样品至20 mL顶空瓶中,加入10.00 mL重蒸馏正己烷稀释。移取1.00 mL稀释后的样品加入填有中性氧化铝的固相萃取柱中净化,使用10 mL重蒸馏正己烷洗脱至比色管中。采用负压溶剂蒸发提取富集装置浓缩洗脱液至1 mL以下,用重蒸馏正己烷定容至1.00 mL上机测试。采用HP-5毛细管色谱柱(5%Phenyl Methyl Siloxane,30.0 m×320μm×0.25μm)分析,对气相色谱仪分析条件进行优化并获得最佳条件,初温90℃出峰时间短,分析总时长为25 min,分离效果好。通过对实际原油样品和标准物质进行测试,结果表明:10种卤代烃石油示踪剂的线性良好,相关系数r2≥0.998;方法精密度好,平行测定10次的相对标准偏差(RSD)均小于2%;根据3倍信噪比确定的检出限介于0.004~0.250 mg·L-1之间;加标回收率介于93.6%~113%之间。该方法快捷简单,精密度高,准确度好,能满足实际需求,适用于原油样品中10种卤代烃石油示踪剂的大批量测定。This paper established a method to simultaneously determine 10 halogentated hydrocarbon petroleum tracer (p-fluoro bromo benzene,bromobenzene,bromocyclohexane,mdichlorobenzene,p-dichlorobenzene,o-dichlorobenzene,p-dibromochlorobenzene,pdibromobenzene,1,2,3-trichlorobenzene,bromododecane) by Al2O3packed solid phase extraction column-vacuum solvent evaporation extraction-gas chromatography-electron capture detector.In Sample pretreatment,1.00 g of petroleum sample was weighted into a 20 mL headspace bottle,and 10.00 mL distilled n-hexane was added to dilute.then 1.00 mL diluted sample was transferred to the solid phase extraction column which filled with neutral Al2O3to purification,and10 mL distill n-hexane was eluted into colorimetric tube.Before the detection,Negative pressure solvent evaporation extraction and enrichment device was used to concentrate the eluent to less than 1 mL,and distilled n-hexane was added to 1.00 mL for test.In the test,HP-5 capillary column (5% Phenyl Methyl Siloxane,30.0 m×320μm×0.25μm) was equipped to analysis.The optimum condition for gas chromatography was obtain:the initial temperature was 90℃ and the total analysis times was 25 min.The result showed that the liner correlation coefficient r~2≥0.998 and relative standard deviation (RSD) was less than 2.0%,the detection limit was 0.004~0.250 mg·L-1and the recovery rates was between 93.6%~113%,which can satisfy the needs of real petroleum samples.Therefore,the study provided a fast,accurate and precise method which can applied to batch-analysis of petroleum samples.

关 键 词：石油示踪剂 中性氧化铝 卤代烃 气相色谱-电子捕获 

分 类 号：TE39[石油与天然气工程—油气田开发工程] O657.71[理学—分析化学]