摘要
采用气相色谱-质谱法(GC/MS)在选择离子监测(SIM)模式下,以对氟溴苯、溴苯、溴代环己烷、对二氯苯、间二氯苯、邻二氯苯、对溴氯苯、1,3,5-三氯苯、1,2,4-三氯苯、对二溴苯、1,2,3-三氯苯和溴代十二烷为研究对象,建立了12种卤代烃石油示踪剂的快速分析方法。采用HP-5色谱柱(phenyl methyl siloxane,60 m×320μm×0.25μm)分离,载气(N 2)流速1.0 mL/min。升温程序:初始温度90℃,保持2 min,以5℃/min升温至100℃,保持2 min,以10℃/min升温至200℃,保持5 min。进样口温度300℃,进样量2μL,离子源温度260℃,辅助加热温度280℃,选择离子监测(SIM)模式定量分析。结果表明,12种卤代烃示踪剂在10~10000μg/L浓度范围内的线性关系良好,最低检出限可达10~4μg/L,准确度和加标回收率均符合要求。该方法样品前处理简单、快速、灵敏,可为石油开发过程中有机物示踪剂检测提供技术参考。
Halogenated hydrocarbon organic tracer is a kind of chemical tracer,which has the characteristics of less adsorption on the bottom surface and easy to be detected.In this research,gas chromatography-mass spectrometry(GC/MS)was applied to analyse p-fluorobromobenzene,bromobenzene,bromocyclohexane,p-dichlorobenzene,m-dichlorobenzene,o-dichlorobenzene,p-bromochlorobenzene,1,3,5-trichlorobenzene,1,2,4-trichlorobenzene,p-dibromobenzene,1,2,3-trichlorobenzene and bromododecane as twelve halogenated hydrocarbon organic petroleum tracer.The separation was performed on a Kromasil HP-5 column(phenyl methyl siloxane,60 m×320μm×0.25μm).The carrier gas(N 2)was at a flow rate of 1.0 mL/min.Quantitative analysis of halogenated hydrocarbon organic petroleum tracer was carried out by electron ionization(EI)source and selective ion monitoring(SIM)mode,the sample inject volume was 2μL,the ion source temperature was 260℃and the auxiliary heating temperature was 280℃.The results showed that twelve halogenated hydrocarbon organic petroleum tracer had good linear relationship in the range of 10-10000μg/L,the limit detection was 10-4μg/L,and the standard addition recovery rate was less than 3%.This method has good precision,sensitive,simple and rapid pretreatment,which is suitable for determine the content of petroleum tracer,also can provide a technical way for petroleum tracer detection in the process of petroleum development.
作者
闫峻
冯硕
李博文
徐静
王志龙
崔建勇
YAN Jun;FENG Shuo;LI Bo-wen;XU Jing;WANG Zhi-long;CUI Jian-yong(Beijing Research Institute of Uranium Geology,Beijing 100029,China)
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2020年第4期379-385,共7页
Journal of Chinese Mass Spectrometry Society
关键词
石油示踪剂
卤代烃
气相色谱-质谱法(GC/MS)
选择离子监测
petroleum tracer
halogenated hydrocarbons
gas chromatography-mass spectrometry(GC/MS)
selective ion monitoring(SIM)
