气相色谱-质谱法测定石油中十二种卤代烃示踪剂

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(N₂)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10～10 000μg/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。

Determination of Twelve Halogenated Hydrocarbon Organic Tracers in Petroleum by GC/MS

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×320 μm×0.25 μm). The carrier gas (N2) 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 2 μL, 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 10-10 000 μg/L, the limit detection was 10.4 μg/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.