页岩油气储层压裂返排液中卤代烃的吹扫捕集-气相色谱/质谱法检测

Determination of halogenated hydrocarbons in outlet fluid for shale oil and gas reservoir fracturing by purge-and-trap and GC-MS

郭威 黄春华 赵雄虎 张小涛 沈斌 汪双清 孙玮琳

Guo Wei Huang Chunhua Zhao Xionghu Zhang Xiaotao Shen Bin Wang Shuangqing Sun Weilin

国家地质实验测试中心 油气能源地球化学研究室, 北京 100037 2. 中国石油大学(北京) 钻井液实验室, 北京 102249

Oil & Gas Geochemistry Department, National Research Center for Geoanalysis, Beijing 100037, China 2. Drilling Fluid Laboratory, China University of Petroleum(Beijing), Beijing 102249, China

在页岩油气开采中，化学示踪技术可以有效应用于评价储层压裂改造效果。化学示踪剂技术推广应用的先决条件在于其相应的分析检测方法。通过研究筛选出了21种化学性质稳定、地层背景值低的卤代烃作为示踪剂，建立了基于吹扫捕集气相色谱-质谱联用（GC-MS）的高灵敏度检测方法。对吹扫捕集、气相色谱-质谱条件进行了优化并获得了最佳条件。结果表明：方法的检出限为0.027~0.162 μg/L，基体加标回收率在74.16%~121.9%之间，精密度（相对标准偏差RSD，n=7）小于12.79%。该方法简单、快捷，适用于页岩油气储层压裂液中所述卤代烃示踪剂的检测。

In shale oil and gas exploration, chemical tracer technology is effectively applied to the evaluation of fracturing technology. The precondition for the application of this technology is the establishment of corresponding analysis method. The authors selected 21 kinds of halogenated hydrocarbons as tracer, with stable chemistry character and low stratigraphic background values. And a high sensitivity detection method for the tracer by purge-and-trap and gas chromatography mass spectrometry (GC-MS) was developed. The conditions of purge-and-trap and GC-MS were optimized and the optimum conditions were obtained. The results showed that the detection limits were 0.027-0.162 μg/L. The average recoveries were 74.16%-121.9% with a precision lower than 12.79% (RSD, n=7). The established method is simple and fast, hence is applicable for the determination of tracer in fracturing outlet fluid samples after reservoir reconstruction.

国家重大科技专项（2016ZX05034-003）和中国地质调查项目（DD20160184）资助。

https://doi.org/10.11781/sysydz201706865