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高真空与脉冲放电气相色谱联用装置研发及其在岩石脱气化学分析中的应用
引用本文:李立武,刘艳,王先彬,张铭杰,曹春辉,邢蓝田,李中平.高真空与脉冲放电气相色谱联用装置研发及其在岩石脱气化学分析中的应用[J].岩矿测试,2017,36(3):222-230.
作者姓名:李立武  刘艳  王先彬  张铭杰  曹春辉  邢蓝田  李中平
作者单位:甘肃省油气资源研究重点实验室/中国科学院油气资源研究重点实验室, 中国科学院地质与地球物理研究所, 甘肃 兰州 730000,甘肃省油气资源研究重点实验室/中国科学院油气资源研究重点实验室, 中国科学院地质与地球物理研究所, 甘肃 兰州 730000,甘肃省油气资源研究重点实验室/中国科学院油气资源研究重点实验室, 中国科学院地质与地球物理研究所, 甘肃 兰州 730000,兰州大学地质科学与矿产资源学院, 甘肃 兰州 730000,甘肃省油气资源研究重点实验室/中国科学院油气资源研究重点实验室, 中国科学院地质与地球物理研究所, 甘肃 兰州 730000,甘肃省油气资源研究重点实验室/中国科学院油气资源研究重点实验室, 中国科学院地质与地球物理研究所, 甘肃 兰州 730000,甘肃省油气资源研究重点实验室/中国科学院油气资源研究重点实验室, 中国科学院地质与地球物理研究所, 甘肃 兰州 730000
基金项目:国家自然科学基金资助项目(41473062)
摘    要:岩石中气体化学组成的分析具有重要意义。载气保护下的岩石脱气,过程比较复杂;高真空下岩石脱气的气相色谱分析报道较少,一般不能测量气体的总量;真空脱气质谱法对于分子量相近的气体,很难进行测量。针对上述问题,本文研制了高真空岩石样品脱气分析装置,该装置真空度10-4Pa,空白样品压强0.1 Pa,N2含量测量精度为0.63%,标准温压下最少可测样品量1 mm3。将其与带脉冲放电检测器的气相色谱仪联用,实现了岩石脱气及其微升量级气体化学组成的高灵敏气相色谱分析。利用本系统分析了五大连池火山岩、松辽盆地储层岩石和四川盆地页岩样品中释放的气体,结果表明:相比以往的实验装置和方法,该系统能够直接测量岩石脱出气体的总量,分段加热脱气分析样品用量更少,气体组成分析灵敏度更高,检测的主要成分是岩石脱气常见的成分,针对性较强。

关 键 词:高真空电磁破碎  微升量气体  脉冲放电检测器  幔源岩  页岩气
收稿时间:2016/9/8 0:00:00
修稿时间:2017/5/29 0:00:00

Development of a Combined Device with High Vacuum and Pulsed Discharge Gas Chromatography and Its Application in Chemical Analysis of Gases from Rock Samples
LI Li-wu,LIU Yan,WANG Xian-bin,ZHANG Ming-jie,CAO Chun-hui,XING Lan-tian and LI Zhong-ping.Development of a Combined Device with High Vacuum and Pulsed Discharge Gas Chromatography and Its Application in Chemical Analysis of Gases from Rock Samples[J].Rock and Mineral Analysis,2017,36(3):222-230.
Authors:LI Li-wu  LIU Yan  WANG Xian-bin  ZHANG Ming-jie  CAO Chun-hui  XING Lan-tian and LI Zhong-ping
Affiliation:Key Laboratory of Petroleum Resources, Gansu Province, Key Laboratory of Petroleum Resources Research, Institute of Geology and Geophysics, Chinese Academy of Sciences, Lanzhou 730000, China,Key Laboratory of Petroleum Resources, Gansu Province, Key Laboratory of Petroleum Resources Research, Institute of Geology and Geophysics, Chinese Academy of Sciences, Lanzhou 730000, China,Key Laboratory of Petroleum Resources, Gansu Province, Key Laboratory of Petroleum Resources Research, Institute of Geology and Geophysics, Chinese Academy of Sciences, Lanzhou 730000, China,School of Earth Sciences, Lanzhou University, Lanzhou 730000, China,Key Laboratory of Petroleum Resources, Gansu Province, Key Laboratory of Petroleum Resources Research, Institute of Geology and Geophysics, Chinese Academy of Sciences, Lanzhou 730000, China,Key Laboratory of Petroleum Resources, Gansu Province, Key Laboratory of Petroleum Resources Research, Institute of Geology and Geophysics, Chinese Academy of Sciences, Lanzhou 730000, China and Key Laboratory of Petroleum Resources, Gansu Province, Key Laboratory of Petroleum Resources Research, Institute of Geology and Geophysics, Chinese Academy of Sciences, Lanzhou 730000, China
Abstract:The chemical composition of gases trapped in rocks is important information sought in a wide variety of earth science studies; therefore, the analysis of chemical composition of gases in rocks is of great significance. It is tedious for releasing and collecting gases from rocks under carrier gas and chemical analyses. Few works were reported about gas chromatography analysis of rock degassing under high vacuum, and the total amount of gas were not measured mostly. It is difficult for mass spectrometer to analyze gases with similar molecular weights. Because of these problems, a high vacuum rock sample degassing device has been developed. The vacuum of the device is <10-4Pa. The blank sample pressure is <0.1Pa, the accuracy for N2 in the air is 0.63%, the minimum measurable quantity is <1mm3 at standard temperature and pressure. It is combined with a gas chromatograph with a pulsed discharge detector. A high sensitive gas chromatographic analysis of the chemical composition of gases in rocks has been realized. The gas released from Wudalianchi volcanic rocks, Songliao Basin reservoirs and shale samples from Sichuan basin is analyzed by using this system. The result shows that the total amount of gas out of the rock can directly be measured, gas composition analysis is more sensitive compared with the previous experimental device and method, and it is more targeted at the common component of gases released from rocks.
Keywords:high vacuum electromagnetic crushing  micro liter gases  pulsed discharge detector  mantle rock  shale gas
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