单个油气包裹体检测技术及应用
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摘要
本文综述了近些年来单个包裹体探测的各种技术,包括显微荧光、显微拉曼、显微傅立叶变换红外光谱、同步辐射x射线荧光、质子诱导x射线荧光(Particle Induced X-ray Emissions)、激光剥蚀(消融)电感耦合等离子质谱(LA-ICP-MS)。在此基础上,提出一种基于普通倒置荧光显微镜的单个油气包裹体的紫外-可见显微荧光光谱测量装置,该装置包括倒置荧光显微镜、反射式显微物镜、微透镜、光纤、紫外-可见荧光分光光度计和计算机,通过光纤基座和反射式显微物镜-微透镜-光纤适配器将所有器件结合为一个整体。通过反射式显微物镜-微透镜-光纤适配器上的三维位移台(空间分辨率2μm),反射式显微物镜与倒置荧光显微经的显微物镜很容易共焦,最小光斑12μm。利用本装置可对单个包裹体进行显微定位、显微照相、外光源激发或显微镜内置汞灯激发、紫外-可见显微荧光光谱测量、光谱分析、包裹体色度分析等。
在成功建立实验系统的基础上,本文以吉林油田南部和西部斜坡区中浅层5口油井钻井取心砂岩为研究对象,通过对砂岩薄片进行偏光/荧光显微镜镜下鉴定、包裹体丰度、包裹体均一温度、盐度测量,发现5口井(白95,花5,检22,农29和伏4)均发育两期包裹体。在此基础上,实测了5口井38个典型第2期次油气包裹体在外光源及显微镜内置汞灯激发下的紫外-可见荧光光谱。测量结果表明汞灯激发下的荧光光谱明显受到包裹体周围颗粒和胶结物荧光的影响,因而该光谱不能真实地反映包裹体所含古油的信息。石英颗粒本身也会发出“背景”荧光,因而当聚焦光斑比包裹体大时,必须考滤“背景”荧光的影响。在250nm激发下,通过与标准芳烃荧光光谱的比较,可定性确定包裹体中古油芳烃主成分,油气包裹体中古油主要以中质油为主,含二环、三环、四环或二环、三环、四环、五环芳烃,并且普遍含有五环以上重质芳烃和非烃,依据古油主成分进而推测古油的成熟度和母源的性质。对365nm激发下的单个油气包裹体的荧光光谱,我们定义了一个反映油成熟度的参数—S390-455/S455-680,并建立了S390-455/S455-680与色谱-质谱分析计算的成熟度参数Rc之间的关系。
除此外,我们还测量了5口井29个原油的荧光光谱,对于250nm激发下的荧光光谱,通过与标准芳烃荧光光谱比较,可知原油普遍以二环、三环芳烃为主,另有一定量的四环芳烃,五环以上重质芳烃和非烃远少于油气包裹体中的古油。但农29井泉四段列外,该层砂岩原油含一定的重质芳烃。通过荧光峰位和半高宽定性地确定原油的成熟度,通过Qi参数确定油水界面,结果表明Qi参数对于重质油含量较多或单环芳烃含量较多的原油并非是一个很好的评价参数。对365nm激发下的原油的荧光光谱,我们也建立了S390-455/S455-680与色谱-质谱分析计算的成熟度参数Rc之间的关系。
依据色度学原理,对于单个油气包裹体和原油在365nm激发及包裹体在自身汞灯紫光激发下的荧光光谱进行了色坐标计算。结果表明,原油的色坐标均小于相应层位的包裹体的色坐标,这表明原油的成熟度大于包裹体中古油的成熟度；外光源365nm激发下的色坐标小于显微镜自身汞灯紫光激发下的油气包裹体的色坐标,原因是后者的荧光光谱不受胶结物和石英颗粒自身荧光的影响,其色坐标更真实地反应了油气包裹体本身的颜色；固液包裹体或液态包裹体所含烃比气液包裹体重；外光源激发下同一层位中不同油气包裹体的色坐标覆盖的较宽范围反应了第2期次充注的油气可能来自两个成熟度不同的烃源岩。
本装置的最大特点是无需对显微镜做任何改造,通过普通倒置荧光显微镜和反射式显微物镜相结合,实现了昂贵的紫外显微镜在测量单个油气包裹体紫外-可见显微荧光光谱方面的功能,总体造价大大降低。该装置在透明材料微区显微荧光光谱测量方面具有潜在的应用价值,由于采用了倒置荧光显微镜,该装置还可以用于生物切片微区(细胞、生物包裹体等)紫外-可见显微荧光光谱的测量。
A review, including in micro-fluorescence, micro-Raman spectroscopy, micro-Fourier transformation infrared spectroscopy, synchrotron radiation X-ray fluorescence microprobe, particle induced X-ray emissions and laser ablation inductively coupled plasma mass spectrometry, was presented about the testing techniques for single inclusions in recent years. Based on above techniques, an experimental setup lied on common inverted fluorescence microscope for measuring UV-VIS spectra of single hydrocarbon inclusions was brought up. This setup includes in an inverted fluorescence microscope(IFM), a reflective objective(RO), a micro-lens(ML), a fiber cable, a UV-VIS spectrometer and a computer. All the elements were integrated into a whole system by a fiber base plate and a RO-ML-fiber adaptor. It is easily to make the RO and the objective of the IFM con-focus by a 3D displacement stage with a 2μm space resolution. The minimum diameter of the focal point is 12um. By using this setup one can localize a single hydrocarbon inclusion in the middle of the vision field of the IFM and take photo for it, excite it using external light source or internal mercury lamp of the IFM, measure and analyze the UV-VIS spectrum or calculate the chromaticity coordinates.
After the setup was successfully established, the sandstones from 5 oil wells localized middle-shallow layers in the south and west of Songliao Basin were under studied. The sandstone thin sections were observed under polarized light/fluorescence microscope. The GOI(grains containing oil inclusions), homogeneous temperature and salinity of the inclusions were measured. The above experiment results show that there were two times hydrocarbon accumulation for the strata of the 5 oil wells (Bai 95, Hua 5, Jian 22, Nong 29 and Fu 4). After above experiments, the UV-VIS spectra of 38 typical hydrocarbon inclusions of secondary charge(excited by the external light source or internal mercury lamp of the IFM) from 5 oil wells were measured. The results showed that the spectra excited by the internal mercury lamp were influenced by the fluorescence of the cement and the silicon grains. So the spectra cann't reflect the real information of the palio-oils in the inclusions. When the size of the focal point of the external light source is larger than that of the inclusion, one has to take into account the "background" fluorescence coming from the silicon grain. For the spectra excited by 250nm external light source, by comparison the spectra of the hydrocarbon inclusions with the standard aromatic hydrocarbons, one can quantitative determine the main aromatic hydrocarbons in the inclusions. The palio-oils in the inclusions are mainly middle weight aromatic hydrocarbon, for example, dicyclic, tricyclic, tetracyclic or dicyclic, tricyclic, tetracyclic and petracyclic aromatic hydrocarbons. They all contained some weight aromatic hydrocarbons and nonhydrocarbons. Further more, the maturities of the palio-oils and the source rocks can be quantitative obtained. And for the spectra excited by 365nm external light source, we defined an index S390-455/S455-680, which reflects the maturity of the oil. A relationship between S390-455/S455-680 and Rc calculated by GC-MS experiment was established.
Except for the spectra of single hydrocarbon inclusions, we also measured the UV-VIS spectra of 29 crude oils from these 5 oil wells. For the spectra excited by 250nm light, by comparison the spectra of the crude oils with the standard aromatic hydrocarbons, one can quantitative determine the main aromatic hydrocarbons in the crude oils. The aromatic hydrocarbons in the crude oils are mainly dicyclic and tricyclic aromatics. There are some tetracyclic aromatics in the crude oils. The crude oils of the Nong 29 well are special. There are some weight aromatic hydrocarbons. The weight aromatics and nonhydrocarbons in the crude oils are far less than that in the palio-oils of the hydrocarbon inclusions. And by the peak positions and the HWFHs (half width of full height) of the spectra, one can quantitative determine the maturities of the crude oils. And by Qi index, the oil-water interface was obtained. But the Qi index was limited. For the samples contained more weight hydrocarbons or more single circle aromatic hydrocarbon, it will lose effect. And for the spectra excited by 365nm light, a relationship between S390-455/S455-680 and Rc calculated by GC-MS experiment was also established.
By Colourometry principle, the chromaticity coordinates of the hydrocarbon inclusions, excited by 365nm of the external light source and the violet light of the internal mercury lamp of the IFM, and the crudes oils were calculated. The results showed that:(1) All the chromaticity coordinates of the crude oil are less than the ones of the single inclusions, this indicates that the maturities of the crude oils are higher than the palio-oils in the inclusions; (2) All the chromaticity coordinates of the single hydrocarbon inclusions excited by the external light source are less than that of the ones by internal mercury lamp, which shows the former wasn't influenced by the fluorescence from the cement and the silicon grains. The chromaticity coordinates of the single hydrocarbon inclusions excited by the external light source reflect the real colors of the inclusions; (3) The UV-VIS spectra show that the hydrocarbons contained in the solid-liquid or pure liquid inclusions are more weight than that in the gas-liquid inclusions; (4) The wider chromaticity coordinates ranges of the single hydrocarbon inclusions from same strata reflect the secondary oil charge may come from two maternal sources with different maturities.
The prominent feature of this setup is not necessary make any rebuilt to the microscope. By combining the microscope and the RO, the setup can be used as an expensive UV microscope in measuring the UV-VIS spectra of single hydrocarbon inclusions. The total cost was greatly lowered. It is promising to measure the UV-VIS spectra of micro-size samples. Because the inverted microscope was assumed, it can also be used to measure UV-VIS spectra of bio-samples, such as cells or bio-inclusions.
在成功建立实验系统的基础上,本文以吉林油田南部和西部斜坡区中浅层5口油井钻井取心砂岩为研究对象,通过对砂岩薄片进行偏光/荧光显微镜镜下鉴定、包裹体丰度、包裹体均一温度、盐度测量,发现5口井(白95,花5,检22,农29和伏4)均发育两期包裹体。在此基础上,实测了5口井38个典型第2期次油气包裹体在外光源及显微镜内置汞灯激发下的紫外-可见荧光光谱。测量结果表明汞灯激发下的荧光光谱明显受到包裹体周围颗粒和胶结物荧光的影响,因而该光谱不能真实地反映包裹体所含古油的信息。石英颗粒本身也会发出“背景”荧光,因而当聚焦光斑比包裹体大时,必须考滤“背景”荧光的影响。在250nm激发下,通过与标准芳烃荧光光谱的比较,可定性确定包裹体中古油芳烃主成分,油气包裹体中古油主要以中质油为主,含二环、三环、四环或二环、三环、四环、五环芳烃,并且普遍含有五环以上重质芳烃和非烃,依据古油主成分进而推测古油的成熟度和母源的性质。对365nm激发下的单个油气包裹体的荧光光谱,我们定义了一个反映油成熟度的参数—S390-455/S455-680,并建立了S390-455/S455-680与色谱-质谱分析计算的成熟度参数Rc之间的关系。
除此外,我们还测量了5口井29个原油的荧光光谱,对于250nm激发下的荧光光谱,通过与标准芳烃荧光光谱比较,可知原油普遍以二环、三环芳烃为主,另有一定量的四环芳烃,五环以上重质芳烃和非烃远少于油气包裹体中的古油。但农29井泉四段列外,该层砂岩原油含一定的重质芳烃。通过荧光峰位和半高宽定性地确定原油的成熟度,通过Qi参数确定油水界面,结果表明Qi参数对于重质油含量较多或单环芳烃含量较多的原油并非是一个很好的评价参数。对365nm激发下的原油的荧光光谱,我们也建立了S390-455/S455-680与色谱-质谱分析计算的成熟度参数Rc之间的关系。
依据色度学原理,对于单个油气包裹体和原油在365nm激发及包裹体在自身汞灯紫光激发下的荧光光谱进行了色坐标计算。结果表明,原油的色坐标均小于相应层位的包裹体的色坐标,这表明原油的成熟度大于包裹体中古油的成熟度；外光源365nm激发下的色坐标小于显微镜自身汞灯紫光激发下的油气包裹体的色坐标,原因是后者的荧光光谱不受胶结物和石英颗粒自身荧光的影响,其色坐标更真实地反应了油气包裹体本身的颜色；固液包裹体或液态包裹体所含烃比气液包裹体重；外光源激发下同一层位中不同油气包裹体的色坐标覆盖的较宽范围反应了第2期次充注的油气可能来自两个成熟度不同的烃源岩。
本装置的最大特点是无需对显微镜做任何改造,通过普通倒置荧光显微镜和反射式显微物镜相结合,实现了昂贵的紫外显微镜在测量单个油气包裹体紫外-可见显微荧光光谱方面的功能,总体造价大大降低。该装置在透明材料微区显微荧光光谱测量方面具有潜在的应用价值,由于采用了倒置荧光显微镜,该装置还可以用于生物切片微区(细胞、生物包裹体等)紫外-可见显微荧光光谱的测量。
A review, including in micro-fluorescence, micro-Raman spectroscopy, micro-Fourier transformation infrared spectroscopy, synchrotron radiation X-ray fluorescence microprobe, particle induced X-ray emissions and laser ablation inductively coupled plasma mass spectrometry, was presented about the testing techniques for single inclusions in recent years. Based on above techniques, an experimental setup lied on common inverted fluorescence microscope for measuring UV-VIS spectra of single hydrocarbon inclusions was brought up. This setup includes in an inverted fluorescence microscope(IFM), a reflective objective(RO), a micro-lens(ML), a fiber cable, a UV-VIS spectrometer and a computer. All the elements were integrated into a whole system by a fiber base plate and a RO-ML-fiber adaptor. It is easily to make the RO and the objective of the IFM con-focus by a 3D displacement stage with a 2μm space resolution. The minimum diameter of the focal point is 12um. By using this setup one can localize a single hydrocarbon inclusion in the middle of the vision field of the IFM and take photo for it, excite it using external light source or internal mercury lamp of the IFM, measure and analyze the UV-VIS spectrum or calculate the chromaticity coordinates.
After the setup was successfully established, the sandstones from 5 oil wells localized middle-shallow layers in the south and west of Songliao Basin were under studied. The sandstone thin sections were observed under polarized light/fluorescence microscope. The GOI(grains containing oil inclusions), homogeneous temperature and salinity of the inclusions were measured. The above experiment results show that there were two times hydrocarbon accumulation for the strata of the 5 oil wells (Bai 95, Hua 5, Jian 22, Nong 29 and Fu 4). After above experiments, the UV-VIS spectra of 38 typical hydrocarbon inclusions of secondary charge(excited by the external light source or internal mercury lamp of the IFM) from 5 oil wells were measured. The results showed that the spectra excited by the internal mercury lamp were influenced by the fluorescence of the cement and the silicon grains. So the spectra cann't reflect the real information of the palio-oils in the inclusions. When the size of the focal point of the external light source is larger than that of the inclusion, one has to take into account the "background" fluorescence coming from the silicon grain. For the spectra excited by 250nm external light source, by comparison the spectra of the hydrocarbon inclusions with the standard aromatic hydrocarbons, one can quantitative determine the main aromatic hydrocarbons in the inclusions. The palio-oils in the inclusions are mainly middle weight aromatic hydrocarbon, for example, dicyclic, tricyclic, tetracyclic or dicyclic, tricyclic, tetracyclic and petracyclic aromatic hydrocarbons. They all contained some weight aromatic hydrocarbons and nonhydrocarbons. Further more, the maturities of the palio-oils and the source rocks can be quantitative obtained. And for the spectra excited by 365nm external light source, we defined an index S390-455/S455-680, which reflects the maturity of the oil. A relationship between S390-455/S455-680 and Rc calculated by GC-MS experiment was established.
Except for the spectra of single hydrocarbon inclusions, we also measured the UV-VIS spectra of 29 crude oils from these 5 oil wells. For the spectra excited by 250nm light, by comparison the spectra of the crude oils with the standard aromatic hydrocarbons, one can quantitative determine the main aromatic hydrocarbons in the crude oils. The aromatic hydrocarbons in the crude oils are mainly dicyclic and tricyclic aromatics. There are some tetracyclic aromatics in the crude oils. The crude oils of the Nong 29 well are special. There are some weight aromatic hydrocarbons. The weight aromatics and nonhydrocarbons in the crude oils are far less than that in the palio-oils of the hydrocarbon inclusions. And by the peak positions and the HWFHs (half width of full height) of the spectra, one can quantitative determine the maturities of the crude oils. And by Qi index, the oil-water interface was obtained. But the Qi index was limited. For the samples contained more weight hydrocarbons or more single circle aromatic hydrocarbon, it will lose effect. And for the spectra excited by 365nm light, a relationship between S390-455/S455-680 and Rc calculated by GC-MS experiment was also established.
By Colourometry principle, the chromaticity coordinates of the hydrocarbon inclusions, excited by 365nm of the external light source and the violet light of the internal mercury lamp of the IFM, and the crudes oils were calculated. The results showed that:(1) All the chromaticity coordinates of the crude oil are less than the ones of the single inclusions, this indicates that the maturities of the crude oils are higher than the palio-oils in the inclusions; (2) All the chromaticity coordinates of the single hydrocarbon inclusions excited by the external light source are less than that of the ones by internal mercury lamp, which shows the former wasn't influenced by the fluorescence from the cement and the silicon grains. The chromaticity coordinates of the single hydrocarbon inclusions excited by the external light source reflect the real colors of the inclusions; (3) The UV-VIS spectra show that the hydrocarbons contained in the solid-liquid or pure liquid inclusions are more weight than that in the gas-liquid inclusions; (4) The wider chromaticity coordinates ranges of the single hydrocarbon inclusions from same strata reflect the secondary oil charge may come from two maternal sources with different maturities.
The prominent feature of this setup is not necessary make any rebuilt to the microscope. By combining the microscope and the RO, the setup can be used as an expensive UV microscope in measuring the UV-VIS spectra of single hydrocarbon inclusions. The total cost was greatly lowered. It is promising to measure the UV-VIS spectra of micro-size samples. Because the inverted microscope was assumed, it can also be used to measure UV-VIS spectra of bio-samples, such as cells or bio-inclusions.
引文
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