CN111751194B - Sampling method for oil gas inclusion components - Google Patents
Sampling method for oil gas inclusion components Download PDFInfo
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- CN111751194B CN111751194B CN201910233764.8A CN201910233764A CN111751194B CN 111751194 B CN111751194 B CN 111751194B CN 201910233764 A CN201910233764 A CN 201910233764A CN 111751194 B CN111751194 B CN 111751194B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
Abstract
The application discloses a sampling method of oil gas inclusion components. The sampling method comprises the following steps: 1) The first organic solvent and the water are mixed with the oil gas inclusion sample; 2) Adding the oil gas inclusion sample and the second organic solvent into the closed first end of the heat transfer container, freezing the second organic solvent into solid, and closing the open second end of the heat transfer container in a vacuum state; 3) Enriching the oil gas component released after bursting the oil gas inclusion sample and the second organic solvent at a second end; 4) Cooling and centrifuging the heat transfer container; 5) And heating the heat transfer container in a water bath, and performing ultrasonic oscillation to obtain a solvent sample enriched with oil gas inclusion components. The application utilizes local heating to realize the immediate enrichment of hydrocarbon components released by the solvent and the oil gas inclusion at the non-heating end after bursting, and overcomes the defect of component change such as thermal cracking of the solvent and the hydrocarbon components after long-term heating.
Description
Technical Field
The application belongs to the field of oil and gas exploration and research, and particularly relates to a sampling method of oil and gas inclusion components, which is further used for efficiently collecting and sampling the oil and gas inclusion components in oil and gas inclusion samples of drilling cores and field geological sections.
Background
The oil-gas inclusion is a geological ancient fluid sample captured in main minerals such as quartz, calcite and the like in the migration path and the reservoir filling process, the components of the oil-gas inclusion embody one of the most important chemical properties of the oil-gas inclusion, reflect key information such as the maturity and sources of the oil gas, and the analysis of the components of the oil-gas inclusion is an important means for carrying out oil-gas reservoir research.
According to the difference of the separation modes of the oil gas inclusion and the main mineral, the oil gas inclusion sampling process can be divided into a grinding method, a micro-drilling method, a thermal explosion method and a laser ablation method. Because of the low content of hydrocarbon inclusions in the geologic sample and the scarcity of the drilling sample, efficient enrichment sampling is an important factor to consider.
Chinese patent application (application number CN 200810101066.4) discloses a quantitative collection system for trace gas in rock group inclusion and a use method thereof: the device comprises a rock sealing grinding unit, a trace gas transferring unit and a trace gas metering unit, wherein a geological sample is placed into the rock sealing grinding unit, and the rock sample is ground and crushed to separate an oil-gas inclusion from main minerals, so that trace gas transfer and metering in the oil-gas inclusion are realized.
Chinese patent application (application number CN 200920108653.6) discloses a hydrocarbon inclusion microcosmic sampler (fig. 1): comprises six parts of a light source system, an objective table 1-2, a micro drill 1-3, a microscopic camera system, a suction pipe system 1-7 and a base 1-1, and is characterized in that: an objective table 1-2 is fixed on the upper plane of the base 1-1. The miniature drill 1-3 is erected on one side surface of the base 1-1, and the light source system comprises a fluorescent light source 1-5, an upper white light source 1-6 and a lower white light source 1-8. The microscopic camera system consists of a camera 1-4, a lens cone, an ocular and an objective lens, and is arranged right above the objective table 1-2. The cameras 1-4 are arranged above the lens barrel and have the same light path with fluorescence. The suction pipe system is fixed on the base 1-1 or is not fixed and independently used. The effect is as follows: the multifunctional performance is realized; sampling the minerals of hydrocarbon inclusion in different periods from a 2cm multiplied by 0.5cm light sheet or inclusion sheet from which asphalt is leached under fluorescence; the method can be used for taking macroscopic vein single minerals from rock samples; microscopic single mineral samples were drilled on rock laminates or rock slide samples.
Chinese patent application (application number CN 201510922506.2) discloses a burst temperature testing instrument for fluid inclusions (fig. 2): the device comprises a helium-neon light source, a beam splitter, a convex lens, a diaphragm, two total reflection mirrors, a quartz test tube, an iron stand, an electronic thermometer, a heating furnace, a photoelectric detector, a USB acquisition card and a computer. Wherein a quartz cuvette is used for holding a geological sample and is subjected to thermal explosion.
Chinese patent application (application number CN 201310690418.5) discloses a method for sampling oil and gas inclusion components (fig. 3): the method comprises the steps of providing a first container and a second container, wherein the outer diameter of the first container is smaller than the inner diameter of the second container, and the first container and the second container are transparent; placing a solvent in a first container and sealing the first container; filling the oil gas inclusion sample into a second container, and filling the obtained sealed first container filled with the solvent into the second container; and (3) degrading the oil gas inclusion sample in the obtained sealed second container by using laser, and then breaking the end, close to the sample, of the first container by using the laser under the condition of keeping the second container intact, so that the solvent in the first container enters the second container, and thus, the components of the oil gas inclusion are fully dissolved in the solvent.
Therefore, the existing experimental device and technology adopt thermal explosion, grinding, micro-drilling and laser ablation to realize the separation of oil gas inclusion and main minerals, the collection of inclusion components is mostly realized by adopting a mode of hot carrier gas blowing or medium-low temperature solvent dissolution, the operation steps are relatively complicated, and the sample consumption is relatively more and inflexible. Therefore, there is a need for a convenient and efficient collection method that uses a small amount of sample and can be flexibly controlled.
Disclosure of Invention
The application aims to solve the problems, and the solvent and the sample are sealed in the heat transfer container at the same time, so that the oil gas inclusion bursts by heating only the sample end during component collection, and the oil gas inclusion components released after bursting and the solvent are enriched at the unheated end by utilizing the temperature difference, thereby avoiding the thermal cracking problem of the oil gas inclusion components and the solvent caused by high temperature.
In order to achieve the above object, the present application provides a sampling method of oil gas inclusion components, the sampling method comprising:
1) Soaking an oil-gas inclusion sample in a first organic solvent, performing ultrasonic cleaning to remove free crude oil and organic matters contained in the oil-gas inclusion sample, and drying to remove the first organic solvent and water;
2) Adding a dried oil gas inclusion sample and a second organic solvent into a heat transfer container, wherein the heat transfer container is an elongated container with one end closed and the other end open, adding the dried oil gas inclusion sample and the second organic solvent into a first end of the heat transfer container closed, immersing the first end into liquid nitrogen to freeze the second organic solvent into solid, vacuumizing to enable the heat transfer container to be in a vacuum state, and then closing the second end of the heat transfer container open;
3) Heating the first end of the heat transfer container to enrich the released oil and gas components and the second organic solvent at the unheated second end of the heat transfer container after bursting the oil and gas inclusion sample;
4) Cooling and centrifuging the heat transfer container to enable the second organic solvent dissolved with the oil gas component and the oil gas inclusion sample to be centrifuged to the same end;
5) And heating the heat transfer container in a water bath and carrying out ultrasonic oscillation to further dissolve residual oil gas inclusion components attached to the surface of the oil gas inclusion sample, thereby obtaining a solvent sample enriched with the oil gas inclusion components.
The proposal utilizes local heating, realizes that hydrocarbon components released by the solvent and the oil gas inclusion after bursting are immediately enriched at a non-heating end (namely a second end), and overcomes the defect that the solvent and the hydrocarbon components are heated for a long time to generate component changes such as thermal cracking, and the like.
According to the method of the application, the oil gas inclusion sample is crushed according to the size of the heat transfer container, and the oil gas inclusion sample is kept at a certain particle size, and preferably, before the step 1), the oil gas inclusion sample is crushed to the particle size of 100-1000 mu m.
According to the method of the present application, in order to sufficiently remove free crude oil and organic matters contained in the oil gas inclusion sample, ultrasonic cleaning and soaking in the first organic solvent are generally alternately performed. The time of ultrasonic cleaning and soaking can be adjusted according to the needs of the person skilled in the art, and as a preferable scheme, the time of ultrasonic cleaning is 20-40 min, and the time of soaking is 16-32 h. In order to ensure that all the free crude oil and organic matters contained therein are removed, the ultrasonic cleaning and soaking modes are preferably carried out for more than 3 times.
According to the method of the application, the drying is aimed at removing the organic solvent and the moisture therefrom. The specific conditions for drying are not particularly limited in the present application, as long as the above requirements are satisfied. Preferably, in step 1), the drying temperature is 70-90 ℃ and the drying time is 20-28 h.
In the preferred scheme, in step 1), after removing the first organic solvent and the water, the method further comprises the step of placing the dried oil gas inclusion sample under a polarized light and/or fluorescence microscope for observation, selecting particles with higher inclusion abundance, and adjusting the particles with higher inclusion abundance according to the needs of a person skilled in the art.
According to the application, in step 2), the amount of the second organic solvent can be adjusted as required by a person skilled in the art, and the smaller the amount, the better the detection requirement is.
Preferably, the first organic solvent and the second organic solvent are each independently selected from at least one of chloroform, dichloromethane and n-hexane.
According to the detection principle of the application, the filling height of the oil gas inclusion sample and the second organic solvent is not more than 10% of the height of the heat transfer container, so that the accuracy of the detection result of the obtained solvent sample enriched in the oil gas inclusion components is ensured. Preferably, the loading height of the oil gas inclusion sample and the second organic solvent should be less than 10% of the height of the heat transfer container and exceed the height of the inclusion sample.
Preferably, in step 3), the heating temperature is 300-400 ℃ and the heating time is 2-5 min.
According to the application, in step 4), the heat transfer vessel is typically cooled to about room temperature.
Preferably, the temperature of the heat transfer container for water bath heating is 70-90 ℃.
According to the method of the application, the size of the container can be flexibly adjusted according to the amount of the sample to be collected.
According to the method of the application, the material of the heat transfer container can be selected according to the requirement, and the material of the heat transfer container is glass or metal as a preferable scheme.
According to the method of the present application, the method of closing the second end of the heat transfer container opening may be a method conventional in the art selected according to the material of the heat transfer container, for example, when the material of the heat transfer container is glass, the method of closing the second end of the heat transfer container opening may be a method of closing with a hydrogen flame gun.
Preferably, the method further comprises: the heat transfer container is ultrasonically cleaned and dried prior to use. More preferably, the number of times of ultrasonic cleaning and drying is not less than 3.
Preferably, the method further comprises withdrawing a solvent sample enriched in oil and gas inclusion components with a sampling needle. The extracted solvent sample can be subjected to analysis such as chromatography-mass spectrometry.
The application has the beneficial effects that:
according to the application, the geological sample and the solvent are placed in the same container, and the container is heated differently, so that after burst components of the oil-gas inclusion in the sample are released, the geological sample and the solvent are spontaneously mixed and enriched together with the solvent at the end far away from the sample (namely the second end), and irreversible changes such as cracking of the solvent and the oil-gas inclusion components caused by overhigh temperature are avoided. The application has simple and flexible operation, and can adopt the heat transfer container with corresponding specification for the sample and the analysis and test means to achieve the experimental purpose.
Compared with the separation characteristic research of a pipeline type oil-water separation system, the method has the greatest characteristics that the method utilizes the solvent to enrich inclusion components in the process of collecting the inclusion components; compared with the Chinese patent application CN200810101066.4, the application solves the problems that trace gas cannot be directly taken out for analysis in a low negative pressure state in a closed container, the transfer and collection are incomplete, the gas taking out analysis is inconvenient, and the quantitative and qualitative analysis of a plurality of subsequent projects cannot be simultaneously carried out in the prior art; compared with the Chinese patent application CN201310690418.5, the application has the greatest characteristics that only a single container is needed in the process of collecting inclusion components, and two containers are not needed for physically separating the solvent and the sample; in contrast to chinese patent application CN200920108653.6, the present application is directed to the collection of inclusion components in a closed rather than open system.
Additional features and advantages of the application will be set forth in the detailed description which follows.
Drawings
The above and other objects, features and advantages of the present application will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings.
Fig. 1 shows a schematic diagram of a hydrocarbon inclusion microcosmic sampler of the prior art.
Fig. 2 shows a schematic diagram of a prior art burst temperature testing instrument for fluid inclusions.
FIG. 3 is a schematic diagram of a prior art method of sampling oil and gas inclusion components.
Fig. 4 shows a schematic diagram of the main steps of the method of the application.
FIG. 5 shows a chromatographic-mass spectrometry analysis of the composition of a hydrocarbon inclusion of a group obtained in one embodiment of the application.
FIG. 6 shows a chromatographic-mass spectrometry analysis of a prior art method for sampling oil and gas inclusion components.
Reference numerals illustrate:
1-1 parts of base, 1-2 parts of object stage, 1-3 parts of micro drill, 1-4 parts of camera, 1-5 parts of fluorescent source, 1-6 parts of upper white light source, 1-7 parts of suction pipe system, 1-8 parts of lower white light source, 1-9 parts of negative pressure pump, 1-10 parts of switch, 1-11 parts of main column.
3-1, an oil gas inclusion sample, 3-2, a second quartz capillary tube, 3-3, n-hexane (about 10 μl), 3-4, and a first quartz capillary tube.
1. The method comprises the steps of (1) centrifuging a heat transfer container (2), a first end (3), an oil-gas inclusion sample (4), a second organic solvent (5), a second end (6), a heating table (7), the second organic solvent and the oil-gas inclusion sample to the same end of the heat transfer container, and (8) extracting a solvent sample enriched with oil-gas inclusion components by using a sampling needle.
Detailed Description
Preferred embodiments of the present application will be described in more detail below. While the preferred embodiments of the present application are described below, it should be understood that the present application may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the application to those skilled in the art.
Fig. 4 shows a schematic diagram of the main steps of the method of the application. As shown in fig. 4, the sampling method includes:
1) Soaking an oil-gas inclusion sample in a first organic solvent, performing ultrasonic cleaning to remove free crude oil and organic matters contained in the oil-gas inclusion sample, and drying to remove the first organic solvent and water;
2) Adding a dried oil gas inclusion sample and a second organic solvent into a heat transfer container 1, wherein the heat transfer container is an elongated container with one end closed and the other end open, adding the dried oil gas inclusion sample and the second organic solvent 4 into a first end 2 of the heat transfer container 1, immersing the first end 2 into liquid nitrogen, freezing the second organic solvent 4 into solid, vacuumizing to enable the heat transfer container to be in a vacuum state, and then sealing a second end 5 of the heat transfer container;
3) Heating the first end of the heat transfer container (which can be heated by a heating table 6) to enrich the released oil and gas components and the second organic solvent after bursting the oil and gas inclusion sample at the unheated second end of the heat transfer container;
4) Cooling and centrifuging the heat transfer container to centrifuge the second organic solvent with the oil and gas components dissolved therein and the oil and gas inclusion sample to the same end 7;
5) Heating the heat transfer container in water bath and ultrasonically oscillating to further dissolve residual oil gas inclusion components attached to the surface of the oil gas inclusion sample to obtain a solvent sample enriched with the oil gas inclusion components;
6) And (3) extracting a solvent sample 9 enriched in the oil gas inclusion components by using a sampling needle to be tested.
Example 1
Selecting a certain drilling core sample to sample the components of the group oil gas inclusion, and performing experimental analysis according to the following steps:
1) Mechanically crushing an oil gas inclusion sample, selecting a particle sample with the particle size smaller than 1mm multiplied by 1mm and larger than 0.1mm multiplied by 0.1mm, placing the particle sample under a polarizing/fluorescence microscope, observing, and selecting particles with high abundance of the oil gas inclusion for later use;
2) Soaking the selected oil-gas inclusion sample in chloroform for ultrasonic cleaning for 30min, soaking for 24 hours, repeating the steps of ultrasonic cleaning and soaking for 3 times to remove free crude oil and organic matters contained in the oil-gas inclusion sample, and drying in an oven at 80 ℃ for 24 hours to remove chloroform and water;
3) Cutting a section of quartz glass tube with the length of 10cm and the inner diameter of 1mm and square interface as a heat transfer container, and adopting the ultrasonic cleaning, soaking and drying modes of the step 2) to clean and dry the quartz glass tube;
4) Sealing one end of a quartz glass tube by utilizing a hydrogen flame gun, and sequentially filling 1mg of oil gas inclusion sample and 10 mu L of n-hexane solvent from the unsealed end to the sealed end;
5) Immersing the sealed end into liquid nitrogen to freeze normal hexane in the sealed end into solid, connecting the unsealed end to a vacuum pump through a nut, a sealing gasket and a pipeline for vacuumizing, and sealing the unsealed end by a hydrogen flame gun;
6) The sample end is locally heated by a heating table, the heating temperature is 400 ℃, and the duration time is 2min, so that the oil gas components and n-hexane released after the oil gas inclusion sample bursts are enriched at the unheated end; after the quartz glass tube is cooled to room temperature, putting the quartz glass tube into a centrifuge to centrifuge n-hexane to the same end;
7) Heating the quartz glass tube in a water bath at 80 ℃ and ultrasonically oscillating for 30 minutes, standing for 24 hours, heating in the water bath again and ultrasonically oscillating for 30 minutes, standing for 24 hours, and further dissolving residual oil gas inclusion components attached to the surface of the oil gas inclusion sample to obtain a solvent sample enriched in the oil gas inclusion components;
8) The non-sample end of the heat transfer vessel was opened and 1.5. Mu.l of the inclusion-enriched solvent was withdrawn with a sampling needle for chromatographic mass spectrometry.
The results of the chromatographic mass spectrometry are shown in FIG. 5.
Comparing the chromatographic mass spectrometry chart of example 1 (fig. 4 of the present application) with fig. 4 (fig. 6 of the present application) of the publication of patent No. ZL201310690418.5, an oil and gas inclusion component sampling method, the method of the present application can obtain similar chromatographic mass spectrometry results in geological samples. The present application differs from the comparative patent in that the present application allows analysis to be accomplished with only one vessel (i.e., heat transfer vessel), whereas the comparative patent requires two vessels.
The foregoing description of embodiments of the application has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described.
Claims (4)
1. A method for sampling oil and gas inclusion components, the method comprising:
1) Mechanically crushing an oil gas inclusion sample, selecting a particle sample with the particle size smaller than 1mm multiplied by 1mm and larger than 0.1mm multiplied by 0.1mm, placing the particle sample under a polarizing/fluorescence microscope, observing, and selecting particles with high abundance of the oil gas inclusion for later use;
2) Soaking the selected oil-gas inclusion sample in a first organic solvent, performing ultrasonic cleaning to remove free crude oil and organic matters contained in the oil-gas inclusion sample, and drying to remove the first organic solvent and water;
3) Adding a dried oil gas inclusion sample and a second organic solvent into a heat transfer container, wherein the heat transfer container is an elongated container with one end closed and the other end open, adding the dried oil gas inclusion sample and the second organic solvent into a first closed end of the heat transfer container, immersing the first end into liquid nitrogen to freeze the second organic solvent into solid, vacuumizing to enable the heat transfer container to be in a vacuum state, then sealing the second open end of the heat transfer container, wherein the heat transfer container is a quartz glass tube with a square interface, and sealing the second open end of the heat transfer container by a hydrogen flame gun;
4) Locally heating the first end of the heat transfer container to enrich the released oil gas component and the second organic solvent after bursting the oil gas inclusion sample at the second end of the unheated heat transfer container, wherein the heating temperature is 400 ℃ and the duration is 2min;
5) Cooling and centrifuging the heat transfer container to enable the second organic solvent dissolved with the oil gas component and the oil gas inclusion sample to be centrifuged to the same end;
6) Heating the quartz glass tube in a water bath at 80 ℃ and ultrasonically oscillating for 30 minutes, standing for 24 hours, heating in the water bath again and ultrasonically oscillating for 30 minutes, standing for 24 hours, and further dissolving residual oil gas inclusion components attached to the surface of the oil gas inclusion sample to obtain a solvent sample enriched in the oil gas inclusion components;
7) Opening a non-sample end of the heat transfer container, and extracting 1.5 microliters of the solvent enriched with inclusion components by using a sampling needle to perform chromatographic mass spectrometry analysis;
the loading height of the oil gas inclusion sample and the second organic solvent is less than 10% of the height of the heat transfer container and exceeds the height of the oil gas inclusion sample.
2. The sampling method according to claim 1, wherein in step 2), the drying temperature is 70-90 ℃ and the time is 20-28 h.
3. The sampling method according to claim 1, wherein the first organic solvent and the second organic solvent are each independently selected from at least one of chloroform, dichloromethane and n-hexane.
4. The sampling method of claim 1, wherein the method further comprises: the heat transfer container is ultrasonically cleaned and dried prior to use.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104198251A (en) * | 2014-09-15 | 2014-12-10 | 西安西北有色地质研究院有限公司 | Test tube assembly for low-temperature quick ashing of organic matter sample |
| CN104713742A (en) * | 2013-12-16 | 2015-06-17 | 中国石油化工股份有限公司 | Oil gas inclusion component sampling method |
| CN108956836A (en) * | 2018-05-18 | 2018-12-07 | 中国石油化工股份有限公司 | The release of hydrocarbon gas and extraction element and method in inclusion enclave |
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2019
- 2019-03-26 CN CN201910233764.8A patent/CN111751194B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104713742A (en) * | 2013-12-16 | 2015-06-17 | 中国石油化工股份有限公司 | Oil gas inclusion component sampling method |
| CN104198251A (en) * | 2014-09-15 | 2014-12-10 | 西安西北有色地质研究院有限公司 | Test tube assembly for low-temperature quick ashing of organic matter sample |
| CN108956836A (en) * | 2018-05-18 | 2018-12-07 | 中国石油化工股份有限公司 | The release of hydrocarbon gas and extraction element and method in inclusion enclave |
Non-Patent Citations (1)
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| 密封石英管爆裂法快速分析包裹体中CO2碳同位素;李洪伟 等;《分析化学》;20140131;第42卷(第1期);第127-130页 * |
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