CN116794007A - Determination method of gas-liquid ratio of fluid inclusion and sub-minerals - Google Patents
Determination method of gas-liquid ratio of fluid inclusion and sub-minerals Download PDFInfo
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- CN116794007A CN116794007A CN202310176122.5A CN202310176122A CN116794007A CN 116794007 A CN116794007 A CN 116794007A CN 202310176122 A CN202310176122 A CN 202310176122A CN 116794007 A CN116794007 A CN 116794007A
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- liquid ratio
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- 239000012530 fluid Substances 0.000 title claims abstract description 87
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 26
- 239000011707 mineral Substances 0.000 title claims abstract description 26
- 239000007788 liquid Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- 238000005259 measurement Methods 0.000 claims abstract description 8
- 230000000877 morphologic effect Effects 0.000 claims abstract description 5
- 239000007791 liquid phase Substances 0.000 claims description 15
- 239000012071 phase Substances 0.000 claims description 14
- 239000007790 solid phase Substances 0.000 claims description 12
- 238000001069 Raman spectroscopy Methods 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 7
- 239000011435 rock Substances 0.000 claims description 4
- 238000000095 laser ablation inductively coupled plasma mass spectrometry Methods 0.000 claims description 3
- 238000004452 microanalysis Methods 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 239000000446 fuel Substances 0.000 abstract 2
- 238000009792 diffusion process Methods 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 7
- 239000002244 precipitate Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 210000003000 inclusion body Anatomy 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000004514 thermodynamic simulation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a method for measuring gas-liquid ratio of fluid inclusion and sub-mineral, which relates to the field of carbon paper of fuel cells, and solves the problems that the existing carbon paper for a gas diffusion layer of the fuel cells is easy to leave clamping marks or damage the carbon paper, and the fixed position of a clamp cannot be coated to cause waste of carbon paper resources; the method comprises the steps of cutting the fluid inclusion sheet layer by layer, then adopting a scanning electron microscope to scan and measure each layer, finally obtaining the morphological structure in the fluid inclusion, then establishing a three-dimensional model through a three-dimensional modeling technology, and calculating the volume of the three-dimensional model. The method has the characteristics of low operation cost, comprehensive measurement data and accurate settlement result.
Description
Technical Field
The invention relates to the field of fluid inclusion determination and analysis, in particular to a determination method of a gas-liquid ratio of a fluid inclusion and a sub-mineral.
Background
Fluid inclusions are original geological fluids in which minerals are historically captured and trapped in mineral crystal defects during crystal growth in a hydrothermal system, often containing gas phase, liquid phase, solid sub-minerals, and the like, within the fluid inclusions. The volume of the fluid inclusions is extremely small, typically elliptical cavities with diameters of 1-10 microns, with small amounts of 20 microns or even larger, and the sub-mineral diameters within the fluid inclusions are typically 1-3 microns. Despite its small volume, the fluid enclosure maintains fluid geochemical information of the current geological environment, such as temperature, pressure, composition, etc. Parameters such as the volume of the fluid package and the ratio of gas to liquid (the ratio of the gas phase part to the liquid phase part) are important parameters for carrying out the thermodynamic simulation of the fluid package, and can be used for calculating physical and chemical conditions such as the pressure of the captured fluid. The sub-minerals in the fluid inclusion are formed by hot fluid minerals which are sealed at the defect of the mineral crystal or by cooling and crystallizing the sealed hot fluid. Analysis of the sub-mineral matter composition may reveal geological information such as the geological history, the matter composition of the original hydrothermal fluid, and the like.
However, when the existing analysis is performed on the gas-liquid ratio in the fluid inclusion, the error is large, because some of the analysis needs to be performed on the volume and the space in the fluid inclusion in a frozen state, so that the volume of a liquid-phase object in the fluid inclusion may also change due to freezing and solidification, and meanwhile, the measurement also causes that solid-phase substances are contained in the fluid inclusion when the substance in the liquid-phase state is measured in the fluid inclusion, so that the error is further increased, and the measurement on the components and the content of each phase of substances in the fluid inclusion cannot be conveniently performed. Therefore, a determination method of the gas-liquid ratio of the fluid inclusion and the sub-minerals is provided.
Disclosure of Invention
The invention aims to provide a method for measuring the gas-liquid ratio of a fluid inclusion and sub-minerals, which solves the problems that solid phase substances are possibly mixed when the gas-liquid ratio of the fluid inclusion is measured, the volume measurement of liquid phase substances is not accurate enough, the error is large, and the components and the content of each phase of substances are inconvenient to measure.
In order to achieve the above purpose, the present invention provides the following technical solutions: a method for determining the gas-liquid ratio of a fluid inclusion and a sub-mineral comprises the following steps:
s1: tabletting the rock sample, grinding the two-sided polished thin sheets, and obtaining a conventional fluid inclusion thin sheet;
s2: performing standard sample correction on a laser Raman spectrometer, and performing gas phase, liquid phase, solid phase components and content test analysis on a fluid inclusion on the Raman spectrometer;
s3: cutting the fluid inclusion sheet layer by layer until the fluid inclusion can penetrate the measurement;
s4: synchronously scanning and measuring each section of the fluid inclusion by using a scanning electron microscope during cutting, and establishing the overall morphological characteristics of the fluid inclusion by using a three-dimensional modeling technology;
s5: and (3) calculating and establishing an internal space of the fluid inclusion by a three-dimensional modeling technology, and calculating the gas-liquid ratio according to the gas phase, the liquid phase, the solid phase components and the content data obtained in the step (S2).
Preferably, the thickness of the fluid inclusion sheet in S1 is 10-120 μm.
Preferably, in S3, the fluid inclusion sheet is polished and cut layer by using a micron-sized polisher.
Preferably, the cutting depth of each layer in the S3 is 10-25 μm.
Preferably, in the step S4, the scanning electron microscope is used to scan each cut fluid inclusion sheet to ensure that the fluid inclusion sheets are located at the same position each time.
Preferably, the determination of the gas phase, liquid phase, solid phase components and content in the fluid inclusion in S2 may also be performed by micro-drilling-ultra-micro analysis, laser ablation inductively coupled plasma mass spectrometry.
Compared with the related art, the method for measuring the gas-liquid ratio of the fluid inclusion and the sub-minerals has the following beneficial effects:
the invention provides a method for determining gas-liquid ratio of fluid inclusion and sub-mineral, which is characterized in that rock is made into a fluid inclusion sheet, then the inclusion of one fluid in the fluid inclusion sheet is directly selected, and the gas phase, liquid phase, solid phase components and content in the fluid inclusion are tested and analyzed on a Raman instrument by using a laser Raman spectroscopy, so that the components and the content in the fluid inclusion are conveniently analyzed directly with high precision.
The invention provides a method for determining the gas-liquid ratio of a fluid inclusion and sub-minerals, which comprises the steps of cutting a fluid inclusion sheet layer by layer, scanning and determining each layer by adopting a scanning electron microscope, finally obtaining a morphological structure in the fluid inclusion, establishing a three-dimensional model by a three-dimensional modeling technology, calculating the volume of the three-dimensional model, and not only effectively improving the accurate calculation of the internal volume of the fluid inclusion, but also improving the calculation of the gas-liquid ratio in the fluid inclusion.
The method has the characteristics of low operation cost, comprehensive measurement data and accurate settlement result.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully, and it is apparent that the embodiments described are only some, but not all, of the embodiments of the present invention; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment one:
the invention provides a technical scheme that: a method for determining the gas-liquid ratio of a fluid inclusion and a sub-mineral comprises the following steps:
s1: tabletting the rock sample, grinding the two polished sheets to obtain a conventional fluid inclusion sheet, and controlling the thickness of the inclusion sheet to be 10-120 mu m;
s2: performing standard sample correction on a laser Raman spectrometer, performing gas phase, liquid phase, solid phase component and content test analysis on the fluid inclusion on the Raman spectrometer, and determining and selecting one of a plurality of fluid inclusions on the fluid inclusion sheet as a target fluid inclusion;
s3: using a micron-sized grinding machine to grind and cut the fluid inclusion sheet layer by layer until the fluid inclusion can be penetrated and measured, wherein the cutting depth of each layer is controlled to be the same and is 10-25 mu m;
s4: scanning and measuring each section of the fluid inclusion by using a scanning electron microscope synchronously during cutting, wherein the scanning electron microscope ensures that each cut fluid inclusion sheet is positioned at the same measuring position when scanning each cut fluid inclusion sheet, and the overall morphological characteristics of the target fluid inclusion which is selected before are established by a three-dimensional modeling technology;
s5: and (3) calculating and establishing an internal space of the fluid inclusion by a three-dimensional modeling technology, and calculating the gas-liquid ratio according to the gas phase, the liquid phase, the solid phase components and the content data obtained in the step (S2).
Embodiment two:
and S2, measuring the gas phase, liquid phase and solid phase components and the content in the fluid inclusion body by a micro-drilling-ultra-micro analysis method and a laser ablation inductively coupled plasma mass spectrometry method.
In particular when using a micro-drill-ultra-micro assay:
before the fluid inclusion is cut layer by layer, the following is performed:
(1) firstly, polishing the polished thin sheet under a binocular (soluble minerals can be dissolved by fine water flow), so that the inclusion to be measured is as close to the surface of the sample as possible, and is generally within tens of micrometers.
(2) Penetrating the inclusion with sharp steel needle or carbon needle, inserting the special conical capillary into the exposed inclusion rapidly, and allowing brine to enter the capillary rapidly or slowly under capillary siphoning action; the measurement of the solution volume was performed under a microscope with a cross-reticle.
(3) Placing the capillary under the binoculars, reacting with a drop of reactant prepared in advance on the microscope stage, and observing the precipitation reaction process under the microscope; and after the reaction is complete, rapidly transferring the capillary to an alcohol lamp for sealing.
(4) And horizontally placing the sealed capillary tube in a centrifuge, centrifuging for 15-20 min, compressing the precipitate to the tail end of the capillary tube, measuring the diameter of the capillary tube under a mirror, estimating the volume of the precipitate, substituting the volume of the precipitate into a mathematical relation in table 1, and calculating the content of the element to be detected.
Table 1:
note that:the average volume of precipitate, expressed in%, relative to the volume of the initial solution; the content unit of the element to be measured is calculated as g/L.
Claims (6)
1. A method for determining the gas-liquid ratio of a fluid inclusion and a sub-mineral, comprising the steps of:
s1: tabletting the rock sample, grinding the two-sided polished thin sheets, and obtaining a conventional fluid inclusion thin sheet;
s2: performing standard sample correction on a laser Raman spectrometer, and performing gas phase, liquid phase, solid phase components and content test analysis on a fluid inclusion on the Raman spectrometer;
s3: cutting the fluid inclusion sheet layer by layer until the fluid inclusion can penetrate the measurement;
s4: synchronously scanning and measuring each section of the fluid inclusion by using a scanning electron microscope during cutting, and establishing the overall morphological characteristics of the fluid inclusion by using a three-dimensional modeling technology;
s5: and (3) calculating and establishing an internal space of the fluid inclusion by a three-dimensional modeling technology, and calculating the gas-liquid ratio according to the gas phase, the liquid phase, the solid phase components and the content data obtained in the step (S2).
2. The method for measuring a gas-liquid ratio of a fluid inclusion and a sub-mineral according to claim 1, wherein the thickness of the fluid inclusion sheet in S1 is 10 to 120 μm.
3. The method for determining gas-liquid ratio of fluid inclusions and sub-minerals according to claim 1, wherein the step S3 is performed by polishing and cutting the fluid inclusion sheet layer by layer using a micron-sized polishing machine.
4. The method for determining gas-liquid ratio and sub-minerals of claim 1, wherein the depth of cut of each layer in S3 is 10-25 μm.
5. The method for determining gas-liquid ratio of fluid inclusion and sub-mineral according to claim 1, wherein the scanning electron microscope is used for scanning each cut fluid inclusion sheet in S4 to ensure that each fluid inclusion sheet is in the same position.
6. The method for determining gas-liquid ratio and sub-minerals of a fluid inclusion according to claim 1, wherein the determination of gas phase, liquid phase, solid phase components and content in the fluid inclusion in S2 is further performed by micro-drilling-ultra micro-analysis, laser ablation inductively coupled plasma mass spectrometry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310176122.5A CN116794007A (en) | 2023-02-28 | 2023-02-28 | Determination method of gas-liquid ratio of fluid inclusion and sub-minerals |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310176122.5A CN116794007A (en) | 2023-02-28 | 2023-02-28 | Determination method of gas-liquid ratio of fluid inclusion and sub-minerals |
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| Publication Number | Publication Date |
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| CN116794007A true CN116794007A (en) | 2023-09-22 |
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| CN202310176122.5A Pending CN116794007A (en) | 2023-02-28 | 2023-02-28 | Determination method of gas-liquid ratio of fluid inclusion and sub-minerals |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117789205A (en) * | 2024-01-05 | 2024-03-29 | 中国矿业大学 | Fluid inclusion analysis method and system based on target detection and semantic segmentation |
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2023
- 2023-02-28 CN CN202310176122.5A patent/CN116794007A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117789205A (en) * | 2024-01-05 | 2024-03-29 | 中国矿业大学 | Fluid inclusion analysis method and system based on target detection and semantic segmentation |
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