Shale oil in-situ determination method and device

Abstract

The invention provides a shale oil in-situ determination method and device, and the method comprises the steps: obtaining a first plate-shaped sample and a second plate-shaped sample from an oil-containing shale sample, carrying out polishing treatment on the second plate-shaped sample, testing the first plate-shaped sample by adopting a nuclear magnetic resonance relaxation spectrum technology, and determining the shale oil in-situ. Acquiring the content of the retained oil of the first plate-shaped sample in an original state, placing the polished second plate-shaped sample in a field emission scanning electron microscope under a preset target acceleration voltage, and observing and recording the occurrence state of the retained oil in pores of the second plate-shaped sample, and analyzing the content of the shale retention oil and the occurrence state of the shale retention oil in different pores based on the content and the occurrence state of the shale retention oil.

Description

Technical Field

[0001] This application relates to the field of shale oil exploration technology, and more specifically, to a method and apparatus for in-situ determination of shale oil. Background Technology

[0002] Shale oil is primarily found in nanoscale pore-throat systems. Within this extremely confined space, the physicochemical properties of the fluid undergo significant changes, leading to exceptionally complex occurrence phases and fluidity of shale oil. Therefore, characterization techniques for the occurrence state and content of shale oil are crucial for determining its efficient exploitation potential.

[0003] Currently, the characterization of shale oil occurrence and content mainly relies on various separation techniques, such as the pyrolysis S1 method (Rock-Eval analysis), and traditional characterization techniques such as field emission scanning electron microscopy (FESEM) or nuclear magnetic resonance (NMR). In addition, in recent years, some studies have attempted to combine multiple techniques (such as FIB-SEM and micro-CT) to analyze pore structure.

[0004] However, while the S1 pyrolysis method determines free hydrocarbon content by heating rock samples to 300℃, light hydrocarbon components (C6-13) are easily lost during sample storage and crushing, leading to serious deviations in oil content evaluation results. FESEM requires carbon plating or oil washing of samples, destroying the original occurrence state of the retained oil. Although NMR can quantitatively analyze oil content, it is difficult to provide spatial distribution and morphological information. Furthermore, combining multiple techniques to analyze pore structure makes it difficult to achieve in-situ characterization of shale oil occurrence state and content. Additionally, it is difficult to simultaneously perform quantitative and imaging analysis on the same sample, and sample pretreatment (such as fluid saturation and cryogenic grinding) may introduce human interference. Summary of the Invention

[0005] In view of this, the purpose of this application is to provide a method and apparatus for in-situ determination of shale oil. The method uses nuclear magnetic resonance relaxation spectroscopy to test a first plate-shaped sample to obtain the content of retained oil in its original state. A polished second plate-shaped sample is then placed in a field emission scanning electron microscope to obtain the occurrence state of retained oil in the pores. Based on the content and occurrence state of the retained oil, the method comprehensively analyzes the content and occurrence state of the shale oil, avoiding serious deviations in oil content evaluation results and damage to the original occurrence state of the retained oil. It can provide spatial distribution and morphological information, enabling in-situ characterization of the occurrence state and content of shale oil. This achieves integrated quantitative and imaging characterization on the same sample simultaneously, and avoids human interference during sample pretreatment.

[0006] In a first aspect, embodiments of this application provide a method for in-situ determination of shale oil, the method comprising: A first plate-shaped sample and a second plate-shaped sample were obtained from the oil-bearing shale sample, and the second plate-shaped sample was polished. The first plate-shaped sample was tested using nuclear magnetic resonance relaxation spectroscopy to obtain the residual oil content of the first plate-shaped sample in its original state. The polished second plate-shaped sample was placed in a field emission scanning electron microscope under a preset target accelerating voltage to observe and record the state of oil retention in the pores of the second plate-shaped sample. The content of shale oil and its occurrence state in different pores are analyzed based on the content of the retained oil and the occurrence state.

[0007] In one possible implementation, obtaining the first plate-shaped sample and the second plate-shaped sample includes: Wire cutting technology was used to obtain plate-shaped samples of the target size from shale cores; The plate-shaped sample is divided into a first plate-shaped sample and a second plate-shaped sample.

[0008] In one possible implementation, the polishing process of the second plate-shaped sample includes: The second plate-shaped sample is fixed on the sample holder, and the second plate-shaped sample is mechanically polished in sequence using sandpaper of different grit sizes; The second plate-shaped sample was polished using an argon ion polisher with preset target parameters.

[0009] In one possible implementation, observing and recording the state of the oil retained in the pores of the second plate-shaped sample includes: The imaging mode of the field emission scanning electron microscope is set to low-voltage secondary electron mode; Under the condition that the second plate-shaped sample is not carbonized, the presence state of the oil retained in the pores of the second plate-shaped sample is directly observed and recorded by the field emission scanning electron microscope.

[0010] In one possible implementation, the testing of the first plate-shaped sample using nuclear magnetic resonance relaxation spectroscopy includes: For the first plate-shaped sample, target test parameters for relaxation spectrum testing of the first plate-shaped sample are determined; wherein, the target test parameters include at least resonance frequency, echo time, waiting time, and number of scans; The relaxation spectrum of the first plate-shaped sample was tested using a preset nuclear magnetic resonance spectrometer under the target test parameters. In one possible implementation, obtaining the retained oil content of the first plate-shaped sample in its original state includes: Obtain the corresponding relaxation signal in the original state; calculate the residual oil content of the first plate-shaped sample based on the relaxation signal.

[0011] In one possible implementation, the method further includes: The first plate-shaped sample and the second plate-shaped sample were tested repeatedly.

[0012] Secondly, embodiments of this application also provide an in-situ shale oil testing device, the device comprising: The acquisition module is used to acquire a first plate-shaped sample and a second plate-shaped sample from an oil-bearing shale sample, and to polish the second plate-shaped sample. The first testing module is used to test the first plate-shaped sample using nuclear magnetic resonance relaxation spectroscopy to obtain the residual oil content of the first plate-shaped sample in its original state. The second test module is used to place the polished second plate-shaped sample in a field emission scanning electron microscope under a preset target accelerating voltage to observe and record the state of oil retention in the pores of the second plate-shaped sample. The analysis module is used to analyze the content of shale oil and its occurrence state in different pores based on the content of the retained oil and the occurrence state.

[0013] In one possible implementation, the acquisition module is specifically used for: Wire cutting technology was used to obtain plate-shaped samples of the target size from shale cores; The plate-shaped sample is divided into a first plate-shaped sample and a second plate-shaped sample.

[0014] In one possible implementation, the acquisition module is specifically used for: The second plate-shaped sample is fixed on the sample holder, and the second plate-shaped sample is mechanically polished in sequence using sandpaper of different grit sizes; The second plate-shaped sample was polished using an argon ion polisher with preset target parameters.

[0015] In one possible implementation, the second test module is specifically used for: The imaging mode of the field emission scanning electron microscope is set to low-voltage secondary electron mode; Under the condition that the second plate-shaped sample is not carbonized, the presence state of the oil retained in the pores of the second plate-shaped sample is directly observed and recorded by the field emission scanning electron microscope.

[0016] In one possible implementation, the first test module is specifically used for: For the first plate-shaped sample, target test parameters for relaxation spectrum testing of the first plate-shaped sample are determined; wherein, the target test parameters include at least resonance frequency, echo time, waiting time, and number of scans; The relaxation spectrum of the first plate-shaped sample was tested using a preset nuclear magnetic resonance spectrometer under the target test parameters. In one possible implementation, the first test module is specifically used for: Obtain the corresponding relaxation signal in the original state; calculate the residual oil content of the first plate-shaped sample based on the relaxation signal.

[0017] In one possible implementation, the device further includes: The third testing module is used to repeatedly test the first plate-shaped sample and the second plate-shaped sample.

[0018] Thirdly, embodiments of this application provide an electronic device, including: a processor, a storage medium, and a bus. The storage medium stores machine-readable instructions executable by the processor. When the electronic device is running, the processor communicates with the storage medium via the bus, and the processor executes the machine-readable instructions to perform the steps of the shale oil in-situ determination method as described in any of the first aspects.

[0019] Fourthly, embodiments of this application provide a computer-readable storage medium storing a computer program, which, when executed by a processor, performs the steps of the shale oil in-situ determination method according to any one of the first aspects.

[0020] This application provides a method and apparatus for in-situ determination of shale oil. A first slab-shaped sample and a second slab-shaped sample are obtained from an oil-bearing shale sample. The second slab-shaped sample is polished. Nuclear magnetic resonance relaxation spectroscopy is used to test the first slab-shaped sample to obtain the content of retained oil in its original state. The polished second slab-shaped sample is placed in a field emission scanning electron microscope at a preset target accelerating voltage to observe and record the occurrence state of retained oil in the pores of the second slab-shaped sample. Based on the retained oil content and occurrence state, the content of shale retained oil and its occurrence state in different pores are analyzed. This application uses nuclear magnetic resonance relaxation spectroscopy to test the content of retained oil in the original state of a first plate-shaped sample. The polished second plate-shaped sample is then placed in a field emission scanning electron microscope to obtain the occurrence state of retained oil in the pores. Based on the content and occurrence state of retained oil, the content and occurrence state of shale retained oil are comprehensively analyzed. This avoids serious deviations in the oil content evaluation results and damage to the original occurrence state of retained oil. It can provide spatial distribution and morphological information, and perform in-situ characterization of shale oil occurrence state and content. It achieves integrated quantitative and imaging characterization on the same sample simultaneously, and avoids human interference during sample pretreatment.

[0021] To make the above-mentioned objectives, features and advantages of this application more apparent and understandable, preferred embodiments are described below in detail with reference to the accompanying drawings. Attached Figure Description

[0022] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0023] Figure 1 This is a flowchart of the shale oil in-situ determination method provided in the embodiments of this application; Figure 2 This is a schematic diagram of the overall process for in-situ shale oil determination; Figure 3 This is a schematic diagram of the first and second plate-shaped samples after preparation; Figure 4 This is a schematic diagram of the crude oil occurrence state in shale pores. Figure 1 ; Figure 5 This is a schematic diagram of the crude oil occurrence state in shale pores. Figure 2 ; Figure 6 This is a schematic diagram of a nuclear magnetic resonance relaxation spectrum plate; Figure 7This is a schematic diagram showing the content of retained oil obtained by nuclear magnetic resonance relaxation spectroscopy. Figure 8 This is a schematic diagram of the structure of the shale oil in-situ testing device provided in the embodiments of this application; Figure 9 This is a schematic diagram of the structure of an electronic device provided according to an embodiment of this application. Detailed Implementation

[0024] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. It should be understood that the accompanying drawings in this application are for illustrative and descriptive purposes only and are not intended to limit the scope of protection of this application. Furthermore, it should be understood that the schematic drawings are not drawn to scale. The flowcharts used in this application illustrate operations implemented according to some embodiments of this application. It should be understood that the operations in the flowcharts may not be implemented in sequence, and steps without logical contextual relationships may be reversed or implemented simultaneously. In addition, those skilled in the art, guided by the content of this application, may add one or more other operations to the flowcharts, or remove one or more operations from the flowcharts.

[0025] Furthermore, the described embodiments are merely some, not all, of the embodiments of this application. The components of the embodiments of this application described and illustrated herein can typically be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of this application provided in the accompanying drawings is not intended to limit the scope of the claimed application, but merely to illustrate selected embodiments of the application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

[0026] It should be noted that the term "comprising" will be used in the embodiments of this application to indicate the presence of the features declared thereafter, but does not exclude the addition of other features.

[0027] Shale oil is primarily found in nanoscale pore-throat systems. Within this extremely confined space, the physicochemical properties of the fluid undergo significant changes, leading to exceptionally complex occurrence phases and fluidity characteristics. Therefore, characterization techniques for the occurrence state and content of shale oil are crucial for assessing its potential for efficient extraction.

[0028] Currently, the characterization of shale oil occurrence and content mainly relies on various separation techniques, such as the pyrolysis S1 method (Rock-Eval analysis), and traditional characterization techniques such as field emission scanning electron microscopy (FESEM) or nuclear magnetic resonance (NMR). In addition, in recent years, some studies have attempted to combine multiple techniques (such as FIB-SEM and micro-CT) to analyze pore structure.

[0029] However, while the S1 pyrolysis method determines free hydrocarbon content by heating rock samples to 300℃, light hydrocarbon components (C6-13) are easily lost during sample storage and crushing, leading to serious deviations in oil content evaluation results. FESEM requires carbon plating or oil washing of samples, destroying the original occurrence state of the retained oil. Although NMR can quantitatively analyze oil content, it is difficult to provide spatial distribution and morphological information. Furthermore, combining multiple techniques to analyze pore structure makes it difficult to achieve in-situ characterization of shale oil occurrence state and content. Additionally, it is difficult to simultaneously perform quantitative and imaging analysis on the same sample, and sample pretreatment (such as fluid saturation and cryogenic grinding) may introduce human interference.

[0030] To address this issue, this application provides a method and apparatus for in-situ determination of shale oil. The method utilizes nuclear magnetic resonance relaxation spectroscopy to test a first plate-shaped sample to obtain the content of retained oil in its original state. A polished second plate-shaped sample is then placed in a field emission scanning electron microscope to obtain the occurrence state of retained oil in the pores. Based on the content and occurrence state of the retained oil, a comprehensive analysis of the shale oil content and its occurrence state is conducted. This avoids serious deviations in oil content evaluation results and damage to the original occurrence state of the retained oil. It provides spatial distribution and morphological information, enabling in-situ characterization of shale oil occurrence state and content. It achieves integrated quantitative and imaging characterization simultaneously on the same sample, and avoids human interference during sample pretreatment.

[0031] Figure 1 This is a flowchart of the in-situ shale oil determination method provided in the embodiments of this application. For example... Figure 1 As shown in the embodiments of this application, the in-situ shale oil determination method may specifically include: S101. Obtain a first plate-shaped sample and a second plate-shaped sample from the oil-bearing shale sample, and polish the second plate-shaped sample.

[0032] S102. The first plate-shaped sample is tested using nuclear magnetic resonance relaxation spectroscopy to obtain the residual oil content of the first plate-shaped sample in its original state.

[0033] S103. Place the polished second plate-shaped sample in a field emission scanning electron microscope under a preset target accelerating voltage, and observe and record the state of oil retention in the pores of the second plate-shaped sample.

[0034] S104. Based on the content and occurrence state of retained oil, analyze the content of retained oil in shale and its occurrence state in different pores.

[0035] In the above-mentioned in-situ shale oil determination method, the content of retained oil in its original state is obtained by testing the first plate-shaped sample using nuclear magnetic resonance relaxation spectroscopy. The polished second plate-shaped sample is then placed in a field emission scanning electron microscope to obtain the occurrence state of retained oil in the pores. Based on the content and occurrence state of retained oil, the content and occurrence state of shale retained oil are comprehensively analyzed. This method avoids serious deviations in the oil content evaluation results and damage to the original occurrence state of retained oil. It can provide spatial distribution and morphological information, perform in-situ characterization of shale oil occurrence state and content, and achieve integrated quantitative and imaging characterization on the same sample simultaneously. Furthermore, it avoids human interference during sample pretreatment.

[0036] The exemplary steps described above in the embodiments of this application are illustrated below with specific examples: S101, Obtain a first plate-shaped sample and a second plate-shaped sample from the oil-bearing shale sample, and polish the second plate-shaped sample.

[0037] In this embodiment, the first plate-shaped sample is a larger plate-shaped sample, and the second plate-shaped sample is a smaller plate-shaped sample. The first plate-shaped sample is used for nuclear magnetic resonance (NMR) testing, and the second plate-shaped sample is used for scanning electron microscopy (SEM) testing. An oil-bearing shale sample from a shale core is divided in two to obtain the first plate-shaped sample and the second plate-shaped sample. The second plate-shaped sample is then polished for subsequent processing. For example, as... Figure 2 As shown.

[0038] Optionally, when obtaining the first and second plate-shaped samples, wire cutting technology is used to obtain plate-shaped samples of the target size from the shale core; the plate-shaped samples are then divided into the first and second plate-shaped samples. For example, taking the Jurassic Lianggaoshan Formation oil-bearing shale from well TY1 in the Sichuan Basin as an example, a 5cm×2cm×0.4cm plate-shaped sample is obtained using a precision wire cutting machine. The same plate-shaped sample is then divided in two, with the larger part (4.5cm×2cm×0.4cm) used for nuclear magnetic resonance (NMR) testing and the smaller part (0.5cm×3cm×0.4cm) used for SEM testing, for example, as... Figure 3 As shown, this represents the first and second plate-shaped samples after preparation.

[0039] Optionally, when polishing the second plate-shaped sample, the second plate-shaped sample is fixed on a sample holder, and mechanically polished using sandpaper of different grit sizes in sequence; the second plate-shaped sample is then polished using an argon ion polisher with preset target parameters. These target parameters include voltage, beam current, and polishing time; the processed second plate-shaped sample has a smooth, uncontaminated observation surface.

[0040] Specifically, for example, the second plate-shaped sample is fixed on the sample holder and mechanically polished sequentially using sandpaper with different grit sizes of 9μm, 2μm, and 0.5μm; then, it is finally polished using an argon ion polisher with parameters of 5kV voltage, 2mA beam current, and 1h polishing time, so that the treated second plate-shaped sample has a flat and uncontaminated observation surface.

[0041] Optionally, when observing and recording the state of oil retention in the pores of the second plate-shaped sample, the imaging mode of the field emission scanning electron microscope (FET) is set to low-voltage secondary electron mode; under the condition that the second plate-shaped sample is not carbon-coated, the state of oil retention in the pores of the second plate-shaped sample is directly observed and recorded by the FET. Here, "not carbon-coated" represents the original surface of the second plate-shaped sample.

[0042] For example, the polished second plate-shaped sample is placed in a field emission scanning electron microscope (SEM), the target accelerating voltage is set to 1.5 kV, and secondary electron (SE) mode is used for imaging to observe and record the state of crude oil occurrence in shale pores, such as "oil film" adhering to the pore wall (e.g., ...). Figure 4 (as shown) or "agglomerated" in small pores (such as...) Figure 5 (As shown).

[0043] S102, the first plate-shaped sample was tested using nuclear magnetic resonance relaxation spectroscopy to obtain the residual oil content of the first plate-shaped sample in its original state.

[0044] In this embodiment, the original state, i.e., the state of unwashed oil and unsaturated fluid, is used to test the first plate-shaped sample obtained in step S101 using nuclear magnetic resonance relaxation spectroscopy to obtain the residual oil content of the first plate-shaped sample in its original state for subsequent processing. For example, as... Figure 2 As shown.

[0045] Optionally, when testing the first plate-shaped sample using nuclear magnetic resonance relaxation spectroscopy, target test parameters for the relaxation spectrum testing of the first plate-shaped sample are determined; and a preset nuclear magnetic resonance spectrometer is used to perform relaxation spectrum testing on the first plate-shaped sample under the target test parameters. The target test parameters include at least the resonance frequency, echo time, waiting time, and number of scans.

[0046] Optionally, when obtaining the retained oil content of the first plate-shaped sample in its original state, the corresponding relaxation signal is obtained in the original state; the retained oil content of the first plate-shaped sample is calculated based on the relaxation signal. The original state is an unwashed, unsaturated fluid, i.e., without washing or saturation / soaking treatment.

[0047] For example, a two-dimensional relaxation spectrum test (T1-T2) was performed on the first plate-shaped sample using an nuclear magnetic resonance (NMR) spectrometer. The test parameters were: resonance frequency 2 MHz, echo time 0.2 ms, waiting time 3 s, and number of scans 64. Based on the relaxation spectrum signal and the NMR plate of that region (e.g., Figure 6 (As shown) Calculate the oil saturation and quantitatively obtain the retained oil content (e.g.) Figure 7 (As shown).

[0048] S103, the polished second plate-shaped sample is placed in a field emission scanning electron microscope under a preset target accelerating voltage to observe and record the state of oil retention in the pores of the second plate-shaped sample.

[0049] In this embodiment, the presence state of the oil retained in the pores of the second plate-shaped sample characterizes the imaging information of the oil film retained in different types of pores. The presence state includes at least the pore type, the presence morphology of the oil retained, the pore size, the morphology, and the distribution characteristics of the oil retained. The second plate-shaped sample after polishing in step S101 is placed in a field emission scanning electron microscope at a target accelerating voltage (e.g., 1.5 kV) to observe the presence state of the oil retained in the pores of the second plate-shaped sample.

[0050] S104, based on the content and occurrence state of retained oil, analyzes the content of retained oil in shale and its occurrence state in different pores.

[0051] In this embodiment of the application, based on the content of retained oil in the first plate-shaped sample in its original state obtained in step S102 and the occurrence state of retained oil in the pores of the second plate-shaped sample obtained in step S103, the content of shale retained oil and its occurrence state in different pores are comprehensively analyzed.

[0052] The in-situ shale oil determination method provided in this application involves obtaining a first plate-shaped sample and a second plate-shaped sample from an oil-bearing shale sample, polishing the second plate-shaped sample, testing the first plate-shaped sample using nuclear magnetic resonance relaxation spectroscopy to obtain the content of retained oil in the first plate-shaped sample in its original state, placing the polished second plate-shaped sample in a field emission scanning electron microscope at a preset target accelerating voltage to observe and record the occurrence state of retained oil in the pores of the second plate-shaped sample, and analyzing the content of retained oil in shale and its occurrence state in different pores based on the content and occurrence state of retained oil. The in-situ shale oil determination method of this application uses nuclear magnetic resonance relaxation spectroscopy to test the first plate-shaped sample to obtain the content of retained oil in its original state. The polished second plate-shaped sample is then placed in a field emission scanning electron microscope to obtain the occurrence state of retained oil in the pores. Based on the content and occurrence state of retained oil, the content and occurrence state of shale retained oil are comprehensively analyzed. This method avoids serious deviations in oil content evaluation results and damage to the original occurrence state of retained oil. It can provide spatial distribution and morphological information, perform in-situ characterization of shale oil occurrence state and content, and achieve integrated quantitative and imaging characterization on the same sample simultaneously. Furthermore, it avoids human interference during sample pretreatment.

[0053] Furthermore, the first plate-shaped sample and the second plate-shaped sample were tested repeatedly.

[0054] Figure 8 This is a schematic diagram of the structure of the shale oil in-situ testing device provided in the embodiments of this application; as shown below. Figure 8 As shown, the shale oil in-situ testing device 800 of this application embodiment may specifically include: The acquisition module 801 is used to acquire a first plate-shaped sample and a second plate-shaped sample from an oil-bearing shale sample, and to polish the second plate-shaped sample. The first test module 802 is used to test the first plate-shaped sample using nuclear magnetic resonance relaxation spectroscopy to obtain the residual oil content of the first plate-shaped sample in its original state. The second test module 803 is used to place the polished second plate-shaped sample in a field emission scanning electron microscope under a preset target accelerating voltage, and observe and record the state of oil retention in the pores of the second plate-shaped sample. Analysis module 804 is used to analyze the content of shale oil and its occurrence state in different pores based on the content of the retained oil and the occurrence state.

[0055] In one possible implementation, the acquisition module is specifically used for: Wire cutting technology was used to obtain plate-shaped samples of the target size from shale cores; The plate-shaped sample was divided into a first plate-shaped sample and a second plate-shaped sample.

[0056] In one possible implementation, the acquisition module is specifically used for: The second plate-shaped sample was fixed on the sample holder, and the second plate-shaped sample was mechanically polished in sequence using sandpaper of different grit sizes. The second plate-shaped sample was polished using an argon ion polisher with preset target parameters.

[0057] In one possible implementation, the second test module is specifically used for: Set the imaging mode of the field emission scanning electron microscope to low-voltage secondary electron mode; Under the condition that the second plate-shaped sample is not carbon-plated, the presence state of the oil retained in the pores of the second plate-shaped sample is directly observed and recorded by field emission scanning electron microscopy.

[0058] In one possible implementation, the first test module is specifically used for: For the first plate-shaped sample, the target test parameters for relaxation spectrum testing of the first plate-shaped sample are determined; wherein, the target test parameters include at least the resonance frequency, echo time, waiting time and number of scans; The relaxation spectrum of the first plate-shaped sample was tested using a preset nuclear magnetic resonance spectrometer under the target test parameters. In one possible implementation, the first test module is specifically used for: The corresponding relaxation signal is obtained in the original state; the residual oil content of the first plate-shaped sample is calculated based on the relaxation signal.

[0059] In one possible implementation, the apparatus further includes: The third testing module is used to perform repeated tests on the first plate-shaped sample and the second plate-shaped sample.

[0060] The shale oil in-situ determination device provided in this application obtains a first plate-shaped sample and a second plate-shaped sample from an oil-bearing shale sample. The second plate-shaped sample is polished, and the first plate-shaped sample is tested using nuclear magnetic resonance relaxation spectroscopy to obtain the content of retained oil in the original state of the first plate-shaped sample. The polished second plate-shaped sample is placed in a field emission scanning electron microscope under a preset target accelerating voltage to observe and record the occurrence state of retained oil in the pores of the second plate-shaped sample. Based on the content and occurrence state of retained oil, the content of shale retained oil and its occurrence state in different pores are analyzed. The shale oil in-situ determination device of this application uses nuclear magnetic resonance relaxation spectroscopy to test the first plate-shaped sample to obtain the content of retained oil in its original state. The polished second plate-shaped sample is placed in a field emission scanning electron microscope to obtain the occurrence state of retained oil in the pores. Based on the content and occurrence state of retained oil, the content and occurrence state of shale retained oil are comprehensively analyzed. This avoids serious deviations in the oil content evaluation results and damage to the original occurrence state of retained oil. It can provide spatial distribution and morphological information, and perform in-situ characterization of shale oil occurrence state and content. It realizes integrated quantitative and imaging characterization on the same sample simultaneously, and avoids human interference during sample pretreatment.

[0061] like Figure 9 As shown in the embodiment of this application, an electronic device 900 includes a processor 901, a memory 902, and a bus. The memory 902 stores machine-readable instructions that can be executed by the processor 901. When the electronic device is running, the processor 901 communicates with the memory 902 via the bus. The processor 901 executes the machine-readable instructions to perform the steps of the shale oil in-situ determination method described above.

[0062] Specifically, the aforementioned memory 902 and processor 901 can be general-purpose memory and processor, without any specific limitations. When the processor 901 runs the computer program stored in the memory 902, it can execute the aforementioned shale oil in-situ measurement method.

[0063] Corresponding to the above-described shale oil in-situ determination method, this application embodiment also provides a computer-readable storage medium storing a computer program, which, when executed by a processor, performs the steps of the above-described shale oil in-situ determination method.

[0064] Those skilled in the art will clearly understand that, for the sake of convenience and brevity, the specific working processes of the systems and devices described above can be referred to the corresponding processes in the method embodiments, and will not be repeated here. In the several embodiments provided in this application, it should be understood that the disclosed systems, devices, and methods can be implemented in other ways. The device embodiments described above are merely illustrative. For example, the division of modules is only a logical functional division, and in actual implementation, there may be other division methods. Furthermore, multiple modules or components can be combined or integrated into another system, or some features can be ignored or not executed. Another point is that the displayed or discussed mutual coupling or direct coupling or communication connection can be through some communication interfaces; the indirect coupling or communication connection of devices or modules can be electrical, mechanical, or other forms.

[0065] The modules described as separate components may or may not be physically separate. The components shown as modules may or may not be physical units; that is, they may be located in one place or distributed across multiple network units. Some or all of the units can be selected to achieve the purpose of this embodiment according to actual needs.

[0066] In addition, the functional units in the various embodiments of this application can be integrated into one processing unit, or each unit can exist physically separately, or two or more units can be integrated into one unit.

[0067] If the aforementioned functions are implemented as software functional units and sold or used as independent products, they can be stored in a processor-executable, non-volatile, computer-readable storage medium. Based on this understanding, the technical solution of this application, in essence, or the part that contributes to the prior art, or a portion of the technical solution, can be embodied in the form of a software product. This computer software product is stored in a storage medium and includes several instructions to cause a computer device (which may be a personal computer, server, or network device, etc.) to execute all or part of the steps of the deployment methods described in the various embodiments of this application. The aforementioned storage medium includes various media capable of storing program code, such as USB flash drives, portable hard drives, ROM, RAM, magnetic disks, or optical disks.

[0068] The above are merely specific embodiments of this application, but the scope of protection of this application is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in this application should be included within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.

Claims

1. A method for in-situ determination of shale oil, characterized in that, The method includes: A first plate-shaped sample and a second plate-shaped sample were obtained from the oil-bearing shale sample, and the second plate-shaped sample was polished. The first plate-shaped sample was tested using nuclear magnetic resonance relaxation spectroscopy to obtain the residual oil content of the first plate-shaped sample in its original state. The polished second plate-shaped sample was placed in a field emission scanning electron microscope under a preset target accelerating voltage to observe and record the state of oil retention in the pores of the second plate-shaped sample. The content of shale oil and its occurrence state in different pores are analyzed based on the content of the retained oil and the occurrence state.

2. The method according to claim 1, characterized in that, The process of obtaining the first plate-shaped sample and the second plate-shaped sample includes: Wire cutting technology was used to obtain plate-shaped samples of the target size from shale cores; The plate-shaped sample is divided into a first plate-shaped sample and a second plate-shaped sample.

3. The method according to claim 1, characterized in that, The polishing process of the second plate-shaped sample includes: The second plate-shaped sample is fixed on the sample holder, and the second plate-shaped sample is mechanically polished in sequence using sandpaper of different grit sizes; The second plate-shaped sample was polished using an argon ion polisher with preset target parameters.

4. The method according to claim 1, characterized in that, The observation and recording of the presence state of the oil retained in the pores of the second plate-shaped sample includes: The imaging mode of the field emission scanning electron microscope is set to low-voltage secondary electron mode; Under the condition that the second plate-shaped sample is not carbonized, the presence state of the oil retained in the pores of the second plate-shaped sample is directly observed and recorded by the field emission scanning electron microscope.

5. The method according to claim 1, characterized in that, The testing of the first plate-shaped sample using nuclear magnetic resonance relaxation spectroscopy includes: For the first plate-shaped sample, target test parameters for relaxation spectrum testing of the first plate-shaped sample are determined; wherein, the target test parameters include at least resonance frequency, echo time, waiting time, and number of scans; The relaxation spectrum of the first plate-shaped sample was tested using a preset nuclear magnetic resonance spectrometer under the target test parameters.

6. The method according to claim 1, characterized in that, Obtaining the residual oil content of the first plate-shaped sample in its original state includes: Obtain the corresponding relaxation signal in the original state; calculate the residual oil content of the first plate-shaped sample based on the relaxation signal.

7. The method according to claim 1, characterized in that, The method further includes: The first plate-shaped sample and the second plate-shaped sample were tested repeatedly.

8. A shale oil in-situ testing device, characterized in that, The device includes: The acquisition module is used to acquire a first plate-shaped sample and a second plate-shaped sample from an oil-bearing shale sample, and to polish the second plate-shaped sample. The first testing module is used to test the first plate-shaped sample using nuclear magnetic resonance relaxation spectroscopy to obtain the residual oil content of the first plate-shaped sample in its original state. The second test module is used to place the polished second plate-shaped sample in a field emission scanning electron microscope under a preset target accelerating voltage to observe and record the state of oil retention in the pores of the second plate-shaped sample. The analysis module is used to analyze the content of shale oil and its occurrence state in different pores based on the content of the retained oil and the occurrence state.

9. An electronic device, characterized in that, include: The device includes a processor, a memory, and a bus. The memory stores machine-readable instructions executable by the processor. When the electronic device is running, the processor communicates with the memory via the bus. When the machine-readable instructions are executed by the processor, they perform the steps of the shale oil in-situ determination method as described in any one of claims 1 to 7.

10. A computer-readable storage medium, characterized in that, The computer-readable storage medium stores a computer program that, when executed by a processor, performs the steps of the shale oil in-situ determination method as described in any one of claims 1 to 7.

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