Method for measuring uniform temperature of inclusion

Abstract

The invention relates to the technical field of reservoir formation evaluation of oil and gas basins, and provides a method for measuring the uniform temperature of an inclusion, which comprises the following steps: cooling a test sample until the test sample generates bubbles; raising the temperature of the test sample until bubbles disappear, and recording the temperature at the moment as a quasi-uniform temperature; cooling the test sample in the preset cooling interval; observing whether bubbles reappear in the test sample or not; if not, taking the current quasi-uniform temperature as the uniform temperature; and if yes, adding one unit experiment precision to the value of the quasi-uniform temperature, heating the test sample until the temperature reaches the quasi-uniform temperature, and repeatedly cooling and heating. According to the invention, the technical problem that the measurement result is easily influenced by the observation ability and subjective factors of measurement personnel to cause errors because the inclusion uniform temperature measurement method in the prior art depends on naked eye observation of whether bubbles disappear can be solved.

Description

Technical Field

[0001] This invention relates to the field of oil and gas basin accumulation evaluation technology, and in particular to a method for measuring the homogenization temperature of inclusions. Background Technology

[0002] In the field of hydrocarbon basin accumulation assessment, fluid inclusions can indicate information such as hydrocarbon charging, accumulation processes, and paleotemperature and pressure. Therefore, the study of fluid inclusions is of great significance in the field of hydrocarbon basin accumulation assessment. Measuring the homogenization temperature of fluid inclusions is one part of fluid inclusion research. Currently, the main methods for measuring the homogenization temperature of fluid inclusions, both domestically and internationally, are as follows:

[0003] Meng Fanwei et al. used cryogenic cryo-thermometry to study the thermometry of pure liquid-phase halite fluid inclusions. Laboratory-synthesized halite crystals were cut into inclusion slices and placed in a freezer at -15°C for 30 days. This caused the original pure liquid-phase halite fluid inclusions to shrink without freezing, altering their size and volume, thus forming gas-liquid two-phase fluid inclusions with bubbles. The homogenization temperature of the gas-liquid two-phase fluid inclusions formed under cryogenic conditions was measured at room temperature (28°C). An international synthetic inclusion standard with a reference temperature of ±1.0°C was used before measurement. During measurement, the halite inclusion slices were quickly removed from the freezer and immediately placed on a hot-cold stage for rapid cooling to -15°C. The temperature of the pure liquid-phase fluid inclusions that developed bubbles during freezing was then measured. A segmented heating method was used during the measurement process: the heating rate was 0.5°C / min below 15°C and 0.1°C / min above 15°C until homogenization was achieved.

[0004] Wang Chunlian et al. chose to freeze single-phase primary fluid inclusions to induce the formation of bubbles in the originally single-phase liquid inclusions. Because brine inclusions are generally small and the liquid is often in a metastable state, bubble formation is not easy. Therefore, freezing was performed at a lower temperature to accelerate bubble formation. Generally, a temperature not lower than -50℃ was chosen for freezing. After about 1-2 hours, some inclusions began to show bubbles. Temperature measurement began once a large number of inclusions showed bubbles. During heating, care was taken to avoid excessively rapid heating. A segmented heating method was used: a heating rate of 0.5℃ / min below 15℃ and 0.1℃ / min above 15℃ until homogeneity was achieved. This ensured more accurate data.

[0005] Before testing single-phase fluid inclusions, Li Haonan et al. first froze the samples in a refrigerator for 1-2 weeks at a temperature of approximately -18°C. This temperature prevents the fluid inclusions from freezing, which could cause them to stretch, deform, or leak, thus damaging the inclusions and affecting the temperature measurement results. After 1-2 weeks of freezing, bubbles were observed in 2%-10% of the fluid inclusions in the samples. This method is effective in most cases, but variations exist between different samples. Bubbles were observed in most samples, while some samples produced fewer or no bubbles. The samples were then removed from the refrigerator and quickly placed on a hot-cold stage for another hour (maintaining a temperature of -18°C). The fluid inclusions with bubbles were located and marked. Subsequently, the temperature was slowly increased at a rate of 0.5°C / min. When the bubbles began to shrink under the microscope, indicating approaching the homogenization temperature, the heating rate was adjusted to 0.1°C / min until the bubbles disappeared. The temperature at this point was recorded as the homogenization temperature of the fluid inclusions.

[0006] Although the above methods can all obtain a uniform temperature of the package, they all rely on visual observation of whether the bubbles have disappeared when determining whether the package is in a uniform state. Therefore, the measurement results are easily affected by the observer's observation ability and subjective factors, which can lead to errors in the measurement results. Summary of the Invention

[0007] The purpose of this invention is to overcome the technical problem that existing methods for measuring the uniformity temperature of inclusions rely on visual observation of whether air bubbles disappear, and the measurement results are easily affected by the observer's observation ability and subjective factors, resulting in errors. This invention provides a method for measuring the uniformity temperature of inclusions.

[0008] In a first aspect, the present invention provides a method for measuring the uniform temperature of an encapsulation, comprising the following steps:

[0009] S1. Cool the test sample until bubbles are generated in the test sample;

[0010] S2. Heat the test sample. When the movement state of the bubbles changes, reduce the heating rate and continue heating until the bubbles disappear. Record the temperature at this time as the pseudo-homogenization temperature.

[0011] S3. Cool the test sample within the predetermined cooling range;

[0012] S4. Observe whether bubbles reappear in the test sample; if not, skip to step S5; if yes, increase the value of the pseudo-homogenization temperature by one unit of experimental precision, heat the test sample until the temperature reaches the pseudo-homogenization temperature, and repeat steps S3 to S4.

[0013] S5. Use the current pseudo-homogenization temperature as the homogenization temperature.

[0014] Compared to the single-heating method of existing technologies, the homogenization temperature measurement method of this scheme involves multiple cycles of cooling and heating of the test sample, with the pseudo-homogenization temperature value increased by one unit of experimental precision in each cycle. When no more bubbles appear after cooling, the pseudo-homogenization temperature of the last heating is used as the homogenization temperature measurement result. Therefore, operators no longer need to accurately judge when the bubbles disappear, but only need to observe whether bubbles reappear after cooling. This greatly reduces the requirements for operator observation and eliminates the influence of subjective factors on the measurement results, thus achieving higher measurement accuracy. At the same time, multiple cycles of cooling and heating can also avoid the influence of some accidental factors during the measurement process, thereby further improving the measurement accuracy of this scheme.

[0015] Furthermore, this solution involves repeated cooling and heating of the test samples, which can overcome the defect that some test samples are difficult to generate bubbles during a single heating process. This ensures that various test samples can generate bubbles stably, thus making this solution applicable to a wide variety of test samples and giving it better versatility than existing technologies.

[0016] Meanwhile, this scheme also sets a predetermined cooling range in step S3, which can prevent the test sample from being damaged due to excessive cooling, such as the rupture of the inclusion. The extent of damage increases with the number of cycles, and ultimately has a negative impact on the measurement results. Thus, this scheme can avoid the shortcomings of repeated cooling and heating, and give full play to the advantages of repeated cooling and heating.

[0017] Preferably, the test sample contains at least one of hydrocarbon inclusions, brine inclusions, and gas-liquid two-phase inclusions.

[0018] This proposal recommends three test samples that are compatible with the measurement method for the homogeneous temperature of the inclusions in this proposal.

[0019] Preferably, step S1 further includes the following step: when the test sample generates bubbles, the bubbles are marked.

[0020] This method allows for quick location and observation of the bubbles generated in step S1 during step S2.

[0021] Preferably, the bubble motion state in step S2 includes at least one of bubble motion speed and bubble motion direction.

[0022] This plan recommends specific criteria for judging changes in the state of bubble motion.

[0023] Preferably, before the movement state of the bubbles changes in step S2, the heating rate of the test sample is greater than or equal to 4℃ / min and less than or equal to 6℃ / min.

[0024] Preferably, after the movement state of the bubble changes in step S2, the heating rate of the test sample is greater than or equal to 1℃ / min and less than or equal to 3℃ / min.

[0025] Preferably, the range of the predetermined cooling range in step S3 is a cooling amplitude of less than or equal to 25°C.

[0026] This solution recommends a specific range of values ​​for the predetermined cooling interval, which can prevent the test samples from being damaged due to excessive cooling.

[0027] Preferably, the unit experimental precision in step S4 is less than or equal to 0.2℃.

[0028] This scheme recommends a specific range of values ​​for the unit experimental precision, which can avoid the measurement accuracy being too low due to excessively large unit experimental precision values.

[0029] Preferably, the test sample is a sheet-like test sample.

[0030] This method allows for easy and clear observation of the morphology of test samples and the air bubbles generated within them using a microscope.

[0031] Preferably, a hot or cold stage is used to cool or heat the test sample.

[0032] This solution can achieve both cooling and heating of test samples using a single device, eliminating the need to repeatedly switch between cooling and heating devices when cooling or heating is required, thereby improving measurement efficiency.

[0033] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0034] This invention provides a method for measuring the uniform temperature of a package. By repeatedly cooling and heating the test sample, the measurement results of the uniform temperature are obtained. This method can greatly reduce the requirements for the operator's observation skills and eliminate the influence of the operator's subjective factors and some accidental factors on the measurement results, thereby obtaining higher measurement accuracy.

[0035] Furthermore, by repeatedly cooling and heating the test samples, this invention can overcome the defect that some test samples are difficult to generate bubbles during a single heating process, ensuring that various test samples can stably generate bubbles. This allows the solution to be applied to various test samples and has better versatility than existing technologies. Attached Figure Description

[0036] Figure 1 This is a flowchart illustrating a method for measuring the uniform temperature of an encapsulated object according to the present invention.

[0037] Figure 2 This is a microscopic schematic diagram of the test sample in Example 2 before cooling;

[0038] Figure 3 This is a microscopic schematic diagram of the test sample in Example 2 after cooling and the generation of bubbles;

[0039] Icons: 1-Test sample; 2-Bubble. Detailed Implementation

[0040] The present invention will be further described in detail below with reference to experimental examples and specific embodiments. However, this should not be construed as limiting the scope of the above-mentioned subject matter of the present invention to the following embodiments; all technologies implemented based on the content of the present invention fall within the scope of the present invention.

[0041] Unless otherwise specified, the use of terms such as "upper," "lower," "left," "right," "center," "inner," and "outer" to indicate orientation or positional relationships in the description of specific embodiments of the present invention is based on the orientation or positional relationships shown in the accompanying drawings, or the orientation or positional relationship in which the product / equipment / device is typically placed during use. These terms are merely for the purpose of facilitating the description of the present invention or simplifying the description in specific embodiments, enabling those skilled in the art to quickly understand the solution, and do not indicate or imply that a particular device / component / element must have a specific orientation, or be constructed and operated in a specific positional relationship. Therefore, they should not be construed as limitations on the present invention.

[0042] Furthermore, the use of terms such as "horizontal," "vertical," "suspended," and "parallel" does not imply that the corresponding device / component / element must be absolutely horizontal, vertical, suspended, or parallel, but rather that it can be slightly tilted or have a deviation. For example, "horizontal" merely means that its direction is more horizontal relative to "vertical," not that the structure must be completely horizontal, but that it can be slightly tilted. Alternatively, it can be simplified to mean that the corresponding device / component / element, when set in a "horizontal," "vertical," "suspended," or "parallel" direction, can have an error / deviation of ±10% relative to the corresponding direction, more preferably within ±8%, more preferably within ±6%, more preferably within ±5%, and more preferably within ±4%. As long as the corresponding device / component / element is within the error / deviation range, it can still achieve its function in the present invention.

[0043] Furthermore, the use of terms such as "first," "second," "third," etc. in terminology is merely for distinguishing identical or similar components and should not be interpreted as emphasizing or implying the relative importance of a particular component.

[0044] Furthermore, in the description of the embodiments of the present invention, "several", "more than", and "a number of" represent at least two. The number can be any number, such as 2, 3, 4, 5, 6, 7, 8, or 9, and can even exceed nine.

[0045] Furthermore, in the description of the technical solution of this invention, unless otherwise explicitly specified / limited / restricted, the terms "set up," "install," "connect," "link," "provided with," "laid out," and "arranged" should be interpreted broadly. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to common connection methods in the art, such as welding, riveting, bolting, and threaded connections. Such connections can be mechanical, electrical, or communication connections; they can be direct connections or indirect connections through an intermediate medium; and they can refer to the internal communication between two components.

[0046] Example 1

[0047] like Figures 1 to 3 As shown, a method for measuring the uniform temperature of an encapsulation includes the following steps:

[0048] S1. Cool down test sample 1 until bubble 2 is generated in test sample 1;

[0049] S2. Heat the test sample 1. When the motion state of bubble 2 changes, reduce the heating rate and continue heating until bubble 2 disappears. Record the temperature at this time as the pseudo-homogenization temperature.

[0050] S3. Cool the test sample 1 within the predetermined cooling range;

[0051] S4. Observe whether bubble 2 reappears in test sample 1. If not, skip to step S5. If yes, increase the value of the pseudo-homogenization temperature by one unit of experimental precision, heat test sample 1 until the temperature reaches the pseudo-homogenization temperature, and repeat steps S3 to S4.

[0052] S5. The current pseudo-homogenization temperature is taken as the homogenization temperature, i.e., the measurement result.

[0053] In an optional implementation, a hot-cold stage is used to cool or heat the test sample 1, such as the MDS600 hot-cold stage.

[0054] In an optional implementation, test sample 1 is a sheet-like test sample 1.

[0055] In an optional implementation, test sample 1 contains at least one of hydrocarbon inclusions, brine inclusions, and gas-liquid two-phase inclusions.

[0056] In an optional implementation, step S1 further includes the following step: when test sample 1 generates bubbles 2, the bubbles 2 are marked. The marking method includes, but is not limited to, marking directly on test sample 1 with a marker or marking on an image of test sample 1 using a computer program.

[0057] In an optional implementation, the motion state of bubble 2 in step S2 includes at least one of bubble 2's motion speed and motion direction. Correspondingly, in step S2, when either the motion speed or the motion direction of bubble 2 changes, the heating rate is reduced.

[0058] In an optional implementation, before the motion state of bubble 2 changes in step S2, the heating rate of test sample 1 is greater than or equal to 4℃ / min and less than or equal to 6℃ / min, for example 5℃ / min.

[0059] In an optional implementation, after the motion state of bubble 2 changes in step S2, the heating rate of test sample 1 is greater than or equal to 1℃ / min and less than or equal to 3℃ / min, for example 2℃ / min.

[0060] In an optional implementation, the predetermined cooling range in step S3 is a cooling amplitude of less than or equal to 25°C. That is, the difference between the temperature of test sample 1 before cooling and the temperature of test sample 1 after cooling is less than or equal to 25°C.

[0061] In an optional implementation, the unit experimental precision in step S4 is less than or equal to 0.2°C, for example, 0.1°C.

[0062] Example 2

[0063] Based on Example 1, taking the Permian Qixia Formation of a certain section as an example, this example provides the following specific implementation steps:

[0064] SA1, Select as follows Figure 2 The rock samples from the field profile of the developmental vein shown were ground into fluid inclusion test sections as test sample 1, sealed in a plastic resealable bag, and placed in a well-sealed plastic box with desiccant added for use;

[0065] SA2. The test sample 1 was cooled using an MDS600 hot and cold stage. The sample 1 was then observed under a microscope at room temperature, and the resulting bubbles 2 were located and marked. Figure 3 As shown;

[0066] SA3. Heat the test sample 1 at a rate of 5℃ / min. When the bubble 2 is observed to start to shrink and its movement pattern changes under the microscope, it indicates that the test sample 1 is close to the homogenization temperature. At this time, reduce the heating rate to 2℃ / min and continue heating until the bubble 2 disappears. Record the temperature at this time as 84.3℃ and set it as the pseudo-homogenization temperature.

[0067] SA4. Within the predetermined cooling range, i.e., within 25℃, the test sample 1 was cooled. When the temperature decreased by 12℃, bubbles 2 were found to reappear, and the test sample 1 returned to the gas-liquid two-phase state. Therefore, the pseudo-homogenization temperature of 84.3℃ was increased by one unit of experimental precision, 0.1℃, to obtain a new pseudo-homogenization temperature of 84.4℃. The test sample 1 was then reheated to the new pseudo-homogenization temperature.

[0068] SA5, repeat step SA4, that is, repeatedly cool down and heat up the test sample 1, and in each cycle, the pseudo-homogenization temperature is increased by one unit of experimental precision; when the pseudo-homogenization temperature reaches 84.7℃, the temperature is lowered again within the range of 25℃, and it is found that bubble 2 no longer appears in the test sample 1. Therefore, 84.7℃ is taken as the accurate and reliable homogenization temperature.

[0069] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method of measuring the uniform temperature of an inclusion, characterized in that, The method comprises the following steps: S1, cooling the test sample (1) until the test sample (1) generates bubbles (2); S2, heating the test sample (1), when the movement state of the bubbles (2) changes, reducing the heating rate, continuing to heat until the bubbles (2) disappear, and recording the temperature at this time as the quasi-uniform temperature; S3, cooling the test sample (1) in a predetermined cooling interval; S4, observing whether the bubbles (2) reappear in the test sample (1); if not, jumping to step S5; if yes, increasing the value of the quasi-uniform temperature by one unit of experimental precision, heating the test sample (1) until the temperature reaches the quasi-uniform temperature, and repeating steps S3 to S4; S5, taking the current quasi-uniform temperature as the uniform temperature.

2. The method of measuring the uniform temperature of a package according to claim 1, wherein, The test sample (1) comprises at least one of a hydrocarbon inclusion, a saltwater inclusion, and a gas-liquid two-phase inclusion.

3. The method of claim 1, wherein the sample is a wrapped body. Step S1 further comprises the following step: when the test sample (1) generates bubbles (2), marking the bubbles (2).

4. The method of claim 1, wherein the sample is a wrapped body. The movement state of the bubbles (2) in step S2 comprises at least one of the movement speed of the bubbles (2) and the movement direction of the bubbles (2).

5. A method of measuring the uniform temperature of an inclusion according to any one of claims 1 to 4, characterized in that, Before the movement state of the bubbles (2) changes in step S2, the heating rate of the test sample (1) is greater than or equal to 4°C / min and less than or equal to 6°C / min.

6. A method of measuring the uniform temperature of a package according to claim 5, wherein After the movement state of the bubbles (2) changes in step S2, the heating rate of the test sample (1) is greater than or equal to 1°C / min and less than or equal to 3°C / min.

7. A method for measuring the uniform temperature of an inclusion according to any one of claims 1 to 4, characterized in that, The predetermined cooling interval in step S3 has a range of a cooling amplitude less than or equal to 25°C.

8. A method for measuring the uniform temperature of an inclusion according to any one of claims 1 to 4, characterized in that, The unit of experimental precision in step S4 is less than or equal to 0.2°C.

9. A method for measuring the uniform temperature of an inclusion according to any one of claims 1 to 4, characterized in that, The test sample (1) is a sheet-shaped test sample (1).

10. A method for measuring a uniform temperature of an inclusion according to any one of claims 1 to 4, characterized in that, A cooling and heating stage is used to cool or heat the test sample (1).

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