CN109580702B - Method for measuring uniform temperature and freezing point temperature of fluid inclusion - Google Patents
Method for measuring uniform temperature and freezing point temperature of fluid inclusion Download PDFInfo
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- CN109580702B CN109580702B CN201811416639.2A CN201811416639A CN109580702B CN 109580702 B CN109580702 B CN 109580702B CN 201811416639 A CN201811416639 A CN 201811416639A CN 109580702 B CN109580702 B CN 109580702B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point
Abstract
The invention discloses a method for measuring uniform temperature and freezing point temperature of a fluid inclusion. When the uniform temperature is measured by the uniform method, when the measured uniform temperature is higher than the reappearance temperature, the measured uniform temperature is determined as the actual uniform temperature of the fluid inclusion; when the freezing point temperature is measured by a freezing method, when the ice crystals in the fluid inclusion are completely melted, the temperature is the freezing point temperature of the fluid inclusion. The invention effectively avoids the adverse effect on experimental data caused by the objective existence of the metastable state, and timely and effectively calibrates the fluid inclusion temperature measurement process and the temperature measurement data in the experiment process through the influence of the metastable state phenomenon on the fluid inclusion temperature measurement process and the temperature measurement data, thereby further improving the reliability and the accuracy of the inclusion temperature measurement data; the method and the device can ensure that an observer can timely verify the temperature measurement data, effectively avoid the influence of human factors on the experimental data, reasonably avoid the interference of the metastable state on the test data, and scientifically convert the interference of the metastable state into the improvement on the precision of the experimental data.
Description
Technical Field
The invention relates to a method for measuring uniform temperature and freezing point temperature of a fluid inclusion, belonging to the technical field of temperature measurement.
Background
The fluid trapped in the process of mineral growth preserves various geological geochemical information (such as temperature, pressure, components and the like) of the geological environment at that time, so that various data and information can be obtained through qualitative or quantitative analysis of the ancient fluid in the inclusion, and various geological action processes in the researched crust and mantle can be further explained. Fluid inclusion analysis has been widely used in the fields of geology, such as mineral deposit science, oil exploration and tectogeology, and is one of the most active fields in the current geoscience research.
The fluid inclusion temperature measuring technology is a method which is the most convenient and fast to directly obtain the temperature, the pressure and the salinity of the captured fluid inclusions in a non-destructive manner, and is also the method which is most widely applied at present. Basic principle of fluid inclusion temperature measurement: (1) principle of homogeneous temperature measurement by homogeneous method: selecting gas-liquid two-phase inclusion (single-phase inclusion in capture), converting the gas-liquid two-phase to single-phase when a cold and hot platform is heated to a certain temperature, recovering the phase state (single-phase) when the inclusion is formed, and obtaining the uniform temperature of the inclusion at the instant temperature in recovery. (2) The principle of freezing point temperature measurement by a freezing method is that the freezing point temperature of the liquid phase of the inclusion is measured by utilizing the principle that saline solutions with different concentrations have different freezing points, and the liquid phase concentration of the inclusion can be obtained by applying a corresponding phase diagram according to the measured freezing point of the inclusion. The method for measuring the temperature of the fluid inclusion is based on observing and identifying various phases (solid phase, liquid phase and gas phase) of the fluid contained in the inclusion in detail, and measures and observes and records various instantaneous phase change temperatures of the inclusion by regulating and controlling temperature rise (or temperature drop), thereby achieving the purpose of measuring the temperature of the fluid inclusion.
In the existing fluid inclusion temperature measuring technology, the chinese patent application (201410792390.0) discloses an inclusion temperature measuring system and a detection method thereof, which utilizes a temperature measuring instrument and an image acquisition system and adopts a uniform method to measure the uniform temperature of an inclusion. The temperature measuring method has the following defects: when the fluid inclusion is used for measuring the temperature, the phase state of the fluid inclusion needs to be identified by naked eyes or an image acquisition system, different people judge the fluid inclusion differently, and particularly when the fluid inclusion is small, a test result has certain errors. Therefore, it is necessary to provide a measuring method to make the measurement result closer to the real temperature, and to effectively avoid the error caused by objective factors or human factors to the temperature measurement experiment.
Disclosure of Invention
The invention aims to provide a method for measuring the uniform temperature of a fluid inclusion, which effectively avoids the adverse effect on experimental data caused by the objective existence of a metastable state, and effectively calibrates in time in the measuring process through the influence of the metastable state phenomenon on the temperature measuring process and the temperature measuring data of the fluid inclusion, thereby further improving the reliability and the accuracy of the temperature measuring data of the inclusion.
In fluid inclusion thermometry, it is an essential condition that the volume of the inclusion be kept constant. The inclusion body is a uniform, closed and constant-volume system without considering the existence of a metastable state phenomenon, and the phase state transformation process is completely reversible along with the change of temperature. However, the entire fully reversible process is delayed due to the presence of meta-stability. The invention just utilizes the phenomenon which exists objectively to calibrate the temperature measurement data in the temperature measurement process of the fluid inclusion. Metastable equilibrium means that the system does not reach its lowest energy state, but it has a tendency to change toward stable equilibrium. Many minerals that grow at high temperature and pressure, such as sanidine, kyanite, chrysolite, etc., are metastable in equilibrium with the ability to remain at ambient temperature and pressure. Metastable state of inclusion means: when the temperature is increased and decreased to a certain temperature, some component of the inclusion should be nucleated (crystal nucleus or bubble, etc.) and the inclusion phase which is not nucleated. The metastable state is caused by the lack of nucleation conditions in the inclusion composition, which is most pronounced in smaller-sized, round or oval inclusions. Fluid inclusions are very small systems, which cannot nucleate normally due to lack of nuclei, and metastable equilibrium phenomena are very common. Therefore, the experimental method for calibrating the temperature measurement of the fluid inclusion in the metastable state is utilized to enable the data of the temperature measurement experiment to be closer to the real temperature, and errors caused by objective factors or human factors to the temperature measurement experiment are effectively avoided.
Specifically, the invention provides a method for measuring the uniform temperature of a fluid inclusion, which comprises the following steps:
(1) placing a sample of the fluid inclusion to be detected in a sample chamber of a calibrated cold and hot platform, and adjusting and focusing an objective lens of a microscope;
(2) adjusting the temperature of the cold and hot table and observing, comprising the following steps:
1) starting temperature rise, and suspending observation of phase state change of the fluid inclusion;
2) when bubbles in the fluid inclusion are obviously reduced and are close to disappear, reducing the temperature rise rate until the fluid inclusion reaches a homogeneous phase, wherein the temperature at the moment is the measured homogeneous temperature of the fluid inclusion;
(3) continuing to heat, then cooling after pausing, and recording the temperature as a reproduction temperature when bubbles in the fluid inclusion are observed to reappear;
(4) comparing the measured uniform temperature and the reproduction temperature, and performing the following steps a) or b):
a) when the measured uniform temperature is greater than the reproduced temperature, identifying the measured uniform temperature as an actual uniform temperature of the fluid enclosure;
b) when the measured uniform temperature is less than the reproduction temperature, repeating steps (2) and (3) until the measured uniform temperature is greater than the reproduction temperature.
In the above-mentioned measuring method, CO may be used in the step (1)2And calibrating the cold and hot table by the temperature of the triple point of the inclusion.
In the determination method, in the step (2)1), the temperature rise rate is 10-20 ℃/min, and the phase state change is observed when the temperature per liter is 5-10 ℃.
In the measuring method, in the step (2)2), the temperature rise rate is 0.5-1 ℃/min.
In the determination method, in the step (3), the temperature is increased by 20-30 ℃; pausing for 3-5 min.
The invention provides a method for measuring the freezing point temperature of a fluid inclusion, which comprises the following steps:
(1) placing a sample of the fluid inclusion to be detected in a sample chamber of a calibrated cold and hot platform, and adjusting and focusing an objective lens of a microscope;
(2) adjusting the temperature of the cold and hot table and observing, comprising the following steps:
1) beginning to cool, and pausing to observe the phase change of the fluid inclusion;
2) reducing the rate of cooling until the fluid inclusions are completely frozen before bubbles in the fluid inclusions disappear;
3) continuously cooling;
(3) in the process of starting heating, when the last ice crystal of the fluid inclusion is about to melt, cooling, and growing the ice crystal again and pushing the bubbles to leave the original position;
(4) continuing heating, wherein the ice crystals are melted and reduced, cooling again when the temperature is increased to 0.1-0.2 ℃ higher than the temperature increased in the step (3), and growing again if the ice crystals are not completely melted;
(5) observing the regrowth condition of the ice crystals in the fluid inclusion after the temperature reduction in the step (4), and carrying out the following steps a) or b):
a) when the liquid is completely melted, ice crystals can not appear quickly due to a metastable state phenomenon, bubbles can not move, and the temperature at the moment is the freezing point temperature of the fluid inclusion;
b) when ice crystals appear, indicating that the ice crystals are not completely melted, repeating the step (4) until the ice crystals in the fluid inclusion are completely melted.
In the above determination method, in step (1), the freezing temperature of the synthetic inclusion with known salinity may be used to calibrate the cold and hot stage.
In the determination method, in the step (2)1), the cooling rate is 5-10 ℃/min, and the phase state change is observed at a temperature of 2.5-5 ℃ per liter.
In the determination method, in the step (2)2), the cooling rate is 0.5-1 ℃/min.
In the determination method, in the step (2)3), the temperature is reduced by 2-5 ℃ to ensure that the fluid inclusion is completely frozen.
In the measuring method, in the step (3), the temperature is reduced by 2-5 ℃.
In the measuring method, in the step (4), the temperature is reduced by 2-5 ℃.
On the basis of the existing fluid inclusion temperature measurement method, the objective phenomenon of metastable state is combined and utilized to calibrate experimental data. According to the principle of temperature measurement of the inclusion, in the experimental process of temperature measurement of the fluid inclusion, the measured uniform temperature or freezing point temperature is effectively calibrated in time by using the typical phenomenon of metastable state. The experimental method for calibrating the temperature measurement of the inclusion of the fluid by using the metastable state greatly improves the accuracy of temperature measurement experimental data, skillfully avoids the adverse effect on the temperature measurement of the inclusion by reasonably using the metastable state phenomenon, and timely and effectively calibrates the temperature measurement data by using the special phenomenon.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1 measurement of Uniform temperature by fluid Inclusion uniformity method
The fluid inclusion measured in this example was a saline inclusion.
The determination was carried out according to the following procedure:
1. starting a host, a microscope and a temperature measuring instrument;
2. and (3) carrying out standard sample calibration: with CO2Calibrating the cold and hot tables according to the three-phase point temperature of the inclusion;
3. putting a sample which is observed in advance and is divided into two parts into a cold and hot platform sample chamber;
4. adjusting the objective lens, adjusting the visual field to the area of the inclusion to be observed, and focusing;
5. observing, describing and photographing the inclusion to be subjected to temperature measurement and making a corresponding record;
6. adjusting the temperature of the cold and hot table and observing:
A. when the temperature is raised, the temperature raising rate is 10 ℃/min, the temperature per liter is 5 ℃, and the phase state change of the temperature is observed in a suspension mode;
B. before bubbles in the critical inclusion disappear, the heating rate is reduced to 0.5 ℃/min until the inclusion reaches a homogeneous phase, and the temperature of 80 ℃ at the moment is recorded as the measured homogeneous temperature of the inclusion;
7. and (3) after the inclusion reaches the uniform temperature, heating to 100 ℃, staying for 5 minutes, cooling, observing until bubbles reappear, wherein the temperature of 75 ℃ is the reappearance temperature.
And when the measured uniform temperature is 80 ℃ higher than the reproduction temperature of 75 ℃, the measured uniform temperature of 80 ℃ is the actual uniform temperature of the fluid inclusion.
EXAMPLE 2 freezing determination of freezing temperature by fluid inclusion freezing method
The fluid inclusion measured in this example was a saline inclusion.
The determination was carried out according to the following procedure:
1. starting a host, a microscope and a temperature measuring instrument;
2. and (3) carrying out standard sample calibration: calibrating the cold and hot tables by using the freezing point temperature of the synthetic inclusion with known salinity;
3. putting a sample which is observed in advance and is divided into two parts into a cold and hot platform sample chamber;
4. adjusting the objective lens, adjusting the visual field to the area of the inclusion to be observed, and focusing;
5. observing, describing and photographing the inclusion to be subjected to temperature measurement and making a corresponding record;
6. adjusting the temperature of the cold and hot table and observing:
A. when the temperature is reduced, the temperature reduction rate is 5 ℃/min, and the phase change of the liquid is observed temporarily every time the temperature is reduced by 2 ℃/min;
B. before bubbles in the inclusion disappear, the cooling rate is reduced to 0.5 ℃/min until the inclusion is completely frozen;
C. when the inclusion is completely frozen, the temperature is still reduced by 5 ℃ to ensure that the inclusion is completely frozen;
7. in the process of temperature return (heating to-5.2 ℃), when the last ice crystal is about to melt, the temperature is quickly reduced by 2 ℃, the ice crystal grows up again and pushes the bubbles to leave the original position;
8. continuing to heat, melting the ice crystals to reduce the temperature, rapidly cooling to 2 ℃ again when the temperature is about 0.1 ℃ higher than the temperature of the last heating, and growing the ice crystals if the ice crystals are not completely melted;
9. observing that the ice crystals in the inclusion are not completely melted, and repeating the step 8; then observing that the ice crystals in the inclusion are completely melted, and due to a metastable state phenomenon, the ice crystals can not appear quickly, bubbles can not move, and the temperature of minus 5.0 ℃ is the most accurate actually measured freezing point temperature.
The metastable nature of fluid inclusions has a very important impact on inclusion thermometry, which mainly uses the observed phase transition temperature to obtain test data, and sometimes even obtains virtual test results. The invention effectively avoids the adverse effect on experimental data caused by the objective existence of the metastable state, and timely and effectively calibrates the fluid inclusion temperature measurement process and the temperature measurement data in the experiment process through the influence of the metastable state phenomenon on the fluid inclusion temperature measurement process and the temperature measurement data, thereby further improving the reliability and the accuracy of the inclusion temperature measurement data. The method not only can enable an observer to verify the temperature measurement data in time, effectively avoids the influence of human factors on the experimental data, but also reasonably avoids the interference of the metastable state on the test data, and scientifically converts the interference of the metastable state into the improvement on the precision of the experimental data.
Claims (4)
1. A method for determining the uniform temperature of a fluid enclosure, comprising the steps of:
(1) placing a sample of a fluid inclusion to be measured in a sample chamber of a cold and hot stage of a calibrated microscope, adjusting an objective lens of the microscope and focusing;
(2) adjusting the temperature of the cold and hot table and observing, comprising the following steps:
1) starting temperature rise, and suspending observation of phase state change of the fluid inclusion;
2) when bubbles in the fluid inclusion are obviously reduced and are close to disappear, reducing the temperature rise rate until the fluid inclusion reaches a homogeneous phase, wherein the temperature at the moment is the measured homogeneous temperature of the fluid inclusion;
(3) continuing to heat, then cooling after pausing, and recording the temperature as a reproduction temperature when bubbles in the fluid inclusion are observed to reappear;
(4) comparing the measured uniform temperature and the reproduction temperature, and performing the following steps a) or b):
a) when the measured uniform temperature is greater than the reproduced temperature, identifying the measured uniform temperature as an actual uniform temperature of the fluid enclosure;
b) when the measured uniform temperature is less than the reproduction temperature, repeating steps (2) and (3) until the measured uniform temperature is greater than the reproduction temperature.
2. The method for measuring according to claim 1, wherein: in the step (2)1), the temperature rising rate is 10-20 ℃/min, and the phase state change is observed when the temperature per liter is 5-10 ℃.
3. The assay method according to claim 1 or 2, characterized in that: in the step (2)2), the temperature rising rate is 0.5-1 ℃/min.
4. The assay method according to claim 1 or 2, characterized in that: in the step (3), heating to 20-30 ℃; pausing for 3-5 min.
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| CN114113198A (en) * | 2020-09-01 | 2022-03-01 | 中国石油化工股份有限公司 | Method and system for testing uniform temperature of rock fluid inclusion |
| CN113252711B (en) * | 2021-04-14 | 2023-12-22 | 成都理工大学 | Determination method of gas-liquid ratio of fluid inclusion and sub-minerals |
| CN113655061A (en) * | 2021-09-23 | 2021-11-16 | 华志(福建)电子科技有限公司 | Method for identifying melting point of substance based on image and melting point instrument |
| CN116337662B (en) * | 2023-05-24 | 2023-07-28 | 山东科技大学 | Temporary plugging phase control test method for alternately injecting low-temperature fluid and water into ice crystals |
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