CN109580702A - A kind of homogenization temperature of fluid inclusion and the measuring method of freezing point temperature - Google Patents
A kind of homogenization temperature of fluid inclusion and the measuring method of freezing point temperature Download PDFInfo
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- 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
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Abstract
The invention discloses the measuring methods of a kind of homogenization temperature of fluid inclusion and freezing point temperature.When homogenization method measures homogenization temperature, when measuring homogenization temperature greater than reproducible temperature, then assert that measurement homogenization temperature is the practical homogenization temperature of fluid inclusion；When freezing measures freezing point temperature, when the ice crystal in fluid inclusion is completely melt, then temperature at this time is the freezing point temperature of fluid inclusion.The present invention effectively evades metastable objective reality adverse effect caused by experimental data, and pass through influence of the metastable state phenomenon to fluid-rock system process and temperature measurement data, it is timely and effectively calibrated during testing and carrying out, further improves reliability, the accuracy of inclusion temperature data；Not only observer can be made to verify temperature measurement data in time, effectively prevent influence of the human factor to experimental data, and interference of the metastable state to test data is reasonably avoided, the raising to test data precision is scientifically converted by the interference of metastable state phenomenon.
Description
Technical field
The present invention relates to the measuring methods of a kind of homogenization temperature of fluid inclusion and freezing point temperature, belong to temperature measurement skill
Art field.
Background technique
The fluid of mineral institute's trap during the growth process saves the various GEOLOGICAL AND GEOCHEMICAL information of geological environment at that time
(such as: temperature, pressure, ingredient), therefore various numbers can be obtained by the qualitative or quantitative analysis to fossil fluid in inclusion enclave
According to, information, the various geologic process in the studied earth's crust and earth mantle are explained further.Fluid-inclusion analysis is extensive
Apply to the ground such as Ore Deposits, oil exploration and structural geology field, is neck the most active in current geoscience research
One of domain.
Fluid-rock system technology be it is nondestructive directly acquire fluid inclusion it is captured when temperature, pressure and salt
Spend most convenient and fast method, and method most widely used at present.The basic principle of fluid-rock system: (1) homogenization method is surveyed
Determine homogenization temperature principle: choosing gas-liquid two-phase inclusion enclave (being the inclusion enclave of single-phase when capture), be warmed to using cold and hot
Gas-liquid two-phase is changed into single-phase when a certain temperature, restores the phase (single-phase) when inclusion enclave formation, moment when recovery
Temperature is the homogenization temperature of inclusion enclave.(2) freezing measurement freezing point temperature principle has using the saline solution of various concentration
The principle of different freezing points can be using corresponding according to the freezing point of surveyed inclusion enclave to measure the freezing point temperature of inclusion enclave liquid phase
Phasor finds out the liquid concentration of inclusion enclave.Fluid-rock system method is in detailed observation and identification inclusion enclave containing fluid
On the basis of various object phases (solid phase, liquid phase, gas phase), is measured by regulation heating (or cooling) and observe and record the various of inclusion enclave
The temperature of moment phase change, to achieve the purpose that fluid-rock system.
In existing fluid-rock system technology, Chinese patent application (201410792390.0) discloses a kind of inclusion enclave
Temp measuring system and its detection method, this method utilize temperature measuring device and image capturing system, and using homogenization method to inclusion enclave
Homogenization temperature is measured.The temp measuring method has the following deficiencies:, need to be by naked eyes when with fluid packet inclusion temperature
Or image capturing system carries out phase to fluid inclusion and identifies, the judgement of different people is different, especially fluid inclusion
When smaller, test result can there is a certain error.Therefore need to provide a kind of measuring method, so that measurement result is more nearly
True temperature effectively avoids error caused by testing because of objective factor or human factor to thermometric.
Summary of the invention
The object of the present invention is to provide a kind of measuring methods of the homogenization temperature of fluid inclusion, and the method for the present invention is effectively
Metastable objective reality adverse effect caused by experimental data is avoided, and fluid inclusion is surveyed by metastable state phenomenon
The influence of warm process and temperature measurement data, is timely and effectively calibrated in continuous mode, further improves inclusion temperature data
Reliability, accuracy.
In fluid-rock system, it is an essential condition that the volume of inclusion enclave, which is kept constant,.It is not examining
Consider metastable state phenomenon in the presence of, inclusion enclave be one it is uniform, closing, etc. appearances system, sent out with the variation of temperature
The transition process of raw phase is completely reversibility.However due to metastable presence, the process of entire completely reversibility is caused to generate
The phenomenon that delay.The phenomenon that present invention exactly utilizes this objective reality, to temperature measurement data during fluid-rock system
It is calibrated.Metastable equilibrium refers to system and is not up to its minimum energy state, but the trend of its oriented stable equilibrium's variation.
The mineral grown under many high temperature and high pressures, such as glassy feldspar, kyanite, coesite still are able to remain behind at normal temperatures and pressures
Just belong to metastable equilibrium.The metastable state of inclusion enclave refers to: when heating up and being cooled to certain temperature, inclusion enclave some ingredient should be at
Core (nucleus or bubble etc.) and the inclusion phase not being nucleated.Cause metastable the reason is that lacking the item of nucleation in Fluid Inclusion Compositions
Part, this phenomenon partial size is smaller, in round or ellipse inclusion enclave it is the most significant.Fluid inclusion is very small system,
Nucleation cannot normally occur due to lacking nucleus, metastable equilibrium phenomenon is very common.Therefore metastable state convection current is utilized
The data that the experimental method that body inclusion temperature is calibrated tests thermometric are more nearly true temperature, effectively avoid because of visitor
Error caused by sight factor or human factor test thermometric.
Specifically, the measuring method of the homogenization temperature of fluid inclusion provided by the invention, includes the following steps:
(1) sample of fluid inclusion to be measured is placed in cold and hot calibrated sample room, is adjusted microscopical
Object lens are simultaneously focused；
(2) the cold and hot temperature and observation are adjusted, is included the following steps:
1) it starts to warm up, during which the phase-state change of the fluid inclusion is observed in pause；
2) before the bubble in the fluid inclusion obviously becomes smaller and closes on disappearance, the rate of the heating is reduced, directly
Reach homogeneous phase to the fluid inclusion, temperature at this time is the measurement homogenization temperature of the fluid inclusion；
(3) continue to heat up, cool down again after then suspending, when observing that the bubble in the fluid inclusion goes out again
Now, temperature at this time is denoted as reproducible temperature；
(4) the measurement homogenization temperature and the reproducible temperature are compared, and carries out following step a) or b):
A) when the measurement homogenization temperature is greater than the reproducible temperature, then assert that the measurement homogenization temperature is the stream
The practical homogenization temperature of body inclusion enclave；
B) when the measurement homogenization temperature is less than the reproducible temperature, then repeatedly step (2) and (3), up to the survey
It measures homogenization temperature and is greater than the reproducible temperature.
In above-mentioned measuring method, in step (1), CO can be used2The triple point of inclusion enclave to described cold and hot into
Row calibration.
In above-mentioned measuring method, step (2) 1) in, the rate of the heating is 10~20 DEG C/min, every heating 5~10
The phase-state change is observed in DEG C pause.
In above-mentioned measuring method, step (2) 2) in, the rate of the heating is 0.5~1 DEG C/min.
In above-mentioned measuring method, in step (3), heat up 20~30 DEG C；Suspend 3~5min.
The measuring method of the freezing point temperature of fluid inclusion provided by the present invention, includes the following steps:
(1) sample of fluid inclusion to be measured is placed in cold and hot calibrated sample room, is adjusted microscopical
Object lens are simultaneously focused；
(2) the cold and hot temperature and observation are adjusted, is included the following steps:
1) start to cool down, during which the phase-state change of the fluid inclusion is observed in pause；
2) before the bubble collapse closed in the fluid inclusion, the rate of the cooling is reduced, until the fluid
Inclusion enclave all freezes；
3) continue to cool down；
(3) it during starting to warm up, when last ice crystal of the fluid inclusion will melt, is dropped
Temperature, the ice crystal grow up again and bubble are pushed to leave original position；
(4) continue to heat up, the ice crystal fusing becomes smaller, higher by 0.1~0.2 than the temperature to heat up in step (3) when being warming up to
DEG C when, cool down again, if the ice crystal still it is unfused completely if again can grow up again；
(5) after step (4) cooling, the situation that regrows of the ice crystal in the fluid inclusion is observed, and carry out down
State step a) or b):
A) when being completely melt, due to metastable state phenomenon, will not occur ice crystal again quickly again, bubble does not also move, then
Temperature at this time is the freezing point temperature of fluid inclusion；
B) when there is ice crystal, illustrate that it is not completely melt, then repeatedly step (4), until in the fluid inclusion
Ice crystal is completely melt.
In above-mentioned measuring method, in step (1), the freezing point temperature of the synthetic inclusion of known salinity can be used to described
Cold and hot is calibrated.
In above-mentioned measuring method, step (2) 1) in, the rate of the cooling is 5~10 DEG C/min, every heating 2.5~5
The phase-state change is observed in DEG C pause.
In above-mentioned measuring method, step (2) 2) in, the rate of the cooling is 0.5~1 DEG C/min.
In above-mentioned measuring method, step (2) 3) in, cool down 2~5 DEG C, it is ensured that the fluid inclusion fully charge.
In above-mentioned measuring method, in step (3), cool down 2~5 DEG C.
In above-mentioned measuring method, in step (4), cool down 2~5 DEG C.
On the basis of existing fluid-rock system method, in conjunction with and the phenomenon that using this objective reality of metastable state pair
Experimental data is calibrated.According to the principle of inclusion temperature, in fluid-rock system experimentation, utilization is metastable
Typical phenomenon timely and effectively calibrates measured homogenization temperature or freezing point temperature.Using metastable state to Fluid inclusions
The experimental method that body thermometric is calibrated greatly improves the accuracy of thermometric experimental data, by reasonable utilization metastable state phenomenon,
Dexterously it rationally avoids inclusion temperature bring adverse effect, and in time, effectively using this special phenomenon
Temperature measurement data is calibrated.
Specific embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1, fluid inclusion homogenization method measure homogenization temperature
The fluid inclusion of the present embodiment measurement is saline solution inclusion enclave.
It is measured as steps described below:
1, start host, microscope and temperature measuring device；
2, it carries out standard specimen calibration: using CO2The triple point of inclusion enclave calibrates cold and hot；
3, by preparatory observation, simultaneously the good sample of dividing processing is put into cold and hot sample room；
4, object lens are adjusted, the region of observation inclusion enclave needed for the ken is adjusted to, and focus；
5, is carried out by observation description, take pictures and carries out corresponding record for the inclusion enclave of quasi- thermometric；
6, it adjusts cold and hot temperature and observes:
A, when starting to warm up, heating rate is 10 DEG C/min, and every 5 DEG C of heating should suspend and observe its phase-state change；
B, in critical inclusion before bubble collapse, the near 0.5 DEG C/min of heating rate, until inclusion enclave reaches uniform
Phase, 80 DEG C of temperature at this time are denoted as the measurement homogenization temperature of inclusion enclave；
7, inclusion enclave is warming up to 100 DEG C after reaching homogenization temperature, stops 5 minutes and cools down again, and observes until bubble
The temperature reappeared, 75 DEG C of temperature at this time are as reproducible temperature.
80 DEG C of homogenization temperature of measurement are greater than 75 DEG C of reproducible temperature, then measuring 80 DEG C of homogenization temperature is the fluid inclusion
Practical homogenization temperature.
Embodiment 2, fluid inclusion freezing measure freezing point temperature
The fluid inclusion of the present embodiment measurement is saline solution inclusion enclave.
It is measured as steps described below:
1, start host, microscope and temperature measuring device；
2, it carries out standard specimen calibration: cold and hot being calibrated with the freezing point temperature of the synthetic inclusion of known salinity；
3, by preparatory observation, simultaneously the good sample of dividing processing is put into cold and hot sample room；
4, object lens are adjusted, the region of observation inclusion enclave needed for the ken is adjusted to, and focus；
5, is carried out by observation description, take pictures and carries out corresponding record for the inclusion enclave of quasi- thermometric；
6, it adjusts cold and hot temperature and observes:
A, when starting cooling, rate of temperature fall is 5 DEG C/min, 2 DEG C/min of every cooling, should suspend and observe its phase-state change；
B, in closing on inclusion enclave before bubble collapse, rate of temperature fall is down to 0.5 DEG C/min, until inclusion enclave all freezes；
C, after inclusion enclave all freezes, 5 DEG C of cooling is still needed to, it is ensured that its fully charge；
7, (- 5.2 DEG C are risen to) during rising again, when last ice crystal will melt, 2 DEG C of fast cooling, ice crystal meeting
Again it grows up and bubble is pushed to leave original position；
8, continue to rise again, which can melt again becomes smaller, when rising again to about high 0.1 DEG C of the temperature risen again than last time, then
2 DEG C of secondary fast cooling, if ice crystal still it is unfused it is complete if again can grow up；
9, the ice crystal observed in inclusion enclave is not completely melt, repeats step 8；Then observe that the ice crystal in inclusion enclave is complete
Fusing, due to metastable state phenomenon, ice crystal will not occurs, bubble does not also move, and -5.0 DEG C of temperature at this time are the most again quickly
Accurately actual measurement freezing point temperature.
The meta-stable behavior of fluid inclusion observes mainly phase transition temperature to obtain the inclusion enclave of test data
For thermometry, there is extremely important influence, can even obtain virtual test result sometimes.The present invention effectively evades Asia
The objective reality of stable state is adversely affected caused by experimental data, and by metastable state phenomenon to fluid-rock system process and
The influence of temperature measurement data is timely and effectively calibrated during testing and carrying out, and further improve inclusion temperature data can
By property, accuracy.This method not only can make observer verify temperature measurement data in time, effectively prevent human factor pair
The influence of experimental data, and interference of the metastable state to test data is reasonably avoided, by the interference science of metastable state phenomenon
Ground is converted into the raising to test data precision.
Claims (10)
1. a kind of measuring method of the homogenization temperature of fluid inclusion, includes the following steps:
(1) sample of fluid inclusion to be measured is placed in calibrated microscopical cold and hot sample room, described in adjusting
Microscopical object lens are simultaneously focused；
(2) the cold and hot temperature and observation are adjusted, is included the following steps:
1) it starts to warm up, during which the phase-state change of the fluid inclusion is observed in pause；
2) before the bubble in the fluid inclusion obviously becomes smaller and closes on disappearance, the rate of the heating is reduced, until institute
It states fluid inclusion and reaches homogeneous phase, temperature at this time is the measurement homogenization temperature of the fluid inclusion；
(3) continue to heat up, cool down again after then suspending, when observing that the bubble in the fluid inclusion reappears
When, temperature at this time is denoted as reproducible temperature；
(4) the measurement homogenization temperature and the reproducible temperature are compared, and carries out following step a) or b):
A) when the measurement homogenization temperature is greater than the reproducible temperature, then assert that the measurement homogenization temperature is the fluid packet
Wrap up in the practical homogenization temperature of body；
B) when the measurement homogenization temperature is less than the reproducible temperature, then repeatedly step (2) and (3), until the measurement is
One temperature is greater than the reproducible temperature.
2. measuring method according to claim 1, it is characterised in that: step (2) 1) in, the rate of the heating is 10~
20 DEG C/min, the phase-state change is observed in every 5~10 DEG C of pauses of heating.
3. measuring method according to claim 1 or 2, it is characterised in that: step (2) 2) in, the rate of the heating is
0.5~1 DEG C/min.
4. measuring method according to any one of claim 1-3, it is characterised in that: in step (3), heating 20~30
℃；Suspend 3~5min.
5. a kind of measuring method of the freezing point temperature of fluid inclusion, includes the following steps:
(1) sample of fluid inclusion to be measured is placed in calibrated microscopical cold and hot sample room, described in adjusting
Microscopical object lens are simultaneously focused；
(2) the cold and hot temperature and observation are adjusted, is included the following steps:
1) start to cool down, during which the phase-state change of the fluid inclusion is observed in pause；
2) before the bubble collapse closed in the fluid inclusion, the rate of the cooling is reduced, until the Fluid inclusions
Body all freezes；
3) continue to cool down；
(3) during starting to warm up, when last ice crystal of the fluid inclusion will melt, cool down, institute
Ice crystal is stated to grow up again and bubble is pushed to leave original position；
(4) continuing to heat up, the ice crystal fusing becomes smaller, when being warming up to 0.1~0.2 DEG C higher than the temperature to heat up in step (3),
Cool down again, if the ice crystal still it is unfused completely if again can grow up again；
(5) after step (4) cooling, the situation that regrows of the ice crystal in the fluid inclusion is observed, and carry out following steps
It is rapid a) or b):
A) when being completely melt, then temperature at this time is the freezing point temperature of fluid inclusion；
B) when there is ice crystal, then repeatedly step (4), the ice crystal in the fluid inclusion are completely melt.
6. measuring method according to claim 5, it is characterised in that: step (2) 1) in, the rate of the cooling is 5~
10 DEG C/min, the phase-state change is observed in every 2.5~5 DEG C of pauses of heating.
7. measuring method according to claim 5 or 6, it is characterised in that: step (2) 2) in, the rate of the cooling is
0.5~1 DEG C/min.
8. the measuring method according to any one of claim 5-7, it is characterised in that: step (2) 3) in, cooling 2~5
℃。
9. the measuring method according to any one of claim 5-8, it is characterised in that: in step (3), cool down 2~5 DEG C.
10. the measuring method according to any one of claim 5-9, it is characterised in that: in step (4), cool down 2~5 DEG C.
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| CN113252711A (en) * | 2021-04-14 | 2021-08-13 | 成都理工大学 | Method for measuring 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 |
| 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 |
| CN116337662A (en) * | 2023-05-24 | 2023-06-27 | 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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| 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 |
| CN113252711A (en) * | 2021-04-14 | 2021-08-13 | 成都理工大学 | Method for measuring gas-liquid ratio of fluid inclusion and sub-minerals |
| 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 |
| CN116337662A (en) * | 2023-05-24 | 2023-06-27 | 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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