CN109580702B - Method for measuring uniform temperature and freezing point temperature of fluid inclusion - Google Patents
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- 239000012530 fluid Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 43
- 230000008014 freezing Effects 0.000 title abstract description 18
- 238000007710 freezing Methods 0.000 title abstract description 18
- 238000001816 cooling Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000003556 assay Methods 0.000 claims 2
- 238000009529 body temperature measurement Methods 0.000 abstract description 28
- 239000013078 crystal Substances 0.000 abstract description 17
- 238000002474 experimental method Methods 0.000 abstract description 8
- 238000012360 testing method Methods 0.000 abstract description 4
- 230000002411 adverse Effects 0.000 abstract description 3
- 238000000265 homogenisation Methods 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 19
- 238000005259 measurement Methods 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000004861 thermometry Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- INJRKJPEYSAMPD-UHFFFAOYSA-N aluminum;silicic acid;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O INJRKJPEYSAMPD-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010443 kyanite Substances 0.000 description 1
- 229910052850 kyanite Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
本发明公开了一种流体包裹体的均一温度和冰点温度的测定方法。均一法测定均一温度时，当测量均一温度大于再现温度时，则认定测量均一温度为流体包裹体的实际均一温度；冷冻法测定冰点温度时，当流体包裹体中的冰晶完全熔化时，则此时的温度即为流体包裹体的冰点温度。本发明有效地规避亚稳态的客观存在对实验数据造成的不利影响，且通过亚稳态现象对流体包裹体测温过程及测温数据的影响，在实验进行过程中及时有效的校准，进一步提高了包裹体测温数据的可靠性、准确性；不仅可以使观测者对测温数据及时地验证，有效避免了人为因素对实验数据的影响，而且合理的避免了亚稳态对测试数据的干扰，将亚稳态现象的干扰科学地转化为对实验数据精度的提高。The invention discloses a method for measuring the uniform temperature and freezing point temperature of fluid inclusions. When the uniform temperature is determined by the homogenization method, when the measured uniform temperature is greater than the reproduction temperature, the measured uniform temperature is determined to be the actual uniform temperature of the fluid inclusions; when the freezing point temperature is determined by the freezing method, when the ice crystals in the fluid inclusions are completely melted, this is the case. The temperature at is the freezing point temperature of the fluid inclusions. The present invention effectively avoids the adverse influence of the objective existence of metastable state on experimental data, and through the influence of metastable state phenomenon on the temperature measurement process and temperature measurement data of fluid inclusions, timely and effective calibration during the experiment is carried out, and further It improves the reliability and accuracy of the temperature measurement data of the inclusions; it not only enables the 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 metastable state to the test data. Interference, scientifically transform the interference of metastable phenomena into the improvement of the accuracy of experimental data.
Description
技术领域technical field
本发明涉及一种流体包裹体的均一温度和冰点温度的测定方法，属于温度测量技术领域。The invention relates to a method for measuring the uniform temperature and freezing point temperature of fluid inclusions, belonging to the technical field of temperature measurement.
背景技术Background technique
矿物在生长过程中所圈闭的流体保存了当时地质环境的各种地质地球化学信息(如：温度、压力、成分等)，因此可以通过对包裹体中古流体的定性或定量分析，获得各种数据、信息，进一步解释所研究的地壳及地幔中的各种地质作用过程。流体包裹体分析已广泛运用于矿床学、石油勘探及构造地质学等地学领域，是目前地球科学研究中最为活跃的领域之一。The fluid trapped by the mineral during the growth process preserves various geological and geochemical information (such as temperature, pressure, composition, etc.) of the geological environment at that time. data and information to further explain the various geological processes in the studied crust and mantle. The analysis of fluid inclusions has been widely used in the fields of geology such as mineral deposits, petroleum exploration and structural geology, and is one of the most active fields in geosciences at present.
流体包裹体测温技术是非破坏性的直接获取流体包裹体被捕获时温度、压力及盐度最便捷的方法，也是目前最广泛应用的方法。流体包裹体测温的基本原理：(1)均一法测定均一温度原理：选取气—液两相包裹体(捕获时为单一相的包裹体)，利用冷热台加温到某一温度时气—液两相转变为单一相，恢复包裹体形成时的相态(单一相)，恢复时的瞬间温度即为包裹体的均一温度。(2)冷冻法测定冰点温度原理利用不同浓度的盐水溶液具有不同冰点的原理，来测定包裹体液相的冰点温度，根据所测包裹体的冰点即可应用相应的相图求出包裹体的液相浓度。流体包裹体测温方法是在详细观察和辨认包裹体中含流体的各种物相(固相、液相、气相)基础上，通过调控升温(或降温)测量并观察记录包裹体的各种瞬间相变化的温度，从而达到流体包裹体测温的目的。Fluid inclusion thermometry is the most convenient and non-destructive method to directly obtain the temperature, pressure and salinity of fluid inclusions when they are captured, and it is also the most widely used method at present. The basic principle of temperature measurement of fluid inclusions: (1) Homogeneous method to measure uniform temperature. - The liquid two phases are transformed into a single phase, and the phase state (single phase) when the inclusions are formed is restored, and the instantaneous temperature during recovery is the uniform temperature of the inclusions. (2) The principle of freezing point temperature determination by freezing method The freezing point temperature of the liquid phase of the inclusions can be determined by using the principle that salt solutions with different concentrations have different freezing points. Liquid concentration. The temperature measurement method of fluid inclusions is based on the detailed observation and identification of various phases (solid phase, liquid phase, gas phase) containing fluids in the inclusions. The temperature of the instantaneous phase change, so as to achieve the purpose of measuring the temperature of fluid inclusions.
现有流体包裹体测温技术中，中国专利申请(201410792390.0)公开了一种包裹体测温系统及其检测方法，该方法利用测温仪器及图像采集系统，并采用均一法对包裹体的均一温度进行测定。该测温方法存在如下不足之处：在用流体包包裹体测温时，需依靠肉眼或图像采集系统对流体包裹体进行相态进行识别，不同人的判断不同，特别是流体包裹体较小时，测试结果会存在一定的误差。因此需要提供一种测定方法，以使测量结果更加接近真实温度，有效避免因客观因素或人为因素对测温实验造成的误差。Among the existing fluid inclusion temperature measurement technologies, Chinese patent application (201410792390.0) discloses an inclusion temperature measurement system and a detection method thereof. temperature is measured. This temperature measurement method has the following shortcomings: when measuring the temperature of fluid inclusions, it is necessary to rely on the naked eye or image acquisition system to identify the phase state of the fluid inclusions. Different people have different judgments, especially when the fluid inclusions are small. , there will be some errors in the test results. Therefore, it is necessary to provide a measurement method, so as to make the measurement result closer to the real temperature, and to effectively avoid errors caused by objective factors or human factors in the temperature measurement experiment.
发明内容SUMMARY OF THE INVENTION
本发明的目的是提供一种流体包裹体的均一温度的测定方法，本发明方法有效地避免了亚稳态的客观存在对实验数据造成的不利影响，且通过亚稳态现象对流体包裹体测温过程及测温数据的影响，在测定过程中及时有效的校准，进一步提高了包裹体测温数据的可靠性、准确性。The object of the present invention is to provide a method for measuring the uniform temperature of fluid inclusions. The method of the present invention effectively avoids the adverse effects caused by the objective existence of metastable states on experimental data, and measures fluid inclusions through metastable state phenomena. The influence of temperature process and temperature measurement data, timely and effective calibration in the measurement process, further improves the reliability and accuracy of inclusion temperature measurement data.
在流体包裹体测温学上，包裹体的体积保持恒定是一个必不可少的条件。在不考虑亚稳态现象存在的情况下，包裹体是一个均一、封闭、等容的体系，随着温度的变化而发生相态的转变过程是完全可逆的。然而由于亚稳态的存在，导致整个完全可逆的过程产生延迟的现象。本发明正是利用这一客观存在的现象，在流体包裹体测温过程中对测温数据进行校准。亚稳平衡是指体系并未达到它的最低能量状态，但它有向稳定平衡变化的趋势。许多高温和高压下生长的矿物，如透长石、蓝晶石、柯石英等在常温常压下仍能够保持下来便属于亚稳平衡。包裹体的亚稳态指：当升温和降温至一定温度时，包裹体某个成分应该成核(晶核或气泡等)而未成核的包裹体相。造成亚稳态的原因是包裹体成分中缺乏成核的条件，这种现象在粒径较小、圆形或椭圆形包裹体中最为显著。流体包裹体是非常小的体系，由于缺乏晶核而不能正常地发生成核作用，亚稳平衡现象十分常见。因此利用亚稳态对流体包裹体测温进行校准的实验方法使得测温实验的数据更加接近真实温度，有效避免因客观因素或人为因素对测温实验造成的误差。In the thermometry of fluid inclusions, it is an essential condition that the volume of the inclusions remains constant. In the case of disregarding the existence of metastable state, the inclusion is a homogeneous, closed and isovolumic system, and the phase transition process with the change of temperature is completely reversible. However, due to the existence of metastable states, the entire fully reversible process is delayed. The present invention utilizes this objectively existing phenomenon to calibrate the temperature measurement data during the temperature measurement process of the fluid inclusions. Metastable equilibrium means that the system has not reached its lowest energy state, but it has a tendency to change towards stable equilibrium. Many minerals grown under high temperature and high pressure, such as feldspar, kyanite, coesite, etc., can still be maintained at normal temperature and pressure, and they belong to metastable equilibrium. The metastable state of the inclusions refers to the inclusion phase in which a certain component of the inclusions should nucleate (crystal nuclei or bubbles, etc.) but not nucleate when the temperature is raised and cooled to a certain temperature. The metastability is caused by the lack of nucleation conditions in the inclusion composition, which is most pronounced in smaller, round or elliptical inclusions. Fluid inclusions are very small systems that cannot nucleate normally due to the lack of nuclei, and metastable equilibrium is very common. Therefore, the experimental method of calibrating the temperature measurement of fluid inclusions by metastable state makes the data of the temperature measurement experiment closer to the real temperature, and effectively avoids the error caused by objective factors or human factors in the temperature measurement experiment.
具体地，本发明提供的流体包裹体的均一温度的测定方法，包括如下步骤：Specifically, the method for measuring the uniform temperature of fluid inclusions provided by the present invention includes the following steps:
(1)将待测的流体包裹体的样品置于经校准的冷热台的样品室中，调节显微镜的物镜并对焦；(1) Place the sample of the fluid inclusion to be measured in the sample chamber of the calibrated hot and cold stage, adjust the objective lens of the microscope and focus;
(2)调节所述冷热台的温度并观察，包括如下步骤：(2) regulate the temperature of described hot and cold stage and observe, comprise the steps:
1)开始升温，期间暂停观察所述流体包裹体的相态变化；1) Start to heat up, and pause to observe the phase change of the fluid inclusions during the period;
2)当所述流体包裹体中的气泡明显变小且临近消失前，降低所述升温的速率，直至所述流体包裹体达到均一相，此时的温度即为所述流体包裹体的测量均一温度；2) When the air bubbles in the fluid inclusions are significantly smaller and are about to disappear, reduce the rate of temperature increase until the fluid inclusions reach a homogeneous phase, and the temperature at this time is the measurement uniformity of the fluid inclusions. temperature;
(3)继续升温，然后暂停后再进行降温，当观察到所述流体包裹体中的气泡重新出现时，此时的温度记为再现温度；(3) continue to heat up, then pause and then lower the temperature, when it is observed that the bubbles in the fluid inclusions reappear, the temperature at this time is recorded as the reproduction temperature;
(4)对比所述测量均一温度和所述再现温度，并进行下述步骤a)或b)：(4) Compare the measured uniform temperature and the reproduction temperature, and carry out the following steps a) or b):
a)当所述测量均一温度大于所述再现温度时，则认定所述测量均一温度为所述流体包裹体的实际均一温度；a) When the measured uniform temperature is greater than the reproduction temperature, the measured uniform temperature is determined to be the actual uniform temperature of the fluid inclusion;
b)当所述测量均一温度小于所述再现温度时，则重复步骤(2)和(3)，直至所述测量均一温度大于所述再现温度。b) When the measurement uniformity temperature is lower than the reproduction temperature, repeat steps (2) and (3) until the measurement uniformity temperature is greater than the reproduction temperature.
上述的测定方法中，步骤(1)中，可采用CO2包裹体的三相点温度对所述冷热台进行校准。In the above determination method, in step (1), the triple point temperature of the CO 2 inclusions can be used to calibrate the cooling and heating stage.
上述的测定方法中，步骤(2)1)中，所述升温的速率为10～20℃/min，每升温5～10℃暂停观察所述相态变化。In the above determination method, in step (2) 1), the heating rate is 10-20°C/min, and the phase state change is suspended for every 5-10°C heating.
上述的测定方法中，步骤(2)2)中，所述升温的速率为0.5～1℃/min。In the above determination method, in step (2) 2), the heating rate is 0.5-1°C/min.
上述的测定方法中，步骤(3)中，升温20～30℃；暂停3～5min。In the above determination method, in step (3), the temperature is increased by 20 to 30° C.; the temperature is suspended for 3 to 5 minutes.
本发明所提供的流体包裹体的冰点温度的测定方法，包括如下步骤：The method for measuring the freezing point temperature of fluid inclusions provided by the present invention comprises the following steps:
(1)将待测的流体包裹体的样品置于经校准的冷热台的样品室中，调节显微镜的物镜并对焦；(1) Place the sample of the fluid inclusion to be measured in the sample chamber of the calibrated hot and cold stage, adjust the objective lens of the microscope and focus;
(2)调节所述冷热台的温度并观察，包括如下步骤：(2) regulate the temperature of described hot and cold stage and observe, comprise the steps:
1)开始降温，期间暂停观察所述流体包裹体的相态变化；1) Start cooling, and pause to observe the phase state change of the fluid inclusions during the period;
2)在临近所述流体包裹体中的气泡消失前，降低所述降温的速率，直至所述流体包裹体全部冻结；2) before the bubbles in the fluid inclusions disappear, reducing the cooling rate until the fluid inclusions are completely frozen;
3)继续降温；3) Continue to cool down;
(3)开始升温的过程中，当所述流体包裹体的最后一粒冰晶即将熔化时，进行降温，所述冰晶重新长大并推动气泡离开原位；(3) in the process of starting to heat up, when the last ice crystal of the fluid inclusion is about to melt, the temperature is lowered, and the ice crystal grows up again and pushes the bubble to leave the original position;
(4)继续升温，所述冰晶熔化变小，当升温至比步骤(3)中升温的温度高0.1～0.2℃时，再次降温，若所述冰晶仍未熔化完全则又会重新长大；(4) continue to heat up, described ice crystal melting becomes smaller, when warming up to 0.1～0.2 ℃ higher than the temperature that heats up in step (3), lower the temperature again, if described ice crystal still does not melt completely, will grow up again;
(5)经步骤(4)降温后，观察所述流体包裹体中的冰晶的重新生长情况，并进行下述步骤a)或b)：(5) After cooling in step (4), observe the regrowth of the ice crystals in the fluid inclusions, and carry out the following steps a) or b):
a)当完全熔化时，由于亚稳态现象，将不会再很快再出现冰晶，气泡也不移动，则此时的温度即为流体包裹体的冰点温度；a) When it is completely melted, due to the metastable phenomenon, ice crystals will not appear again soon, and the bubbles will not move, then the temperature at this time is the freezing point temperature of the fluid inclusions;
b)当出现冰晶时，说明其未完全熔化，则重复步骤(4)，直至所述流体包裹体中的冰晶完全熔化。b) When ice crystals appear, it means that they are not completely melted, and step (4) is repeated until the ice crystals in the fluid inclusions are completely melted.
上述的测定方法中，步骤(1)中，可采用已知盐度的合成包裹体的冰点温度对所述冷热台进行校准。In the above determination method, in step (1), the freezing point temperature of the synthetic inclusions with known salinity can be used to calibrate the hot and cold stage.
上述的测定方法中，步骤(2)1)中，所述降温的速率为5～10℃/min，每升温2.5～5℃暂停观察所述相态变化。In the above determination method, in step (2) 1), the cooling rate is 5-10° C./min, and the phase state change is suspended for every 2.5-5° C. temperature increase.
上述的测定方法中，步骤(2)2)中，所述降温的速率为0.5～1℃/min。In the above determination method, in step (2) 2), the cooling rate is 0.5-1°C/min.
上述的测定方法中，步骤(2)3)中，降温2～5℃，确保所述流体包裹体完全冻结。In the above determination method, in step (2) 3), the temperature is lowered by 2 to 5° C. to ensure that the fluid inclusions are completely frozen.
上述的测定方法中，步骤(3)中，降温2～5℃。In the above determination method, in step (3), the temperature is lowered by 2 to 5°C.
上述的测定方法中，步骤(4)中，降温2～5℃。In the above determination method, in step (4), the temperature is lowered by 2 to 5°C.
在现有流体包裹体测温方法的基础上，结合并利用亚稳态这一客观存在的现象对实验数据进行校准。根据包裹体测温的原理，在流体包裹体测温实验过程中，利用亚稳态的典型现象，及时有效地对所测得的均一温度或冰点温度进行校准。利用亚稳态对流体包裹体测温进行校准的实验方法大大提高测温实验数据的准确性，通过合理运用亚稳态现象，巧妙地将其对包裹体测温带来的不利影响合理避免，并利用这一特殊的现象及时、有效的对测温数据进行校准。Based on the existing temperature measurement methods of fluid inclusions, the experimental data is calibrated by combining and using the objective phenomenon of metastability. According to the principle of temperature measurement of inclusions, in the process of temperature measurement of fluid inclusions, the typical phenomenon of metastable state is used to timely and effectively calibrate the measured uniform temperature or freezing point temperature. The experimental method of calibrating the temperature measurement of fluid inclusions by metastable state greatly improves the accuracy of temperature measurement experimental data. This special phenomenon calibrates the temperature measurement data in a timely and effective manner.
具体实施方式Detailed ways
下述实施例中所使用的实验方法如无特殊说明，均为常规方法。The experimental methods used in the following examples are conventional methods unless otherwise specified.
下述实施例中所用的材料、试剂等，如无特殊说明，均可从商业途径得到。The materials, reagents, etc. used in the following examples can be obtained from commercial sources unless otherwise specified.
实施例1、流体包裹体均一法测定均一温度Embodiment 1, fluid inclusion homogenization method measures homogenization temperature
本实施例测定的流体包裹体为盐水溶液包裹体。The fluid inclusions measured in this example are saline solution inclusions.
按照下述步骤进行测定：Follow the steps below to measure:
1、启动主机、显微镜及测温仪器；1. Start the host, microscope and temperature measuring instrument;
2、进行标样校准：用CO2包裹体的三相点温度对冷热台进行校准；2. Carry out standard sample calibration: use the triple point temperature of CO 2 inclusions to calibrate the hot and cold stage;
3、将预先观察并分割处理好的样品放入冷热台样品室中；3. Put the pre-observed and divided samples into the sample chamber of the hot and cold stage;
4、调节物镜，将视域调节至所需观测包裹体的区域，并对焦；4. Adjust the objective lens, adjust the field of view to the area where the inclusions need to be observed, and focus;
5、对拟测温的包裹体进行观察描述、拍照并做好相应的记录；5. Observe and describe the inclusions to be temperature-measured, take pictures and make corresponding records;
6、调节冷热台温度并观察：6. Adjust the temperature of the hot and cold table and observe:
A、开始升温时，升温速率为10℃/min，每升温5℃，应暂停观察其相态变化；A. When the temperature rises, the heating rate is 10°C/min, and the phase state change should be suspended for every 5°C temperature rise;
B、在临界包裹体中气泡消失前，升温速率将至0.5℃/min，直至包裹体达到均一相，此时的温度80℃记为包裹体的测量均一温度；B. Before the bubbles disappear in the critical inclusions, the heating rate will be 0.5°C/min until the inclusions reach a homogeneous phase, and the temperature at this time of 80°C is recorded as the measured homogeneous temperature of the inclusions;
7、包裹体达到均一温度后升温至100℃，停留5分钟再进行降温，并观测直到气泡重新出现的温度，此时的温度75℃即为即再现温度。7. After the inclusions reach a uniform temperature, heat up to 100°C, stay for 5 minutes and then cool down, and observe the temperature until the bubbles reappear. The temperature at this time of 75°C is the reappearance temperature.
测量均一温度80℃大于再现温度75℃，则测量均一温度80℃即为该流体包裹体的实际均一温度。If the measured uniform temperature of 80°C is greater than the reproduction temperature of 75°C, the measured uniform temperature of 80°C is the actual uniform temperature of the fluid inclusion.
实施例2、流体包裹体冷冻法测定冰点温度Example 2. Determination of freezing point temperature by fluid inclusion freezing method
本实施例测定的流体包裹体为盐水溶液包裹体。The fluid inclusions measured in this example are saline solution inclusions.
按照下述步骤进行测定：Follow the steps below to measure:
1、启动主机、显微镜及测温仪器；1. Start the host, microscope and temperature measuring instrument;
2、进行标样校准：用已知盐度的合成包裹体的冰点温度对冷热台进行校准；2. Carry out standard sample calibration: use the freezing point temperature of synthetic inclusions with known salinity to calibrate the hot and cold stage;
3、将预先观察并分割处理好的样品放入冷热台样品室中；3. Put the pre-observed and divided samples into the sample chamber of the hot and cold stage;
4、调节物镜，将视域调节至所需观测包裹体的区域，并对焦；4. Adjust the objective lens, adjust the field of view to the area where the inclusions need to be observed, and focus;
5、对拟测温的包裹体进行观察描述、拍照并做好相应的记录；5. Observe and describe the inclusions to be temperature-measured, take pictures and make corresponding records;
6、调节冷热台温度并观察：6. Adjust the temperature of the hot and cold table and observe:
A、开始降温时，降温速率为5℃/min，每降温2℃/min，应暂停观察其相态变化；A. When cooling starts, the cooling rate is 5°C/min, and the phase state change should be suspended for every 2°C/min cooling;
B、在临近包裹体中气泡消失前，降温速率降至0.5℃/min，直至包裹体全部冻结；B. Before the bubbles in the inclusions disappear, the cooling rate is reduced to 0.5°C/min until the inclusions are completely frozen;
C、当包裹体全部冻结后，仍需降温5℃，确保其完全冻结；C. When the inclusions are completely frozen, it is still necessary to cool down by 5 °C to ensure that they are completely frozen;
7、回温过程中(升至-5.2℃)，当最后一粒冰晶即将熔化时，快速降温2℃，冰晶会重新长大并推动气泡离开原位；7. During the temperature recovery process (rising to -5.2°C), when the last ice crystal is about to melt, rapidly cool down by 2°C, the ice crystal will grow again and push the bubbles away from the original position;
8、继续回温，该冰晶又会熔化变小，当回温至比上次回温的温度约高0.1℃时，再次快速降温2℃，若冰晶仍未熔化完则又会长大；8. Continue to return to temperature, and the ice crystals will melt and become smaller. When the temperature is returned to about 0.1°C higher than the last temperature, the temperature will be rapidly lowered by 2°C again. If the ice crystals are not completely melted, they will grow again;
9、观察包裹体中的冰晶未完全熔化，重复步骤8；然后观察到包裹体中的冰晶完全熔化，由于亚稳态现象，将不会很快再出现冰晶，气泡也不移动，此时的温度-5.0℃是最为准确的实测冰点温度。9. Observe that the ice crystals in the inclusions are not completely melted, and repeat step 8; then observe that the ice crystals in the inclusions are completely melted. Due to the metastable phenomenon, ice crystals will not appear again soon, and the bubbles will not move. The temperature of -5.0℃ is the most accurate measured freezing point temperature.
流体包裹体的亚稳态特性对主要以观测相态转变温度来获取测试数据的包裹体测温学来说，有着极其重要的影响，有时甚至会得出虚拟的测试结果。本发明有效地规避亚稳态的客观存在对实验数据造成的不利影响，且通过亚稳态现象对流体包裹体测温过程及测温数据的影响，在实验进行过程中及时有效的校准，进一步提高了包裹体测温数据的可靠性、准确性。这一方法不仅可以使观测者对测温数据及时地验证，有效避免了人为因素对实验数据的影响，而且合理的避免了亚稳态对测试数据的干扰，将亚稳态现象的干扰科学地转化为对实验数据精度的提高。The metastable properties of fluid inclusions have an extremely important influence on the thermometry of inclusions, which mainly obtains test data by observing the phase transition temperature, and sometimes even obtains virtual test results. The present invention effectively avoids the adverse influence of the objective existence of metastable state on experimental data, and through the influence of metastable state phenomenon on the temperature measurement process and temperature measurement data of fluid inclusions, timely and effective calibration during the experiment is carried out, and further The reliability and accuracy of the temperature measurement data of the inclusions are improved. This method not only enables the observer to verify the temperature measurement data in a timely manner, 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 understands the interference of the metastable state phenomenon. This translates into an improvement in the accuracy of experimental data.
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