CN106500877B - A kind of thermal station temperature correction method - Google Patents
A kind of thermal station temperature correction method Download PDFInfo
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- CN106500877B CN106500877B CN201611020222.5A CN201611020222A CN106500877B CN 106500877 B CN106500877 B CN 106500877B CN 201611020222 A CN201611020222 A CN 201611020222A CN 106500877 B CN106500877 B CN 106500877B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K15/00—Testing or calibrating of thermometers
- G01K15/002—Calibrated temperature sources, temperature standards therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K15/00—Testing or calibrating of thermometers
- G01K15/005—Calibration
Abstract
The invention discloses a kind of thermal station temperature correction method, configuration specific components, concentration sulfate solution, and melting capillary silicone tube capsule is made in enclosed melting capillary silicone tube；The melting capillary silicone tube capsule containing different component, the sulfate solution of concentration prepared is placed in the thermal station of calibrated mistake and is heated, until liquid liquid phase separation occurs in melting capillary silicone tube capsule, record the generation temperature of liquid liquid phase separation and establishes corresponding database；The melting capillary silicone tube capsule of containing sulfate aqueous solution is placed in the thermal station of not calibrated mistake and is heated, the generation temperature of liquid liquid phase separation is recorded, is then compared with database, to be corrected to thermal station temperature.Temperature stabilization occurs for the sulfuric acid brine system liquid liquid phase separation of the present invention and range is more wide in range, can meet the temperature correction demand of conventional thermal station.It is convenient, fast to melt capillary silicone tube synthetic inclusion.
Description
Technical field
The present invention relates to temperature correction fields, and in particular to a kind of thermal station temperature correction method.
Background technology
High temperature and pressure simulated experiment is to study the important means of Earth geologic process.Currently, high temperature and pressure simulation is real
The enrichment and migration for being widely used in metallic element in mineralization are tested, hydrocarbon simulation and Water-rock interaction mechanism and dynamics are ground
Study carefully.Fluid inclusion is the movable positive evidence of geology fossil fluid, the original geology of in store fossil fluid, geochemical information.
Using the analysis means such as homogenization method, decrepitation method and freezing can obtain inclusion enclave capture when temperature and pressure and its at
Point, the information such as salinity and density, contribute to geologic process that is more intuitive and clearly recognizing earth interior, such as geologic process
Temperature, pressure condition recovery, BIFhosted gold deposit and mineralizing genesis research etc..In recent years, Fluid-inclusion analysis is led in oil exploration
Domain is also widely used, to explain hydrocarbon generation history, Oil and gas charging period and Oil charge history etc..It is simulated in high temperature and pressure
During experiment and fluid-rock system, temperature controls whether accurately to affect the accuracy of experimental result to a certain extent
And reliability.Therefore, either high temperature and pressure simulated experiment or fluid inclusion microthermometry analysis, all needs before experiment
Temperature correction is carried out to Temperature-controlled appliance.
Laboratory temperature truing tool (or standard specimen) mainly has mercurial thermometer, standard reagent and thermocouple etc..Wherein, water
Silver-colored thermometer temperature-measuring range is relatively low, and precision is not high, few to use.Standard reagent such as utilizes sulphur, sodium nitrate, nitric acid
The fusing point of the substances such as potassium carries out temperature correction to instrument, and this method is very high to reagent purity requirement, and during the experiment
It is also possible to pollute equipment and even damage.Quartzy crack healing method synthetic inclusion standard specimen can also be used for thermal station temperature school
Just, such as pure H2O inclusion enclaves freezing point (0 DEG C) and super critical point (374 DEG C), pure CO2Inclusion enclave three phase point (- 56.6 DEG C) etc..With H2O
Supercritical temperature for, due to artificial inclusion enclave formed the time differ, not every inclusion enclave, which all meets temperature calibration, to be wanted
It asks.In addition, the quartzy crack of application is healed, it is relative complex to prepare artificial inclusion enclave program for method, also relatively time-consuming.Thermocouple, which has, to be surveyed
The advantages that warm precision is higher, temperature-measuring range wide (- 200~1300 DEG C), also becomes a kind of more commonly used temperature measurement tool, but its
The disadvantage is that probe may be contaminated influence, especially temperature equilibrium time is longer in static gaseous medium.And it is long
Time uses, and pyroelecthc properties often change, therefore in order to obtain higher temperature measurement accuracy, after a period of use
It needs to examine and determine thermocouple and calibrated.Thermal resistance be the common temperature measurement tool of middle low-temperature space (<200 DEG C), but its temperature-sensitive
Portion size is larger, and reaction rate is relatively slow, and temperature measurement accuracy is also vulnerable to the influence of resistance wire aging.In conclusion
All there is different degrees of defect and apply upper limitation in existing temperature correction method, this calibrates work to laboratory temperature
Bring inconvenience.
Unmixing or phenomenon of phase separation is relatively conventional during magmatic evolution and hydrothermal process, as melt-fluid does not mix
Molten and liquid-gas phase is unmixing etc..And the research of liquid-liquid phase separation is relatively fewer in Hydrothermal System, at present about inorganic solution
The research of high temperature liquid-liquid phase separation is concentrated mainly on sulfate-aqueous systems.Sulfate is the second largest solute component in seawater,
It is the important component of lithosphere fluid and melt.In the subduction zone of oxidizing condition, sulfate can be for transmission to great depth
(~40km), then it is released in plate dehydration in fluid phase.The research of liquid-liquid phase separation in early stage inorganic solution
It is concentrated mainly on UO2SO4-H2O systems, because of UO2SO4It is the fuel of aqueous homogeneous reactor, the generation temperature of liquid-liquid phase separation is
The upper limit of reactor operating temperature.
Some researches show that the presence of low-k component, and the liquid-liquid phase point of sulfate solution can be greatly lowered
From temperature.Such as 0.5m CdSO4The temperature of liquid-liquid phase separation is 224.5 DEG C, by methanol and CdSO4Solution is with 0.8 volume
After solution is added, the temperature of liquid-liquid phase separation is down to 151.4 DEG C；And H is added2SO4Afterwards, the liquid-liquid phase of sulfate solution
Separation temperature can then increase.Such as 0.1m LiSO4The temperature that liquid-liquid phase separation occurs is 352 DEG C, and 0.1m LiSO4-
0.01m H2SO4The liquid-liquid phase separation temperature of solution is 353 DEG C.Some researches show that, in the case where sulfate concentration is certain,
The H of addition2SO4More, the temperature of liquid-liquid phase separation is higher.By taking pure aquatic system as an example, saturated vapor pressure is only at 350 DEG C
16.5MPa, and the pressure that common melting capillary silicone tube can be born is up to 100MPa or more.Under identical temperature condition, sulfuric acid brine
The saturated vapor pressure of solution is smaller than pure water, therefore, observes the liquid-liquid phase separation of sulfate solution under the conditions of saturated vapor pressure
Phenomenon will not cause to melt the explosion of capillary silicone tube capsule.
Invention content
Goal of the invention：In order to overcome the deficiencies in the prior art, the present invention to provide a kind of thermal station temperature correction method,
According to MgSO4、ZnSO4、CdSO4、Li2SO4Liquid-liquid phase separation phenomenon can occur under the high temperature conditions for equal sulfate liquors, i.e.,
Uniform solution is mutually gradually disengaged out two liquid phases of enrichment sulfate and poor sulfate under the high temperature conditions.Sulfate-aqueous systems
The temperature of liquid-liquid phase separation and fluid components and pressure are closely related, show more wide in range temperature range (150~360
℃).Sulfur-bearing can be easily synthesized using I-Ming Chou et al. melting capillary silicone tube synthetic fluid inclusion technologies developed
The transparent cavity of acid salt solution coordinates Linkam cold and hot generation temperature that can accurately measure its liquid-liquid phase separation of CAP500
Degree.In addition, having found out that sulfate-aqueous systems liquid-liquid phase separation occurs for packing density the influence of temperature, and analyze liquid-liquid phase
The standard deviation of temperature occurs for separation.On the basis of above-mentioned work, new thermal station temperature correction method is established.
Technical solution：
A kind of thermal station temperature correction method, including step：
Step 1：The sulfate solution of certain component, concentration is configured, and melting capillary is made in enclosed melting capillary silicone tube
Silicone tube capsule；
Step 2：The melting capillary silicone tube capsule that step 1 prepares is placed in the thermal station of calibrated mistake and is heated, until
Liquid-liquid phase separation occurs in melting capillary silicone tube capsule, and records the generation temperature of liquid-liquid phase separation as the component, concentration
" normal temperature " of liquid-liquid phase separation occurs for sulfate solution；
Step 3：Step 1 and step 2 are repeated, measures different component, liquid-liquid phase separation occurs for the sulfate solution of concentration
Temperature, and establish corresponding database；
Step 4：Melting capillary silicone tube capsule containing main constituent, concentration sulphuric acid saline solution is placed in the heat of not calibrated mistake
It is heated on platform, and records the generation temperature of liquid-liquid phase separation, be then compared with database, to be carried out to thermal station temperature
Correction.
The sulfate solution is matched by analyzing pure grade chemicals and deionized water by molality (mol/kg)
It makes.
The melting capillary silicone tube specification is as follows：100 μm of internal diameter, 300 μm of outer diameter, section are circle, can be born
The pressure of 100MPa or more.
The melting capillary silicone tube capsule manufacturing process is as follows：
Step 11：The polyimide covercoat for being covered in melting capillary tube surface is burnt up with oxyhydrogen flame, hair will be melted
One end oxyhydrogen flame sealing of thin silicone tube；
Step 12：Prepared sulfate solution is dropped on clean evaporating dish, with electric iron close to melting capillary
Silicone tube drives the air in melting capillary silicone tube, then immerses in solution melting capillary silicone tube open end, electricity is removed after 1-2 seconds
Soldering iron simultaneously takes out melting capillary silicone tube；
Step 13：Sulfate solution is centrifuged to sealing end using centrifuge, is then attached to melting capillary silicone tube
Vacuum pipeline vacuumizes, and is used in combination oxyhydrogen flame by open end sealing, that is, is prepared into the melting capillary silicone tube capsule of containing sulfate solution.
In the sealing stage of step 13, cold water or liquid nitrogen are immersed into the melting capillary silicone tube part of containing sulfate aqueous solution
In.
A concentration of 1mol/kg or more of sulfate solution that the melting capillary silicone tube capsule prepared in the step 1 uses.
Melting capillary silicone tube capsule prepared by the step 1 selects the sulfuric acid containing specific components, concentration according to actual needs
Saline solution is prepared.
The thermal station rate of heat addition is as follows in the step 2：When target temperature is less than 200 DEG C, heating rate is 5 DEG C/min,
When target temperature is higher than 200 DEG C, heating rate is 0.5 DEG C/min.
Advantageous effect：
(1) temperature stabilization occurs for sulfate-aqueous systems liquid-liquid phase separation and range is more wide in range (150-360 DEG C), can
To meet the temperature correction demand of conventional thermal station.The corrosion resistance of capillary silicone tube is stronger, especially in acid condition, SiO2
Corrosion is very weak under the conditions of experimental temperature, will not be made a significant impact on liquid-liquid phase separation temperature.
(2) compared with method is healed in quartzy crack, melting capillary silicone tube synthetic inclusion is convenient, fast.Using melting capillary
Silicone tube can synthesize various inorganic, Organic Inclusions in a short time, and its size it is more typical fluid inclusion it is big, phase transformation
Observation is also relatively sharp.
(3) melting capillary silicone tube capsule has stronger mechanical strength, can bear higher temperature, pressure, non-explosive
It splits, experiment safety is reliable.
(4) moderate dimensions for melting capillary silicone tube capsule, can be placed in common thermal station, meet different type thermal station
Use demand.Contain only the melting capillary silicone tube capsule of solution sample if prepared, length can control in 1.5cm hereinafter, and its
Outer diameter is generally less than 0.3mm.Therefore, in addition to the Linkam CAP500 and INSTEC that are designed for melting capillary silicone tube experiment are cold
Outside thermal station, melting capillary silicone tube capsule can easily be placed in other common cold and hot, and (such as 600 types of Linkam THMSG are cold
Thermal station).And the larger thermal resistance of volume is then difficult to work in narrow regions.
Description of the drawings
Fig. 1 is thermal station structure and sample stage Temperature Distribution.
Fig. 2 is the relationship that temperature and fluid composition occur for different system liquid-liquid phase separations.
Fig. 3 is packing density to 1.0m CdSO4The influence of temperature occurs for liquid-liquid phase separation.
Specific implementation mode
The present invention is further described below in conjunction with the accompanying drawings.
The present invention provides a kind of thermal station temperature correction method, includes the following steps：
Step 1：The sulfate solution of certain component, concentration is configured, and melting capillary is made in enclosed melting capillary silicone tube
Silicone tube capsule.
Sulfate solution is by analyzing pure grade chemicals (MgSO4, Fisher Certified Reagent；Li2SO4,
ZnSO4, CdSO4, Sigma-Aldrich) and deionized water (~18.2k Ω) be formulated by molality (mol/kg,
m).Sulfate solution concentration can be 1mol/kg or more.Alkali metal soln is in alkalescent under the high temperature conditions, to which meeting is molten
Lose silicone tube.In order to weaken Li2SO4Corrosion of the solution to silicone tube inner wall, is added a small amount of H in the solution2SO4, Li is made2SO4With
H2SO4Molar ratio is 10:1 Li2SO4-H2SO4Mixed solution, wherein Li2SO4Concentration may be selected 0.1m, 0.5m, 1.0m,
1.5m and 2.0m.
Optical clear chamber is prepared using melting capillary silicone tube (Polymicro Technologies, LLC), the present invention uses
Melting capillary silicone tube specification it is as follows：100 μm of internal diameter, 300 μm of outer diameter, section are circle, can bear the pressure of 100MPa or more
Power.First the polyimide covercoat for being covered in tube surface is burnt up with oxyhydrogen flame, then by one end oxyhydrogen welding of silicone tube
Envelope.Prepared solution is dropped on clean evaporating dish, the air in silicone tube is driven close to silicone tube with electric iron, then by silicon
Tube opening end is immersed in solution, and electric iron is removed after 1-2 seconds and takes out silicone tube.Solution is centrifuged to sealing end using centrifuge,
Then silicone tube is attached to vacuum pipeline to vacuumize, is used in combination oxyhydrogen flame by open end sealing, that is, be prepared into containing sulfate solution
Melt capillary silicone tube capsule.In the last sealing stage, in order to prevent in silicone tube solution boiling and effusion, will generally contain solution
Silicone tube part immerse in cold water or liquid nitrogen.The length of the melting capillary silicone tube capsule sample prepared is generally less than 2cm.
Since the repeatability that liquid-liquid phase separation occurs for sulfate-aqueous systems is strong, and same sample liquid-liquid phase separation temperature
The standard deviation of degree is smaller, is repeated 1-2 times when measuring same sample liquid-liquid phase separation temperature.In addition, sulfate liquor is dense
Degree is higher, and the high concentration phase volume that liquid-liquid phase separation is formed after occurring is bigger, therefore, in order to reduce production during phase transformation observation
Raw error, it is proposed that the melting capillary silicone tube capsule (such as >=1m) for preparing the sulfate liquor containing higher concentration, as thermal station temperature
The standard specimen of calibration.
Step 2：The sample prepared is placed in the thermal station of calibrated mistake and is heated, until liquid-liquid phase separation occurs, note
The generation temperature for recording liquid-liquid phase separation occurs " normal temperature " of liquid-liquid phase separation as the component sulfate solution.
Temperature-controlled appliance used in the present invention is the CAP500 type thermal station of Linkam companies of Britain production.Inside thermal station
Sample stage by metallic silver at.After melting capillary silicone tube is placed on sample stage, lid one carries the silver strip of trepanning on it, is convenient for light
Learn observation (Fig. 1 a).Metallic silver has good thermal conductivity, therefore the thermal station has good thermal stability (± 0.1 DEG C), sample
Sample platform internal temperature differential is less than 1 DEG C.In order to detect the Temperature Distribution of sample stage in thermal station used in this experiment, Type-K thermoelectricity is utilized
The temperature (Fig. 1 b) of equally distributed 5 points within the scope of even 4cm when measuring different target temperature.Before experiment, Type-K thermocouples
It is corrected by Wuxi City measurement verification test center.As illustrated in figure 1 c, when thermal station target temperature be respectively set as 100 DEG C, 200
DEG C, 300 DEG C, 400 DEG C when, the temperature difference within the scope of sample stage 4cm is respectively smaller than 0.1,0.2,0.5 and 0.9 DEG C.Due to thermal station temperature
It is 500 DEG C to spend the upper limit, and the temperature difference is larger in thermal station on the temperature spot, but again smaller than 2 DEG C within the scope of 4cm.
By the melting capillary silicone tube capsule prepared merging thermal station heating.It balances and accurately measures in order to ensure system reaches
The generation temperature of liquid-liquid phase separation, when target temperature is less than 200 DEG C, heating rate is 5 DEG C/min, when target temperature is higher than
At 200 DEG C, heating rate is 0.5 DEG C/min.The high temperature phase behavior of sulfate-aqueous systems, object lens are observed using Leica microscope
Multiple is 10 × and 20 ×.In order to ensure the repeatability of experimental phenomena, the phase behavior of each sample is observed 2-5 times.
Step 3：The temperature of liquid-liquid phase separation, Ke Yijian occur for the sulfate solution by measuring different component, concentration
Found corresponding database.Other laboratories can select the sulfate solution containing specific components, concentration according to the needs of oneself
Standard specimen of the melting capillary silicone tube capsule as the laboratory thermal station temperature correction.
Step 4：The melting capillary of main constituent, concentration sulphuric acid saline solution is heated using the thermal station for not carrying out temperature correction
When silicone tube capsule, the generation temperature of liquid-liquid phase separation is recorded, is then compared with database, to be carried out to thermal station temperature
Correction.
Fig. 2 summarizes the relationship that temperature and solution concentration occur for part of sulfuric acid salt-aqueous systems high temperature liquid-liquid phase separation.
In low strength range, the generation temperature of liquid-liquid phase separation is reduced with the raising of solution concentration, and in highly concentrated solution,
The temperature of the generation of liquid-liquid phase separation increases (table 1) with the raising of solution concentration, and typical lower critical solution temperature is presented
Phenomenon (lower critical solution temperature, LCST).Li in the present invention2SO4-H2SO4Mixed solution
LCST is about 339.5 DEG C.LCST is the typical macroscopic property of polymer solution, therefore, the liquid-liquid phase separation characterized by LCST
Appearance imply these sulfate liquors complicated ion complexation have occurred under the high temperature conditions.In alkali metal sulfates
In solution, SO4 2-It under the high temperature conditions can be with SiO2Interaction forms Si (OH)4·SO4 2-Complex compound, to improve SiO2's
Solubility.The ingredient for melting capillary silicone tube is almost pure SiO2, and contain Li2SO4The melting capillary silicone tube capsule of solution is at 350 DEG C
H is added in following tube wall corrosion phenomenon unobvious2SO4Afterwards, tube wall corrosion is weaker.Therefore, SiO2Dissolving is to Li2SO4-H2O/H2SO4
The influence of system liquid-liquid phase separation effect can be ignored.In addition, the sulfate liquor for the generation liquid-liquid phase separation reported at present,
The solubility of its sulfate, higher than after certain value, is reduced with the raising of temperature in temperature.Such as pressure be 0.1MPa
When, MgSO4·H2O be high-temperature stable mineral facies (>68℃),MgSO4·H2The solubility of O is significantly dropped with the raising of temperature
It is low.Under the conditions of saturated vapor pressure, anhydrous Li2SO4It is Li2SO4-H2O systems high-temperature stable phase (>233℃).Li2SO4Dissolving
Degree is reduced when temperature is higher than 233 DEG C with the raising of temperature.From phasor, Li2SO4-H2SO4-H2Liquid-occurs for O systems
The temperature of liquid phase separation is higher than corresponding Li2SO4Solubility curve, this also indicates that the structure of solution occurs under the high temperature conditions
Variation.
Different system liquid-liquid phase separation temperature (DEG C) under the conditions of 1. saturated vapor pressure of table
*Li2SO4And H2SO4Molar ratio is 10:1.
When preparing the melting capillary silicone tube capsule containing sulfate liquor, it is difficult to ensure the vapor/liquid ratio of all samples (i.e.
Compactedness) unanimously, therefore, it is necessary to which to specific components sulfate liquor liquid-liquid phase separation temperature occurs for evaluate sample compactedness
Influence.The packing density of sample refers to the percentage that the volume of solution phase accounts for melting capillary silicone tube capsule total volume.With 1m
CdSO4For, it has made packing density and has melted capillary silicone tube capsule, as shown in figure 3 and table 2,1m CdSO between 30-70%4Liquid-
Liquid phase separation occurs that apparent correlation is not present between temperature and the packing density of sample, and packing density is to liquid-liquid phase separation
The influence very little of temperature occurs, maximum deviation is only 0.3 DEG C.From 1m ZnSO4,1m CdSO4With 1m Li2SO4-0.1m H2SO4
From the point of view of the measurement result of solution, the generation temperature of same sample liquid-liquid phase separation has good repeatability, 5 measurements
Standard deviation is respectively less than 0.1 DEG C (table 3).To sum up, the generation temperature repeatability of sulfate-aqueous systems liquid-liquid phase separation is strong, and
Liquid-liquid phase separation occurs for sample packing density the influence very little of temperature.Therefore, liquid-liquid phase separation in typical sulfate solution
Generation temperature can be as the standard specimen of thermal station temperature correction.
2. 1.0m CdSO of table4The temperature of liquid-liquid phase separation occurs when packing density is between 32~67.80% for solution
(℃)
The standard deviation of liquid-liquid phase separation temperature (DEG C) occurs for the typical sulfate solution of table 3.
The above is only a preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of thermal station temperature correction method, it is characterised in that：Including step：
Step 1：The sulfate solution of certain component, concentration is configured, and melting capillary silicone tube is made in enclosed melting capillary silicone tube
Capsule；
Step 2：The melting capillary silicone tube capsule that step 1 prepares is placed in the thermal station of calibrated mistake and is heated, until melting
Liquid-liquid phase separation occurs in capillary silicone tube capsule, and records the generation temperature of liquid-liquid phase separation as the component, concentration sulphuric acid
" normal temperature " of liquid-liquid phase separation occurs for saline solution；
Step 3：Step 1 and step 2 are repeated, measures different component, the temperature of liquid-liquid phase separation occurs for the sulfate solution of concentration
Degree, and establish corresponding database；
Step 4：Melting capillary silicone tube capsule containing main constituent, concentration sulphuric acid saline solution is placed in the thermal station of not calibrated mistake
Heating, and the generation temperature of liquid-liquid phase separation is recorded, it is then compared with database, to be corrected to thermal station temperature.
2. thermal station temperature correction method according to claim 1, it is characterised in that：The sulfate solution is pure by analyzing
Grade chemicals and deionized water are formulated by molality.
3. thermal station temperature correction method according to claim 1, it is characterised in that：The melting capillary silicone tube specification is such as
Under：100 μm of internal diameter, 300 μm of outer diameter, section are circle.
4. thermal station temperature correction method according to claim 1, it is characterised in that：It is prepared by the melting capillary silicone tube capsule
Process is as follows：
Step 11：The polyimide covercoat for being covered in melting capillary tube surface is burnt up with oxyhydrogen flame, capillary silicon will be melted
One end of pipe oxyhydrogen flame sealing；
Step 12：Prepared sulfate solution is dropped on clean evaporating dish, with electric iron close to melting capillary silicone tube
The air in melting capillary silicone tube is driven, then melting capillary silicone tube open end is immersed in solution, electric iron is removed after 1-2 seconds
And take out melting capillary silicone tube；
Step 13：Sulfate solution is centrifuged to sealing end using centrifuge, melting capillary silicone tube is then attached to vacuum
Pipeline vacuumizes, and is used in combination oxyhydrogen flame by open end sealing, that is, is prepared into the melting capillary silicone tube capsule of containing sulfate solution.
5. thermal station temperature correction method according to claim 4, it is characterised in that：In the sealing stage of step 13, will contain
The melting capillary silicone tube part of sulfate solution is immersed in cold water or liquid nitrogen.
6. thermal station temperature correction method according to claim 1, it is characterised in that：The melting hair prepared in the step 1
A concentration of 1mol/kg or more of sulfate solution that thin silicone tube capsule uses.
7. thermal station temperature correction method according to claim 1, it is characterised in that：Melting capillary prepared by the step 1
Silicone tube capsule selects the sulfate solution containing certain component, concentration to be prepared according to actual needs.
8. thermal station temperature correction method according to claim 1, it is characterised in that：The thermal station rate of heat addition in the step 2
It is as follows：When target temperature is less than 200 DEG C, heating rate is 5 DEG C/min, when target temperature is higher than 200 DEG C, heating rate
It is 0.5 DEG C/min.
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Citations (3)
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|---|---|---|---|---|
| WO2010092137A2 (en) * | 2009-02-11 | 2010-08-19 | Institut National De La Recherche Agronomique - Inra | Methods for testing the accuracy and thermal reliability of a pcr thermal cycler, and a means for implementing said methods |
| CN105097420A (en) * | 2014-05-05 | 2015-11-25 | 无锡华润上华科技有限公司 | Temperature calibration method for MASSON quick heat treatment stock |
| WO2016038425A1 (en) * | 2014-09-10 | 2016-03-17 | Braster Sa | Device and method for controlling the calibration of thermochromic liquid-crystal matrices |
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2016
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010092137A2 (en) * | 2009-02-11 | 2010-08-19 | Institut National De La Recherche Agronomique - Inra | Methods for testing the accuracy and thermal reliability of a pcr thermal cycler, and a means for implementing said methods |
| CN105097420A (en) * | 2014-05-05 | 2015-11-25 | 无锡华润上华科技有限公司 | Temperature calibration method for MASSON quick heat treatment stock |
| WO2016038425A1 (en) * | 2014-09-10 | 2016-03-17 | Braster Sa | Device and method for controlling the calibration of thermochromic liquid-crystal matrices |
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| Title |
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| In situ observations of liquid–liquid phase separation in aqueous ZnSO4 solutions;Xiaolin Wang等;《Geochimica et Cosmochimica Acta》;20160302;第1-59页 * |
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