A sample preparation device for a high-pressure crucible of a differential scanning calorimeter (DSC) under a special atmosphere and a sample preparation method thereof

Abstract

The application discloses a kind of special atmosphere under DSC high-pressure crucible sample preparation device and its sample preparation method, sample preparation device includes the external operation box that can provide multi-component gas sample preparation environment, sample preparation platform, sampling tool box, analytical balance, shock pad, modular high-pressure crucible pressure sample device and the like.The external operation box includes transparent airtight box, sample temporary storage warehouse, multiple adjustable gas paths and pipe valves, external lead wire grounding;Sample preparation platform is the smooth table top of corrosion-resistant coating;Sampling tool box includes solid sample feeder and other commonly used tools.The sample preparation device structure is light and compact, which overcomes the shortcomings of large size and heavy weight of existing pressure sample device, can simulate the operating atmosphere in the laboratory conditions to characterize the potential thermal risk of the sample under actual working conditions, and has the characteristics of easy quantization of operation process control parameters, strong crucible specification adaptability and the like.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of thermal analysis equipment, in particular to a sample preparation device for DSC high-pressure crucible under special atmosphere and a sample preparation method thereof. BACKGROUND

[0002] As an important tool for studying the thermal effect and thermal hazard behavior of substances, DSC is often used to obtain thermodynamic and kinetic parameters and thermal safety characteristic parameters of substances, and plays an irreplaceable role in the research of thermal stability of substances, chemical synthesis and process thermal risk research in the process of drug development. Strictly regulated sample preparation process is the basis for accurate acquisition of thermal effect information and thermal dynamics analysis of samples.

[0003] In the study of thermal hazard behavior of substances, the main carrier of DSC test is high-pressure crucible, in order to achieve mass conservation during sample testing and exclude the influence of evaporation, volatilization and other factors on test results. At present, international mainstream thermal analysis equipment manufacturers can provide disposable high-pressure crucibles or reusable high-pressure crucibles of different specifications, and the materials are generally stainless steel or gold-plated stainless steel. The sealing method is punch type or spiral type gasket sealing, and the structure is two-section or three-section. The related crucible types and schematic diagrams are shown in FIGS. 1-3. Figure 1 As shown in the figures, the experimental personnel select the crucible type according to the experimental design requirements.

[0004] However, the high-pressure crucible sealing tool generally has the problems of complex structure, large space occupation, difficult quantification in the operation process, high dependence on the experience of the test personnel, and poor crucible specification adaptability. In view of the fact that the samples to be studied in the current new energy industry, biomedicine industry and other cutting-edge scientific research fields have special properties, they are extremely sensitive to the environment, such as easy to absorb moisture, easy to volatilize, avoid oxygen, avoid water, etc. The limitations of using existing sample preparation devices to carry out sample preparation operations in thermal analysis laboratories are more significant.

[0005] Therefore, there is an urgent need in the art for a sample preparation device for DSC high-pressure crucible under special atmosphere and a sample preparation method thereof, which has a light structure, an easy-to-quantify operation process and strong crucible specification applicability, and can effectively solve the problem of sample preparation using DSC high-pressure crucible under special atmosphere. SUMMARY

[0006] To solve the above technical problems, the present application provides a sample preparation device for DSC high-pressure crucible under special atmosphere, which comprises an external operation box, a sample preparation table, an analytical balance, a shock pad and a modular high-pressure crucible sample pressing device.

[0007] The external operation box is a transparent closed box body, the external operation box is provided with an air inlet and an air outlet, a plurality of adjustable air paths are connected to the air inlet, and a stop valve is fixedly installed on the adjustable air path, the air outlet is connected with a vacuum pump and a waste gas treatment device through a three-way valve, and the external operation box is connected with ground wires;

[0008] The sample preparation table is located in the internal operation box, the material of the sample preparation table is hard plate, and the surface of the sample preparation table is coated with a corrosion-resistant coating.

[0009] One side of the external operation box is provided with a sample temporary storage bin, and the other side of the external operation box is provided with a sampling tool box, the sampling tool box stores a metal powder funnel, a pressing rod, a tweezers, a micro spatula, a pipette gun and a capillary quartz tube.

[0010] The analytical balance is located on one side of the internal operation box, the anti-vibration pad is arranged at the bottom of the analytical balance, and a wind deflector is arranged between the analytical balance and the sampling tool box.

[0011] The modular high-pressure crucible sample pressing device is located on the other side of the internal operation box, and the modular high-pressure crucible sample pressing device comprises a sample preparation tool, a variable shaft transmission device, an adjustable high-hardness crucible groove holder and a cone head, a pre-set torque screwdriver insertion hole and a pre-set torque wrench.

[0012] Specifically, the main operation surface of the external operation box is provided with a plurality of clamping grooves, and a long-sleeved glove is fixed on each clamping groove, which is used for facilitating the sample preparation operation of the operator.

[0013] Specifically, the two sides of the sample temporary storage bin are respectively provided with an inner side window and an outer side window, and the inner side window and the outer side window are both closable movable windows.

[0014] Specifically, the adjustable air path comprises an air inlet pipeline and an air outlet pipeline, a first stop valve is arranged on the air inlet pipeline, and a second stop valve is arranged on the air outlet pipeline.

[0015] Specifically, the gas type of the adjustable air path is argon, nitrogen or oxygen.

[0016] Specifically, the depth scale of the digital distance meter is connected to the cross bar of the cone head of the modular high-pressure crucible sample pressing device, and the two ends of the inner measuring claw of the digital distance meter are respectively connected with the cone head and the bottom plate of the adjustable high-hardness crucible groove holder.

[0017] Specifically, the sample preparation tool, the variable shaft transmission device, the adjustable high-hardness crucible groove holder and the cone head are all made of hard alloy material.

[0018] Specifically, the variable shaft transmission device is fixedly installed in the modular high-pressure crucible sample preparation device, the variable shaft transmission device is in a threaded helical gear transmission mode, the preset torque screwdriver insertion hole is arranged at the top of the modular high-pressure crucible sample preparation device, the preset torque wrench is fixed to one side of the modular high-pressure crucible sample preparation device, the cone head is connected with a cone head connecting piece, the cone head connecting piece is a driven shaft, and the cone head connecting piece is radially displaced with the rotation of the preset torque wrench.

[0019] The application also provides a sample preparation method of the sample preparation device of the DSC high-pressure crucible under a special atmosphere, based on the sample preparation device of the DSC high-pressure crucible under a special atmosphere.

[0020] S1, determining the crucible specification and adjusting zero: according to the sample preparation requirements, the specification of the required crucible is determined, the adjustable high-hardness crucible groove holder corresponding to the specification is selected for installation, the plane of the cone head is adjusted to be parallel to the bottom of the adjustable high-hardness crucible groove holder, the reading of the digital distance meter at this time is recorded and taken as "0";

[0021] S2, a set of blank crucibles are sequentially placed in the adjustable high-hardness crucible groove holder, step S1 is repeated, the torque value of the preset torque wrench is adjusted and slightly overloaded, the reading of the digital distance meter is just zero, the torque value at this time is recorded, the above steps are repeated five times, and three crucibles are randomly selected, the above steps are repeated, and the maximum torque value is taken as the torque reference value T refer , if a larger value appears subsequently, the new larger value is taken as the torque reference value T refer ;

[0022] S3, determining the test atmosphere and introducing the gas: according to the sample preparation requirements, the atmosphere environment required by the sample during the transfer and use process is determined, the external gas source of the gas inlet pipeline is adjusted, the first stop valve is opened, and the air in the external operation box and the sample temporary storage bin is replaced with the determined gas, so that the external operation box and the sample temporary storage bin are filled with the required gas;

[0023] S4, sample weighing under a special atmosphere: the analytical balance is opened, the crucible is placed in the analytical balance, the mass m0 of the blank crucible at this time is recorded, the skin is removed, and the sample is placed in the crucible; the solid sample or the powder sample is weighed by using a metal powder funnel, and the sample is compacted by using a sample pressing rod, and the sample quality m1 is recorded by using a liquid gun or a capillary quartz tube.

[0024] S5, sample preparation: the crucible is sequentially placed in the adjustable high-hardness crucible groove holder, the variable shaft transmission device is rotated to make the cone head tightly contact with the top of the crucible, and the torque value of the preset torque wrench is adjusted to T refer, through the "0" point positioning method, when the digital display of the digital distance measuring instrument is exactly "0", continue to apply force and slightly overload twice, then change the shaft transmission device, take out the crucible and weigh m2, record the sample mass m s = m2-m0, finally, put the pressed crucible into the sample temporary storage bin, and complete the sample preparation.

[0025] Compared with the prior art, the special atmosphere DSC high-pressure crucible sample preparation device has the following beneficial effects:

[0026] 1. The special atmosphere DSC high-pressure crucible sample preparation device provided by the present application has a compact structure and is easy to realize, overcoming the shortcomings of large size and heavy weight of the existing sample preparation device, and effectively solving the problem of difficulty in sample preparation using a DSC high-pressure crucible under special atmosphere in a thermal analysis laboratory.

[0027] 2. The high-hardness crucible groove and the cone head are modularized, and the crucible specification has strong adaptability. After standard sample preparation zero adjustment, whether the digital display of the digital distance measuring instrument is "0" during sample preparation can be used as an auxiliary judgment. This method eliminates the potential torque loss caused by the static friction between the transmission shafts. At this time, the operator directly and accurately completes the sample preparation operation through the "0" value positioning method of the preset torque wrench or the number display measuring instrument, and the sample preparation process is quantized, which can effectively eliminate the influence of human factors on the airtightness of the high-pressure crucible sample preparation process.

[0028] 3. The sample preparation device and the sample preparation method provided by the present application are applied to process flow thermal risk identification research, can simulate the factory operating atmosphere under laboratory conditions, can characterize the potential thermal risk of the sample under actual working conditions, can improve the pertinence and practicality of process engineering control measures, and has guiding significance for the reasonable construction of the protection layer. BRIEF DESCRIPTION OF DRAWINGS

[0029] Figure 1 is a typical DSC high-pressure crucible schematic diagram of a mainstream thermal analysis manufacturer;

[0030] Figure 2 is a schematic diagram of the special atmosphere DSC high-pressure crucible sample preparation device provided by the present application;

[0031] Figure 3 is a schematic diagram of the modular high-pressure crucible sample preparation device in the present application;

[0032] Figure 4 is a schematic diagram of the internal structure of the modular high-pressure crucible sample preparation device in the present application;

[0033] Figure 5 is a schematic diagram of the cone head of the modular high-pressure crucible sample preparation device in the present application;

[0034] Figure 6 is a schematic diagram of the variable shaft transmission device of the modular high-pressure crucible sample preparation device in the present application;

[0035] In the diagram, 1-external operating box, 2-vibration pad, 3-analytical balance, 4-grounding wire, 5-power cord hole, 6-wind baffle, 7-second shut-off valve, 8-air outlet pipe, 9-sampling tool box, 10-modular high-pressure crucible sample pressing device, 11-first shut-off valve, 12-air inlet pipe, 13-preset torque screwdriver insertion hole, 14-preset torque wrench, 15, 17 and 21-long-sleeved gloves, 16-stainless steel base plate, 18-inner window, 19-sample storage chamber, 20-outer window, 22-sample preparation table. Detailed Implementation

[0036] The technical solution of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Unless otherwise specified, the materials, instruments, and reagents used in the following embodiments can be obtained commercially. Unless otherwise specified, the technical means used in the embodiments are conventional means well known to those skilled in the art.

[0037] The structures, proportions, sizes, etc., illustrated in the accompanying drawings of this specification are only for illustrative purposes to aid those skilled in the art and are not intended to limit the implementation conditions of this invention. Therefore, they have no substantial technical significance. Any modifications to the structure, changes in proportions, or adjustments to size, without affecting the effectiveness and purpose of this invention, should still fall within the scope of the technical content disclosed in this invention. Furthermore, the terms such as "upper," "lower," "left," "right," "middle," and "one" used in this specification are merely for clarity of description and are not intended to limit the scope of this invention. Changes or adjustments to their relative relationships, without substantially altering the technical content, should also be considered within the scope of this invention.

[0038] Example 1

[0039] like Figures 2-6 As shown in the figure, this embodiment illustrates a sample preparation device for a DSC high-pressure crucible under a special atmosphere, including an external operation box 1, a sample preparation stage 22, an analytical balance 3, an anti-vibration pad 2, and a modular high-pressure crucible sample pressing device 10;

[0040] The external operation box 1 is a transparent closed box, and the material thereof includes but is not limited to organic glass or acrylic material. The external operation box 1 is provided with an air inlet and an air outlet. The air inlet is connected with a plurality of adjustable air paths, and a stop valve is fixedly installed on the adjustable air path. The air outlet is connected with a vacuum pump and a waste gas treatment device through a three-way valve. The external operation box 1 is provided with a rubber-sealed power line hole 5, and the external lead 4 is grounded to avoid static electricity.

[0041] The sample preparation table 22 is located in the internal of the external operation box 1. The sample preparation table 22 is a flat table surface made of hard plate material, and the surface is coated with a corrosion-resistant coating.

[0042] A sample temporary storage bin 19 is arranged on one side of the external operation box 1, and a sampling tool box 9 is arranged on the other side of the external operation box 1. The sampling tool box 9 stores a metal powder funnel, a pressing rod, a tweezers, a micro spatula, a pipette gun and a capillary quartz tube.

[0043] The analytical balance 3 is located on one side of the internal of the external operation box 1, and is a high-precision analytical balance with a display precision of not less than 0.01 mg. The anti-vibration pad 2 is arranged at the bottom of the analytical balance 3, and is made of fluororubber or rubber, which is used to eliminate the weak vibration of the table surface caused by external force. A wind deflector 6 is arranged between the analytical balance 3 and the sampling tool box 9.

[0044] The modular high-pressure crucible sample pressing device 10 is located on the other side of the internal of the external operation box 1. A stainless steel plate 16 is arranged below the modular high-pressure crucible sample pressing device 10 for support. The modular high-pressure crucible sample pressing device 10 includes a sample preparation tool, a variable shaft transmission device, an adjustable high-hardness crucible groove holder and a tapered head, a pre-set torque screwdriver insertion hole 13 and a pre-set torque wrench 14.

[0045] The main operation surface of the external operation box 1 is provided with a plurality of clamping grooves. A long-sleeved glove 15 / 17 / 21 is fixedly arranged on each clamping groove. The long-sleeved glove 15 / 17 / 21 is used for conveniently operating personnel to perform sample preparation operations, such as sampling, weighing and sample pressing.

[0046] The sample temporary storage bin 19 is provided with an internal side window 18 and an external side window 20 on both sides. The internal side window 18 and the external side window 20 are both closable and movable windows. The adjustable air path includes an air inlet pipeline 12 and an air outlet pipeline 8. The air inlet pipeline 12 is provided with a first stop valve 11, and the air outlet pipeline 8 is provided with a second stop valve 7. The air inlet type of the adjustable air path is argon, nitrogen or oxygen.

[0047] First, the sample is put into the sample temporary storage bin 19 by opening the external side window 20. Then, the external side window 20 is closed, and the air atmosphere is replaced by connecting the air inlet pipeline 12 and the air outlet pipeline 8 of the sample temporary storage bin 19. Then, the sample is transferred to the sample preparation table by opening the internal side window 18, so that the air atmosphere in the bin is consistent with the air atmosphere in the external operation box 1.

[0048] The gas inlet is connected with a gas supply pipeline, and the gas outlet is connected with a vacuum pump and a laboratory exhaust gas aftertreatment device through a three-way joint. The device is operated for 2-3 times alternately to realize the full replacement of the gas in the device. After the gas is replaced, the three-way joint at the gas outlet is switched to connect the laboratory exhaust gas aftertreatment device.

[0049] The depth scale of the digital distance meter is connected to the cross bar of the cone head of the modular high-pressure crucible sample pressing device 10, and the two ends of the inner measuring claw of the digital distance meter are connected to the cone head and the bottom plate of the adjustable high-hardness crucible groove holder, respectively.

[0050] The sample preparation holder, the variable shaft transmission device, the adjustable high-hardness crucible groove holder, and the cone head are all made of hard alloy material.

[0051] The variable shaft transmission device is fixedly installed in the modular high-pressure crucible sample pressing device 10, and the variable shaft transmission device is a threaded helical gear transmission. The top of the driven shaft assembly of the modular high-pressure crucible sample pressing device 10 is a threaded helical gear, and below it is a positioning ring. The inside of the positioning ring is connected to the cone head connecting piece through a thread. The cone head assembly is tightly connected to the cone head connecting piece through a limiting bolt. The two limiting ears on the side surface of the cone head connecting piece are used to limit the axial displacement of the cone head, and the cone head connecting piece can be detached. The top of the cone head connecting piece has an internal hexagonal groove, and the internal hexagonal groove is connected to the internal hexagonal hole of the preset torque wrench inserted into the top of the modular high-pressure crucible sample pressing device 10.

[0052] The preset torque wrench insertion hole 13 is arranged at the top of the modular high-pressure crucible sample pressing device 10, and the preset torque wrench 14 is fixed on one side of the modular high-pressure crucible sample pressing device 10. The cone head is connected to the cone head connecting piece, and the cone head connecting piece is a driven shaft. The cone head connecting piece occurs radial displacement with the rotation of the preset torque wrench 14.

[0053] Based on the above sample preparation device, the method for preparing samples by using 25 μL three-section punch type disposable high-pressure crucible is as follows:

[0054] Step 1: Before using the sample press, determine the crucible specification and perform debugging and zero setting. In this embodiment, a 25 μL three-section punch type disposable high-pressure crucible is selected. Figure 1 (b) Three-section punch type disposable high-pressure crucible, the crucible specification is 25 μL, a groove holder corresponding to the specification is taken out and fixed by a hexagonal screw. During the debugging process, the plane of the cone head is controlled to be parallel to the bottom groove holder. Rotate the top pentagonal handle to raise the cone head, take out a set of high-pressure crucibles to be used, the height of which is 4.72 mm, the corresponding bottom groove holder depth is 2.27 mm, and the distance between the cone head and the bottom groove holder should be 2.45 mm. Adjust the thickness of the difference scale to 2.45 mm, place it on the groove holder, rotate the top pentagonal handle to make the cone head tightly contact with the difference scale, and record the reading of the digital distance meter at this time and set it to "0".

[0055] Step 2: Put a set of empty crucibles into the groove holder in order, repeat the above steps, adjust the torque value of the preset torque wrench 14 and slightly overload, wait for the digital distance meter to show exactly zero, record the torque value at this time. Repeat five times, and randomly select three crucibles, repeat the above steps, take the maximum value of the previous process as the torque reference value T of the crucible of this type refer . If a larger value appears later, use the new larger value as the torque reference value T refer .

[0056] Step 3: Determine the test atmosphere. Two samples to be tested are solid powder and colorless transparent liquid. According to the requirements of the research and development process, the samples must be in argon protection during transfer and use, and strict oxygen and water avoidance is required during storage and use.

[0057] Step 4: Connect the argon gas source to the gas inlet pipeline 12, open the exhaust valve, then open the first stop valve 11, and use argon to replace the air in the external operation box 1 and the sample temporary storage bin 19 by the upward air exhaust method. First, open the outside window 20 of the sample temporary storage bin 19 to put in the sample, close the outside window 20 of the sample temporary storage bin 19, and complete the argon replacement by connecting the gas inlet pipeline 12 and the gas outlet pipeline 8 through the sample temporary storage bin 19, then open the inside window 18 of the sample temporary storage bin 19 to move the sample to the sample preparation table, so that the atmosphere in the bin is consistent with the argon atmosphere in the external operation box 1.

[0058] Step 5: Sample weighing under special atmosphere. Open the analytical balance 3, place a 25 μL crucible on the analytical balance 3, record the mass of the empty crucible m0 at this time, remove the skin, and place the sample in the crucible. For solid samples or powder samples, use a metal powder funnel to weigh and use a sample pressing rod to compact the sample. For homogeneous liquid samples, use a pipette gun (10 μL tip) or a capillary quartz tube to transfer. Record the mass of the added sample m1. It should be noted that if the sample is heterogeneous during testing, it should be mixed as evenly as possible before being taken with a capillary quartz tube or a micro spatula. The sample taking process should avoid wall sticking or adhesion.

[0059] Step 6: Place the crucible in the crucible groove holder, rotate the top pentagonal star handle to make the cone head tightly contact with the dry top, adjust the torque value of the preset torque wrench to T refer , position by "0" point, continue to apply force and slightly overload twice when the digital distance meter shows exactly "0", then loosen the top pentagonal star handle, take out the crucible and weigh m2, record the sample mass m s = m2 - m0. Place the pressed crucible in the sample disc.

[0060] Step 7: open the inner side window 20, put the sample tray containing the crucible into the sample temporary storage bin 19, close the inner side window 20, open the sample temporary storage bin outer side window (18) from the outside, take out the sample tray, and use tweezers to place the pressed crucible to be tested in the designated position of the sample tray of the DSC automatic sample injector.

[0061] Step 8: input the recorded sample mass to be tested and the automatic sample injector position into the DSC device, and set the test program according to the requirements.

[0062] The embodiment is a method for sampling under an argon atmosphere using a 25 μL three-section punch type disposable high-pressure crucible. If a threaded crucible is used, replace the corresponding modular cone head and groove holder, remove the movable ear of the cone head connector, and the sealing process can be completed by inserting a preset torque screwdriver into the top preset torque screwdriver insertion hole 13.

[0063] In summary, the above embodiments are only preferred embodiments of the present application and do not limit the protection scope of the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims

1. A sample preparation device for a high pressure crucible for DSC under special atmosphere, characterized in that, The device comprises an external operation box (1), a sample preparation table (22), an analysis balance (3), an anti-vibration pad (2) and a modular high-pressure crucible sample pressing device (10); The external operation box (1) is a transparent sealed box body, the external operation box (1) is provided with an air inlet and an air outlet, the air inlet is connected with a plurality of adjustable air paths, and a stop valve is fixedly installed on the adjustable air path, the air outlet is connected with a vacuum pump and a waste gas treatment device through a three-way valve, and the external operation box (1) is connected with a grounding wire (4). The sample preparation table (22) is located in the internal of the external operation box (1), the material of the sample preparation table (22) is hard plate, and the surface of the sample preparation table (22) is coated with a corrosion-resistant coating. One side of the external operation box (1) is provided with a sample temporary storage bin (19), and the other side of the external operation box (1) is provided with a sampling tool box (9), the sampling tool box (9) stores a metal powder funnel, a pressing rod, a tweezers, a micro spatula, a pipette gun and a capillary quartz tube. The analysis balance (3) is located on one side of the internal of the external operation box (1), the anti-vibration pad (2) is arranged at the bottom of the analysis balance (3), and the analysis balance (3) and the sampling tool box (9) are provided with a wind deflector (6). The modular high-pressure crucible sample pressing device (10) is located on the other side of the internal of the external operation box (1), and the modular high-pressure crucible sample pressing device (10) comprises a sample preparation support, a variable shaft transmission device, an adjustable high-hardness crucible groove support and a taper head, a pre-set torque screwdriver insertion hole (13) and a pre-set torque wrench (14). The variable shaft transmission device is fixedly installed in the modular high-pressure crucible sample pressing device (10), and the variable shaft transmission device is a threaded helical gear transmission, the pre-set torque screwdriver insertion hole (13) is arranged at the top of the modular high-pressure crucible sample pressing device (10), the pre-set torque wrench (14) is fixed on one side of the modular high-pressure crucible sample pressing device (10), the taper head is connected with a taper head connecting piece, the taper head connecting piece is a driven shaft, and the taper head connecting piece is radially displaced with the rotation of the pre-set torque wrench (14).

2. The sample preparation apparatus for special atmosphere DSC high pressure crucible according to claim 1, characterized by, A plurality of clamping grooves are arranged on the main operation surface of the external operation box (1), and a long-sleeved glove is fixedly arranged on each clamping groove.

3. The sample preparation apparatus for special atmosphere DSC high pressure crucible according to claim 1, characterized by, The two sides of the sample temporary storage bin (19) are respectively provided with an inner side window (18) and an outer side window (20), and the inner side window (18) and the outer side window (20) are both closable movable windows.

4. The sample preparation apparatus for special atmosphere DSC high pressure crucible according to claim 1, characterized by, The adjustable air path comprises an air inlet pipeline (12) and an air outlet pipeline (8), the air inlet pipeline (12) is provided with a first stop valve (11), and the air outlet pipeline (8) is provided with a second stop valve (7).

5. The sample preparation apparatus for special atmosphere DSC high pressure crucible according to claim 1, characterized by, The adjustable air path comprises an air inlet pipeline (12) and an air outlet pipeline (8), the air inlet pipeline (12) is provided with a first stop valve (11), and the air outlet pipeline (8) is provided with a second stop valve (7).

6. The sample preparation apparatus for special atmosphere DSC high pressure crucible according to claim 4, characterized by, The adjustable air path comprises an air inlet pipeline (12) and an air outlet pipeline (8), the air inlet pipeline (12) is provided with a first stop valve (11), and the air outlet pipeline (8) is provided with a second stop valve (7). The cross bar of the taper head of the modular high-pressure crucible sample pressing device (10) is connected with a depth scale of a digital distance measuring instrument, and the two ends of the inner measuring claw of the digital distance measuring instrument are connected with the taper head and the bottom plate of the adjustable high-hardness crucible groove support.

7. The sample preparation apparatus for special atmosphere DSC high pressure crucible according to claim 1, characterized by, The sample preparation fixture, the variable shaft transmission device, the adjustable high-hardness crucible groove holder and the cone head are all made of hard alloy material.

8. A method of sample preparation for a special atmosphere DSC high pressure crucible sample preparation device, characterized by, Based on the sample preparation device of the high-pressure crucible of DSC under a special atmosphere according to claim 6, the sample preparation method steps are as follows: S1, determining the crucible specification and adjusting zero: according to the sample preparation requirements, the specification of the required crucible is determined, and the adjustable high-hardness crucible groove holder corresponding to the specification is selected for installation, the plane of the cone head is adjusted to be parallel to the bottom of the adjustable high-hardness crucible groove holder, and the reading of the digital distance meter at this time is recorded and marked as "0"; S2, take a set of blank crucible in order to put into adjustable high hardness crucible slot, repeat step S1, adjust the preset torque wrench torque value and slightly overload, when the digital distance meter shows the number is exactly zero, record the torque value at this time, repeat five times, and randomly selected three crucible, repeat the previous steps, take the maximum torque as the torque reference value T refer , if the subsequent emergence of a larger value, with the new larger value as the torque reference value T refer ; S3, determining the test atmosphere and introducing the gas: according to the sample preparation requirements, the required atmosphere environment of the sample during the transfer and use is determined, the external gas source of the gas inlet pipeline is adjusted, the first stop valve is opened, and the air in the external operation box and the sample temporary storage bin is replaced with the determined gas, so that the external operation box and the sample temporary storage bin are filled with the required gas; S4, sample weighing under special atmosphere: open the analytical balance, place the crucible in the analytical balance, record the mass m0 of the blank crucible, peel, and place the sample in the crucible; solid sample or powder sample is weighed using a metal powder funnel, and the sample is compacted using a sample pressing rod, and homogeneous liquid sample is transferred using a pipette or a capillary quartz tube and the mass m1 of the added sample is recorded; S5, sample preparation: the crucible is placed in the adjustable high-hardness crucible slot holder, the rotating variable shaft transmission device is used to make the cone head tightly contact with the top of the crucible, the torque value of the preset torque wrench is adjusted to T refer , through the "0" point positioning method, when the digital display distance meter shows "0", continue to apply force and slightly overload twice, then rotate the variable shaft transmission device, take out the crucible and weigh m2, record the sample mass m s = m2- m0, finally, the pressed crucible is placed in the sample temporary storage bin, and the sample preparation is completed.

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