CN112946008A - Sample loading device and method for evaluating thermal stability of energetic compound - Google Patents
Sample loading device and method for evaluating thermal stability of energetic compound Download PDFInfo
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- CN112946008A CN112946008A CN201911258193.XA CN201911258193A CN112946008A CN 112946008 A CN112946008 A CN 112946008A CN 201911258193 A CN201911258193 A CN 201911258193A CN 112946008 A CN112946008 A CN 112946008A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
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Abstract
The invention discloses a sample loading device for evaluating the thermal stability of an energetic compound, which comprises an inert gas purging and displacing device, a glass sample bottle, a disposable bottle cap and a bottle cap sealing device. And one side of the inert gas purging and replacing device is provided with an air inlet vacuum valve, the other side of the inert gas purging and replacing device is provided with an air exhaust vacuum valve, the top of the inert gas purging and replacing device is provided with a rubber plug, and a vacuum meter is placed in the rubber plug. The glass sample bottle is placed in an inert gas purge and displacer and the disposable vial cap is sealed with a vial cap sealer after the energetic compound is loaded. The invention also discloses a sample loading method of the energetic compound. The sample loading device and the method for evaluating the thermal stability of the energetic compound are simple to use, can prevent the energetic compound from interacting with oxygen in the air to release heat and even explode in the process of evaluating the thermal stability, and improve the accuracy and the repeatability of measurement.
Description
Technical Field
The invention belongs to the technical field of energetic compound thermal stability evaluation, and particularly relates to a sample loading device and method for energetic compound thermal stability evaluation2、H2O and CO2And the interaction between the isogas and the energetic compound.
Background
The energy-containing compound is widely used in the fields of aviation and aerospace aircraft propulsion, weapons, explosives and the like, and because the energy density is high and the explosion is easy to occur, the determination of the storage stability of the energy-containing compound under the normal temperature condition is very important. In order to accelerate the evaluation of stability, it is generally necessary to weigh a certain mass of the energetic compound, store it hermetically in a glass sample vial, place it in a highly sensitive heat flow calorimeter, and measure the cumulative exotherm of the energetic compound over a certain period of time (days to months) under high temperature conditions (typically 60-90 ℃) (in order to accelerate the reaction of the energetic compound). If the cumulative exotherm is below the index, it can be determined that the energetic compound can be stably stored at ambient conditions for ten years (StaNAG 4582, North Jun Ltd). In the detection process of the method, the energy-containing compound is usually sealed in the glass sample bottle, and in order to ensure the safety in the test process, the energy-containing compound in the glass sample bottle is usually only put into a small part. Residual air in the sample bottle can react with the energetic compound under the high-temperature condition, so that heat change is caused, and the measurement result is changed. Moreover, due to the difference of the sample quality of each measurement, the batch accuracy of the test result is obviously different.
Therefore, the invention eliminates and avoids the problems of measurement accuracy and repeatability caused by air interference in the thermal stability evaluation process by establishing the sample loading device and the method for evaluating the thermal stability of the energetic compound.
Disclosure of Invention
The invention aims to provide an energy-containing compound sample loading device capable of eliminating the influence of air in the process of evaluating the thermal stability of an energy-containing compound.
Another object of the present invention is to provide a method for loading an energetic compound using the above-described detection apparatus.
In order to achieve the purpose, the specific technical scheme of the invention is as follows:
a sample loading device for evaluating thermal stability of an energetic compound, comprising: inert gas purge and displacer, glass sample bottle, disposable vial cap, vial cap sealer.
And one side of the inert gas purging and replacing device is provided with an air inlet vacuum valve, the other side of the inert gas purging and replacing device is provided with an air exhaust vacuum valve, the top of the inert gas purging and replacing device is provided with a rubber plug, and a vacuum meter is arranged in the rubber plug.
The glass sample bottle is placed in an inert gas purging and replacing device and is used for containing energetic compounds;
the disposable bottle cap realizes the sealing of the glass sample bottle by the bottle cap sealer after the energy-containing compound is filled.
The bottle cap sealer comprises a clamping piece 1 ', a top rod 2', springs 3 'and 4', a fixing rod 5 'and a pressure rod 6', and when the bottle cap sealer does not work, the mouth of the clamping piece is opened under the action of the two springs, and a sample bottle covered with a disposable bottle cap is sleeved in the bottle cap sealer. When the disposable bottle cap is in work, the push rod can be pushed through a lever formed by the fixed rod and the press rod, so that the clamping piece is closed, and the disposable bottle cap is sealed on the sample bottle.
And the air suction vacuum valve of the inert gas purging and replacing device is connected with the mechanical pump, and the air inlet vacuum valve is connected with the high-purity argon pipeline.
The invention provides a sample loading method for evaluating the thermal stability of an energy-containing compound by using the sample loading device, which comprises the following steps:
the introduced gas is high-purity Ar gas, and the gas flow is set to be 50-100 mL/min.
Further, the complete removal of air in the inert gas purging and the displacer is realized, which specifically comprises:
the glass sample vial was placed in an inert gas purge and displacer and a rubber stopper with a vacuum gauge was inserted into the top of the displacer to seal it. And closing the air inlet vacuum valve, opening the air exhaust vacuum valve and the mechanical pump to start evacuating the inert gas purging and displacer, closing the air exhaust vacuum valve after the vacuum gauge shows that the vacuum degree in the displacer meets the vacuum requirement, opening the air inlet vacuum valve, introducing high-purity Ar gas, and closing the air inlet vacuum valve after the pressure of the vacuum gauge reaches normal pressure. The evacuation and Ar gas replacement operations were repeated at least 3 times.
Further, the weighing and sealing of the energetic compound are realized, and the method specifically comprises the following steps:
and disconnecting the inert gas purging and displacer from the vacuum pump, keeping the gas inlet vacuum valve open and Ar gas introduced all the time, and taking down the rubber plug from the gas purging and displacer. And then placing an inert gas purging and displacing device on a balance, weighing the energetic compound with the required mass under the protection of Ar gas, and sealing the disposable bottle cap on the glass sample bottle by using a bottle cap sealing device after the weighing is finished.
The energy-containing compound is one or more of Ammonium Dinitramide and hydroxylamine nitrate.
The invention has the following advantages:
1. the calorimetric research on the storage stability of the energetic compound is realized by matching with a TAM III type heat flow calorimeter of TA company.
2. The operation steps are simple, and the introduction of air in the sample loading process of the energetic compound can be effectively avoided.
3. Suitable for sealing and loading all types (solid and liquid) of energetic compounds.
Drawings
FIG. 1 is a schematic diagram of a sample loading device for evaluating thermal stability of an energetic compound provided by the invention: 1-inert gas purge and displacer; 2-glass sample bottle; 3-rubber stopper; 4-vacuum meter; 5-a vacuum valve for air intake; 6-evacuating the vacuum valve; 7-disposable bottle cap; 8-bottle cap sealer.
Fig. 2 is a schematic view of the principle of the closure sealer.
Detailed Description
Example 1
The apparatus will be described in detail with reference to fig. 1.
A sample loading device for evaluating the thermal stability of an energetic compound comprises an inert gas purging and displacing device 1, a glass sample bottle 2, a disposable bottle cap 7 and a bottle cap sealing device 8.
An air inlet vacuum valve is arranged on one side of the inert gas purging and replacing device 1, an air exhaust vacuum valve is arranged on the other side of the inert gas purging and replacing device, a rubber plug 3 is arranged at the top of the inert gas purging and replacing device, and a vacuum meter 4 is arranged in the rubber plug.
The glass sample bottle 2 is arranged in an inert gas purging and replacing device 1 and is used for containing energetic compounds;
the disposable cap 7 is sealed by the cap sealer 8 after the energetic compound is filled in the glass sample bottle.
When the device works, the inert gas purging and air suction vacuum valve of the displacer 1 is connected with the mechanical pump, and the air inlet vacuum valve is connected with the high-purity argon pipeline. And the gas flow of the high-purity Ar gas is set to be 80-100 mL/min.
The glass sample bottle 2 was placed in an inert gas purge and displacer 1, and a rubber stopper 3 with a vacuum gauge 2 was inserted into the top end of the displacer to close it. And closing the air inlet vacuum valve, opening the air exhaust vacuum valve and the mechanical pump to start evacuating the inert gas purging and displacer, closing the air exhaust vacuum valve after the vacuum gauge shows that the vacuum degree in the displacer meets the vacuum requirement, opening the air inlet vacuum valve, introducing high-purity Ar gas, and closing the air inlet vacuum valve after the pressure of the vacuum gauge reaches normal pressure. The evacuation and Ar gas replacement operations were repeated at least 3 times.
Subsequently, the inert gas purge and displacer 1 is disconnected from the vacuum pump, the gas inlet vacuum valve 5 is kept open and Ar gas is constantly introduced, and the rubber stopper 3 is removed from the gas purge and displacer 1. And then placing the inert gas purging and displacing device 1 on a balance, weighing the energetic compound with the required mass under the protection of Ar gas, and sealing the disposable bottle cap 7 on the glass sample bottle 2 by using a bottle cap sealing device 8 after weighing.
The bottle cap sealer 8 comprises a clamping piece 1 ', a mandril 2 ', a first spring, a second spring, a fixing rod 3 ', a second spring, a fixing rod 5 ' and a pressing rod 6 ', wherein the clamping piece 1 ' is formed by cutting a cylinder with an opening at the upper end and the lower end in the axial direction and is formed by four quarter cylinders with the same shape and size, arc-shaped bulges are arranged on the inner wall surfaces of the upper ends of the four 1/4 cylinders in the circumferential direction, the upper end and the lower end of the four 1/4 cylinders are sequentially hinged at intervals in sequence through hinges in the circumferential direction (namely the upper end and the lower end of the adjacent 2 1/4 cylinders are hinged at intervals in sequence), and the second spring 4 ' is wound on the outer side wall of the lower part of the four. Namely, a second spring 4' is wound around the narrow opening (the upper bottom surface below) of the inverted cone-shaped platform, so that the clamping piece is always inverted cone-shaped under the condition of no external force, and the wide opening (the lower bottom surface above) of the inverted cone-shaped platform is always opened. An ejector rod is placed in the inverted cone-shaped narrow opening of the clamping piece in a penetrating and sleeving mode, the upper end portion of the ejector rod is the same as the inner diameter of the inverted cone-shaped narrow opening, the ejector rod gradually becomes thick downwards, a first spring 3 ' is sleeved outside the ejector rod, the ejector rod is coaxial with the spring, under the condition that no external force exists, under the action of the spring 3 ', the ejector rod 2 ' cannot enter the inverted cone-shaped narrow opening, and opening and closing of the wide opening of the clamping piece are not affected. The lower end of the ejector rod 2 'is fixed on the pressing rod 6', the right end of the fixed rod 5 'is provided with a guide cylinder with an upper end and a lower end opened, the lower end of the clamping piece 1', the second spring 4 'is arranged on the upper part in the guide cylinder, the upper end of the ejector rod 2' is sleeved on the lower part in the guide cylinder, the right ends of the pressing rod 6 'and the fixed rod 5' are rotatably connected, when the bottle cap needs to be sealed, the pressing rod 6 'is pressed, a lever is formed by the fixed rod 5' and the pressing rod 6 ', the ejector rod 2' is pushed to move upwards to extrude into the inverted cone-shaped narrow opening, the inverted cone is gradually changed into a cylinder shape along with the entering of the ejector rod, the four-flap clamping
Example 2
2.706, 0.688 and 1.656 g of ammonium dinitramide propellant solutions with different masses are respectively weighed by the sample loading device and the method provided by the invention, TAM III thermal activity micro calorimeter is used for evaluating the thermal stability of the propellant, the evaluation result is shown in Table 1, the accumulated heat flow values (Max. heat flow with time of evaluation) are 94.23, 96.19 and 95.50 muW/g respectively, and the difference of heat flow measurement values caused by different air contents in different sample measurement bottles is eliminated.
Table 1 results of thermal stability evaluation of different mass Ammonium Dinitramide (ADN) propellant solutions.
Claims (7)
1. A sample loading device for evaluating thermal stability of an energetic compound, comprising: inert gas purging and displacing device, glass sample bottle and disposable bottle cap;
one side of the inert gas purging and displacer (1) is provided with an air inlet vacuum valve (5), the other side of the inert gas purging and displacer is provided with an air outlet with an air exhaust vacuum valve (6), the top of the inert gas purging and displacer is provided with a sample loading port with a sealing rubber plug (3), and the rubber plug is provided with a vacuum meter (4) for measuring the pressure in the inert gas purging and displacer (1); the glass sample bottle (2) is arranged in an inert gas purging and replacing device and is used for containing energetic compounds;
after the energetic compound is filled into the glass sample bottle (2), the glass sample bottle (2) is sealed by the disposable bottle cap.
2. The sample loading device for evaluating the thermal stability of an energetic compound according to claim 1, wherein: and the air suction vacuum valve of the inert gas purging and replacing device is connected with an air suction port of the mechanical pump, and the air inlet vacuum valve is connected with a high-purity argon source pipeline.
3. The sample loading device for evaluating the thermal stability of an energetic compound according to claim 1, wherein:
the inert gas purging and displacing device and the glass sample bottle are containers made of transparent materials (quartz glass).
4. A sample loading device for thermal stability evaluation of energetic compounds according to claim 1 or 3, characterized in that:
the glass sample bottle (2) is a sample bottle with an upper opening and an outer wall surface provided with a circular ring-shaped outer edge along the radial direction;
the disposable bottle cap is a cylindrical metal bottle cap with an opening at the lower end and a sealed upper end;
the disposable bottle cap is arranged at the opening of the sample bottle and is pressed by the bottle cap sealer to seal the bottle opening;
the bottle cap sealer (8) consists of a clamping piece (1 '), a push rod (2'), a first spring (3 '), a second spring (4'), a fixing rod (5 ') and a pressure lever (6'), wherein the clamping piece (1 ') consists of a cylinder body which is formed by axially cutting a cylinder with openings at the upper end and the lower end and has 4, 5 or 6 petals 1/4, 1/5 or 1/6 with the same shape and size, an arc-shaped bulge is arranged on the inner wall surface of the upper end of the cylinder 1/4, 1/5 or 1/6 along the circumferential direction, the upper end and the lower end of the cylinder 1/4, 1/5 or 1/6 are sequentially hinged at intervals along the circumferential direction through hinges, and the outer side wall of the lower part of the cylinder is wound with the second spring (4') along the circumferential direction to enable the cylinder to be placed in an inverted; a mandril is sleeved in the inverted cone-shaped narrow opening of the clamping piece, the upper end part of the mandril has the same diameter as the inner diameter of the inverted cone-shaped narrow opening, and gradually becomes thicker downwards and is in a frustum shape; a first spring (3') is sleeved outside the ejector rod, and the ejector rod is coaxial with the spring; the lower end of the ejector rod (2 ') is fixed on the pressure rod (6'), the right end of the fixed rod (5 ') is provided with a guide cylinder with an opening at the upper end and the lower end, the lower end of the clamping piece (1') and the second spring (4 ') are arranged at the upper part in the guide cylinder, the upper end of the ejector rod (2') is sleeved at the lower part in the guide cylinder, and the pressure rod (6 ') is rotatably connected with the right end of the fixed rod (5').
5. The loading device of claim 1, wherein the loading device is used for evaluating the thermal stability of the energetic compound, and the loading device is characterized in that: the introduced gas is high-purity Ar or N2The gas flow is set to be 80-100 mL/min.
6. A sample loading method for evaluating the thermal stability of an energetic compound by using the sample loading device as claimed in any one of claims 1 to 5,
1) the method for realizing inert gas purging and complete removal of air in the displacer specifically comprises the following steps:
placing the glass sample bottle in an inert gas purging and replacing device, and inserting a rubber plug with a vacuum meter into the top end of the replacing device to seal the glass sample bottle; closing the air inlet vacuum valve, opening the air exhaust vacuum valve and the mechanical pump to start evacuating the inert gas purging and displacer, closing the air exhaust vacuum valve after the vacuum gauge shows that the vacuum degree in the displacer meets the vacuum requirement, opening the air inlet vacuum valve, introducing high-purity Ar gas, and closing the air inlet vacuum valve after the pressure of the vacuum gauge reaches normal pressure; repeating the operations of evacuating and replacing Ar gas for at least 3 times;
2) weighing and sealing the energetic compound in the absence of air, and specifically comprises the following steps:
disconnecting the inert gas purging and displacer from the vacuum pump, keeping the gas inlet vacuum valve open and Ar gas always introduced, and taking down the rubber plug from the gas purging and displacer; and then placing an inert gas purging and displacing device on a balance, weighing the energetic compound with the required mass under the protection of Ar gas, and sealing the disposable bottle cap on the glass sample bottle by using a bottle cap sealing device after the weighing is finished.
7. The loading device of claim 6, wherein the loading device is used for evaluating the thermal stability of the energetic compound, and the loading device is characterized in that: the introduced gas is high-purity Ar or N2The gas flow is set to be 80-100 mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911258193.XA CN112946008B (en) | 2019-12-10 | 2019-12-10 | Sample loading device and method for evaluating thermal stability of energetic compound |
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| CN201911258193.XA CN112946008B (en) | 2019-12-10 | 2019-12-10 | Sample loading device and method for evaluating thermal stability of energetic compound |
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| CN112946008A true CN112946008A (en) | 2021-06-11 |
| CN112946008B CN112946008B (en) | 2022-11-29 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH44504A (en) * | 1908-05-15 | 1909-08-16 | Ludwig Mueller | Apparatus for filling bottles |
| CN2065188U (en) * | 1990-03-12 | 1990-11-07 | 杨书魁 | Hand-pressed can seamer |
| CN2127382Y (en) * | 1992-07-08 | 1993-02-24 | 中南制药机械二厂 | Sealing pliers |
| CN202164086U (en) * | 2011-07-25 | 2012-03-14 | 临安香聚日用品有限公司 | Manual cap pressing pincers |
| CN107037070A (en) * | 2016-02-04 | 2017-08-11 | 固安鼎材科技有限公司 | A kind of method and test device and system for being used to detect small molecule material heat endurance |
| CN107621169A (en) * | 2017-09-30 | 2018-01-23 | 中南大学 | A kind of small size vacuum induction melting furnace and its method of smelting |
| CN109455651A (en) * | 2018-12-29 | 2019-03-12 | 苏州凌耀制药设备有限公司 | A kind of bottle cap locking mechanism |
| CN208932934U (en) * | 2018-09-18 | 2019-06-04 | 浙江东方绍兴酒有限公司 | A kind of yellow rice wine envelope bottle |
-
2019
- 2019-12-10 CN CN201911258193.XA patent/CN112946008B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH44504A (en) * | 1908-05-15 | 1909-08-16 | Ludwig Mueller | Apparatus for filling bottles |
| CN2065188U (en) * | 1990-03-12 | 1990-11-07 | 杨书魁 | Hand-pressed can seamer |
| CN2127382Y (en) * | 1992-07-08 | 1993-02-24 | 中南制药机械二厂 | Sealing pliers |
| CN202164086U (en) * | 2011-07-25 | 2012-03-14 | 临安香聚日用品有限公司 | Manual cap pressing pincers |
| CN107037070A (en) * | 2016-02-04 | 2017-08-11 | 固安鼎材科技有限公司 | A kind of method and test device and system for being used to detect small molecule material heat endurance |
| CN107621169A (en) * | 2017-09-30 | 2018-01-23 | 中南大学 | A kind of small size vacuum induction melting furnace and its method of smelting |
| CN208932934U (en) * | 2018-09-18 | 2019-06-04 | 浙江东方绍兴酒有限公司 | A kind of yellow rice wine envelope bottle |
| CN109455651A (en) * | 2018-12-29 | 2019-03-12 | 苏州凌耀制药设备有限公司 | A kind of bottle cap locking mechanism |
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| CN112946008B (en) | 2022-11-29 |
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