Detection method for gas generated by aging of solid propellant and application

Abstract

The invention provides a method for detecting gas generated by aging of a solid propellant, which comprises the following steps: aging the propellant at a specific temperature in a specific device, and detecting by adopting a gas chromatography-mass spectrometry technology, so that gas components with very low content can be detected; and the collected multi-component gas is effectively separated and qualitatively and quantitatively analyzed. According to the invention, a headspace sampling mode is adopted, so that the influence of air introduction caused by manual sampling can be eliminated, and the change rule of the component content can be analyzed more accurately. The detection method provided by the invention has the characteristics of high sensitivity and accuracy, the test environment can be accurately controlled, and the test process is convenient to implement.

Description

Technical Field

[0001] The present invention relates to the technical field of solid propellant aging and evaluation of aging generated gas, and in particular to a method for detecting solid propellant aging generated gas and its application. Background Art

[0002] The safe storage life of solid propellants is an important part of storage performance research and is of great significance in the entire process of propellant formulation research. In terms of propellant initial sample formulation and propellant storage performance screening formulation, the safe storage life of solid propellants is an important performance basis. The storage life of solid propellants can be estimated by accelerating their aging process and studying the performance of aged products.

[0003] The methods used in the study of propellant aging performance mainly use FTIR, nuclear magnetic resonance and X-ray detection methods. For example, the changes in infrared, nuclear magnetic resonance and other characteristic peaks of aged solid propellants can be used to study the correlation with macroscopic mechanical properties, providing a basis for estimating the storage life of solid propellants. In addition, solid propellants undergo a variety of complex chemical reactions during the aging process, which will generate gases. Detecting the changes in the composition and content of these gases can obtain information on the state of propellant aging, and is of guiding significance for studying the aging mechanism of solid propellants and improving the storage performance and service life of propellants. However, there are relatively few studies on solid propellant aging gas detection methods, and due to the small amount of gas precipitated during the aging process, it is difficult to collect, and it is impossible to accurately perform qualitative or quantitative analysis on the generated gas.

[0004] Therefore, there is an urgent need in the art to develop an effective method for detecting solid propellant aging gas. Summary of the invention

[0005] The present invention aims to provide a method for detecting gas generated by solid propellant aging. The method adopts gas chromatography-mass spectrometry combined with detection technology, can detect gas components with very low content, and effectively separate and qualitatively and quantitatively analyze the collected multi-component gas.

[0006] In a first aspect of the present invention, a method for detecting gas generated by aging of solid propellant is provided, the method comprising:

[0007] (1) providing a solid propellant, placing the solid propellant in a sampling bottle, and placing the bottle in a constant temperature oven for accelerated aging, wherein the sampling bottle is placed in a sealed bag;

[0008] (2) during the aging process, at intervals of a certain aging time t, the sampling bottle is taken out, and the gas generated by the aged solid propellant in the sampling bottle is tested using a gas chromatography-mass spectrometry technique to obtain a gas chromatogram, wherein all the gas generated by the aged solid propellant enters the testing system; and

[0009] (3) obtaining the components of the gas generated by solid propellant aging according to the gas chromatogram obtained by gas chromatography and mass spectrometry scanning; and calculating the relative content of the gas generated by solid propellant aging according to the ratio of the integrated area of ​​each component to the total integrated area;

[0010] The sampling bottle is provided with a sealing gasket, the materials of the sampling bottle and the sealing gasket do not react with the aging generated gas, and the volume of the sampling bottle is 10mL-30mL.

[0011] In another preferred embodiment, the mass of the solid propellant is 5 to 50 g.

[0012] In another preferred embodiment, the step (1) further comprises: placing the sampling bottle in a sealed bag, and then placing the sampling bottle and the sealed bag together in a constant temperature oven for aging.

[0013] In another preferred embodiment, the sampling bottle is made of a material that does not react with the aging generated gas.

[0014] In another preferred embodiment, the sampling bottle is selected from a glass bottle.

[0015] In another preferred embodiment, the volume of the sampling bottle is 10mL-30mL.

[0016] In another preferred embodiment, the sampling bottle has a sealing gasket, wherein the sealing gasket is made of a material that does not react with the aging generated gas.

[0017] In another preferred embodiment, the sealing gasket is made of tetrafluoroethylene.

[0018] In another preferred embodiment, the sealing bag is made of a material that does not react with the aging generated gas.

[0019] In another preferred embodiment, the number of the sampling bottles in the sealed bag is n, where n≥1.

[0020] In another preferred embodiment, the accelerated aging temperature is 40-70°C.

[0021] In another preferred embodiment, the testing steps of the gas chromatography-mass spectrometry technology include:

[0022] (a) setting the condition parameters of gas chromatography and mass spectrometry, wherein the gas chromatography condition column is a non-polar gas chromatography column, and the injection method is headspace injection;

[0023] (b) placing the sampling bottle on the sample tray for equilibrium, and after equilibrium at a certain temperature T, the quantitative loop takes a gas mass M and enters the gas chromatography-mass spectrometry inlet with the condition parameters set in step (a) for testing, wherein the sampling bottle contains aged solid propellant or air, and the test number of the test is m, m≥2; and

[0024] (c) Analyze the gas components produced by solid propellant aging using gas chromatography-mass spectrometry.

[0025] In another preferred embodiment, the mass M in step (b) is 800-1200 μL, preferably 900-1100 μL, and most preferably 950-1050 μL.

[0026] In another preferred embodiment, the gas component in step (c) may be but is not limited to carbon dioxide, nitrous oxide, isobutylene, benzene and other gases, and the gas is generated during the aging process of the solid propellant sample.

[0027] In another preferred embodiment, the condition parameters of the gas chromatography and mass spectrometry include the column temperature program parameter setting: starting temperature 30-50°C, maintaining for 3-15 minutes, increasing to 200-250°C at a constant rate, maintaining for 1-10 minutes, wherein the constant rate is 10-20°C / min;

[0028] In another preferred embodiment, the temperature T is the same as the accelerated aging test temperature, and the equilibrium time is 10 to 30 minutes.

[0029] In another preferred embodiment, the mass spectrometry conditions for gas component analysis include:

[0030] (i) the ionization mode is electron ionization;

[0031] (ii) the scanning mode is full scan;

[0032] (iii) scanning mass range m / z 20 to 550 amu; and

[0033] (iv) The transmission line temperature is 200-250°C.

[0034] In a second aspect of the present invention, a method for detecting the aging degree of a solid propellant is provided, the method comprising the steps of:

[0035] (S1) using the method described in the first aspect to detect the gas generated by the aged solid propellant in the sampling bottle, and determine the type or composition of the gas;

[0036] (S2) collecting various gas components in a sampling bottle to obtain the gas contents m01, m02, ... of the corresponding types in the sampling bottle;

[0037] (S3) Using the method described in the first aspect, the gas content of the same sampling bottle containing solid propellant is detected to obtain the content m of the corresponding gas in the sampling bottle. t 1. m t 2. ...; and

[0038] (S4) Calculate each gas m t -m0 value, get the gas content generated by aging;

[0039] Preferably, the method further comprises: taking out the sampling bottle for testing at certain aging time intervals, and analyzing the change pattern of the relative content of each component with the extension of aging time, so as to reflect the aging degree of the solid propellant; more preferably, the gas components include: carbon dioxide, nitrous oxide, isobutylene, and benzene.

[0040] In the third aspect of the present invention, there is provided an application of the method described in the first aspect, wherein the sampling bottles are taken out at certain aging intervals for testing, and the variation of the relative content of each component with the extension of aging time is analyzed, which is used to detect the aging degree of solid propellant.

[0041] It should be understood that within the scope of the present invention, the above-mentioned technical features of the present invention and the technical features specifically described below (such as embodiments) can be combined with each other to form a new or preferred technical solution. Due to space limitations, they will not be described one by one here. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] Figure 1 A gas chromatogram of the gas in an empty sampling bottle is shown.

[0043] Figure 2 A gas chromatogram of gases generated by solid propellant aging is shown. DETAILED DESCRIPTION

[0044] After extensive and in-depth research and a large number of experiments, the inventor unexpectedly developed a method for detecting solid propellant aging and aging-generated gas for the first time. The method adopts gas chromatography-mass spectrometry technology for detection, which can detect gas components with very low content and effectively separate and qualitatively and quantitatively analyze the collected multi-component gas. The invention adopts the headspace sampling method, which can eliminate the influence of air introduced by manual sampling and can more accurately analyze the change law of component content. The detection method provided by the present invention has the characteristics of high sensitivity and precision, the test environment can be accurately controlled, and the test process is easy to implement. The present invention was completed on this basis.

[0045] Gas generation from solid propellant aging

[0046] (1) Sample preparation

[0047] Sample: Provide 5-50 gg of solid propellant and set n groups of identical parallel samples;

[0048] Sampling bottle: glass material, with polytetrafluoroethylene sealing pad, volume 20mL, can be used for headspace sampling, where the material of the sampling bottle is a material that does not react with the aging generated gas.

[0049] Preferably, the volume of the sampling bottle is 10mL-30mL.

[0050] Preferably, the sampling bottle is made of glass.

[0051] Preferably, n≥3.

[0052] In the present invention, the sampling bottle is provided with a sealing gasket, wherein the sealing gasket is made of a material that does not react with the aging generated gas.

[0053] Preferably, the sealing gasket of the sampling bottle is made of polytetrafluoroethylene.

[0054] (2) Aging

[0055] The parallel samples of the solid propellant samples are placed in a sampling bottle, and then the sampling bottle is placed in a sealed bag. After sealing, it is placed in a constant temperature oven for accelerated aging, wherein the sealed bag is made of a material that does not react with the aging generated gas.

[0056] Preferably, the sealing bag is made of tetrafluoroethylene.

[0057] In the present invention, the number of sampling bottles placed in the sealed bag is single or multiple.

[0058] In the present invention, the temperature of the accelerated aging in the thermostat is 40-70°C.

[0059] In the present invention, the aging process is carried out in a sealed manner, and the aging gas is generated and stored in a sampling bottle.

[0060] (3) Sampling

[0061] In the present invention, during the aging process, some sampling bottles are taken out for testing at intervals, and the remaining sampling bottles continue to undergo accelerated aging tests; wherein the method and conditions for each test are the same.

[0062] In the present invention, the gas generated during the aging process can be completely stored in the sampling bottle and can be completely obtained.

[0063] (4) Aging gas detection

[0064] In the present invention, the collected gas samples are tested by using gas chromatography-mass spectrometry technology.

[0065] In the present invention, the head space sampling method is adopted to ensure that no aging gas overflows during the sampling process.

[0066] Detection method of gas generated during solid propellant aging

[0067] The method for detecting gas generated during the aging process of solid propellant in the present invention comprises the following steps:

[0068] 1) Place the solid propellant sample in a sampling bottle and place it in a constant temperature oven for accelerated aging;

[0069] 2) After a certain aging time, take out the sampling bottle and test the collected gas samples using gas chromatography-mass spectrometry to analyze the composition and relative content of the gas generated by the aging of the solid propellant.

[0070] Furthermore, in step 1), the solid propellant sample is placed in a sampling bottle, wherein the mass of the solid propellant sample placed in the sampling bottle is 5 to 50 g, and the mass of the sample in each sampling bottle is the same; wherein the sampling bottle is made of a material that does not react with the aging gas, including glass, with a sealing gasket, wherein the sealing gasket is made of a material that does not react with the aging gas, including polytetrafluoroethylene; and the volume is 10 mL-30 mL.

[0071] Furthermore, in step 1), the sampling bottle containing the solid propellant sample is placed in a sealed bag, which is then sealed and placed in a constant temperature oven for accelerated aging. The sealed bag is made of a material that does not react with the aging generated gas, including tetrafluoroethylene; and the number of sampling bottles placed in the sealed bag is single or multiple.

[0072] Furthermore, in step 1), the sampling bottle containing the propellant sample is placed in a sealed bag, which is then sealed and placed in a constant temperature oven for accelerated aging. The temperature for accelerated aging is any temperature between 40 and 70°C, and the temperature is constant during accelerated aging; at a certain interval, some sampling bottles are taken out for testing, and the remaining sampling bottles continue to undergo accelerated aging tests; the method conditions for each test are the same.

[0073] Furthermore, in step 2), after aging, the sampling bottle is taken out and the collected gas sample is tested using gas chromatography-mass spectrometry. The test includes the following steps:

[0074] 1) setting the condition parameters of gas chromatography and mass spectrometry, wherein the gas chromatography condition column is a non-polar gas chromatography column; and the injection method is headspace injection;

[0075] II) placing the sampling bottle on the sample tray for equilibrium, and after equilibrium at a certain temperature, taking gas through a quantitative loop and entering the inlet of a gas chromatograph-mass spectrometer;

[0076] III) Analyze the gas components produced by solid propellant aging using gas chromatography-mass spectrometry.

[0077] In the present invention, the head space sampling method is adopted to inject all the gas generated by the aged solid propellant into the test system, thereby avoiding the escape of the aged gas and making the experimental results more reliable.

[0078] Specifically, the samples and reference substances are tested using gas chromatography-mass spectrometry, wherein the samples are the samples collected in the bottles described in step 1), and the number of parallel tests each time is greater than or equal to 2; and the reference substances are empty sampling bottles without solid propellants.

[0079] Specifically, the column temperature increase program in the gas chromatography condition parameters of step I) is:

[0080] The starting temperature is 30-50°C, maintained for 3-15 minutes, then raised to 200-250°C at a constant rate, maintained for 1-10 minutes, wherein the constant rate is 10-20°C / min.

[0081] Specifically, in step II), the temperature condition for equilibrating the sampling bottle on the sample plate is the same as the accelerated aging test temperature, and the equilibrating time is 10 to 30 minutes.

[0082] Specifically, the mass spectrometry conditions for qualitatively analyzing the gas components generated by aging of the solid propellant using gas chromatography-mass spectrometry in step III) are:

[0083] Ionization mode: electron ionization; Scanning mode: full scan; Scanning mass range m / z: 20~550amu; Transmission line temperature: 200~250℃.

[0084] Furthermore, in step 2), the collected gas samples are tested using gas chromatography-mass spectrometry technology to analyze the composition and relative content of the gas generated by solid propellant aging. The composition of the gas generated by solid propellant aging is determined based on the results of gas chromatography and mass spectrometry scanning; the relative content of the gas generated by solid propellant aging is calculated based on the ratio of the integral area of ​​each component to the total integral area.

[0085] Specifically, the carbon dioxide content in the sample is analyzed, and the portion of the carbon dioxide content in the sample that is increased compared to the carbon dioxide content in the control sample is identified as the carbon dioxide content generated when the sample is aged. The control sample is an empty sampling bottle without solid propellant.

[0086] Furthermore, in step 2), the sampling bottles are taken out for testing at certain aging time intervals, and the change of each component of the gas generated during the aging process of the solid propellant is analyzed according to the increase of aging time, and the change of the relative content of each component is analyzed.

[0087] Compared with the prior art, the present invention has the following beneficial effects:

[0088] 1. The present invention adopts the method of sealing and aging the sampling bottle and headspace sampling, which can perform continuous sampling to avoid aging gas loss and ensure the accuracy of the test results.

[0089] 2. The method for detecting gas generated by aging of solid propellant of the present invention adopts gas chromatography-mass spectrometry combined technology for detection, which can detect gas components with very low content, and effectively separate and qualitatively and quantitatively analyze the collected multi-component gas, and can accurately evaluate the components of gas generated by aging of solid propellant and its change law.

[0090] 3. The method for detecting gas generated by solid propellant aging of the present invention has the characteristics of high sensitivity, precision and simple operation, the test environment can be accurately controlled and the test process is easy to implement.

[0091] The present invention will be further described below in conjunction with specific examples. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. The experimental methods in the following examples without specifying specific conditions are usually based on conventional conditions or the conditions recommended by the manufacturer. Unless otherwise stated, percentages and parts are by weight.

[0092] Example 1 Detection of Gas Generated by Solid Propellant Aging

[0093] In this experiment, the propellant was aged at 70°C for 10 days. During the aging process, the generated gas was collected. At specific time intervals, the generated gas was detected, the gas data was obtained, and the type and relative content of the gas were determined.

[0094] Sample: A certain azide solid propellant, in the shape of a cuboid, each sample weighs 8.0g, and there are 3 samples in total.

[0095] Sampling bottle: glass material, with polytetrafluoroethylene sealing pad, volume 20mL, can be used for headspace sampling.

[0096] Sealed bag: Made of PTFE with sealed mouth.

[0097] 1. Solid propellant aging and gas collection.

[0098] Specific steps:

[0099] 1) Put three samples into three sampling bottles respectively;

[0100] 2) Put three sampling bottles into a sealed bag, seal it and put it into a constant temperature oven;

[0101] 3) The temperature of the constant temperature oven is set to 70°C, and the sealed bags are aged at this temperature for 10 days.

[0102] 2. Detection of gas generated by solid propellant aging.

[0103] Specific steps:

[0104] 1) Set the column temperature rise program in the gas chromatography condition parameters as follows:

[0105] The initial temperature was 30°C, maintained for 5 min, then increased at a rate of 20°C / min to 200-250°C, and maintained for 5 min.

[0106] 2) Set the mass spectrometry conditions: ionization mode: electron ionization; scanning mode: full scan; scanning mass range m / z: 20-550 amu; transmission line temperature: 230°C.

[0107] 3) Place the sampling bottle on the sample tray and equilibrate at 70°C for 30 minutes.

[0108] 4) Injection method: headspace injection, sampling volume: 1 mL.

[0109] 5) Use gas chromatography-mass spectrometry to conduct qualitative analysis on the empty sampling bottle. After analysis and identification of the gas components, the following are obtained: Figure 1 The gas chromatogram shown in FIG. 1 is analyzed according to the standard mass spectrum library, and the results are shown in Table 1.

[0110] Table 1 Gas components and peak areas in empty sampling bottles

[0111]

[0112]

[0113] 6) The sampling bottle containing the aged solid propellant sample was analyzed by gas chromatography-mass spectrometry. The gas components were analyzed and identified as follows: Figure 2 The gas chromatogram shown in FIG. 2 is analyzed according to the standard mass spectrum library and the results are shown in Table 2.

[0114] Table 2 Gas components and peak areas generated by solid propellant aging

[0115] Retention time Component name Chemical formula Peak area 1.730 carbon dioxide <![CDATA[CO2]]> 36834297 1.820 Nitrous oxide <![CDATA[N2O]]> 21452 8.213 Isobutylene <![CDATA[C4H8]]> 2568093 11.832 benzene <![CDATA[C6H6]]> 116833312

[0116] Depend on Figure 1 From Table 1, we can see that the gas component carbon dioxide was detected in the empty sample bottle. Figure 2As shown in Table 2, carbon dioxide can be detected in the samples of solid propellant aging gas, and its peak area is significantly higher than that of the empty sample bottle, indicating that carbon dioxide is generated during the aging process of solid propellant. In addition, it can be detected that solid propellant produces gaseous products such as nitrous oxide, isobutylene and benzene during the aging process.

[0117] Example 2 Detection of Gas Generated by Solid Propellant Aging

[0118] In this experiment, the propellant was aged at 70°C for 150 days. During the aging process, the generated gas was collected. At specific time intervals, the generated gas was detected, the gas data was obtained, and the type and relative content of the gas were determined.

[0119] Sample: A certain azide solid propellant, in the shape of a cuboid, each sample weighs 8.0g, and there are 14 samples in total.

[0120] Sampling bottle: glass material, with polytetrafluoroethylene sealing pad, volume 20mL, can be used for headspace sampling.

[0121] Sealed bag: Made of PTFE with sealed mouth.

[0122] 1. Solid propellant aging and gas collection.

[0123] Specific steps:

[0124] 1) Place 14 samples into 14 sampling bottles respectively;

[0125] 2) Put two sampling bottles into one sealed bag, a total of 7 sealed bags, seal them and put them into a constant temperature oven;

[0126] 3) The temperature of the constant temperature oven is set at 70°C, and the sealed bags are aged at this temperature for 150 days; among them, a sampling bag is taken out for testing on the 10th day, 20th day, 30th day, 60th day, 90th day, 120th day and 150th day respectively.

[0127] 2. Detection of gas generated by solid propellant aging.

[0128] Specific steps:

[0129] 1) Set the column temperature rise program in the gas chromatography condition parameters as follows:

[0130] The initial temperature was 30°C, maintained for 5 min, then increased at a rate of 20°C / min to 200-250°C, and maintained for 5 min.

[0131] 2) Set the mass spectrometry conditions: ionization mode: electron ionization; scanning mode: full scan; scanning mass range m / z: 20-550 amu; transmission line temperature: 230°C.

[0132] 3) Place the sampling bottle on the sample tray and equilibrate at 70°C for 30 minutes.

[0133] 4) Injection method: headspace injection, sampling volume: 1 mL.

[0134] 5) The empty sampling bottle and the sampling bottle with the aged solid propellant sample were analyzed by gas chromatography-mass spectrometry. The analysis was performed according to the standard mass spectrometry library. Two samples were taken at different aging times for testing. The obtained gas composition is shown in Table 3.

[0135] Table 3. Gas components generated by solid propellant aging

[0136] Time (day) carbon dioxide / % Nitrous oxide / % Isobutylene / % benzene / % 10 17 0.01 1.7 79 20 27 0.02 2.6 68 30 23 0.02 3.1 72 60 14 0.01 7.9 75 90 18 0.03 9.1 69 120 12 0.02 34.6 42 150 12 0.02 35.0 43

[0137] From the test results, we can see that the samples in the sampling bottles all detected gaseous products such as carbon dioxide, nitrous oxide, isobutylene and benzene, which indicates that these gases will be generated during the aging process of solid propellants.

[0138] According to the ratio of the gas integral area to the total integral area, the relative content of various gases is calculated, and the results are shown in Table 3. According to the data analysis in Table 3, the change law of each component of the gaseous aging product within 150 days of propellant aging is that the relative content of carbon dioxide is higher after aging for 20 days, and then gradually decreases. It shows that the propellant releases more carbon dioxide aging products at the beginning of the aging experiment, and then the release rate gradually stabilizes. The relative content of isobutylene gradually increases with the extension of aging time, indicating that it is continuously produced during the aging process. The relative content of nitrous oxide in the aging products changes steadily, and the relative content of benzene has a decreasing trend.

[0139] All documents mentioned in the present invention are cited as references in this application, just as each document is cited as reference individually. In addition, it should be understood that after reading the above teachings of the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the claims attached to this application.

Claims

1. A method for detecting gas generated by solid propellant aging, characterized in that: The method comprises: (1) providing a solid propellant, placing the solid propellant in a sampling bottle, and placing the bottle in a constant temperature oven for accelerated aging, wherein the sampling bottle is placed in a sealed bag; (2) during the aging process, at intervals of a certain aging time t, the sampling bottle is taken out, and the gas generated by the aged solid propellant in the sampling bottle is tested using a gas chromatography-mass spectrometry technique to obtain a gas chromatogram, wherein all the gas generated by the aged solid propellant enters the testing system; and (3) obtaining the components of the gas generated by solid propellant aging according to the gas chromatogram obtained by gas chromatography and mass spectrometry scanning; and calculating the relative content of the gas generated by solid propellant aging according to the ratio of the integrated area of ​​each component to the total integrated area; The sampling bottle is provided with a sealing gasket, the materials of the sampling bottle and the sealing gasket do not react with the aging generated gas, and the volume of the sampling bottle is 10mL-30mL.

2. The method according to claim 1, characterized in that The step (1) also includes: placing the sampling bottle in a sealed bag, and then placing the sampling bottle and the sealed bag together in a constant temperature oven for aging.

3. The method according to claim 1, characterized in that The accelerated aging temperature is 40-70°C.

4. The method according to claim 1, characterized in that The testing steps of the gas chromatography-mass spectrometry technique include: (a) setting the condition parameters of gas chromatography and mass spectrometry, wherein the gas chromatography condition column is a non-polar gas chromatography column, and the injection method is headspace injection; (b) placing the sampling bottle on the sample tray for equilibrium, and after equilibrium at a certain temperature T, the quantitative loop takes a gas mass M and enters the gas chromatography-mass spectrometry inlet with the condition parameters set in step (a) for testing, wherein the sampling bottle contains aged solid propellant or air, and the test number of the test is m, m≥2; and (c) Analyze the gas components produced by solid propellant aging using gas chromatography-mass spectrometry.

5. The method according to claim 4, characterized in that The gas component in step (c) is selected from the following group: carbon dioxide, nitrous oxide, isobutylene, benzene; preferably, the gas is the gas generated during the aging process of the solid propellant sample.

6. The method according to claim 4, characterized in that The condition parameters of the gas chromatography and mass spectrometry include the column temperature rising program parameter setting: starting temperature 30-50°C, maintaining for 3-15 minutes, rising to 200-250°C at a constant rate, maintaining for 1-10 minutes, wherein the constant rate is 10-20°C / min.

7. The method according to claim 4, characterized in that The temperature T is the same as the accelerated aging test temperature, and the equilibrium time is 10 to 30 minutes.

8. The method according to claim 4, characterized in that The mass spectrometry conditions for the gas composition analysis include: (i) the ionization mode is electron ionization; (ii) the scanning mode is full scan; (iii) scanning mass range m / z 20 to 550 amu; and (iv) The transmission line temperature is 200-250°C.

9. A method for detecting the aging degree of solid propellant, characterized in that: The method comprises the steps of: (S1) using the method of claim 1 to detect the gas generated by the aged solid propellant in the sampling bottle to determine the type or composition of the gas; (S2) collecting various gas components in a sampling bottle to obtain the gas contents m01, m02, ... of the corresponding types in the sampling bottle; (S3) Using the method described in claim 1, the gas content of the same sampling bottle containing solid propellant is detected to obtain the content m of the corresponding gas in the sampling bottle. t 1. m t 2. ...; and (S4) Calculate each gas m t -m0 value, get the gas content generated by aging; Preferably, the method further comprises: taking out the sampling bottle for testing at certain aging time intervals, and analyzing the change pattern of the relative content of each component with the extension of aging time, so as to reflect the aging degree of the solid propellant; more preferably, the gas components include: carbon dioxide, nitrous oxide, isobutylene, and benzene.

10. Use of the method according to claim 1, characterized in that: Used to detect the aging degree of solid propellants.

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