Propellant storage safety detection method

Abstract

The invention discloses a propellant storage safety detection method, which comprises the following steps of: establishing a propellant near-infrared spectrum quantitative analysis model by combining a portable near-infrared spectrum tester with propellant component near-infrared spectrum data test software and chemometrics software, and detecting a propellant retest period by using the analysis model. The problems of long time consumption, high danger, serious pollution and the like of propellant component content detection in ammunition quality monitoring can be solved. A near infrared spectrum detection analysis technology is used for replacing a traditional chemical analysis method or a gas chromatography method, dangerous chemical reagents do not need to be used, and toxic and harmful emissions are not generated.

Description

Technical Field

[0001] The invention relates to the technical field of safety detection of explosives and propellants, and in particular to a method for detecting the safety of propellant storage. Background Art

[0002] Propellant is an important component of ammunition and provides energy for the launch of ammunition. In order to ensure the absolute reliability of the quality of ammunition, timely propellant quality testing has become an important part of the work of explosive production units and ammunition technical support departments in various countries around the world. At present, most of the detection of propellant storage safety at home and abroad still adopts classic chemical analysis methods such as bromination method or instrumental analysis methods such as gas chromatography and Vienna. The common feature of these methods is that the sample needs to be destroyed or dissolved in a specific solvent before testing. The sample pretreatment process is long and time-consuming. The preparation time for a single batch is at least 4-8 hours, and only one characterization parameter of the sample can be measured each time, which makes the propellant detection workload large and inefficient, and it is not convenient to carry out on-site mobile detection of propellants under field conditions. It cannot meet the needs of modern warfare for rapid detection of ammunition, which restricts the further improvement of the combat effectiveness of the troops. After consulting literature and patent retrieval, no relevant technical solutions were found. Summary of the invention

[0003] The purpose of the present invention is to provide a method for detecting the storage safety of propellant to solve the problems in the above-mentioned background technology.

[0004] To achieve the above object, the technical solution adopted by the present invention is:

[0005] A method for detecting the storage safety of propellant, wherein the method uses a portable near-infrared spectrometer combined with a propellant component near-infrared spectrum data testing software and chemometrics software to establish a near-infrared spectrum quantitative analysis model for propellant, and then uses the analysis model to detect the propellant retest period, and specifically comprises the following steps:

[0006] (1) Establishing the near-infrared spectroscopy quantitative analysis model of the propellant

[0007] Prepare samples and set values, select different batches of single-base propellant, and analyze the single-base propellant stabilizer content by gas chromatography after crushing, sieving, weighing, and soaking;

[0008] Aging samples: heating and aging the treated samples to obtain the single-base drug stabilizer content with different concentration gradients;

[0009] Collect near-infrared spectra, take the aged samples into the sample pool, collect spectra in diffuse reflectance mode through a near-infrared spectrum detection instrument, collect spectra for each sample in parallel, and obtain a near-infrared spectrum set for modeling;

[0010] Establish and evaluate the model, use general chemometrics software to establish a calibration model for the collected near-infrared spectra and the corresponding single-base drug tranquilizer content, and use the calibration sample prediction standard deviation and calibration sample correlation coefficient to evaluate the effectiveness of the analytical model establishment;

[0011] To verify the model, the near-infrared spectra of the samples used for modeling were recollected and the near-infrared predicted values ​​of the single-base propellant stabilizer content were obtained, which were compared with the values ​​measured by the chromatographic method and the relative deviation was calculated. In addition, different batches of single-base propellants that were not involved in the modeling were selected, and the spectra were collected by the near-infrared instrument to obtain the predicted values ​​of the stabilizer content, which were compared with the values ​​measured by the chromatographic method and the relative deviation was calculated to verify the feasibility of the calibration model.

[0012] (2) Analysis and determination of propellant storage safety performance

[0013] The propellant sample to be tested is placed in a sample pool, and the spectrum is collected by a near-infrared spectrum detection instrument in a diffuse reflectance manner. The stabilizer content of the sample to be tested is analyzed using the propellant near-infrared spectrum quantitative analysis model, and the detected stabilizer and stability content are input into the propellant retest period analysis system to obtain the retest period of the propellant and judge the storage safety performance of the propellant.

[0014] Furthermore, in the sample aging step, the sample is heated and aged at 90°.

[0015] Furthermore, during the aging process of the samples, the samples were placed in a constant temperature heating apparatus for heating aging, and the aging time was controlled to be 24 hours, 48 ​​hours and 72 hours respectively.

[0016] Furthermore, in the process of collecting near-infrared spectra, when the aged sample is placed in the sample pool, the sample height is 2 / 3 of the sample pool height.

[0017] Furthermore, when the sample is placed in the sample pool, the height of the sample is 2 / 3 of the height of the sample pool.

[0018] Furthermore, the sample pool has a diameter of 36 mm.

[0019] Furthermore, in the process of collecting the near-infrared spectrum, the spectral resolution of the near-infrared spectrum detector is 8nm, and the scanning range is 1300nm-2600nm.

[0020] Furthermore, before using general chemometrics software to establish a correction model for the collected near-infrared spectra and the corresponding single-base drug tranquilizer content, the collected near-infrared spectra are judged and abnormal spectra are eliminated, and then preprocessing is performed through spectral characteristic optimization selection.

[0021] Furthermore, the preprocessing method includes SG convolution smoothing, SG convolution derivative and multivariate scattering correction.

[0022] Furthermore, the partial least squares method is used as a correction method in the steps of establishing and evaluating the model.

[0023] Furthermore, the indicator method of the correction sample prediction standard deviation and the correction sample correlation coefficient in the steps of establishing and evaluating the model is implemented in accordance with the ASTM-1655 standard.

[0024] Beneficial effects:

[0025] The propellant storage safety detection method of the present invention can solve the problems of long time consumption, high risk and large pollution in the detection of propellant component content in ammunition quality monitoring. The near infrared spectrum detection and analysis technology replaces the traditional chemical analysis method or gas chromatography method, and no chemical dangerous goods reagents are needed, and no toxic and harmful emissions are generated. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 It is a flow chart of the present invention.

[0027] Figure 2 It is a flow chart of establishing a near-infrared spectrum quantitative analysis model for propellant in the present invention. DETAILED DESCRIPTION

[0028] The present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0029] Example

[0030] A method for detecting the storage safety of propellant, wherein the method uses a portable near-infrared spectrometer combined with propellant component near-infrared spectrum data testing software and chemometrics software to establish a near-infrared spectrum quantitative analysis model for propellant, and then uses the analysis model to detect the propellant retest period. The portable near-infrared spectrometer includes a MEMS-FTNIR spectrometer, a diffuse reflection probe group, a light source and circuit control component, an optical fiber component, a communication and control system, a housing and a computer system, and control software.

[0031] Specifically, the MEMS-FTNIR spectrometer adopts a MEMS chip-level Michelson interferometer, which has the characteristics of wide spectral distribution, high energy, low optical noise, high wavelength repeatability, and excellent long-term stability and reliability.

[0032] The main function of the diffuse reflectance probe group is to perform diffuse reflectance spectrum detection on samples. During the detection, in order to ensure the representativeness and uniformity of the sample spectrum collection, the sample chamber must be rotated at a controllable periodic constant speed to achieve the purpose of uniformly collecting the sample spectrum.

[0033] Light source and circuit control components, this part mainly provides high stability lighting source and lighting power supply for the spectrometer. In this embodiment, a long-life metal reflector bowl halogen tungsten lamp light source imported from the United States is used, and a low drift high stability tungsten lamp power supply circuit is matched.

[0034] The optical fiber component plays the role of optical path series in this system, transmitting the spectral slight change information collected by the diffuse reflection probe to the input end of the spectrometer through a special 600u diameter low-hydroxyl quartz optical fiber, and then the spectrometer performs spectral scanning and analysis.

[0035] The communication and control system performs combined control of the spectrometer system of this project, including steering and speed control, multi-channel communication distribution control, power secondary distribution control, etc.

[0036] The housing and computer system provide hardware and software support for the portable near-infrared spectrometer, ensuring the orderly operation of the entire system.

[0037] The control software establishes a numerical sequence analysis model, converts the detected spectrum into the stabilizer and stability content of the propellant components, and calculates the retest period of the propellant.

[0038] like Figure 1 and Figure 2 As shown, the propellant storage safety detection method in this embodiment specifically includes the following steps:

[0039] (1) S1, establishing the near infrared spectrum quantitative analysis model of the propellant

[0040] S11, prepare samples and set values, select 60 different batches of single-base propellants, and analyze the single-base propellant stabilizer content by gas chromatography after crushing, screening, weighing and soaking.

[0041] S12, aging samples, placing the 60 samples treated in step S11 into a constant temperature heating apparatus, heating and aging at 90°, and controlling the aging time to be 24 hours, 48 ​​hours, and 72 hours, respectively, to obtain 18 single-base drug stabilizer contents with different concentration gradients.

[0042] S13, collect near-infrared spectra, preheat the near-infrared spectrometer for 30 minutes, take an appropriate amount of aged samples into a sample pool with a diameter of 36mm, and the sample height is about 2 / 3 of the sample pool height. Shake it gently and compact it with a weight to make the bottom surface uniform and flat. Use the near-infrared spectrometer to collect spectra in diffuse reflectance mode. The spectral resolution is 8nm and the scanning range is 1300nm-2600nm. Each sample is collected in parallel 3 times to obtain a near-infrared spectrum set for modeling.

[0043] S14, establish and evaluate the model, use general chemometrics software to establish a calibration model for the collected near-infrared spectrum and the corresponding single-base drug tranquilizer content, select partial least squares as the calibration method, and use the calibration sample prediction standard deviation and calibration sample correlation coefficient to evaluate the effect of the analytical model establishment. Among them, before using general chemometrics software to establish a calibration model for the collected near-infrared spectrum and the corresponding single-base drug tranquilizer content, the collected near-infrared spectrum is judged and the abnormal spectrum is eliminated, and then pre-processing is performed by optimizing the spectral characteristics. The pre-processing method includes SG convolution smoothing, SG convolution derivative and multivariate scattering correction. The wavelength range selection is optimized according to the functional group properties and the correlation coefficient. The selection of the number of main factors is dominated by the software recommended value and appropriately fine-tuned. The indicator method for the calibration sample prediction standard deviation and the calibration sample correlation coefficient is implemented in accordance with the ASTM-1655 standard.

[0044] S15, verify the model, re-collect near-infrared spectra of 5 samples used for modeling and obtain near-infrared predicted values ​​of the single-base propellant stabilizer content, compare with the values ​​measured by the chromatographic method, and calculate the relative deviation; in addition, select 5 different batches of single-base propellants that do not participate in the modeling, collect spectra with near-infrared instruments to obtain predicted values ​​of the stabilizer content, compare with the values ​​measured by the chromatographic method, calculate the relative deviation, and verify the feasibility of the correction model.

[0045] (2) S2, analysis and determination of propellant storage safety performance

[0046] The propellant sample to be tested is placed in a sample pool with the sample height being about 2 / 3 of the sample pool height. The sample is gently shaken and compacted with a weight to make the bottom surface uniform and flat. The spectrum is collected by a near-infrared spectrum detection instrument in a diffuse reflection manner. The stabilizer content of the sample to be tested is analyzed using the propellant near-infrared spectrum quantitative analysis model. The detected stabilizer and stability content are input into the propellant retest period analysis system to obtain the retest period of the propellant and judge the storage safety performance of the propellant.

[0047] The propellant storage safety detection method proposed by the present invention uses a near-infrared spectroscopy detection and analysis method to quantitatively analyze the propellant components, thereby realizing rapid, accurate, and environmentally friendly detection of the stabilizer content in the propellant, and inputting the detected stabilizer and stability content into the propellant retest period analysis system, so as to quickly obtain the retest period of the propellant, and then judge the storage safety performance of the propellant. Specifically, the present invention can complete the rapid acquisition and analysis modeling of sample data within 10 minutes, generate a retest period report within 1 minute, and reduce the detection time from 4-6 hours to 2-10 minutes; the total volume of the box is 0.025 cubic meters, and the weight is about 3 kilograms. It is light in weight and high in strength, and is easy for a single soldier to carry.

[0048] Although the embodiments of the present invention are described in the specification, these embodiments are only for reference and should not limit the protection scope of the present invention. Various omissions, substitutions and changes within the scope of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for detecting the safety of propellant storage, characterized in that: The detection method uses a portable near-infrared spectrometer combined with a near-infrared spectrum data test software for propellant components and chemometrics software to establish a near-infrared spectrum quantitative analysis model for propellant, and then uses the analysis model to detect the propellant retest period, specifically comprising the following steps: (1) Establishing the near-infrared spectroscopy quantitative analysis model of the propellant Prepare samples and set values, select different batches of single-base propellant, and analyze the single-base propellant stabilizer content by gas chromatography after crushing, sieving, weighing, and soaking; Aging samples: heating and aging the treated samples to obtain the single-base drug stabilizer content with different concentration gradients; Collect near-infrared spectra, take the aged samples into the sample pool, collect spectra in diffuse reflectance mode through a near-infrared spectrum detection instrument, collect spectra for each sample in parallel, and obtain a near-infrared spectrum set for modeling; Establish and evaluate the model, use general chemometrics software to establish a calibration model for the collected near-infrared spectra and the corresponding single-base drug tranquilizer content, and use the calibration sample prediction standard deviation and calibration sample correlation coefficient to evaluate the effectiveness of the analytical model establishment; To verify the model, the near-infrared spectra of the samples used for modeling were recollected and the near-infrared predicted values ​​of the single-base propellant stabilizer content were obtained, which were compared with the values ​​measured by the chromatographic method and the relative deviation was calculated. In addition, different batches of single-base propellants that were not involved in the modeling were selected, and the spectra were collected by the near-infrared instrument to obtain the predicted values ​​of the stabilizer content, which were compared with the values ​​measured by the chromatographic method and the relative deviation was calculated to verify the feasibility of the calibration model. (2) Analysis and determination of propellant storage safety performance The propellant sample to be tested is placed in a sample pool, and the spectrum is collected by a near-infrared spectrum detection instrument in a diffuse reflectance manner. The stabilizer content of the sample to be tested is analyzed using the propellant near-infrared spectrum quantitative analysis model, and the detected stabilizer and stability content are input into the propellant retest period analysis system to obtain the retest period of the propellant and judge the storage safety performance of the propellant.

2. The method for detecting the storage safety of propellant according to claim 1, characterized in that: In the sample aging step, the sample is heated and aged at 90°.

3. The method for detecting the storage safety of propellant according to claim 1, characterized in that: During the aging process of the samples, the samples were placed in a constant temperature heating apparatus for heating aging, and the aging time was controlled to be 24 hours, 48 ​​hours and 72 hours respectively.

4. The method for detecting the storage safety of propellant according to claim 1, characterized in that: When placing the sample in the sample cell, the sample height is 2 / 3 of the sample cell height.

5. The method for detecting the storage safety of propellant according to claim 1, characterized in that: The sample pool has a diameter of 36 mm.

6. The method for detecting the storage safety of propellant according to claim 1, characterized in that: In the process of collecting near-infrared spectra, the spectral resolution of the near-infrared spectrometer is 8nm, and the scanning range is 1300nm-2600nm.

7. The method for detecting the storage safety of propellant according to claim 1, characterized in that: Before using general chemometrics software to establish a correction model for the collected near-infrared spectra and the corresponding single-base drug tranquilizer content, the collected near-infrared spectra are judged and abnormal spectra are eliminated, and then preprocessing is performed through spectral characteristic optimization selection.

8. The method for detecting the storage safety of propellant according to claim 7, characterized in that: The preprocessing method includes SG convolution smoothing, SG convolution derivative and multivariate scattering correction.

9. The method for detecting the storage safety of propellant according to claim 1, characterized in that: The partial least squares method is used as a correction method in the steps of establishing and evaluating the model.

10. The method for detecting the storage safety of propellant according to claim 1, characterized in that: The indicator method of the correction sample prediction standard deviation and the correction sample correlation coefficient in the steps of establishing and evaluating the model is implemented in accordance with the ASTM-1655 standard.

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