CN111929155A - Near infrared spectrum analysis method for uniaxial tension initial modulus of composite solid propellant - Google Patents
Near infrared spectrum analysis method for uniaxial tension initial modulus of composite solid propellant Download PDFInfo
- Publication number
- CN111929155A CN111929155A CN202010683262.8A CN202010683262A CN111929155A CN 111929155 A CN111929155 A CN 111929155A CN 202010683262 A CN202010683262 A CN 202010683262A CN 111929155 A CN111929155 A CN 111929155A
- Authority
- CN
- China
- Prior art keywords
- solid propellant
- near infrared
- composite solid
- infrared spectrum
- standard
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004449 solid propellant Substances 0.000 title claims abstract description 255
- 239000002131 composite material Substances 0.000 title claims abstract description 251
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 175
- 238000004458 analytical method Methods 0.000 title claims abstract description 14
- 238000012360 testing method Methods 0.000 claims abstract description 68
- 239000007787 solid Substances 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims description 57
- 238000001228 spectrum Methods 0.000 claims description 57
- 239000000126 substance Substances 0.000 claims description 37
- 239000004014 plasticizer Substances 0.000 claims description 22
- 239000007800 oxidant agent Substances 0.000 claims description 21
- 239000000853 adhesive Substances 0.000 claims description 20
- 230000001070 adhesive effect Effects 0.000 claims description 20
- 230000001590 oxidative effect Effects 0.000 claims description 20
- 238000010183 spectrum analysis Methods 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 10
- 238000012795 verification Methods 0.000 claims description 10
- 230000002452 interceptive effect Effects 0.000 claims description 9
- 239000003380 propellant Substances 0.000 claims description 7
- 238000012569 chemometric method Methods 0.000 claims description 6
- 230000003595 spectral effect Effects 0.000 claims description 6
- 238000010561 standard procedure Methods 0.000 claims description 6
- 238000004497 NIR spectroscopy Methods 0.000 claims description 4
- 238000007796 conventional method Methods 0.000 claims description 4
- 238000012935 Averaging Methods 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 3
- 238000012845 near infrared spectroscopy analysis Methods 0.000 claims 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract description 2
- 238000011416 infrared curing Methods 0.000 abstract 1
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 40
- 230000007547 defect Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 239000004322 Butylated hydroxytoluene Substances 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- 229940095259 butylated hydroxytoluene Drugs 0.000 description 1
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003333 near-infrared imaging Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
- G01N3/06—Special adaptations of indicating or recording means
- G01N3/068—Special adaptations of indicating or recording means with optical indicating or recording means
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
A near infrared spectrum analysis method of the uniaxial tension initial modulus of a composite solid propellant. Firstly, designing a certain amount of composite solid propellant formulas with known proportions according to a certain composite solid propellant formula and a uniform distribution principle; secondly, preparing a sample according to a design formula to obtain a certain amount of composite solid propellant standard products with known proportion, using part of the obtained composite solid propellant standard products for testing near infrared spectrum, curing and forming part of the obtained composite solid propellant standard products, and testing the initial modulus of the composite solid propellant standard products in uniaxial tension; and establishing a relation model between the near infrared spectrum of the composite solid propellant standard product and the uniaxial tension initial modulus of the composite solid propellant standard product, and obtaining the uniaxial tension initial modulus of the solid composite solid propellant sample. The invention can realize the purpose of high-efficiency and nondestructive analysis, and provides a convenient and rapid detection method for the production quality and safe manufacture of the composite solid propellant.
Description
Technical Field
The invention relates to the field of composite solid propellants, in particular to a near infrared spectrum analysis method for testing the uniaxial tensile initial modulus of a composite solid propellant in a non-contact manner.
Background
The initial modulus of uniaxial tension of the composite solid propellant is a physical quantity describing the resistance of the composite solid propellant to deformation. The initial modulus of uniaxial tension of the composite solid propellant is defined as the ratio of stress strain of the initial straight line part on a tensile curve. The initial modulus of the composite solid propellant in unidirectional stretching is a main index for characterizing the composite solid propellant, and the initial modulus of the composite solid propellant in unidirectional stretching directly influences the performance of a product. The initial modulus of the uniaxial tension at the present stage is mainly a uniaxial tension method. The method for testing the initial modulus of the composite solid propellant in the uniaxial tension process comprises the steps of solidifying the slurry of the composite solid propellant at 50 ℃ for 7 days, preparing the slurry into medicine strips under corresponding conditions according to corresponding testing methods, and testing the initial modulus of the composite solid propellant in the uniaxial tension process by using corresponding testers. The method has the defects that the curing process is long, and the uniaxial tensile initial modulus of the composite solid propellant cannot be judged by means of the composite solid propellant slurry.
Near infrared spectroscopy is an analysis method of secondary measurement, namely an indirect measurement technology, and a correction model is established by correlating the near infrared spectrum of a sample with quality parameters of the sample. The relevant quality parameters of the test sample are quickly given by means of the model. In recent years, the application of near infrared spectroscopy in the field of composite solid propellants mainly aims at component research of the butylated hydroxytoluene propellant, and a non-contact test for the uniaxial tensile initial modulus of the composite solid propellant is not reported.
Disclosure of Invention
To overcome the existing in the prior art
The invention provides a near infrared spectrum analysis method of the uniaxial tension initial modulus of a composite solid propellant, which overcomes the defect of long curing time in the testing process of the uniaxial tension initial modulus of the composite solid propellant.
The specific process of the invention is as follows:
the samples required by the relation model comprise 50 parts of near infrared spectrum test samples and 50 parts of solid composite solid propellant standard;
the near infrared spectrum test sample and the solid composite solid propellant standard are both prepared by changing the mass percentage of the components influencing the initial modulus of uniaxial tension in the formula of the composite solid propellant;
the components influencing the initial modulus of uniaxial tension comprise an adhesive, a plasticizer and an oxidant. The components of the adhesive, the plasticizer and the oxidant are changed, so that the content of the adhesive in the formula is changed to +/-10%, the content of the plasticizer in the formula is changed to +/-20%, and the content of the oxidant in the formula is changed to +/-3%. According to the changed content, 50 standard formulations of certain type of composite solid propellant are obtained through orthogonal experiments. 1/5 medicinal slurry is respectively taken from 50 parts of prepared standard substance for near infrared spectrum test, and 50 parts of near infrared spectrum test samples are obtained. The remaining 4/5 of each standard was used for curing and molding to obtain 50 parts of solid composite solid propellant standard for testing the initial modulus of uniaxial tension of the composite solid propellant standard.
the acquisition parameters comprise scanning times, spectral range and resolution.
And adjusting the spectrum acquisition parameters of the near-infrared spectrometer by the near-infrared spectrometer. Taking any one part of the near infrared spectrum test sample obtained in the step 1 as a test sample; and carrying out near infrared spectrum test on the infrared spectrum test sample by using a near infrared spectrometer.
Determining the near infrared spectrum acquisition parameters of a certain type of composite solid propellant as follows:
wave number range: 4000-120000cm-1；
The scanning times are as follows: 120 times;
resolution ratio: 4cm-1。
When determining the optimal number of scans: adjusting the scanning times of the near-infrared spectrometer to be 50 times, 100 times, 120 times, 160 times and 200 times respectively, and performing near-infrared spectrum acquisition on the samples used by the acquisition parameters according to the determined scanning times respectively; acquiring a near infrared spectrum after each acquisition of the near infrared spectrum; and sequentially arranging the five pieces of near infrared spectrum noise according to the obtained five pieces of near infrared spectrum noise values from large to small. And selecting a near infrared spectrum with the minimum scanning frequency from the near infrared spectra with similar noise values, and taking the scanning frequency of the near infrared spectrum as the optimal scanning frequency.
Determining the optimal resolution by: the resolution ratios of the near-infrared spectrometers are respectively adjusted to be 2cm-1、4cm-1、 8cm-1Sequentially carrying out near infrared spectrum collection on the samples used by the collection parameters, and obtaining a near infrared spectrum after each near infrared spectrum collection; and sequentially arranging the three near infrared spectrums from large to small according to the noise value of each near infrared spectrum. And selecting one near infrared spectrum with the minimum noise value from the three near infrared spectrums, and taking the scanning times of the near infrared spectrum as the optimal resolution.
And 3, collecting the near infrared spectrum of 50 parts of certain type composite solid propellant standard:
and (3) respectively acquiring the near infrared spectrum of 50 parts of standard substance of the certain type of composite solid propellant according to the near infrared spectrum acquisition parameters of the certain type of composite solid propellant determined in the step (2).
In the near infrared spectrum collection, the room temperature of the collection environment is 25 +/-2 ℃, and the relative humidity is less than or equal to 65%.
And taking the average spectrum of 50 parts of the standard substance of the certain type of composite solid propellant as the near infrared spectrum of the standard substance of the certain type of composite solid propellant in a relational model.
The specific process for collecting 50 parts of near infrared spectrum of certain type of composite solid propellant standard comprises the following steps:
collecting a near infrared spectrum of a first certain type of composite solid propellant standard; the first type of composite solid propellant standard collected three spectra. And averaging the three spectra of the sample by using a near infrared spectrometer to obtain the average spectrum of the composite solid propellant standard product of the certain type.
And repeating the process of collecting the near infrared spectrum of the first certain type of composite solid propellant standard until the near infrared spectrum collection of 50 parts of certain type of composite solid propellant standard is completed, so as to obtain 50 parts of average spectrum of certain type of composite solid propellant standard. And (4) completing the acquisition of the near infrared spectrum of 50 parts of certain type of composite solid propellant standard.
Step 4, testing the uniaxial tensile initial modulus of a certain type of composite solid propellant standard:
and (3) testing the uniaxial tension initial modulus of 50 parts of the solid composite solid propellant standard obtained in the step (1). During testing, the uniaxial tension initial modulus of 50 parts of the solid composite solid propellant standard is respectively tested by using a uniaxial tension initial modulus tester, and the uniaxial tension initial modulus of 50 parts of the solid composite solid propellant standard is respectively obtained. And taking the obtained 50 parts of solid composite solid propellant standard uniaxial tension initial modulus as uniaxial tension initial modulus data associated with the near infrared spectrum of a certain type of composite solid propellant standard in a relational model.
Step 5, collecting the near infrared spectrum of the components influencing the uniaxial tension initial modulus
And (3) acquiring the near infrared spectrum of the component influencing the initial modulus of uniaxial tension according to the optimal acquisition parameters of the near infrared spectrum of the composite solid propellant determined in the step (2), and respectively obtaining near infrared spectrograms of the adhesive, the plasticizer and the oxidant influencing the initial modulus of uniaxial tension.
Step 6, selecting parameters of the optimal model and establishing a relation model:
and inputting the average spectrum of 50 parts of the obtained standard solid propellant of a certain type and the initial modulus of the unidirectional stretching of 50 parts of the standard solid propellant of a solid propellant into near infrared spectrum analysis software in a one-to-one correspondence manner, and selecting the optimal modeling parameters through the near infrared spectrum analysis software. The modeling parameters comprise standard substance spectral analysis interval selection, spectrum pretreatment, chemometric method selection and optimal main factor number selection.
The final determined optimal relational model parameters are as follows:
spectral analysis interval: 4000cm-1～9000cm-1；
Spectrum pretreatment: none;
the stoichiometric method comprises the following steps: partial least squares;
number of optimal factors: 9.
the concrete process of establishing the optimal model parameter selection and relation model in the step 6 is as follows:
selecting a spectral analysis interval of 50 certain type composite solid propellant standard products:
obtaining near infrared spectrograms of the adhesive, the plasticizer and the oxidant through the step 5, and determining a spectral analysis interval of a certain type of composite solid propellant standard product, wherein the spectral analysis interval of the certain type of composite solid propellant standard product is determined by taking the range of the peak position of the near infrared spectrum of the adhesive, the peak position of the near infrared spectrum of the plasticizer, the peak position of the near infrared spectrum of the oxidant and the peak position of the near infrared spectrum of any one certain type of composite solid propellant standard product obtained in the step 3 as the spectral analysis interval of the certain type of composite solid propellant standard product, and the range of the near infrared spectral peak position of the adhesive, the peak position of the near infrared spectrum of the plasticizer and the peak position of the near infrared spectrum of the oxidant; the spectral analysis interval of the certain type of composite solid propellant standard is 4000cm-1～9000cm-1。
II, certain type of composite solid propellant standard substance spectrum pretreatment:
and establishing a relation model of the spectra of the 50 certain type of composite solid propellant standard products through near infrared processing software. And (3) performing derivative and smooth pretreatment on the spectrum of 50 parts of certain type of composite solid propellant standard substance by a conventional method, and establishing a relation model of the spectrum of the pretreated certain type of composite solid propellant standard substance.
And comparing the relation model of the spectrum of the 50 parts of certain type of composite solid propellant standard substance with the relation model of the spectrum of the pretreated certain type of composite solid propellant standard substance, and selecting a pretreatment mode with a correlation coefficient closer to 1 and a small standard deviation as a pretreatment method of the relation model.
III selection of the stoichiometric method:
a partial least square method is adopted as a chemometric method established by a relation model between a spectrum of a certain type of composite solid propellant standard product and the uniaxial tension initial modulus of the solid composite solid propellant standard product.
IV, selecting the optimal main factor number:
the main factor number is the square of the prediction residual obtained by the interactive verification method, and the optimal factor number is the main factor number with the minimum sum of the squares of the prediction residual obtained by the interactive verification method. And calculating the square sum of the prediction residuals obtained by the interactive verification method to obtain the minimum corresponding optimal main factor number 9 of the square sum of the residuals.
Step 7, verifying the relation model
And the relational model is a relational model between the spectrum of the certain type of composite solid propellant standard product obtained in the step 6 and the uniaxial tensile initial modulus of the solid composite solid propellant standard product.
10 samples of certain type of composite solid propellant with the weight of 2 kilograms are taken for verification of the relation model.
1/5 of the mass of each certain type of composite solid propellant sample is taken as a sample for collecting near infrared spectrum data; acquiring 10 near infrared spectrums of certain type composite solid propellant samples; and inputting the obtained 10 near infrared spectrums of the certain type of solid composite propellant samples into the relation model to obtain the initial modulus of the 10 solid composite propellant samples in the uniaxial tension.
4/5 mass of each certain type of composite solid propellant sample is taken, and after being cured, the solid composite solid propellant sample becomes a solid composite solid propellant sample for testing the uniaxial tensile initial modulus. And (3) testing the uniaxial tension initial modulus by adopting a standard method to obtain 10 uniaxial tension initial moduli of the solid composite solid propellant samples.
And comparing the deviation between the uniaxial tension initial modulus of the solid composite solid propellant sample obtained by the standard method and the uniaxial tension initial modulus of the solid composite solid propellant sample obtained by the near infrared spectrum method. The obtained deviation is less than 3%, and the test result of the relation model is proved to be accurate.
When the solid composite solid propellant sample uniaxial tension initial modulus is tested, the solid composite solid propellant sample uniaxial tension initial modulus is tested by adopting a near infrared spectrum method: and inputting the 10 near infrared spectrums of the certain type of composite solid propellant samples into a relation model of the spectrum of the certain type of composite solid propellant standard and the uniaxial tension initial modulus of the solid composite solid propellant standard to obtain the uniaxial tension initial modulus of the solid composite solid propellant sample measured by the model.
Therefore, near infrared spectrum analysis of the initial modulus of the composite solid propellant in uniaxial tension is completed, and the obtained relation model is used for testing the initial modulus of the composite solid propellant in uniaxial tension.
Firstly, designing a certain amount of composite solid propellant formulas with known proportions according to a certain composite solid propellant formula and a uniform distribution principle; secondly, preparing a sample according to a design formula to obtain a certain amount of composite solid propellant slurry with a known proportion, which is referred to as a composite solid propellant standard, wherein one part of the obtained composite solid propellant standard is used for testing a near infrared spectrum, and the other part is cured and formed to test the unidirectional tensile initial modulus of the composite solid propellant standard; then establishing a relation model between the near infrared spectrum of the composite solid propellant standard product and the uniaxial tension initial modulus of the composite solid propellant standard product by means of professional quantitative software; and finally, performing unidirectional stretching initial modulus of the composite solid propellant sample, wherein the unidirectional stretching initial modulus refers to the unidirectional stretching initial modulus of the solidified composite solid propellant sample, and is hereinafter referred to as the unidirectional stretching initial modulus of the solid composite solid propellant sample. In the process of detecting the composite solid propellant sample, the test conditions are ensured to be the same as those of the standard product.
The near infrared accessory used in the invention is a diffuse reflection optical fiber, and the sample measurement adopts a non-contact type. The non-contact sampling mode overcomes the problem that the composite solid propellant is enriched on the surface of the optical fiber probe in a contact mode.
According to the invention, the cured composite solid propellant uniaxial tension initial modulus is directly obtained by testing the composite solid propellant slurry, so that the problem that the conventional test composite solid propellant slurry needs to be cured for 7 days at 50 ℃ is solved, and the sample curing time is greatly saved.
The test conditions of the composite solid propellant sample described in the invention should be consistent with the test conditions of the composite solid propellant standard.
In the present invention, 4000 to 120000cm is used-1The establishment of the wave band relation model causes the defects of large noise signal, low operation speed and poor stability of the relation model, so that the spectral analysis region of the composite solid propellant standard substance needs to be selected.
In the invention, the quality of the model is judged by mainly referring to the correlation coefficient and the standard deviation of the model, the closer the correlation coefficient of the model is to 1, the better, namely, the closer the predicted value and the practical value of the model are, the better, which is shown in fig. 1: the abscissa of the 1 represents a uniaxial tension initial model of the solid composite solid propellant measured by the method QJ 1812-89; 2, the ordinate represents a uniaxial tension initial model measured by a relation model of a certain type of solid propellant standard; 3, representing points corresponding to the predicted value and the actual value, wherein the closer the numerical values of the predicted value and the actual value are, the better the model is; 4 represents a 45 degree line, with 3 being closer to the 4 model the better. The smaller the standard deviation, the better. The relation model with the optimal correlation coefficient and standard deviation is the optimal model, and the model parameter corresponding to the optimal relation model is the optimal modeling parameter.
The invention utilizes the near infrared technology to analyze the initial modulus of the composite solid propellant in the uniaxial tension, and the specified detection precision is completely achieved. The method for detecting the initial modulus of the composite solid propellant in the uniaxial tension can realize the purpose of high-efficiency and nondestructive analysis, thoroughly overcomes the defect that the curing and forming time is long in the traditional test, and provides a convenient and quick detection method for the production quality and the safe manufacture of the composite solid propellant.
Drawings
FIG. 1 is a graph of the correlation of initial modulus in uniaxial tension using a near infrared method and using a standard test.
Fig. 2 is a flow chart of the present invention.
In the figure: 1, the solid composite solid propellant standard has the initial modulus of uniaxial tension; 2. testing the uniaxial tension initial modulus by using a composite solid propellant standard product model; 3. points corresponding to the predicted values and the actual values of the model samples; 4.45 degree line.
Detailed Description
The embodiment is a method for testing the initial modulus of the unidirectional stretching of a certain type of composite solid propellant, and the specific process is as follows:
the composite solid propellant comprises more than ten components, and the standard product formula of 50 parts of the composite solid propellant is obtained by changing the mass percentage of the components influencing the initial modulus of unidirectional stretching in the composite solid propellant formula.
The components influencing the initial modulus of uniaxial tension comprise an adhesive, a plasticizer and an oxidant.
The components affecting the initial modulus of uniaxial tension are changed, the content of the adhesive in the formula is changed within +/-10%, the content of the plasticizer in the formula is changed within +/-20%, and the content of the oxidant in the formula is changed within +/-3%. According to the changed content, a standard formulation of 50 parts of the composite solid propellant is obtained through orthogonal experiments.
And preparing the materials one by using a 3-liter vertical mixer according to a mixing process to obtain a standard substance of 50 parts of the composite solid propellant. The standard substance is composite solid propellant slurry.
1/5 medicinal slurry is respectively taken from 50 parts of prepared standard substance for near infrared spectrum test, and 50 parts of near infrared spectrum test samples are obtained. The remaining 4/5 of each standard was used for cure molding to give 50 parts of solid composite solid propellant standard for testing the uniaxial tensile initial modulus of the composite solid propellant standard. The cured form was cured at 50 ℃ for 7 days.
the acquisition parameters comprise scanning times, spectral range and resolution.
And adjusting the spectrum acquisition parameters of the near-infrared spectrometer by the near-infrared spectrometer. Taking any one part of the near infrared spectrum test sample obtained in the step 1 as a test sample; and carrying out near infrared spectrum test on the infrared spectrum test sample by using a near infrared spectrometer.
The test process is as follows:
determining the optimal scanning times: adjusting the scanning times of the near-infrared spectrometer to be 50 times, 100 times, 120 times, 160 times and 200 times respectively, and performing near-infrared spectrum acquisition on the samples used by the acquisition parameters according to the determined scanning times respectively; obtaining a near infrared spectrum after each near infrared spectrum acquisition; five near infrared spectra were obtained in this example. And sequentially arranging the five pieces of near infrared spectrum noise according to the obtained five pieces of near infrared spectrum noise values from large to small. And selecting a near infrared spectrum with the minimum scanning frequency from the near infrared spectra with similar noise values, and taking the scanning frequency of the near infrared spectrum as the optimal scanning frequency.
Determining the optimal resolution: the resolution ratios of the near-infrared spectrometers are respectively adjusted to be 2cm-1、4cm-1、8cm-1Sequentially carrying out near infrared spectrum collection on the samples used by the collection parameters, and obtaining a near infrared spectrum after each near infrared spectrum collection; in this example, three pieces of resolution of 2cm were obtained-1、4cm-1、8cm-1Near infrared spectrum of (a). And sequentially arranging the three near infrared spectrums from large to small according to the noise value of each near infrared spectrum. And selecting one near infrared spectrum with the minimum noise value from the three near infrared spectrums, and taking the scanning times of the near infrared spectrum as the optimal resolution.
Selecting a spectral interval: the selected spectral interval is the near infrared band of the near infrared spectrometer employed. In this embodiment, the near infrared band is 4000-120000cm-1。
Through the process, the composite solid propellant near infrared spectrum acquisition parameters are determined as follows:
wave number range: 4000-120000cm-1；
The scanning times are as follows: 120 times;
resolution ratio: 4cm-1。
And 3, collecting near infrared spectrums of 50 parts of composite solid propellant standard:
and (3) respectively acquiring the near infrared spectrum of 50 parts of the composite solid propellant standard according to the near infrared spectrum acquisition parameters of the composite solid propellant determined in the step (2). The method comprises the following steps:
the near infrared spectrometer is started up and preheated for one hour. To pair
Collecting a near infrared spectrum of a first composite solid propellant standard; three spectra were collected for the first composite solid propellant standard. And averaging the three spectra of the sample by using test software carried by a near infrared spectrometer to obtain the average spectrum of the composite solid propellant standard.
And repeating the process of acquiring the near infrared spectrum of the first composite solid propellant standard until the near infrared spectrum acquisition of 50 parts of the composite solid propellant standard is completed, so as to obtain an average spectrum of 50 parts of the composite solid propellant standard.
Thus, the near infrared spectrum collection of 50 parts of the composite solid propellant standard is completed.
In the near infrared spectrum collection, the room temperature of the collection environment is 25 +/-2 ℃, and the relative humidity is less than or equal to 65%.
And taking the obtained average spectrum of 50 parts of the composite solid propellant standard as the near infrared spectrum of the composite solid propellant standard in a relational model.
Step 4, testing the uniaxial tensile initial modulus of the composite solid propellant standard:
and (3) testing the uniaxial tension initial modulus of 50 parts of the solid composite solid propellant standard obtained in the step (1). The method comprises the following steps:
respectively testing the initial modulus of the unidirectional stretching of 50 parts of solid composite solid propellant standard products by using a unidirectional stretching initial modulus tester by adopting a conventional method to respectively obtain the initial modulus of the unidirectional stretching of 50 parts of solid composite solid propellant standard products. The test method executes the national ministry of aviation standard of the people's republic of China, and the standard number is as follows: QJ1812-89, standard name: a method for measuring the initial modulus of the composite solid propellant in uniaxial tension.
And taking the obtained 50 parts of solid composite solid propellant standard uniaxial tension initial modulus as uniaxial tension initial modulus data associated with the near infrared spectrum of the composite solid propellant standard in a relational model.
Step 5, collecting the near infrared spectrum of the components influencing the uniaxial tension initial modulus
The components influencing the initial modulus of the uniaxial tension are respectively an adhesive, a plasticizer and an oxidant.
And (3) acquiring the near infrared spectrum of the component influencing the initial modulus of uniaxial tension according to the optimal acquisition parameters of the near infrared spectrum of the composite solid propellant determined in the step (2), and respectively obtaining near infrared spectrograms of the adhesive, the plasticizer and the oxidant.
Step 6, selecting parameters of the optimal model and establishing a relation model:
and inputting the average spectrum of the obtained 50 parts of the composite solid propellant standard and the initial modulus of the unidirectional stretching of the 50 parts of the solid composite propellant standard into near infrared spectrum analysis software in a one-to-one correspondence manner, and selecting the optimal modeling parameters through the near infrared spectrum analysis software. The modeling parameters comprise standard substance spectral analysis interval selection, spectrum pretreatment, chemometric method selection and optimal main factor number selection.
The specific process is as follows:
selecting a spectral analysis interval of 50 parts of composite solid propellant standard:
obtaining near infrared spectrograms of the adhesive, the plasticizer and the oxidant through the step 5, and determining a spectral analysis interval of the standard product of the composite solid propellant, wherein the method specifically comprises the steps of enabling the peak position of the near infrared spectrum of the adhesive, the peak position of the near infrared spectrum of the plasticizer and the peak position of the near infrared spectrum of the oxidant to be in the same range as the peak position of the near infrared spectrum of any one standard product of the composite solid propellant obtained in the step 3, and enabling the peak position of the near infrared spectrum of the standard product of the composite solid propellant and the peak position of the near infrared spectrum of the adhesiveThe range of the peak position of the near infrared spectrum of the plasticizer and the range of the peak position of the near infrared spectrum of the oxidant are used as the spectral analysis interval of the composite solid propellant standard substance; the spectral analysis interval of the composite solid propellant standard product is 4000cm-1～9000cm-1。
II, spectrum pretreatment of a composite solid propellant standard product:
and establishing a relation model of the spectrum of the 50 parts of the composite solid propellant standard substance through near infrared processing software. And (3) performing derivative and smooth pretreatment on the spectrum of 50 parts of the composite solid propellant standard substance according to a conventional method, and establishing a relation model of the spectrum of the pretreated composite solid propellant standard substance.
And comparing the relation model of the spectrum of the 50 parts of composite solid propellant standard substance with the relation model of the spectrum of the pretreated composite solid propellant standard substance, and selecting a pretreatment mode with a correlation coefficient closer to 1 and a small standard deviation as a pretreatment method of the relation model. The comparison result proves that the relation model without spectrum pretreatment is better.
III selection of the stoichiometric method:
and a partial least square method is adopted as a chemometric method established by a relation model between the spectrum of the standard substance of the composite solid propellant and the uniaxial tensile initial modulus of the standard substance of the solid composite solid propellant.
IV, selecting the optimal main factor number:
the main factor number is the square of the prediction residual obtained by the interactive verification method, and the optimal factor number is the main factor number with the minimum sum of the squares of the prediction residual obtained by the interactive verification method. If the number of the main factors selected for establishing the model is too small, insufficient fitting can occur, and more useful information of the original spectrum can be lost, but if too many main factors are selected, overfitting can be caused, measurement noise is introduced, the prediction error of the established model can be obviously increased, and the quality of the model is reduced. And calculating the square sum of the prediction residuals obtained by the interactive verification method to obtain the minimum corresponding main factor number of the square sum of the residuals as 9, namely the optimal factor number as 9.
The final determined optimal relational model parameters are as follows:
spectral analysis interval: 4000cm-1～9000cm-1；
Spectrum pretreatment: none;
the stoichiometric method comprises the following steps: partial least squares;
number of optimal factors: 9.
and inputting the optimal relation model parameters by means of chemometrics software to obtain a relation model between the spectrum of the standard solid propellant and the uniaxial tension initial modulus of the standard solid propellant. The relation model is a relation model between the near infrared spectrum of the composite solid propellant standard product and the uniaxial tension initial modulus of the composite solid propellant standard product, the correlation coefficient of the relation model is 0.99896, and the standard deviation is 0.117.
Step 7, verifying the relation model
And the relational model is a relational model between the spectrum of the standard solid propellant and the uniaxial tensile initial modulus of the standard solid composite propellant obtained in the step 6.
10 samples of composite solid propellant with a weight of 2 kg each were taken for the validation of the relational model.
1/5 of the mass of each composite solid propellant sample is taken as a sample for collecting near infrared spectrum data; acquiring 10 composite solid propellant samples near infrared spectra after collection; and inputting the obtained 10 composite solid propellant samples into the relation model by near infrared spectroscopy to obtain the initial modulus of the 10 solid composite solid propellant samples in the uniaxial tension.
4/5 of the mass of each composite solid propellant sample is taken, and after solidification, the solid composite solid propellant sample becomes a tested solid composite solid propellant sample with the uniaxial tensile initial modulus. And (3) testing the initial modulus of uniaxial tension by adopting a standard method to obtain the initial modulus of uniaxial tension of 10 solid composite solid propellant samples.
And comparing the deviation between the uniaxial tension initial modulus of the solid composite solid propellant sample obtained by the standard method and the uniaxial tension initial modulus of the solid composite solid propellant sample obtained by the near infrared spectrum method. The obtained deviation is less than 3%, and the test result of the relation model is proved to be accurate.
Therefore, near infrared spectrum analysis of the initial modulus of the composite solid propellant in uniaxial tension is completed, and the obtained relation model is used for testing the initial modulus of the composite solid propellant in uniaxial tension.
Claims (7)
1. A near infrared spectrum analysis method for the uniaxial tension initial modulus of a composite solid propellant is characterized by comprising the following specific processes:
step 1, preparation of a sample required by a relation model:
the samples required by the relation model comprise 50 parts of near infrared spectrum test samples and 50 parts of solid composite solid propellant standard;
the near infrared spectrum test sample and the solid composite solid propellant standard are both prepared by changing the mass percentage of the components influencing the initial modulus of uniaxial tension in the composite solid propellant formula;
step 2, determining the optimal acquisition parameters of the near infrared spectrum of the composite solid propellant:
the acquisition parameters comprise scanning times, spectral range and resolution;
adjusting the spectrum acquisition parameters of the near-infrared spectrometer by the near-infrared spectrometer; taking any one part of the near infrared spectrum test sample obtained in the step 1 as a test sample; performing near infrared spectrum test on the infrared spectrum test sample by using a near infrared spectrometer;
determining the near infrared spectrum acquisition parameters of a certain type of composite solid propellant as follows:
wave number range: 4000-120000cm-1；
The scanning times are as follows: 120 times;
resolution ratio: 4cm-1；
And 3, collecting the near infrared spectrum of 50 parts of certain type composite solid propellant standard:
respectively collecting the near infrared spectrum of 50 parts of standard substance of the certain type of composite solid propellant according to the near infrared spectrum collection parameters of the certain type of composite solid propellant determined in the step 2;
in the near infrared spectrum collection, the room temperature of the collection environment is 25 +/-2 ℃, and the relative humidity is less than or equal to 65%;
taking the obtained average spectrum of 50 parts of standard substance of certain type of composite solid propellant as the near infrared spectrum of the standard substance of certain type of composite solid propellant in a relational model;
step 4, testing the uniaxial tensile initial modulus of a certain type of composite solid propellant standard:
testing the initial modulus of uniaxial tension of 50 parts of the solid composite solid propellant standard obtained in the step 1;
during testing, respectively testing the uniaxial tension initial modulus of 50 parts of the solid composite solid propellant standard by using a uniaxial tension initial modulus tester to respectively obtain the uniaxial tension initial modulus of 50 parts of the solid composite solid propellant standard; taking the obtained 50 parts of solid composite solid propellant standard substance uniaxial tension initial modulus as uniaxial tension initial modulus data associated with the near infrared spectrum of a certain type of composite solid propellant standard substance in a relational model;
step 5, collecting the near infrared spectrum of the components influencing the uniaxial tension initial modulus
Acquiring the near infrared spectrum of the component influencing the initial modulus of uniaxial tension according to the optimal acquisition parameters of the near infrared spectrum of the composite solid propellant determined in the step 2, and respectively obtaining near infrared spectrograms of the adhesive, the plasticizer and the oxidant influencing the initial modulus of uniaxial tension;
step 6, selecting parameters of the optimal model and establishing a relation model:
inputting the average spectrum of 50 parts of the obtained standard solid propellant of a certain type and the initial modulus of the unidirectional stretching of 50 parts of the standard solid propellant of a solid propellant into near infrared spectrum analysis software in a one-to-one correspondence manner, and selecting the optimal modeling parameters through the near infrared spectrum analysis software; the modeling parameters comprise standard substance spectral analysis interval selection, spectrum pretreatment, selection of a chemometric method and optimal main factor number selection;
the final determined optimal relational model parameters are as follows:
spectral analysis interval: 4000cm-1～9000cm-1；
Spectrum pretreatment: none;
the stoichiometric method comprises the following steps: partial least squares;
number of optimal factors: 9;
step 7, verifying the relation model
The relation model is a relation model between the spectrum of the certain type of composite solid propellant standard product obtained in the step 6 and the uniaxial tensile initial modulus of the solid composite solid propellant standard product;
taking 10 samples of certain type of composite solid propellant with the weight of 2 kilograms respectively for verifying a relation model;
1/5 of the mass of each certain type of composite solid propellant sample is taken as a sample for collecting near infrared spectrum data;
acquiring 10 near infrared spectrums of certain type composite solid propellant samples; inputting the obtained 10 near infrared spectrums of the certain type of solid composite propellant samples into the relation model to obtain the initial modulus of the 10 solid composite propellant samples in the unidirectional stretching direction;
4/5 of the mass of each certain type of composite solid propellant sample is taken, and the solid composite solid propellant sample becomes a solid composite solid propellant sample for testing the uniaxial tensile initial modulus after being solidified; testing the initial modulus of uniaxial tension by adopting a standard method to obtain the initial modulus of uniaxial tension of 10 solid composite solid propellant samples;
comparing the deviation between the initial modulus of the solid composite solid propellant sample obtained by the standard method and the initial modulus of the solid composite solid propellant sample obtained by the near infrared spectrum method; the obtained deviation is less than 3%, and the test result of the relation model is proved to be accurate;
therefore, near infrared spectrum analysis of the initial modulus of the composite solid propellant in uniaxial tension is completed, and the obtained relation model is used for testing the initial modulus of the composite solid propellant in uniaxial tension.
2. The method for near infrared spectroscopic analysis of the initial modulus of uniaxial tension of the composite solid propellant according to claim 1, wherein the components affecting the initial modulus of uniaxial tension are adhesives, plasticizers and oxidants; changing the components of the adhesive, the plasticizer and the oxidant to change the content of the adhesive within +/-10 percent of the formula, the content of the plasticizer within +/-20 percent of the formula and the content of the oxidant within +/-3 percent of the formula; obtaining 50 standard product formulas of certain type of composite solid propellant through orthogonal experiments according to the changed content; respectively taking 1/5 medicinal slurry from 50 parts of prepared standard substance for near infrared spectrum test to obtain 50 parts of near infrared spectrum test samples; the remaining 4/5 of each standard was used for curing and molding to obtain 50 parts of solid composite solid propellant standard for testing the initial modulus of uniaxial tension of the composite solid propellant standard.
3. The method for near infrared spectroscopic analysis of the uniaxial tension initial modulus of the composite solid propellant according to claim 1, wherein in step 2, when the optimal number of scans is determined: adjusting the scanning times of the near-infrared spectrometer to be 50 times, 100 times, 120 times, 160 times and 200 times respectively, and performing near-infrared spectrum acquisition on the samples used by the acquisition parameters according to the determined scanning times respectively; acquiring a near infrared spectrum after each acquisition of the near infrared spectrum; sequentially arranging the five pieces of near infrared spectrum noise according to the five obtained near infrared spectrum noise values from large to small; and selecting a near infrared spectrum with the minimum scanning frequency from the near infrared spectra with similar noise values, and taking the scanning frequency of the near infrared spectrum as the optimal scanning frequency.
4. The method for near infrared spectroscopic analysis of the uniaxial tensile initial modulus of the composite solid propellant according to claim 1, wherein in step 2, when determining the optimal resolution: the resolution ratios of the near-infrared spectrometers are respectively adjusted to be 2cm-1、4cm-1、8cm-1Sequentially carrying out near infrared spectrum collection on the samples used by the collection parameters, and obtaining a near infrared spectrum after each near infrared spectrum collection; push buttonSequentially arranging the three near infrared spectrums from large to small in noise value of each near infrared spectrum; and selecting one near infrared spectrum with the minimum noise value from the three near infrared spectrums, and taking the scanning times of the near infrared spectrum as the optimal resolution.
5. The near infrared spectrum analysis method for the uniaxial tension initial modulus of the composite solid propellant as claimed in claim 1, wherein the specific process of collecting 50 parts of near infrared spectrum of the standard substance of the certain type of composite solid propellant in the step 3 is as follows: collecting a near infrared spectrum of a first certain type of composite solid propellant standard; collecting three spectra of a first certain type of composite solid propellant standard; averaging the three spectra of the sample by a near infrared spectrometer to obtain an average spectrum of the composite solid propellant standard product;
repeating the process of acquiring the near infrared spectrum of the first certain type of composite solid propellant standard until the near infrared spectrum acquisition of 50 parts of certain type of composite solid propellant standard is completed, so as to obtain an average spectrum of 50 parts of certain type of composite solid propellant standard; and (4) completing the acquisition of the near infrared spectrum of 50 parts of certain type of composite solid propellant standard.
6. The near infrared spectroscopy analysis method for the uniaxial tension initial modulus of the composite solid propellant according to claim 1, wherein the specific process of establishing the optimal model parameter selection and relation model in the step 6 is as follows:
selecting a spectral analysis interval of 50 certain type composite solid propellant standard products:
obtaining a near infrared spectrogram of the adhesive, the plasticizer and the oxidant through the step 5, determining a spectral analysis interval of a certain type of composite solid propellant standard, specifically, enabling a peak position of a near infrared spectrum of the adhesive, a peak position of a near infrared spectrum of the plasticizer and a peak position of a near infrared spectrum of the oxidant to be in a range of the near infrared spectrum of any one certain type of composite solid propellant standard obtained in the step 3, and enabling the peak position of the near infrared spectrum of the certain type of composite solid propellant standard, the peak position of the near infrared spectrum of the adhesive, the peak position of the near infrared spectrum of the plasticizer and the near red of the plasticizer to exist atThe range of the peak position of the external spectrum and the range of the peak position of the near infrared spectrum of the oxidant is used as the spectral analysis interval of the certain type of composite solid propellant standard substance; the spectral analysis interval of the certain type of composite solid propellant standard is 4000cm-1～9000cm-1；
II, certain type of composite solid propellant standard substance spectrum pretreatment:
establishing a relation model of the spectra of the 50 certain type of composite solid propellant standard products through near-infrared processing software;
performing derivative and smooth pretreatment on 50 parts of certain type of composite solid propellant standard substance spectrum according to a conventional method, and establishing a relation model of the pretreated certain type of composite solid propellant standard substance spectrum;
comparing the relation model of the spectrum of the 50 parts of certain type of composite solid propellant standard substance with the relation model of the spectrum of the pretreated certain type of composite solid propellant standard substance, and selecting a pretreatment mode with a correlation coefficient closer to 1 and a small standard deviation as a pretreatment method of the relation model;
III selection of the stoichiometric method:
a partial least square method is adopted as a chemometric method established by a relation model between the spectrum of a certain type of composite solid propellant standard and the uniaxial tension initial modulus of the solid composite solid propellant standard;
IV, selecting the optimal main factor number:
the main factor number is the square of the prediction residual obtained by the interactive verification method, and the optimal factor number is the main factor number with the minimum sum of the squares of the prediction residual obtained by the interactive verification method; and calculating the square sum of the prediction residuals obtained by the interactive verification method to obtain the minimum corresponding optimal main factor number of the square sum of the residuals as 9.
7. The method for near infrared spectroscopic analysis of the uniaxial tension initial modulus of the composite solid propellant according to claim 1, wherein when the solid composite solid propellant sample is tested for the uniaxial tension initial modulus in step 7,
the method comprises the following steps of (1) testing the uniaxial tension initial modulus of a solid composite solid propellant sample by adopting a near infrared spectrum method: and inputting the 10 near infrared spectrums of the certain type of composite solid propellant samples into a relation model of the spectrum of the certain type of composite solid propellant standard and the uniaxial tension initial modulus of the solid composite solid propellant standard to obtain the uniaxial tension initial modulus of the solid composite solid propellant sample measured by the model.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010683262.8A CN111929155A (en) | 2020-07-16 | 2020-07-16 | Near infrared spectrum analysis method for uniaxial tension initial modulus of composite solid propellant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010683262.8A CN111929155A (en) | 2020-07-16 | 2020-07-16 | Near infrared spectrum analysis method for uniaxial tension initial modulus of composite solid propellant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111929155A true CN111929155A (en) | 2020-11-13 |
Family
ID=73313083
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010683262.8A Pending CN111929155A (en) | 2020-07-16 | 2020-07-16 | Near infrared spectrum analysis method for uniaxial tension initial modulus of composite solid propellant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111929155A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5668374A (en) * | 1996-05-07 | 1997-09-16 | Core Laboratories N.V. | Method for stabilizing near-infrared models and determining their applicability |
| CN103760130A (en) * | 2014-01-03 | 2014-04-30 | 广州中大南沙科技创新产业园有限公司 | Method for measuring tween-80 content in compound musk injection by using near-infrared spectrum |
| CN104568828A (en) * | 2015-01-30 | 2015-04-29 | 云南中烟工业有限责任公司 | Method for determining tensile strength of reproduced tobacco leaves of papermaking method by near-infrared diffuse reflection spectrum |
| CN107121409A (en) * | 2017-06-16 | 2017-09-01 | 西安航天化学动力厂 | A kind of method of test NEPE solid propellant combustion rates |
| CN108020526A (en) * | 2017-12-13 | 2018-05-11 | 西安航天化学动力厂 | A kind of HTPB propellant medicine slurry component near infrared detection method |
-
2020
- 2020-07-16 CN CN202010683262.8A patent/CN111929155A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5668374A (en) * | 1996-05-07 | 1997-09-16 | Core Laboratories N.V. | Method for stabilizing near-infrared models and determining their applicability |
| CN103760130A (en) * | 2014-01-03 | 2014-04-30 | 广州中大南沙科技创新产业园有限公司 | Method for measuring tween-80 content in compound musk injection by using near-infrared spectrum |
| CN104568828A (en) * | 2015-01-30 | 2015-04-29 | 云南中烟工业有限责任公司 | Method for determining tensile strength of reproduced tobacco leaves of papermaking method by near-infrared diffuse reflection spectrum |
| CN107121409A (en) * | 2017-06-16 | 2017-09-01 | 西安航天化学动力厂 | A kind of method of test NEPE solid propellant combustion rates |
| CN108020526A (en) * | 2017-12-13 | 2018-05-11 | 西安航天化学动力厂 | A kind of HTPB propellant medicine slurry component near infrared detection method |
Non-Patent Citations (1)
| Title |
|---|
| 张爱科: "固体火箭发动机装药和总装的批生产工艺及质量控制研究", 《豆丁网 HTTPS://WWW.DOCIN.COM/P-537713348.HTML》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1982872B (en) | Near-infrared diffuse reflection spectral method for fastly inspecting drop water content | |
| CN103018195B (en) | Method for determination of PCTFE content in PBX explosive by near infrared spectrum | |
| CN111811932B (en) | Near infrared spectrum analysis method for unidirectional stretching mechanical property of composite solid propellant | |
| CN104749132A (en) | Method for measuring content of azodicarbonamide in flour | |
| CN101216419A (en) | Method for quickly detecting yellow wine quality index | |
| CN109142263B (en) | Component dispersion uniformity online test method in solid propellant preparation process | |
| CN108020526A (en) | A kind of HTPB propellant medicine slurry component near infrared detection method | |
| CN105021564A (en) | Method for determining content of ergosterol in tobacco based on near infrared spectroscopic analysis technology | |
| CN104596979A (en) | Method for measuring cellulose of reconstituted tobacco by virtue of near infrared reflectance spectroscopy technique | |
| CN104596975A (en) | Method for measuring lignin of reconstituted tobacco by paper-making process by virtue of near infrared reflectance spectroscopy technique | |
| CN112179871A (en) | Method for nondestructive detection of caprolactam content in sauce food | |
| CN104596976A (en) | Method for determining protein of paper-making reconstituted tobacco through ear infrared reflectance spectroscopy technique | |
| CN104596980A (en) | Method for measuring hot water solvends of reconstituted tobacco by paper-making process by virtue of near infrared reflectance spectroscopy technique | |
| CN111929155A (en) | Near infrared spectrum analysis method for uniaxial tension initial modulus of composite solid propellant | |
| CN107121409A (en) | A kind of method of test NEPE solid propellant combustion rates | |
| CN108872127A (en) | A kind of nano-cellulose film measurement of water ratio method based on Subtractive Infrared Spectroscopy | |
| CN103048290A (en) | Method for detecting filling value of cut tobacco | |
| CN117740721A (en) | Method for detecting non-protein nitrogen content in feed raw material | |
| CN111811991A (en) | Near infrared spectrum analysis method for non-contact testing density of composite solid propellant | |
| CN109709060B (en) | Method for measuring asphalt softening point, penetration degree and mass loss | |
| CN109374566B (en) | Method and system for measuring content of mixed alcohol | |
| Li et al. | Rapid and nondestructive analysis of quality of prepreg cloth by near-infrared spectroscopy | |
| CN104596978A (en) | Method for determining quantitative physical indexes of paper-making tobacco sheet by virtue of near-infrared reflectance spectroscopy | |
| CN115436315A (en) | Near infrared spectrum-based cement additive detection method | |
| CN1712937A (en) | Nondestructive rapid detection for contents of multiple element components in composite fertilizer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20201113 |
|
| WD01 | Invention patent application deemed withdrawn after publication |