CN112557570A - Method for distinguishing components of combustion residues of gasoline and styrene butadiene rubber by GC-MS (gas chromatography-Mass spectrometer) quantitative method - Google Patents
Method for distinguishing components of combustion residues of gasoline and styrene butadiene rubber by GC-MS (gas chromatography-Mass spectrometer) quantitative method Download PDFInfo
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Abstract
The invention relates to a method for distinguishing components of combustion residues of gasoline and styrene butadiene rubber by using a GC-MS (gas chromatography-Mass spectrometer) quantitative method, belonging to the technical field of fire identification. The method comprises the following steps: the method comprises the following steps: respectively placing a first sample and a second sample in a crucible, igniting, and respectively taking combustion residues of the first sample and the second sample after the combustion is naturally extinguished; step two: sample processing and instrument setting; step three: after the sample is processed in the second step, the extracted experimental sample enters a GC-MS instrument from a sample inlet to obtain a total ion current chromatogram; step four: repeating the first step to the third step to obtain three groups of total ion current chromatograms; step five: identifying and analyzing the similarity of the styrene butadiene rubber combustion residues and the gasoline combustion residue total ion flow graph; step six: and distinguishing components of the combustion residues of the gasoline and the styrene butadiene rubber by using a GC-MS quantitative method for analysis. The method for rapidly identifying the gasoline components by adopting the GC-MS spectrogram greatly improves the accuracy of identifying the gasoline components.
Description
Technical Field
The invention relates to an identification method, in particular to a method for distinguishing components of combustion residues of gasoline and styrene butadiene rubber by using a GC-MS (gas chromatography-Mass spectrometer) quantitative method, belonging to the technical field of fire identification.
Background
After a fire accident occurs, the fire reason is scientifically and reasonably determined, the fire property is timely and accurately judged, the fire property is distinguished, the fire disaster detection method is an important task of fire investigation work, and the fire disaster detection method has important significance for researching fire accident responsibility, summarizing experience teaching and training and maintaining life and property safety of people.
Gasoline is one of combustion improvers which are common in fire cases, and the existence of gasoline components in the fire residue inspection and identification results is key evidence for identifying cases, so that the gasoline is of great importance to extraction of residues in fire fields and chemical composition analysis. The common method for detecting the residual gasoline in the fire scene mainly comprises thin layer chromatography, ultraviolet spectroscopy, gas chromatography-mass spectrometry (GC-MS) and college liquid chromatography. Researchers use different methods to analyze the types of the actual fire scene extract material evidence according to related methods specified in GB/T18294-2010 fire technical identification method, wherein gas chromatography-mass spectrometry is the most common method with the highest sensitivity and accuracy.
However, the organic matters in the fire scene are various, especially petroleum product derivatives, and the organic materials often cause great background interference on GC-MS detection of combustion improvers, so that inaccuracy of identification results is increased. Therefore, the Netherlands court scientific institute (NFI) establishes an international database of common interferents, researchers study chromatograms of the common interferents in a fire scene under different conditions, and the results show that factors such as the type of a combustion improver, the type of a combustible interferent, the combustion time, the air flow and the like all affect the components of the combustion improver residues. The domestic scholars also study the influence of various interferents on gasoline identification, establish a related database and play an important guiding role in eliminating the influence of partial organic matter combustion or decomposition products on the gasoline component identification. A great deal of research finds that the combustion or decomposition product containing alkylbenzene has large background interference on gasoline identification, and the main component of organic matters capable of generating a large amount of alkylbenzene after combustion or thermal decomposition often contains alkylbenzene monomers, wherein Styrene Butadiene Rubber (SBR), also called polystyrene butadiene copolymer, is widely applied to the market as typical synthetic rubber, and is one of the most common materials in the fields of automobile tires, adhesive tapes, rubber tubes, wires and cables, medical appliances and the like. However, the styrene-butadiene rubber combustion residue GC-MS total ion chromatogram contains characteristic peaks of gasoline combustion residue GC-MS total ion chromatogram, such as C2 benzene, C3 benzene, C4 benzene and polycyclic aromatic hydrocarbon, so that the styrene-butadiene rubber combustion residue has a great influence on gasoline identification. How to eliminate the influence of the styrene butadiene rubber combustion residues in the material evidence extracted in a fire scene on the inspection and identification of gasoline is one of the important subjects of the fire inspection and identification research works at home and abroad at present.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for distinguishing components of combustion residues of gasoline and styrene butadiene rubber by using a GC-MS (gas chromatography-mass spectrometry) quantitative method, which is used for solving the problems that in fire identification, an artificial identification chromatogram is uncertain and random, and the combustion or decomposition product of styrene butadiene rubber in the fire residues has great interference on the chromatogram.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for distinguishing gasoline and styrene butadiene rubber combustion residue components by using a GC-MS quantitative method comprises the following steps:
the method comprises the following steps: in order to enable the environment of the experimental sample to be as close to a real fire scene as possible, the simulation experiment is carried out in a mode of igniting the experimental sample a and the experimental sample b in a crucible, and the method specifically comprises the following steps: respectively placing an experimental sample a and two experimental samples a in a crucible, igniting, and respectively taking combustion residues of the experimental samples a after the combustion is naturally extinguished; wherein the experimental sample a in the first step comprises one or more of organic substances containing styrene butadiene rubber and gasoline; the experimental sample b in the step one is gasoline;
step two: sample processing and instrument set-up
The method for treating the combustion residues of the experimental sample by adopting a solvent extraction method comprises the following steps: placing each experimental sample prepared in the step one in a beaker, adding n-hexane, placing the beaker in an ultrasonic cleaner, shaking the beaker for 10min, taking out the sample, naturally evaporating the sample to 0.5ml, and extracting the sample into a sample injection bottle for detection, wherein the sample injection amount is 0.1 mu l; setting analysis conditions of the gas chromatography-mass spectrometer for the combustion residues of the experimental sample a and the experimental sample b, namely the analysis conditions of each experimental sample of the GC-MS instrument;
step three: after the sample is processed in the second step, the extracted experimental sample enters a GC-MS instrument from an injection port, the experimental sample enters a mass spectrometer after being separated by a chromatographic column, different ions enter a mass analyzer and a detector after being ionized by an ion source, a detection signal is transmitted to a computer, the detection signal is processed by using data analysis software carried by the GC-MS instrument to obtain a total ion current chromatogram, the analysis of extracted ion peaks is carried out aiming at different characteristic components, and the identification and comparative analysis are carried out on each substance peak through a standard spectrum library;
step four: repeating the first step to the third step, and performing GC-MS analysis repeated tests on the combustion residues of the experimental sample a and the experimental sample b to obtain three groups of total ion current chromatograms;
step five: the similarity identification analysis of the styrene butadiene rubber combustion residue and the gasoline combustion residue total ion flow diagram specifically comprises the following steps: comparing and identifying each characteristic peak in the total ion current chromatogram with a standard spectrogram library, analyzing the types, names, molecular formulas and retention time of characteristic components of aromatic hydrocarbon and polycyclic aromatic hydrocarbon in the experimental sample, and judging whether the experimental sample contains one or two of gasoline combustion residues or butadiene styrene rubber combustion residues;
step six: an analysis method for distinguishing components of combustion residues of gasoline and styrene butadiene rubber by using a GC-MS quantitative method specifically comprises the following steps: if the experimental sample is analyzed and judged to contain one or two of gasoline combustion residues or styrene butadiene rubber combustion residues through the four steps, selecting three characteristic peaks of C2 benzene in the total ion current chromatogram, integrating the areas of the three characteristic peaks through data analysis software carried by a GC-MS instrument, or solving the peak value, and synthesizing data in the repeated test in the fourth step to obtain the average value of the area ratios of the three characteristic peaks, namely the ratio of the three kinds of C2 benzene; comparing the content ratios of three types of C2 benzene in the combustion residue of the experimental sample a and the combustion residue of a certain styrene butadiene rubber, and if the ratios are consistent, determining that the main component of the experimental sample a is the styrene butadiene rubber; comparing the content ratios of three types of C2 benzene in the combustion residue of the experimental sample a and the combustion residue of the experimental sample b, if the ratios are consistent, the main component of the experimental sample a can be proved to be gasoline, and if the ratios are inconsistent, the experimental sample a is proved to contain one or more organic matters in the styrene butadiene rubber.
Further, the organic matter containing styrene butadiene rubber in the first step is specifically: one or more of styrene-butadiene SBR1502, styrene-butadiene SBR 1712, styrene-butadiene SBR1502E, industrial styrene-butadiene cushion, thermoplastic styrene-butadiene rubber particle SBS, butadiene rubber BR9000, solution polymerized styrene-butadiene rubber SSBR 303 and thermoplastic styrene-butadiene rubber SBS 1401.
Further, in the second step, the GC-MS instrument analysis conditions of the combustion residue of the experimental sample a and the experimental sample b are as follows: the split ratio is 10: 1, the flow rate of He gas is 20mL/min, and the pressure in front of the column is 800 kpa; the column temperature is increased to 260 ℃ in a step-like manner from 50 ℃, and the specific process is as follows: firstly keeping the column temperature at 50 ℃ for 2min, then raising the column temperature to 150 ℃ at 10 ℃/min, keeping the column temperature at 2min, then raising the column temperature to 186 ℃ at 6 ℃/min, keeping the column temperature at 2min, finally raising the column temperature to 260 ℃ at 4 ℃/min, and keeping the column temperature at 2 min.
Further, the gasoline in the experimental sample a and the gasoline in the experimental sample b are both 92# gasoline.
Compared with the prior art, the invention has the following technical effects:
the method disclosed by the invention effectively solves the uncertainty and randomness of manual chromatogram identification around the complex situation of combustion improver identification in the process of analyzing the fire residues, effectively eliminates the interference of styrene butadiene rubber combustion or decomposition products in the fire residues on the chromatogram, greatly improves the accuracy of gasoline component identification by adopting a method for quickly identifying the gasoline component by a GC-MS (gas chromatography-mass spectrometry) chromatogram, and has reliable identification data and better application prospect.
Drawings
FIG. 1 is a total ion current chromatogram of the combustion residue of SBR No. 1502E in sample a;
FIG. 2 is a total ion current chromatogram of the combustion residue of sample b;
FIG. 3 is a total ion flow chromatogram of the combustion residue of sample c;
FIG. 4 is a total ion flow chromatogram of the combustion residue of sample d.
Detailed Description
The invention will be further illustrated with reference to the following specific examples and the accompanying figures 1-4.
The invention relates to a method for distinguishing components of combustion residues of gasoline and styrene butadiene rubber by using a GC-MS (gas chromatography-Mass spectrometer) quantitative method, which comprises the following steps of:
the method comprises the following steps: in order to enable the environment of the experimental sample to be as close to a real fire scene as possible, the simulation experiment is carried out in a mode of igniting the experimental sample a and the experimental sample b in a crucible, and the method specifically comprises the following steps: respectively placing an experimental sample a and two experimental samples a in a crucible, igniting, and respectively taking combustion residues of the experimental samples a after the combustion is naturally extinguished; the experimental sample a in the first step comprises one or more of styrene butadiene rubber-containing organic matters and No. 92 gasoline, wherein the styrene butadiene rubber-containing organic matters are specifically as follows: one or more of styrene-butadiene SBR1502, styrene-butadiene SBR 1712, styrene-butadiene SBR1502E, industrial styrene-butadiene cushion, thermoplastic styrene-butadiene rubber particle SBS, butadiene rubber BR9000, solution polymerized styrene-butadiene rubber SSBR 303 and thermoplastic styrene-butadiene rubber SBS 1401; the experimental sample b in the first step is 92# gasoline;
step two: sample processing and instrument set-up
The method for treating the combustion residues of the experimental sample by adopting a solvent extraction method comprises the following steps: placing each experimental sample prepared in the step one in a beaker, adding n-hexane, placing the beaker in an ultrasonic cleaner, shaking the beaker for 10min, taking out the sample, naturally evaporating the sample to 0.5ml, and extracting the sample into a sample injection bottle for detection, wherein the sample injection amount is 0.1 mu l; setting the analysis conditions of the gas chromatography-mass spectrometer for the combustion residues of the experimental sample a and the experimental sample b, namely the analysis conditions of each experimental sample of the GC-MS instrument: the split ratio is 10: 1, the flow rate of He gas is 20mL/min, and the pressure in front of the column is 800 kpa; the column temperature is increased to 260 ℃ in a step-like manner from 50 ℃, and the specific process is as follows: firstly, keeping the column temperature at 50 ℃ for 2min, then increasing the temperature to 150 ℃ at 10 ℃/min, keeping the temperature for 2min, then increasing the temperature to 186 ℃ at 6 ℃/min, keeping the temperature for 2min, and finally increasing the temperature to 260 ℃ at 4 ℃/min, keeping the temperature for 2 min;
step three: after the sample is processed in the second step, the extracted experimental sample enters a GC-MS instrument from an injection port, the experimental sample enters a mass spectrometer after being separated by a chromatographic column, different ions enter a mass analyzer and a detector after being ionized by an ion source, a detection signal is transmitted to a computer, the detection signal is processed by using data analysis software carried by the GC-MS instrument to obtain a total ion current chromatogram, the analysis of extracted ion peaks is carried out aiming at different characteristic components, and the identification and comparative analysis are carried out on each substance peak through a standard spectrum library;
step four: repeating the first step to the third step, and performing GC-MS analysis repeated tests on the combustion residues of the experimental sample a and the experimental sample b to obtain three groups of total ion current chromatograms;
step five: the similarity identification analysis of the styrene butadiene rubber combustion residue and the gasoline combustion residue total ion flow diagram specifically comprises the following steps: comparing and identifying each characteristic peak in the total ion current chromatogram with a standard spectrogram library, analyzing the types, names, molecular formulas and retention time of characteristic components of aromatic hydrocarbon and polycyclic aromatic hydrocarbon in the experimental sample, and judging whether the experimental sample contains one or two of gasoline combustion residues or butadiene styrene rubber combustion residues;
step six: an analysis method for distinguishing components of combustion residues of gasoline and styrene butadiene rubber by using a GC-MS quantitative method specifically comprises the following steps: if the experimental sample is analyzed and judged to contain one or two of gasoline combustion residues or styrene butadiene rubber combustion residues through the four steps, selecting three characteristic peaks of C2 benzene in the total ion current chromatogram, integrating the areas of the three characteristic peaks through data analysis software carried by a GC-MS instrument, or solving the peak value, and synthesizing data in the repeated test in the fourth step to obtain the average value of the area ratios of the three characteristic peaks, namely the ratio of the three kinds of C2 benzene; comparing the content ratios of three types of C2 benzene in the combustion residue of the experimental sample a and the combustion residue of a certain styrene butadiene rubber, and if the ratios are consistent, determining that the main component of the experimental sample a is the styrene butadiene rubber; comparing the content ratios of three types of C2 benzene in the combustion residue of the experimental sample a and the combustion residue of the experimental sample b, if the ratios are consistent, the main component of the experimental sample a can be proved to be gasoline, and if the ratios are inconsistent, the experimental sample a is proved to contain one or more organic matters in the styrene butadiene rubber.
The process of the present invention is further illustrated in tables 1-4 below in conjunction with FIGS. 1-4.
Fig. 1 is a total ion current chromatogram of the combustion residue of SBR1502E in sample a, and table 1 is an average value of the peak area ratios of three characteristic peaks of C2 benzene as the combustion residue of SBR1502E in sample a. At present, an unknown sample possibly containing the styrene butadiene rubber combustion residue is detected by the method, an ion current chromatogram is extracted by GC-MS analysis, and the similarity of the sample and the characteristic peak of the styrene butadiene rubber or gasoline combustion product is qualitatively analyzed by comparing with a standard spectrum library, if the sample is one or more of the styrene butadiene rubbers. The unknown sample can be excluded or not excluded from containing the styrene-butadiene rubber combustion residue component by comparing the peak area ratios or peak ratios of the three C2 benzenes.
TABLE 1
The specific operation flow is as follows:
example 1:
(1) sample processing method
Treating the combustion residues of an unknown sample c (known as one or more of the samples a) by adopting a solvent extraction method, putting the sample in a beaker, adding n-hexane, putting the beaker into an ultrasonic cleaner, shaking the beaker for 10min, taking out the beaker, naturally evaporating the beaker to 0.5ml, extracting the beaker into a sample feeding bottle, and detecting the sample feeding amount of 0.1 mu l.
(2) GC-MS analysis conditions
The split ratio is 10: 1, He gas flow rate of 20mL/min, and pre-column pressure of 800 kpa. The column temperature was increased stepwise from 50 ℃ to 260 ℃. The specific process is as follows: firstly keeping the column temperature at 50 ℃ for 2min, then raising the column temperature to 150 ℃ at 10 ℃/min, keeping the column temperature at 2min, then raising the column temperature to 186 ℃ at 6 ℃/min, keeping the column temperature at 2min, finally raising the column temperature to 260 ℃ at 4 ℃/min, and keeping the column temperature at 2 min.
(3) Analysis of results
And analyzing by GC-MS (gas chromatography-mass spectrometry) self-contained software to obtain a total ion chromatogram of the combustion residue of the sample C, wherein the total ion chromatogram of the test analysis result is shown in figure 3, performing correlation analysis on the total ion chromatogram and a standard library chromatogram to find that the chromatogram contains a gasoline or styrene butadiene rubber characteristic component, and comparing the area ratio of three characteristic peaks of C2 benzene with the area ratio of the characteristic peak of the combustion residue of the sample b to find that the ratios are consistent, so that the main component of the sample C is gasoline. Wherein the ratio of the three characteristic peak areas of the combustion residue C2 benzene of the sample b and the average value are shown in Table 2, the average value of the three characteristic peak areas of the combustion residue C2 benzene of the sample C is shown in Table 3,
TABLE 2
TABLE 3
| Serial number | C2 benzene species | Peak area ratio average |
| 1 | Ethyl benzene | 0.39 |
| 2 | Para-meta-xylene | 1 |
| 3 | Ortho-xylene | 0.36 |
Example 2:
the treatment of the combustion residue of the unknown sample d (which is known to be one or more of the samples a) and the GC-MS analysis were carried out according to the procedure of example 1.
And (4) analyzing results: and analyzing by GC-MS self-contained software to obtain a sample d aromatic hydrocarbon extraction ion chromatogram shown in figure 4, carrying out correlation analysis on the extraction ion chromatogram of the test analysis result and a standard library chromatogram to find that the chromatogram contains gasoline or styrene butadiene rubber characteristic components, and comparing the average value of the area ratios of three characteristic peaks of C2 benzene with the characteristic peak area ratio of the combustion residue of styrene butadiene SBR 1712 in the sample a to find that the ratios are consistent, so that the sample d is styrene butadiene SBR 1712. Table 4 shows the average of the three characteristic peak-to-peak area ratios of the combustion residue C2 benzene of sample d.
TABLE 4
| Serial number | C2 benzene species | Peak area ratio |
| 1 | Ethyl benzene | 18.04 |
| 2 | Para-meta-xylene | 1 |
| 3 | Ortho-xylene | 1.85 |
The above-mentioned embodiments are only given for the purpose of more clearly illustrating the technical solutions of the present invention, and are not meant to be limiting, and variations of the technical solutions of the present invention by those skilled in the art based on the common general knowledge in the art are also within the scope of the present invention.
Claims (4)
1. A method for distinguishing components of combustion residues of gasoline and styrene butadiene rubber by using a GC-MS quantitative method is characterized by comprising the following steps:
the method comprises the following steps: in order to enable the environment of the experimental sample to be as close to a real fire scene as possible, the simulation experiment is carried out in a mode of igniting the experimental sample a and the experimental sample b in a crucible, and the method specifically comprises the following steps: respectively placing an experimental sample a and two experimental samples a in a crucible, igniting, and respectively taking combustion residues of the experimental samples a after the combustion is naturally extinguished; wherein the experimental sample a in the first step comprises one or more of organic substances containing styrene butadiene rubber and gasoline; the experimental sample b in the step one is gasoline;
step two: sample processing and instrument set-up
The method for treating the combustion residues of the experimental sample by adopting a solvent extraction method comprises the following steps: placing each experimental sample prepared in the step one in a beaker, adding n-hexane, placing the beaker in an ultrasonic cleaner, shaking the beaker for 10min, taking out the sample, naturally evaporating the sample to 0.5ml, and extracting the sample into a sample injection bottle for detection, wherein the sample injection amount is 0.1 mu l; setting analysis conditions of the gas chromatography-mass spectrometer for the combustion residues of the experimental sample a and the experimental sample b, namely the analysis conditions of each experimental sample of the GC-MS instrument;
step three: after the sample is processed in the second step, the extracted experimental sample enters a GC-MS instrument from an injection port, the experimental sample enters a mass spectrometer after being separated by a chromatographic column, different ions enter a mass analyzer and a detector after being ionized by an ion source, a detection signal is transmitted to a computer, the detection signal is processed by using data analysis software carried by the GC-MS instrument to obtain a total ion current chromatogram, the analysis of extracted ion peaks is carried out aiming at different characteristic components, and the identification and comparative analysis are carried out on each substance peak through a standard spectrum library;
step four: repeating the first step to the third step, and performing GC-MS analysis repeated tests on the combustion residues of the experimental sample a and the experimental sample b to obtain three groups of total ion current chromatograms;
step five: the similarity identification analysis of the styrene butadiene rubber combustion residue and the gasoline combustion residue total ion flow diagram specifically comprises the following steps: comparing and identifying each characteristic peak in the total ion current chromatogram with a standard spectrogram library, analyzing the types, names, molecular formulas and retention time of characteristic components of aromatic hydrocarbon and polycyclic aromatic hydrocarbon in the experimental sample, and judging whether the experimental sample contains one or two of gasoline combustion residues or butadiene styrene rubber combustion residues;
step six: an analysis method for distinguishing components of combustion residues of gasoline and styrene butadiene rubber by using a GC-MS quantitative method specifically comprises the following steps: if the experimental sample is analyzed and judged to contain one or two of gasoline combustion residues or styrene butadiene rubber combustion residues through the four steps, selecting three characteristic peaks of C2 benzene in the total ion current chromatogram, integrating the areas of the three characteristic peaks through data analysis software carried by a GC-MS instrument, or solving the peak value, and synthesizing data in the repeated test in the fourth step to obtain the average value of the area ratios of the three characteristic peaks, namely the ratio of the three kinds of C2 benzene; comparing the content ratios of three types of C2 benzene in the combustion residue of the experimental sample a and the combustion residue of a certain styrene butadiene rubber, and if the ratios are consistent, determining that the main component of the experimental sample a is the styrene butadiene rubber; comparing the content ratios of three types of C2 benzene in the combustion residue of the experimental sample a and the combustion residue of the experimental sample b, if the ratios are consistent, the main component of the experimental sample a can be proved to be gasoline, and if the ratios are inconsistent, the experimental sample a is proved to contain one or more organic matters in the styrene butadiene rubber.
2. The method of claim 1, wherein: the organic matter containing styrene butadiene rubber in the first step is specifically as follows: one or more of styrene-butadiene SBR1502, styrene-butadiene SBR 1712, styrene-butadiene SBR1502E, industrial styrene-butadiene cushion, thermoplastic styrene-butadiene rubber particle SBS, butadiene rubber BR9000, solution polymerized styrene-butadiene rubber SSBR 303 and thermoplastic styrene-butadiene rubber SBS 1401.
3. The method of claim 1, wherein: in the second step, the GC-MS instrument analysis conditions of the combustion residues of the experimental sample a and the experimental sample b are as follows: the split ratio is 10: 1, the flow rate of He gas is 20mL/min, and the pressure in front of the column is 800 kpa; the column temperature is increased to 260 ℃ in a step-like manner from 50 ℃, and the specific process is as follows: firstly keeping the column temperature at 50 ℃ for 2min, then raising the column temperature to 150 ℃ at 10 ℃/min, keeping the column temperature at 2min, then raising the column temperature to 186 ℃ at 6 ℃/min, keeping the column temperature at 2min, finally raising the column temperature to 260 ℃ at 4 ℃/min, and keeping the column temperature at 2 min.
4. The method of claim 1, wherein: the gasoline in the experimental sample a and the gasoline in the experimental sample b are both 92# gasoline.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113848268A (en) * | 2021-09-27 | 2021-12-28 | 中国人民警察大学 | Method for eliminating rubber interference gasoline identification by utilizing back propagation neural network method |
| CN113848268B (en) * | 2021-09-27 | 2024-03-08 | 中国人民警察大学 | Method for eliminating rubber interference gasoline identification by using back propagation neural network method |
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