CN114894932A - Method for detecting trace amount peculiar smell gas components in automobile textile fabric - Google Patents
Method for detecting trace amount peculiar smell gas components in automobile textile fabric Download PDFInfo
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- 239000004744 fabric Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 54
- 239000004753 textile Substances 0.000 title claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 40
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 20
- 238000001514 detection method Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000004458 analytical method Methods 0.000 claims description 9
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 7
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 6
- -1 divinylbenzene-polydimethylsiloxane Chemical class 0.000 claims description 5
- KRTXVCMNWAMYGT-UHFFFAOYSA-N [C].C(=C)C1=C(C=CC=C1)C=C Chemical compound [C].C(=C)C1=C(C=CC=C1)C=C KRTXVCMNWAMYGT-UHFFFAOYSA-N 0.000 claims description 3
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- 238000004949 mass spectrometry Methods 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 10
- 238000009825 accumulation Methods 0.000 abstract 1
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 14
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- 238000002347 injection Methods 0.000 description 10
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- 238000010586 diagram Methods 0.000 description 8
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- GTEXIOINCJRBIO-UHFFFAOYSA-N 2-[2-(dimethylamino)ethoxy]-n,n-dimethylethanamine Chemical compound CN(C)CCOCCN(C)C GTEXIOINCJRBIO-UHFFFAOYSA-N 0.000 description 6
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- 229910052734 helium Inorganic materials 0.000 description 4
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- 239000000463 material Substances 0.000 description 4
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- 239000000126 substance Substances 0.000 description 4
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- 230000004048 modification Effects 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- FEUFEGJTJIHPOF-UHFFFAOYSA-N 2-butyl acrylic acid Chemical compound CCCCC(=C)C(O)=O FEUFEGJTJIHPOF-UHFFFAOYSA-N 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
- UDSFAEKRVUSQDD-UHFFFAOYSA-N Dimethyl adipate Chemical compound COC(=O)CCCCC(=O)OC UDSFAEKRVUSQDD-UHFFFAOYSA-N 0.000 description 1
- MUXOBHXGJLMRAB-UHFFFAOYSA-N Dimethyl succinate Chemical compound COC(=O)CCC(=O)OC MUXOBHXGJLMRAB-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- RNOOHTVUSNIPCJ-UHFFFAOYSA-N butan-2-yl prop-2-enoate Chemical compound CCC(C)OC(=O)C=C RNOOHTVUSNIPCJ-UHFFFAOYSA-N 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 1
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- 239000012895 dilution Substances 0.000 description 1
- XTDYIOOONNVFMA-UHFFFAOYSA-N dimethyl pentanedioate Chemical compound COC(=O)CCCC(=O)OC XTDYIOOONNVFMA-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 150000005826 halohydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
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- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 230000008786 sensory perception of smell Effects 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
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- 125000003003 spiro group Chemical group 0.000 description 1
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
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- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
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Abstract
The invention discloses a method for detecting trace odor gas components in automobile textile fabric, which relates to the technical field of trace gas component detection and comprises the following steps: using CO 2 Constructing a polar extraction environment, increasing the pressure intensity of the extraction environment to 1-1.6 MPa, enriching the trace gas by using an extraction head, detecting and analyzing by using a gas chromatography-mass spectrometry combined method, detecting at least three times by using the gas chromatography-mass spectrometry combined method, and accumulating and superposing detection signals. The invention effectively adsorbs and desorbs trace organic matters and tests the peak intensity of a signalThe accumulation of (2) can more accurately measure trace peculiar smell organic matters in the textile fabric.
Description
Technical Field
The invention relates to the technical field of trace gas component detection, in particular to a method for detecting trace peculiar smell gas components in an automobile textile fabric.
Background
With the increasing environmental awareness and self-protection awareness of people, the air quality in the vehicle environment directly related to the health of people is concerned more and more. Various adhesive materials, seat cushion fabrics and the like used for automotive interior trims can slowly and durably release trace volatile peculiar smell organic matters such as benzene series, halohydrocarbon, aldehyde ketone and the like, particularly, the interior temperature of an automobile is higher, the environment is more complex, the requirements of people on the concentration and the main components of peculiar smell in the automotive textile fabric are stricter under the condition, and the health of people is seriously harmed. How to rapidly and accurately detect trace amount of peculiar smell gas components in the textile fabric for the automobile relates to the control and reduction of the automobile manufacturer on the peculiar smell in the environment in the automobile, can also provide technical support for market supervision departments, and has great practical significance.
At present, the peculiar smell of the textile fabric for the automotive interior is mainly evaluated by a man-made olfaction method, and the textile fabric is greatly influenced by subjective factors and has poor stability. In addition, researchers can qualitatively and quantitatively determine odor compounds of the textile fabric by a gas chromatography-mass spectrometry combined method, although the method is objective, the content and concentration of a plurality of volatile odor organic matters in the odor are low, the trace organic matters in the odor are difficult to detect by the existing method and are often ignored by people, and the health of the body is seriously injured. In addition, some researchers use a liquid phase extraction method to extract organic matters from the fabric for detection and analysis, and as the purity of organic or inorganic extraction liquid used by the extraction method is usually less than 100%, the system contains a very small amount of other substances, and the volume of the required extraction liquid is large, volatile odor organic matters in the fabric extracted into the extraction liquid are infinitely diluted, and meanwhile, environmental pollution is caused; these factors pose great difficulty in accurately detecting trace volatile odor organic compounds in the fabric. It is worth to be noted that, in the existing method for determining the odor compound components of the textile fabric by using the gas chromatography-mass spectrometer, the volatile odor compound is detected only once, and the collected signals are easily covered by the miscellaneous peaks and are also easily submerged by the strong signal peaks, so that part of trace organic matters are omitted and ignored, and the detection is inaccurate.
Therefore, how to detect the trace amount of odor gas components in the textile fabric and establish a sensitive, accurate, efficient and objective detection method becomes a problem to be solved urgently at present.
Disclosure of Invention
The invention aims to provide a sensitive, accurate, efficient and objective method for detecting trace odor gas components in automobile textile fabric aiming at the defects of the prior art.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a method for detecting trace amount of peculiar smell gas components in textile fabric for an automobile, which comprises the following steps: using CO 2 The method comprises the steps of constructing a polar extraction environment, increasing the pressure intensity of the extraction environment to 1-1.6 MPa, completely extracting trace volatile peculiar smell organic matters in the fabric, using an extraction head to enrich trace gas, then using a gas chromatography-mass spectrometry combined method to perform detection and analysis, using the gas chromatography-mass spectrometry combined method to perform at least three times of detection, and accumulating and superposing detection signals.
In the detection method of the present invention, CO is first constructed 2 Polar extraction environment, these CO 2 Molecules can enter the gaps of the fibers, volatile peculiar smell organic matters adsorbed in the gaps of the fibers are almost polar gases, and the trace polar gases can be dissolved in CO 2 In the extraction system constructed by gas, thereby extracting the volatile peculiar smell organic matters adsorbed in the fiber gaps into the closed environment of the reactor, and in addition, CO is added into the extraction environment by changing 2 The content of the gas can effectively adjust the air pressure in the extraction system and increase the effective extraction of volatile peculiar smell organic matters adsorbed in fiber gaps; on the other hand, after the extraction head in the extraction system reaches adsorption balance, gas chromatography mass spectrometry detection analysis is carried out on the extraction head, volatile odor organic matters adsorbed in the extraction head can be completely released through the desorption process for 3 times, then detection signals are acquired for 3 times, the signal peak intensity acquired for 3 times is accumulated, and the original unobservable weak peaks of the trace organic matters are accumulated into a stronger peak, so that the trace odor gas in the textile fabric is more accurately detected and analyzed.
Further, the application temperature is increased to 50 ℃ at a heating rate of 5 ℃/min, and is kept for 10-20 minutes, and then is increased to 80 ℃ at a heating rate of 2 ℃/min, and is kept for 10-20 minutes.
Further, the extraction head is 30 micron divinylbenzene-carbon molecular sieve-polydimethylsiloxane, 65 micron divinylbenzene-polydimethylsiloxane, 75 micron carbon molecular sieve-polydimethylsiloxane, or 100 micron polydimethylsiloxane.
Further, in the enrichment process, the ambient temperature is reduced to 20-35 ℃ at a cooling rate of 3-5 ℃/min.
Further, after the enrichment is finished, taking out the extraction head, and desorbing for 2-4 minutes at 230-260 ℃.
Further, the extraction head is repeatedly desorbed for 1-3 times, and the gas chromatography-mass spectrometry method is continuously used for analysis.
Further, the parameters of the gas chromatography-mass spectrometry combined method are as follows: the temperature rise program is that the temperature is preserved for 10min at 50 ℃, and then the temperature is raised to 250 ℃ at the temperature rise rate of 10 ℃/min; the chromatographic column is Rtx-5ms (30m × 0.25um × 0.25 um); the carrier gas was high purity helium (99.9999%), column flow: 1.5 mL/min; the sample injection mode is divided sample injection, and the division ratio is 10: 1; EI source with voltage of 70eV and temperature of 200 ℃; the temperature of a sample inlet is 250 ℃; quadrupole temperature 150 ℃, scanning mode: q3 Scan m/z is 25.00-250.00.
The invention discloses the following technical effects:
according to the invention, trace volatile peculiar smell organic matters which are difficult to detect in the textile fabric are extracted by a high-pressure gas-phase extraction method for detection and analysis; the volatile odorous organic compounds are almost all polar gases, and CO is used 2 The method comprises the steps of constructing a polar extraction environment, increasing the pressure intensity of the extraction environment, completely extracting trace volatile odor organic matters in the fabric, then adsorbing by an extraction head, and then detecting and analyzing by using a gas chromatography-mass spectrometer, detecting by using the gas chromatography-mass spectrometer for multiple times through multiple adsorption-desorption processes, accumulating and superposing multiple detection signals, so that the peak intensity of the trace organic matters is increased, the analysis of the trace organic matters is greatly facilitated, and the trace odor gas in the textile fabric is more accurately detected and analyzed. Wherein CO is 2 The gas is used as a solvent, is non-toxic and harmless, and no other impurities are introduced into the test system. In addition, trace odor organic matters in the textile fabric can be more accurately tested by effectively adsorbing and desorbing the trace organic matters and accumulating the peak intensity of the test signal.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a total ion flow diagram of the main odor-emitting components of the automobile interior fabric of example 1, in which 1-cyclopentanone, 2-butylacrylate, 3-1, 4-dioxaspiro [4.4] -nonane, 4-phenol, dimethyl 5-succinate, 6-nonanal, dimethyl 7-glutarate, 8-decanal, dimethyl 9-adipate, 10-lauryl/dodecanol, 11-2, 6-di-tert-butyl-p-cresol, 12-bis (dimethylaminoethyl) ether;
FIG. 2 is a total ion flow graph of the odor-emitting principle component of the automobile interior fabric of example 2, wherein 1-nonanal, 2-bis (dimethylaminoethyl) ether;
FIG. 3 is a total ion flow diagram of the main odor-emitting components of the automobile interior fabric of example 3, in which 1-cyclopentanone, butyl 2-acrylate, 3-1, 4-dioxaspiro [4.4] -nonane, 4-phenol, dimethyl 5-succinate, 6-nonanal, dimethyl 7-glutarate, 8-decanal, dimethyl 9-adipate, 10-lauryl/dodecanol, 11-2, 6-di-tert-butyl-p-cresol, and 12-bis (dimethylaminoethyl) ether;
FIG. 4 is a total ion flow diagram for testing volatile odorous organic compounds in a liquid phase extraction textile fabric of comparative example 1;
FIG. 5 is a total ion flow diagram of a test for heating and extracting volatile odorous organic compounds in a textile fabric in comparative example 2;
fig. 6 is a total ion flow diagram of major components emitting an offensive odor of the automobile interior fabric of comparative example 3, in which 1-cyclopentanone, dimethyl 2-succinate, dimethyl 3-glutarate, dimethyl 4-adipate, 5-lauryl alcohol/lauryl alcohol, and 6-2, 6-di-t-butyl-p-cresol.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every intervening value, to the extent any stated or intervening value in a stated range, and every other stated or intervening value in that stated range, is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including but not limited to.
Example 1
0.1g of a textile fabric for automobile interior was placed in a reactor, and vacuum was applied, followed by charging CO in the reactor 2 Gas so that the reactor is filled with CO 2 Gas, and the pressure in the reactor reaches 1.3MPa, and the reactor is sealed. And then heating the reactor to 50 ℃ at the heating rate of 5 ℃/min, preserving the heat for 15 min, heating to 80 ℃ at the heating rate of 2 ℃/min, and preserving the heat for 20 min, so that the trace gas in the fabric is fully volatilized into the reactor. Then, 30-micron divinylbenzene-carbon molecular sieve-polydimethylsiloxane with an extraction head arranged in the reactor is used for enriching the trace gas in the reactor, the ambient temperature in the reactor is reduced to 30 ℃ at the cooling rate of 3 ℃/min in the enriching process, the extraction head is taken out and then desorbed for 4 min at the temperature of 240 ℃, and then the analysis is carried out by adopting a gas chromatography-mass spectrometry combined method. And (3) repeatedly desorbing the extraction head for 3 times, continuously analyzing by using a gas chromatography-mass spectrometry combined method, acquiring gas chromatography-mass spectrometry signals for 3 times, accumulating the signal intensity of each substance, and determining the trace odor gas component in the textile fabric according to each retention time in the map after the signal intensity is finally accumulated. Wherein the parameters of the gas chromatography-mass spectrometry combined method are as follows: the temperature rise program is that the temperature is preserved for 10min at 50 ℃, and then the temperature is raised to 250 ℃ at the temperature rise rate of 10 ℃/min; the chromatographic column is Rtx-5ms (30m × 0.25um × 0.25 um); the carrier gas was high purity helium (99.9999%), column flow: 1.5 mL/min; the sample injection mode is divided sample injection, and the division ratio is 10: 1; EI source with voltage of 70eV and temperature of 200 ℃; the injection port temperature is 250 ℃; quadrupole temperature 150 ℃, scanning mode: q3 Scan m/z is 25.00-250.00.
Fig. 1 shows a total ion flow diagram of main components of the peculiar smell emitted by the automobile interior fabric, and 12 main components of the peculiar smell emitted by the automobile interior fabric can be accurately analyzed by the method, wherein the main components are cyclopentanone, butyl acrylate, 1, 4-dioxyspiro [4.4] -nonane, phenol, dimethyl succinate, nonanal, dimethyl glutarate, decanal, dimethyl adipate, lauryl alcohol/lauryl alcohol, 2, 6-di-tert-butyl-p-cresol and bis (dimethylaminoethyl) ether.
Example 2
Same procedure as in example 1, except for changing the CO addition 2 The amount of gas was such that the pressure in the reactor was 1.0MPa, the results being shown in FIG. 2. From fig. 2, it can be seen that 2 main components of the odor emitted from the interior fabric of the automobile, which can be analyzed by the method of comparative example 3, are 1-nonanal and 2-bis (dimethylaminoethyl) ether, respectively.
Example 3
Same procedure as in example 1, except for changing the CO addition 2 The amount of gas was such that the pressure in the reactor was 1.6MPa, the results are shown in FIG. 3. From fig. 3, it can be seen that, in accordance with the results of example 1, the method of example 3 can analyze that 12 main components of the odor emitted from the interior fabric of the automobile are 1-cyclopentanone, 2-butyl acrylate, and 3-1, 4-dioxaspiro [4.4] spiro [ 1, 2-butyl acrylate ], respectively]Nonane, 4-phenol, dimethyl 5-succinate, 6-nonanal, dimethyl 7-glutarateEster, 8-decanal, 9-adipic acid dimethyl ester, 10-lauryl alcohol/dodecanol, 11-2, 6-di-tert-butyl-p-cresol, 12-bis (dimethylaminoethyl) ether.
Comparative example 1
Placing 0.1g of the textile fabric for the automotive interior in 30 ml of ethanol solution with the mass concentration of 99.7%, sealing, keeping the temperature for 2h under the conditions of magnetic stirring at the rotating speed of 300 revolutions per minute and 50 ℃, and analyzing the ethanol extract by using a gas chromatography-mass spectrometry method, wherein the parameters of the gas chromatography-mass spectrometry method are as follows: the temperature rise program is that the temperature is preserved for 10min at 50 ℃, and then the temperature is raised to 250 ℃ at the temperature rise rate of 10 ℃/min; the chromatographic column is Rtx-5ms (30m × 0.25um × 0.25 um); the carrier gas was high purity helium (99.9999%), column flow: 1.5 mL/min; the sample injection mode is divided sample injection, and the division ratio is 10: 1; EI source with voltage of 70eV and temperature of 200 ℃; the temperature of a sample inlet is 250 ℃; quadrupole temperature 150 ℃, scanning mode: q3 Scan m/z 25.00-250.00. The total ion flow diagram of the liquid phase extraction textile fabric volatile odor organic matter test is shown in fig. 4. As a result, it was found that no organic matter was detected in the chromatogram of fig. 4, because more extraction liquid was required in the process of extracting organic matter from the textile fabric, which resulted in infinite dilution of volatile odorous organic matter in the fabric extracted into the extraction liquid, exceeding the detection limit of the test equipment and system.
Comparative example 2
0.1g of the textile fabric for automobile interior decoration was placed in a closed reactor, and the pressure in the reactor was kept at normal pressure, and sealed. And then heating the reactor to 50 ℃ at the heating rate of 5 ℃/min, preserving the heat for 15 min, heating to 80 ℃ at the heating rate of 2 ℃/min, and preserving the heat for 20 min, so that the trace gas in the fabric is fully volatilized into the reactor. And then analyzing the air in the reactor by using a gas chromatography-mass spectrometry method, wherein the parameters of the gas chromatography-mass spectrometry method are as follows: the temperature rise program is that the temperature is preserved for 10min at 50 ℃, and then the temperature is raised to 250 ℃ at the temperature rise rate of 10 ℃/min; the chromatographic column is Rtx-5ms (30m × 0.25um × 0.25 um); the carrier gas was high purity helium (99.9999%), column flow: 1.5 mL/min; the sample injection mode is divided sample injection, and the division ratio is 10: 1; EI source with voltage of 70eV and temperature of 200 ℃; the injection port temperature is 250 ℃; quadrupole temperature 150 ℃, scanning mode: q3 Scan m/z is 25.00-250.00. The total ion flow diagram of the test of heating and extracting volatile odor organic compounds in the textile fabric is shown in fig. 5.
From FIG. 5, no signal peak belonging to organic substances could be found. This indicates that the trace organic substances in the textile fabric cannot be effectively extracted by using the traditional heating method, and cannot be effectively detected and analyzed.
Through comparison of test results of examples 1-3 and comparative example 2, it is found that CO is added 2 After the gas is generated, the peculiar smell volatile gas adsorbed in the automobile interior fabric can be effectively extracted into a reaction system, and the components of the gas can be detected; furthermore, by changing CO 2 The pressure intensity in the reactor is changed by the adding amount of the gas, so that various peculiar smell volatile gases can be extracted into the reaction system and can be detected more accurately.
Comparative example 3
The same procedure as in example 1 was followed except that the number of times of collecting the GC-MS signal was changed to 1, and the results are shown in FIG. 6. As can be seen from fig. 6, when only 1 gc-ms signal is collected, 6 main components, which are 1-cyclopentanone, dimethyl 2-succinate, dimethyl 3-glutarate, dimethyl 4-adipate, 5-lauryl alcohol/lauryl alcohol, and 6-2, 6-di-t-butyl-p-cresol, can be analyzed for the odor emitted from the interior fabric of an automobile by the method of comparative example 3.
According to the results of the embodiment 1 and the comparative example 3, the fact that the superposed detection signal intensity can be accumulated by increasing the acquisition times of the gas chromatography-mass spectrum signal is found, so that the peak intensity of trace organic matters is increased, the analysis of the trace organic matters is greatly facilitated, and the trace odor gas in the textile fabric is more accurately detected and analyzed.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (7)
1. A method for detecting trace amount of peculiar smell gas components in textile fabric for automobiles is characterized by comprising the following steps: using CO 2 Constructing a polar extraction environment, increasing the pressure intensity of the extraction environment to 1-1.6 MPa, enriching the trace gas by using an extraction head, detecting and analyzing by using a gas chromatography-mass spectrometry combined method, detecting at least three times by using the gas chromatography-mass spectrometry combined method, and accumulating and superposing detection signals.
2. The method for detecting the trace odor gas components in the automobile textile fabric according to claim 1, wherein the applying temperature is increased to 50 ℃ at a heating rate of 5 ℃/min, and is kept for 10-20 minutes, and then increased to 80 ℃ at a heating rate of 2 ℃/min, and is kept for 10-20 minutes.
3. The method for detecting the trace odorous gas components in the textile fabric for the automobiles as claimed in claim 1, wherein the extraction head is 30 microns of divinylbenzene-carbon molecular sieve-polydimethylsiloxane, 65 microns of divinylbenzene-polydimethylsiloxane, 75 microns of carbon molecular sieve-polydimethylsiloxane or 100 microns of polydimethylsiloxane.
4. The method for detecting the trace amount of the odor gas components in the automobile textile fabric according to claim 1, wherein the ambient temperature is reduced to 20-35 ℃ at a cooling rate of 3-5 ℃/min in the enrichment process.
5. The method for detecting the trace amount of the odor gas components in the automobile textile fabric according to claim 1, wherein after the enrichment is finished, the extraction head is taken out and desorbed for 2-4 minutes at 230-260 ℃.
6. The method for detecting the trace odorous gas components in the automobile textile fabric is characterized in that the extraction head is desorbed repeatedly for 1-3 times, and the analysis is carried out by continuously using a gas chromatography-mass spectrometry combined method.
7. The method for detecting the trace odor gas components in the automobile textile fabric according to claim 1, characterized in that a scanning mode of a mass spectrometry method is Q3 Scan m/z 25.00-250.00, and the voltage is 70 eV.
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