CN109270193A - A kind of method that automatic headspace sampling-gas chromatography mass spectrometry measures volatile organic matter in polyvinyl alcohol - Google Patents
A kind of method that automatic headspace sampling-gas chromatography mass spectrometry measures volatile organic matter in polyvinyl alcohol Download PDFInfo
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- CN109270193A CN109270193A CN201811357396.XA CN201811357396A CN109270193A CN 109270193 A CN109270193 A CN 109270193A CN 201811357396 A CN201811357396 A CN 201811357396A CN 109270193 A CN109270193 A CN 109270193A
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- polyvinyl alcohol
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- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 34
- 239000005416 organic matter Substances 0.000 title claims abstract description 19
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 title claims abstract description 14
- 238000005259 measurement Methods 0.000 claims abstract description 13
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000002347 injection Methods 0.000 claims abstract description 4
- 239000007924 injection Substances 0.000 claims abstract description 4
- 238000004090 dissolution Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 230000003068 static effect Effects 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 14
- 238000005070 sampling Methods 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 230000008676 import Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 238000002203 pretreatment Methods 0.000 abstract description 4
- 239000000470 constituent Substances 0.000 abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 238000004458 analytical method Methods 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 210000004907 gland Anatomy 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229960001866 silicon dioxide Drugs 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 230000003694 hair properties Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000003859 hyphenated technique Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- SQYNKIJPMDEDEG-UHFFFAOYSA-N paraldehyde Chemical compound CC1OC(C)OC(C)O1 SQYNKIJPMDEDEG-UHFFFAOYSA-N 0.000 description 1
- 229960003868 paraldehyde Drugs 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Classifications
-
- 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
- G01N30/24—Automatic injection systems
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8804—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 automated systems
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
- G01N2030/885—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds involving polymers
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- 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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses the methods of volatile organic matter in a kind of automatic headspace sampling-gas chromatography mass spectrometry measurement polyvinyl alcohol, and sample is placed in container first, solvent is added, dissolution is uniformly mixed；Then Static Headspace method is used, heating evaporates volatile component from sample, reaches biphase equilibrium；Then ml headspace bottle upper gas injection gas chromatograph is separated, mass detector is finally imported and carries out qualitative analysis.The present invention detects volatile organic matter in polyvinyl alcohol using HS-GC/MS, sample pre-treatments are simple, and method is effective and rapid, and qualitative results are accurate, the blank of volatile organic matter full constituent qualitative analysis in polyvinyl alcohol has been filled up, the promotion of polyvinyl alcohol product quality can be more effectively instructed.
Description
Technical field
The present invention relates to volatility in a kind of automatic headspace sampling (HS)-gas chromatography mass spectrometry (GC-MS) measurement polyvinyl alcohol to have
The method of machine object belongs to detection and analysis technical field.
Background technique
Polyvinyl alcohol is a kind of water soluble polymer, it is caused through initiator poly- using vinyl acetate as monomer
Be combined into polyvinyl acetate, then with alkali (prepare) that the processes such as catalyzed alcoholysis, crushing, squeezing, drying are process with methanol it is cotton-shaped,
Sheet or granular solids.
The entire production technology of polyvinyl alcohol is complicated, and raw material is brought into and subsequent reactions generate plurality of impurities, seriously affects poly-
The characteristics such as the degree of polymerization, the degree of staining of vinyl alcohol, especially organic volatile impurities such as methanol, acetone etc. have certain toxicity and
Penetrating odor, can storage to polyvinyl alcohol product, use environment pollutes and security risk.Therefore, it is necessary to establish phase
The method answered measures organic volatile component in PVA, preferably to instruct process modification, to promote product quality.
Currently, the method for volatile component is mainly gas chromatography or low-polarity components in measurement high molecular material.
Headspace technique uses gas direct injected, extracts without organic solvent, interferes small, obtained spectrogram letter small to chromatographic column pollution
It is single, clean, it is one of the preferred method for analyzing volatile component.Unite States Standard ASTM D4526-1996 uses headspace gas color
Spectrometry measures the volatile component in polymer, and the standard of most of automobile interior decoration volatile component measurements also uses head space-gas
Phase chromatography, for example, VDA277 PV3341 etc., but this method is mainly used for quantitative point of volatile component in high molecular material
Analysis, qualitative analysis have some limitations, for example carry out qualitative, complicated for operation, low efficiency and knot by addition standard substance
Fruit reliability is still to be tested.Herein using waving in HS GC mass spectrometric hyphenated technique qualitative determination polyvinyl alcohol sample
Hair property component combines head space-low-polarity components advantage, and analysis efficiency height, wide coverage, detection limit is low, result is quasi-
True property is high, easy to operate, the blank of volatile organic matter full constituent qualitative analysis in polyvinyl alcohol has been filled up, for Product Process
There is the directive significance of reality with the improvement of formula, while also laying a good foundation for quantitative determination volatile component.
Summary of the invention
The object of the present invention is to provide volatile organic matters in a kind of automatic headspace sampling-gas chromatography mass spectrometry measurement polyvinyl alcohol
Method, this method is easy to operate, quick, qualitative results are accurate and reliable.
The method of volatile organic matter in automatic headspace sampling of the present invention-gas chromatography mass spectrometry measurement polyvinyl alcohol, without
Sample pre-treatments, directly take detection sample, real-time detection, are heated and are balanced using automatic headspace sample injector, after reaching balance, head space into
Sample (takes upper air body injection gas chromatograph in ml headspace bottle to be separated), and mass spectrograph is entered after separation and is detected, using group
Dtex levies mass spectrogram and the comparison of NIST standard spectrum library carries out composition analysis.
The method of volatile organic matter in automatic headspace sampling of the present invention-gas chromatography mass spectrometry measurement polyvinyl alcohol, first by sample
Product are placed in container, and solvent is added, and dissolution is uniformly mixed；Then Static Headspace method is used, heating makes volatile component from sample
In evaporate, reach biphase equilibrium；Then ml headspace bottle upper gas injection gas chromatograph is separated, finally imports matter
It composes detector and carries out qualitative analysis.Specifically comprise the following steps:
Step 1: 0.2g polyvinyl alcohol sample is weighed, is put into 20mL ml headspace bottle, addition 2mLN, N- dimethyl acetamide,
It covers silicagel pad and aluminium lid and is sealed against with gland device, ml headspace bottle is put into sample disc designated position according to requirement of experiment, push up
Empty bottle is in 90 DEG C of balance 45min, and 100 DEG C of quantitative loop temperature, 110 DEG C of transmission line temperature, sampling volume 1mL, using Agilent
7697 automatic headspace sample injector sample introductions；
Step 2: sample being divided using Agilent CP-Wax 52CB (50m × 0.32mm × 1.2um) chromatographic column
From column temperature: 52~200 DEG C, initial temperature retains 5min since 52 DEG C, then is warming up to 110 DEG C with 15 DEG C/min, retains 3min, most
200 DEG C of reservation 5min are warming up to 60 DEG C/min afterwards.Carrier gas: helium (purity is greater than 99.999%)；Flow velocity: 1.5mL/min；Point
Stream ratio 20:1；200 DEG C of injector temperature.
Step 3: volatile organic matter in polyvinyl alcohol being examined using Agilent 7890A-5977B gas chromatograph-mass spectrometer
Survey analysis, MS condition: the source EI: 70eV；220 DEG C of transmission line；250 DEG C of ion source；150 DEG C of quadrupole rod；Scanning mode: full scan；
Mass scan range m/z 10~300；Solvent delay 3min；Detector setting is closed after 14.5min.
Step 4: being compared using component characteristics mass spectrogram and NIST standard spectrogram, carry out qualitative analysis.
Wherein, 90 DEG C of head-space sampler platform temperature, balance 45min, 100 DEG C of quantitative loop temperature, transfer tube temperature 110
DEG C, sampling volume 1mL.
The present invention detects volatile organic matter in polyvinyl alcohol using HS-GC/MS, and sample pre-treatments are simple, side
Method is simple and quick, can effectively determine Volatile Organic Components in polyvinyl alcohol, extracts without organic solvent, pre-treatment letter
Single, qualitative results are accurate, the blank of volatile organic matter full constituent qualitative analysis in polyvinyl alcohol filled up, for Product Process
There is the directive significance of reality with the improvement of formula, while also laying a good foundation for quantitative determination volatile component.
Detailed description of the invention
Fig. 1 is volatile organic matter total ion chromatogram in polyvinyl alcohol 04-99 sample in the embodiment of the present invention 1.From
As can be seen that each component can be kept completely separate, and peak shape is preferable, be waved in the sample under the analysis condition that the present invention uses in Fig. 1
Hair property impurity composition type is more, from the point of view of table 1, in addition to the relatively high methyl acetate of content, methanol etc., in sample also
Detect acetaldehyde, methyl propionate, acetone and the 2- crotonaldehyde of trace.
Fig. 2 is volatile organic matter total ion chromatogram in polyvinyl alcohol 17-88 sample in the embodiment of the present invention 2.From
As can be seen that each group separating degree is preferable in sample in Fig. 2, peak shape is symmetrical, and from the point of view of table 2, methanol, acetic acid first are removed in the sample
Exceptionally, 9.250min has also appeared the fine impurity peaks of isobutyl to the groups such as ester, and still remains a small amount of acetone and para-acetaldehyde in sample.
Specific implementation method
Below with reference to specific embodiment, technical scheme is described further, these embodiments cannot understand
For the limitation to technical solution.
Embodiment 1:
The method of volatile organic matter is as follows in automatic headspace sampling-gas chromatography mass spectrometry measurement polyvinyl alcohol in the present embodiment:
1,0.2g polyvinyl alcohol 04-99 sample is weighed, is put into 20mL ml headspace bottle, addition 2mLN, N- dimethyl acetamide,
It covers silicagel pad and aluminium lid and is sealed against with gland device, ml headspace bottle is put into sample disc designated position according to requirement of experiment.
Automatic headspace sampling condition are as follows:
90 DEG C of head-space sampler platform temperature, balance 45min, 100 DEG C of quantitative loop temperature, 110 DEG C of transfer tube temperature, sample introduction
Volume is 1mL.
2, the sample after headspace sampling is analyzed using gas chromatograph-mass spectrometer (GC-MS), gas chromatograph-mass spectrometer (GC-MS) point
Analysis condition are as follows:
GC conditions: column temperature: initial temperature retains 5min since 52 DEG C, then is warming up to 110 DEG C with 15 DEG C/min, retains
3min is finally warming up to 200 DEG C of reservation 5min with 60 DEG C/min；Carrier gas: helium (purity is greater than 99.999%)；Flow velocity:
1.5mL/min；Split ratio 20:1；200 DEG C of injector temperature.
Mass Spectrometry Conditions: the source EI: 70eV；220 DEG C of transmission line；250 DEG C of ion source；150 DEG C of quadrupole rod；Scanning mode: it sweeps entirely
It retouches；Mass scan range m/z 10~300；Solvent delay 3min；Detector setting is closed after 14.5min.
Qualitative fashion: it is compared using component characteristics mass spectrogram and NIST standard spectrum library.
According to the method for volatile organic components in automatic headspace sampling-gas chromatography mass spectrometry measurement polyvinyl alcohol, polyethylene
The spectrogram of each volatile organic matter Gc-mss is as shown in Figure 1, qualitative results are as shown in table 1 in alcohol.
Volatile organic components qualitative results in 1 polyvinyl alcohol 04-99 sample of table
Embodiment 2:
The method of volatile organic matter is as follows in automatic headspace sampling-gas chromatography mass spectrometry measurement polyvinyl alcohol in the present embodiment:
1,0.2g polyvinyl alcohol 17-88 sample is weighed, is put into 20mL ml headspace bottle, addition 2mLN, N- dimethyl acetamide,
It covers silicagel pad and aluminium lid and is sealed against with gland device, ml headspace bottle is put into sample disc designated position according to requirement of experiment.
Automatic headspace sampling condition are as follows:
90 DEG C of head-space sampler platform temperature, balance 45min, 100 DEG C of quantitative loop temperature, 110 DEG C of transfer tube temperature, sample introduction
Volume is 1mL.
2, the sample after headspace sampling is analyzed using gas chromatograph-mass spectrometer (GC-MS), gas chromatograph-mass spectrometer (GC-MS) point
Analysis condition are as follows:
GC conditions: column temperature: initial temperature retains 5min since 52 DEG C, then is warming up to 110 DEG C with 15 DEG C/min, retains
3min is finally warming up to 200 DEG C of reservation 5min with 60 DEG C/min；Carrier gas: helium (purity is greater than 99.999%)；Flow velocity:
1.5mL/min；Split ratio 20:1；200 DEG C of injector temperature.
Mass Spectrometry Conditions: the source EI: 70eV；220 DEG C of transmission line；250 DEG C of ion source；150 DEG C of quadrupole rod；Scanning mode: it sweeps entirely
It retouches；Mass scan range m/z 10~300；Solvent delay 3min；Detector setting is closed after 14.5min.
Qualitative fashion: it is compared using component characteristics mass spectrogram and NIST standard spectrum library.
According to the method for volatile organic components in automatic headspace sampling-gas chromatography mass spectrometry measurement polyvinyl alcohol, polyethylene
The spectrogram of each volatile organic matter Gc-mss is as shown in Fig. 2, qualitative results are as shown in table 2 in alcohol.
Volatile organic components qualitative results in 2 polyvinyl alcohol 17-88 sample of table
Claims (5)
1. the method for volatile organic matter in a kind of automatic headspace sampling-gas chromatography mass spectrometry measurement polyvinyl alcohol, it is characterised in that: first
First sample is placed in container, solvent is added, dissolution is uniformly mixed；Then Static Headspace method is used, heating makes volatile component
It is evaporated from sample, reaches biphase equilibrium；Then ml headspace bottle upper gas injection gas chromatograph is separated, finally
It imports mass detector and carries out qualitative analysis.
2. according to the method described in claim 1, it is characterized by comprising following steps:
Step 1: weighing 0.2g polyvinyl alcohol sample, be put into 20mL ml headspace bottle, 2mLN, N- dimethyl acetamide, sealing is added
Ml headspace bottle is put into sample disc designated position afterwards, using 7697 automatic headspace sample injector sample introduction of Agilent；
Step 2: sample being separated using Agilent CP-Wax 52CB chromatographic column；
Step 3: volatile organic matter in polyvinyl alcohol being detected using Agilent 7890A-5977B gas chromatograph-mass spectrometer；
Step 4: being compared using component characteristics mass spectrogram and NIST standard spectrogram, carry out qualitative analysis.
3. according to the method described in claim 2, it is characterized by:
In step 1, ml headspace bottle is in 90 DEG C of balance 45min, and 100 DEG C of quantitative loop temperature, 110 DEG C of transmission line temperature, sampling volume is
1mL。
4. according to the method described in claim 2, it is characterized by:
In step 2, Agilent CP-Wax 52CB chromatographic column separation parameter is provided that column temperature: 52~200 DEG C, initial temperature is from 52
DEG C start to retain 5min, then be warming up to 110 DEG C with 15 DEG C/min, retains 3min, 200 DEG C of reservations are finally warming up to 60 DEG C/min
5min.Carrier gas: helium (purity is greater than 99.999%)；Flow velocity: 1.5mL/min；Split ratio 20:1；200 DEG C of injector temperature.
5. according to the method described in claim 2, it is characterized by:
In step 3, detection parameters are provided that MS condition: the source EI: 70eV；220 DEG C of transmission line；250 DEG C of ion source；Quadrupole rod
150℃；Scanning mode: full scan；Mass scan range m/z 10~300；Solvent delay 3min；14.5min later detector
Setting is closed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811357396.XA CN109270193B (en) | 2018-11-15 | 2018-11-15 | Method for measuring volatile organic compounds in polyvinyl alcohol by automatic headspace sample injection-gas chromatography-mass spectrometry |
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| CN112444617A (en) * | 2019-09-04 | 2021-03-05 | 中国石油化工股份有限公司 | Method for evaluating odor of polyolefin resin and use thereof |
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| CN112444617A (en) * | 2019-09-04 | 2021-03-05 | 中国石油化工股份有限公司 | Method for evaluating odor of polyolefin resin and use thereof |
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