CN109270193B - Method for measuring volatile organic compounds in polyvinyl alcohol by automatic headspace sample injection-gas chromatography-mass spectrometry - Google Patents
Method for measuring volatile organic compounds in polyvinyl alcohol by automatic headspace sample injection-gas chromatography-mass spectrometry Download PDFInfo
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- CN109270193B CN109270193B CN201811357396.XA CN201811357396A CN109270193B CN 109270193 B CN109270193 B CN 109270193B CN 201811357396 A CN201811357396 A CN 201811357396A CN 109270193 B CN109270193 B CN 109270193B
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- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 39
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000012855 volatile organic compound Substances 0.000 title claims abstract description 24
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 title claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000001819 mass spectrum Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 230000003068 static effect Effects 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- 238000002347 injection Methods 0.000 claims description 11
- 239000007924 injection Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 238000005070 sampling Methods 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
- 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
- 238000007789 sealing Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 3
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 claims description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 2
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 claims description 2
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 claims description 2
- LRDFRRGEGBBSRN-UHFFFAOYSA-N isobutyronitrile Chemical compound CC(C)C#N LRDFRRGEGBBSRN-UHFFFAOYSA-N 0.000 claims description 2
- 229940017219 methyl propionate Drugs 0.000 claims description 2
- SQYNKIJPMDEDEG-UHFFFAOYSA-N paraldehyde Chemical compound CC1OC(C)OC(C)O1 SQYNKIJPMDEDEG-UHFFFAOYSA-N 0.000 claims description 2
- 229960003868 paraldehyde Drugs 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 claims 2
- 229940022682 acetone Drugs 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000004458 analytical method Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000741 silica gel Substances 0.000 description 4
- 229910002027 silica gel Inorganic materials 0.000 description 4
- 238000004817 gas chromatography Methods 0.000 description 3
- 238000011067 equilibration Methods 0.000 description 2
- 238000003988 headspace gas chromatography Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035943 smell Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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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
- G01N30/24—Automatic injection systems
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—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
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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
- G01N30/88—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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Abstract
The invention discloses a method for measuring volatile organic compounds in polyvinyl alcohol by automatic headspace sample injection-gas chromatography-mass spectrometry, which comprises the steps of firstly placing a sample in a container, adding a solvent, and dissolving and mixing uniformly; then heating by adopting a static headspace method to volatilize the volatile components from the sample so as to reach two-phase balance; and injecting the gas at the upper part of the headspace bottle into a gas chromatograph for separation, and finally introducing the gas into a mass spectrum detector for qualitative analysis. The method adopts HS-GC/MS to detect the volatile organic compounds in the polyvinyl alcohol, has simple sample pretreatment, quick and effective method and accurate qualitative result, fills the blank of qualitative analysis of all components of the volatile organic compounds in the polyvinyl alcohol, and can more effectively guide the improvement of the quality of the polyvinyl alcohol product.
Description
Technical Field
The invention relates to a method for determining volatile organic compounds in polyvinyl alcohol by automatic Headspace Sampling (HS) -gas chromatography-mass spectrometry (GC-MS), belonging to the technical field of detection and analysis.
Background
Polyvinyl alcohol is a water-soluble high-molecular polymer, which is a flocculent, flaky or granular solid prepared by using vinyl acetate as a monomer, initiating polymerization by an initiator to obtain polyvinyl acetate, and then using alkali (prepared by methanol) to catalyze alcoholysis, crushing, squeezing, drying and the like.
The whole production process of the polyvinyl alcohol is complex, various impurities are brought by raw materials and generated in subsequent reactions, the characteristics of the polyvinyl alcohol such as polymerization degree, coloring degree and the like are seriously influenced, and especially organic volatile impurities such as methanol, acetone and the like have certain toxic and pungent smells, so that the storage and use environment of the polyvinyl alcohol product are polluted and potential safety hazards are caused. Therefore, it is necessary to establish a corresponding method for determining the volatile organic components in PVA, so as to better guide the process improvement and improve the product quality.
At present, the method for measuring volatile components in high molecular materials mainly adopts gas chromatography or gas chromatography-mass spectrometry technology. The headspace technology adopts gas direct injection, does not need organic solvent extraction, has small interference and small pollution to chromatographic columns, and obtains simple and clean spectrogram, which is one of the preferred methods for analyzing volatile components. The American standard ASTM D4526-1996 adopts headspace gas chromatography to measure volatile components in polymers, and most standards for measuring volatile components in automotive interiors also adopt headspace gas chromatography, such as VDA277\ PV3341 and the like, but the method is mainly used for quantitative analysis of volatile components in high molecular materials, and the qualitative analysis has certain limitations, such as qualitative analysis by adding standard substances, complex operation, low efficiency and yet to be verified result reliability. The method adopts the headspace-gas chromatography-mass spectrometry combined technology to qualitatively determine the volatile components in the polyvinyl alcohol sample, combines the advantages of the headspace-gas chromatography-mass spectrometry combined technology, has high analysis efficiency, wide coverage range, low detection limit, high result accuracy and simple and convenient operation, fills the blank of all-component qualitative analysis of volatile organic compounds in the polyvinyl alcohol, has practical guiding significance for the improvement of product technology and formula, and lays a foundation for quantitatively determining the volatile components.
Disclosure of Invention
The invention aims to provide a method for measuring volatile organic compounds in polyvinyl alcohol by automatic headspace sampling-gas chromatography-mass spectrometry, which is simple and rapid to operate and has accurate and reliable qualitative results.
The method for determining volatile organic compounds in polyvinyl alcohol by automatic headspace sampling-gas chromatography-mass spectrometry has the advantages that the detection sample is directly taken without sample pretreatment, the detection sample is detected in real time, an automatic headspace sampler is used for heating and balancing, after the balance is achieved, headspace sampling (the upper air in a headspace bottle is injected into a gas chromatograph for separation), the headspace sampling enters a mass spectrometer for detection after the separation, and the composition analysis is carried out by comparing a component characteristic mass spectrogram with an NIST standard library.
The invention relates to a method for measuring volatile organic compounds in polyvinyl alcohol by automatic headspace sampling-gas chromatography-mass spectrometry, which comprises the steps of firstly placing a sample in a container, adding a solvent, and dissolving and mixing uniformly; then heating by adopting a static headspace method to volatilize the volatile components from the sample so as to reach two-phase balance; and injecting the gas at the upper part of the headspace bottle into a gas chromatograph for separation, and finally introducing the gas into a mass spectrum detector for qualitative analysis. The method specifically comprises the following steps:
step 1: weighing 0.2g of polyvinyl alcohol sample, putting the polyvinyl alcohol sample into a 20mL headspace bottle, adding 2mLN, N-dimethylacetamide, covering a silica gel pad and an aluminum cover, sealing the silica gel pad and the aluminum cover by using a capping device, putting the headspace bottle into a specified position of a sample tray according to experimental requirements, balancing the headspace bottle at 90 ℃ for 45min, quantitatively circulating the temperature of 100 ℃, the transmission line temperature of 110 ℃, and the sample injection volume of 1mL, and injecting the sample by using an Agilent 7697 automatic headspace sample injector;
step 2: the sample was separated using an Agilent CP-Wax 52CB (50 m.times.0.32 mm. times.1.2 um) column, column temperature: keeping the initial temperature at 52-200 ℃ for 5min from 52 ℃, then heating to 110 ℃ at 15 ℃/min, keeping for 3min, and finally heating to 200 ℃ at 60 ℃/min, and keeping for 5 min. Carrier gas: helium (purity greater than 99.999%); flow rate: 1.5 mL/min; the split ratio is 20: 1; the injection port temperature was 200 ℃.
And step 3: detecting and analyzing volatile organic compounds in polyvinyl alcohol by adopting an Agilent 7890A-5977B gas chromatograph-mass spectrometer, wherein the MS conditions are as follows: EI source: 70 eV; a transmission line is 220 ℃; an ion source of 250 ℃; a quadrupole rod is 150 ℃; the scanning mode is as follows: full scanning; the mass scanning range m/z is 10-300; delaying the solvent for 3 min; after 14.5min the detector is set off.
And 4, step 4: and comparing the component characteristic mass spectrogram with an NIST standard spectrogram to perform qualitative analysis.
Wherein the temperature of the headspace sample injector platform is 90 ℃, the balance time is 45min, the quantitative loop temperature is 100 ℃, the temperature of the transmission tube is 110 ℃, and the sample injection volume is 1 mL.
The method adopts HS-GC/MS to detect the volatile organic compounds in the polyvinyl alcohol, has simple sample pretreatment, simple and quick method, can effectively determine the components of the volatile organic compounds in the polyvinyl alcohol, does not need organic solvent extraction, has simple pretreatment and accurate qualitative result, fills the blank of qualitative analysis of all the components of the volatile organic compounds in the polyvinyl alcohol, has practical guiding significance for the improvement of product process and formula, and lays a foundation for quantitative determination of the volatile components.
Drawings
FIG. 1 is a total ion flow chromatogram of volatile organic compounds in a sample of polyvinyl alcohol 04-99 in example 1 of the present invention. As can be seen from fig. 1, under the analysis conditions adopted in the present invention, the components can be completely separated, the peak shape is better, the variety of the volatile impurity components in the sample is more, and in combination with table 1, trace amounts of acetaldehyde, methyl propionate, acetone and 2-butenal are detected in the sample in addition to methyl acetate, methanol and the like with relatively high contents.
FIG. 2 is a total ion flow chromatogram of volatile organics in a sample of polyvinyl alcohol 17-88 in example 2 of the present invention. As can be seen from fig. 2, the separation degree of each component in the sample is good, the peak shape is symmetrical, and in combination with table 2, in the sample, besides components such as methanol, methyl acetate and the like, a peak of an isobutyronitrile impurity appears at 9.250min, and a small amount of acetone and paraldehyde still remains in the sample.
Detailed description of the invention
The technical solutions of the present invention are further described below with reference to specific examples, which should not be construed as limiting the technical solutions.
Example 1:
the method for measuring the volatile organic compounds in the polyvinyl alcohol by the automatic headspace sample injection-gas chromatography-mass spectrometry in the embodiment comprises the following steps:
1. weighing 0.2g of polyvinyl alcohol 04-99 sample, putting the sample into a 20mL headspace bottle, adding 2mLN, N-dimethylacetamide, covering a silica gel pad and an aluminum cover, sealing the sample by using a capping device, and putting the headspace bottle into a specified position of a sample tray according to the experimental requirements.
The automatic headspace sampling conditions were:
the headspace sample injector platform temperature is 90 ℃, the equilibration time is 45min, the quantitative loop temperature is 100 ℃, the transfer tube temperature is 110 ℃, and the sample injection volume is 1 mL.
2. Analyzing the sample subjected to headspace sample injection by using a gas chromatography-mass spectrometer, wherein the analysis conditions of the gas chromatography-mass spectrometer are as follows:
gas chromatography conditions: column temperature: keeping the initial temperature for 5min from 52 ℃, then heating to 110 ℃ at 15 ℃/min, keeping for 3min, and finally heating to 200 ℃ at 60 ℃/min, and keeping for 5 min; carrier gas: helium (purity greater than 99.999%); flow rate: 1.5 mL/min; the split ratio is 20: 1; the injection port temperature was 200 ℃.
Mass spectrum conditions: EI source: 70 eV; a transmission line is 220 ℃; an ion source of 250 ℃; a quadrupole rod is 150 ℃; the scanning mode is as follows: full scanning; the mass scanning range m/z is 10-300; delaying the solvent for 3 min; after 14.5min the detector is set off.
Qualitative mode: and comparing the component characteristic mass spectrogram with an NIST standard spectrum library.
According to the method for measuring the volatile organic compounds in the polyvinyl alcohol by automatic headspace sampling-gas chromatography-mass spectrometry, the spectrogram of gas chromatography-mass spectrometry analysis of each volatile organic compound in the polyvinyl alcohol is shown in figure 1, and the qualitative result is shown in table 1.
TABLE 1 qualitative results of volatile organic components in the PVA 04-99 samples
Example 2:
the method for measuring the volatile organic compounds in the polyvinyl alcohol by the automatic headspace sample injection-gas chromatography-mass spectrometry in the embodiment comprises the following steps:
1. weighing 0.2g of polyvinyl alcohol 17-88 sample, putting the sample into a 20mL headspace bottle, adding 2mLN, N-dimethylacetamide, covering a silica gel pad and an aluminum cover, sealing the sample by using a capping device, and putting the headspace bottle into a specified position of a sample tray according to the experimental requirements.
The automatic headspace sampling conditions were:
the headspace sample injector platform temperature is 90 ℃, the equilibration time is 45min, the quantitative loop temperature is 100 ℃, the transfer tube temperature is 110 ℃, and the sample injection volume is 1 mL.
2. Analyzing the sample subjected to headspace sample injection by using a gas chromatography-mass spectrometer, wherein the analysis conditions of the gas chromatography-mass spectrometer are as follows:
gas chromatography conditions: column temperature: keeping the initial temperature for 5min from 52 ℃, then heating to 110 ℃ at 15 ℃/min, keeping for 3min, and finally heating to 200 ℃ at 60 ℃/min, and keeping for 5 min; carrier gas: helium (purity greater than 99.999%); flow rate: 1.5 mL/min; the split ratio is 20: 1; the injection port temperature was 200 ℃.
Mass spectrum conditions: EI source: 70 eV; a transmission line is 220 ℃; an ion source of 250 ℃; a quadrupole rod is 150 ℃; the scanning mode is as follows: full scanning; the mass scanning range m/z is 10-300; delaying the solvent for 3 min; after 14.5min the detector is set off.
Qualitative mode: and comparing the component characteristic mass spectrogram with an NIST standard spectrum library.
According to the method for measuring the volatile organic compounds in the polyvinyl alcohol by automatic headspace sampling-gas chromatography-mass spectrometry, the spectrogram of gas chromatography-mass spectrometry analysis of each volatile organic compound in the polyvinyl alcohol is shown in figure 2, and the qualitative result is shown in table 2.
TABLE 2 qualitative results of volatile organic components in the PVA 17-88 samples
Claims (1)
1. A method for measuring volatile organic compounds in polyvinyl alcohol by automatic headspace sampling-gas chromatography-mass spectrometry is characterized by comprising the following steps: firstly, putting a sample into a container, adding a solvent, and dissolving and mixing uniformly; then heating by adopting a static headspace method to volatilize the volatile components from the sample so as to reach two-phase balance; injecting the gas at the upper part of the headspace bottle into a gas chromatograph for separation, and finally introducing the gas into a mass spectrum detector for qualitative analysis; the method specifically comprises the following steps:
step 1: weighing 0.2g of polyvinyl alcohol sample, putting the polyvinyl alcohol sample into a 20mL headspace bottle, adding 2mLN, N-dimethylacetamide, sealing, putting the headspace bottle into a specified position of a sample tray, and sampling by adopting an Agilent 7697 automatic headspace sampler;
step 2: separating the sample by adopting an Agilent CP-Wax 52CB chromatographic column;
and step 3: detecting volatile organic compounds in polyvinyl alcohol by adopting an Agilent 7890A-5977B gas chromatograph-mass spectrometer;
and 4, step 4: comparing the component characteristic mass spectrogram with an NIST standard spectrogram, and performing qualitative analysis;
in the step 1, the headspace bottle is balanced at 90 ℃ for 45min, the quantitative loop temperature is 100 ℃, the transmission line temperature is 110 ℃, and the sample injection volume is 1 mL;
in step 2, the Agilent CP-Wax 52CB chromatographic column separation parameters are set as follows: column temperature: keeping the initial temperature at 52-200 ℃ for 5min from 52 ℃, then heating to 110 ℃ at 15 ℃/min, keeping for 3min, and finally heating to 200 ℃ at 60 ℃/min, and keeping for 5 min; carrier gas: helium with purity greater than 99.999%; flow rate: 1.5 mL/min; the split ratio is 20: 1; the temperature of a sample inlet is 200 ℃;
in step 3, the detection parameters are set as follows: MS conditions: EI source: 70 eV; a transmission line is 220 ℃; an ion source of 250 ℃; a quadrupole rod is 150 ℃; the scanning mode is as follows: full scanning; the mass scanning range m/z is 10-300; delaying the solvent for 3 min; after 14.5min the detector is set to off;
the volatile organic compounds include methanol, methyl acetate, acetaldehyde, methyl formate, water, ethanol, 2-butenal, paraldehyde, acetone, methyl propionate and isobutyronitrile.
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Denomination of invention: A method for automatic headspace injection gas chromatography-mass spectrometry determination of volatile organic compounds in polyvinyl alcohol Effective date of registration: 20231120 Granted publication date: 20201222 Pledgee: Industrial and Commercial Bank of China Limited Chaohu sub branch Pledgor: ANHUI WANWEI UPDATED HIGH-TECH MATERIAL INDUSTRY Co.,Ltd. Registration number: Y2023980066338 |
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