CN102507773A - Method for selectively determining residual vinyl acetate in white latex for cigarette through static headspace gas and chromatography mass spectrometry - Google Patents
Method for selectively determining residual vinyl acetate in white latex for cigarette through static headspace gas and chromatography mass spectrometry Download PDFInfo
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Abstract
The invention relates to a method for selectively determining residual vinyl acetate in white latex for cigarette through static headspace and gas chromatography mass spectrometry, belonging to the technical field of physical and chemical inspection of materials for the cigarette, and provides a quantitative selected ion determining method through the static headspace and gas chromatography mass spectrometry, aiming at selectively determining the residual vinyl acetate in white latex for the cigarette. A sample of the white latex for the cigarette after static headspace at 80 DEG C for 15 minutes is detected by taking 2-hexanone as an internal standard through HP-INNOWAX column in a GC-MS/SIM (Gas Chromatography Mass Spectrometry/Selected Ion Monitoring) mode, and is quantified through an internal standard method. According to the method for selectively determining the residual vinyl acetate in the white latex for the cigarette through the static headspace gas chromatography mass spectrometry, disclosed by the invention, detection limit, labeling recovery ratio and RSD (Relative Standard Deviation) of the method are respectively 0.63mg/kg, 104-107% and 2.5-4.9%; in addition, the method disclosed by the invention has the characteristics of simpleness, fastness, accuracy, sensitiveness and the like, and is especially suitable for quantitative analysis on the residual vinyl acetate in the white latex for the cigarette.
Description
Technical field
The present invention relates to the method for a kind of static head space-gaschromatographic mass spectrometry selective determination cigarette, belong to the physical and chemical inspection technical field of cigarette with material with remaining vinyl acetate in the white glue with vinyl.
Background technology
At present; The tackifier that uses in the domestic production of cigarettes is to be the synthetic a kind of thermoplasticity white glue with vinyl of primary raw material with vinyl acetate mostly; Wherein residual vinyl acetate monomer both had been unfavorable for the stability of emulsion; Can bring being an unpleasant jar to nerves property smell to product again, thereby have a strong impact on the aesthetic quality of cigarette product, international cancer research association classifies it as 2B class carcinogen.Therefore, analyze and the monitoring cigarette has important meaning with vinyl acetate residual in the white glue with vinyl to the security of sucking of cigarette.Cigarette mainly contains near infrared method, titrimetry, iodimetric titration etc. with the residual traditional analysis method of vinyl acetate in the white glue with vinyl, but receives the restriction of its precision and accuracy, and these methods can not satisfy the needs of analysis.The method that some are new such as head space-gas chromatography are just attempted being used for relevant analysis and research with gas chromatography/mass spectroscopy.Static headspace analysis (static headspace; SHS) be a kind of method that the head space gas that is in liquid or solid sample in the closed container that reaches balance is analyzed; It is directly got head space gas the volatile ingredient in the sample is analyzed, and need not the complicated sample preprocessing process, can get rid of the interference of sample substrate to analyzing effectively; The mensuration process is easy, quick, has obtained widespread use at a plurality of analysis fields such as food security, medicine analysis, industrial products in recent years.The present invention combines SHS the deficiency of existing cigarette with vinyl acetate residue analysis method in the white glue with vinyl with gas chromatography-mass spectrum (GC-MS), to set up a kind of easy, accurate, fast detecting cigarette with the residual SHS-GC-MS method of vinyl acetate in the glue.
Summary of the invention
The purpose of this invention is to provide the method for a kind of static head space-gaschromatographic mass spectrometry selective determination cigarette with remaining vinyl acetate in the white glue with vinyl.The present invention is directed to the deficiency of existing cigarette with remaining vinyl acetate analytical approach in the white glue with vinyl; Static head space SHS is combined with gaschromatographic mass spectrometry (GC/MS), set up a kind of easy, accurate, fast selective and detect the SHS-GC/MS method of cigarette with remaining vinyl acetate in the white glue with vinyl.
Static head space of the present invention-gaschromatographic mass spectrometry selective determination cigarette is with the method for remaining vinyl acetate in the white glue with vinyl; With the methyl-n-butyl ketone is internal standard compound; Adopt static head space balance, gas chromatography-mass spectrum to select ion mode to measure the content of cigarette with remaining vinyl acetate in the white glue with vinyl; Wherein, gas chromatography adopts the HP-INNOWAX chromatographic column, and assay adopts inner mark method ration.
Said static head space-gaschromatographic mass spectrometry selective determination cigarette specifically comprises the steps: with the method for remaining vinyl acetate in the white glue with vinyl
(1) preparation of vinyl acetate standard solution: accurately take by weighing the pure material of vinyl acetate, use N, dinethylformamide is made into standard solution;
(2) be added with in the preparation of target matrix correction agent: accurately take by weighing the internal standard compound methyl-n-butyl ketone, use N, dinethylformamide is made into the N of methyl-n-butyl ketone, and dinethylformamide solution obtains to be added with interior target matrix correction agent, and subsequent use as the matrix solvent;
(3) drafting of the detection of vinyl acetate standard solution and typical curve: many parts of the standard solution of accurately removing step (1) acquisition; Add the matrix solvent that a certain amount of step (2) obtains respectively; And use N; The dinethylformamide constant volume obtains the vinyl acetate standard solution of a series of variable concentrations gradients, respectively the vinyl acetate standard solution of these a series of variable concentrations gradients is carried out static head space balance after, put into head-space sampler respectively and carry out SHS-GC/MS and detect; Chromatographic peak area and interior mark peak area ratio Y with vinyl acetate are that ordinate, its respective quality concentration X (μ g/mL) are the typical curve that horizontal ordinate is drawn vinyl acetate, calculate the regression equation of vinyl acetate typical curve;
(4) the static head space of sample is handled: cigarette is placed the head space bottle with the white glue with vinyl sample, add institute's matrix prepared solvent, the testing sample solution of acquisition is sealed rapidly, carry out after the static head space balance to be measured;
(5) cigarette is with the assay of remaining vinyl acetate in the white glue with vinyl sample: the testing sample solution after the static head space balance is put into head-space sampler carry out SHS-GC/MS and detect; In the said regression equation of ratio substitution with the peak area of the vinyl acetate that obtains and the peak area of interior mark methyl-n-butyl ketone, can obtain the residual content of cigarette with vinyl acetate in the white glue with vinyl sample.
Preferable, in the step (1), the concentration of vinyl acetate is 5mg/mL-50mg/mL in the vinyl acetate standard solution.
Preferable, in the step (2), the concentration of methyl-n-butyl ketone is 100 μ g/mL-500 μ g/mL in the matrix solvent.
Preferable, in the step (3), the umber of the vinyl acetate standard solution that accurately pipettes is 6 parts; And in the vinyl acetate standard solution of a series of variable concentrations gradients that obtain, the concentration of vinyl acetate is respectively 10 μ g/mL, 20 μ g/mL; 40 μ g/mL, 80 μ g/mL, 160 μ g/mL; 400 μ g/mL, the concentration of methyl-n-butyl ketone is 120 μ g/mL.
Preferable, in step (3) neutralization procedure (4), the equilibrium temperature of static head space balance is 80 ℃, equilibration time is 10-30min; Be preferably 15min.
Preferable, in the step (4), in the said testing sample solution every 0.1g cigarette with white glue with vinyl generally add 1-5ml be added with in target matrix solvent.
Preferable, in step (3) neutralization procedure (5), the static head space condition that SHS-GC/MS detects is:
Sample equilibrium temperature: 80 ℃; Sample loop temperature: 100 ℃; Transmission line temperature: 120 ℃; Sample equilibration time: 15min; Sample bottle moulding pressure: 15psi; Nebulizer gas pressure: 15psi; Pressing time: 0.20min; Inflationtime: 0.20min; Sample loop equilibration time: 0.05min; Sample injection time: 0.5min.
Preferable, in step (3) neutralization procedure (5), the GC/MS condition that SHS-GC/MS detects is:
GC conditions is: chromatographic column: HP-INNOWAX (30m * 0.25mm * 0.25 μ m); Injector temperature: 150 ℃; Carrier gas: high-purity helium, purity >=99.999%; The constant current mode of flow velocity: 1.0mL/min; Split ratio: 10: 1; Heating schedule: initial temperature keeps 3min for 40 ℃, and the speed with 10 ℃/min rises to 180 ℃ again, and the speed with 20 ℃/min rises to 200 ℃ then, keeps 1min;
The mass spectrum condition is: the transmission line temperature: 250 ℃; Ion source temperature: 230 ℃; Quadrupole rod temperature: 150 ℃; Solvent delay: 3min; Ionization mode: EI source; Ionizing energy: 70eV; Scan mode: select ion monitoring (SIM).
The present invention with the special physicochemical property of white glue with vinyl, optionally measures cigarette with remaining vinyl acetate in the white glue with vinyl according to cigarette, has set up the content of static head space-gas chromatography-mass spectrum technology coupling selective determination cigarette with remaining vinyl acetate in the white glue with vinyl.Sample is interior mark with methyl-n-butyl ketone behind the static head space of 80 ℃, 15min, adopts the HP-INNOWAX post, and gas chromatography-mass spectrum selects ion mode to detect inner mark method ration.The detection of this assay method is limited to 0.63mg/kg, and recovery of standard addition is 104%～107%, and relative standard deviation (RSD) is 2.5%～4.9%.This assay method has characteristics such as simple quick, accurate sensitivity, is applied to the actual sample detection and has obtained good result.
Assay method of the present invention is directly got head space gas residual acetic acid vinyl acetate composition in the sample is analyzed; Can get rid of the interference of sample substrate effectively to analyzing; Need not the complicated sample preprocessing process; This assay method has been avoided loaded down with trivial details solvent extraction, and has quantitatively remedied the not high defective of GC-flame ionization ditector sensitivity through SIM.Experimental result shows: assay method of the present invention has characteristics such as good reproducibility, accuracy height, rapid sensitive, is particularly suitable for the mensuration of cigarette with residual vinyl acetate in the white glue with vinyl.
Description of drawings
Fig. 1 head space equilibration time is to the figure that influences of peak area.
Fig. 2 head space equilibrium temperature is to the figure that influences of peak area.
Four kinds of matrix of Fig. 3 are proofreaied and correct the selection chromatography of ions figure that solvent is used for sample determination
A:N, dinethylformamide; B: glyceryl triacetate; C: cyclohexane; D: normal hexane; Wherein in each collection of illustrative plates,
1: vinyl acetate; 2:N, dinethylformamide; 3: cyclohexane; 4: normal hexane.
Selection chromatography of ions Fig. 4 a of Fig. 4 methyl-n-butyl ketone, selection chromatography of ions Fig. 4 b of vinyl acetate standard items and cigarette are with selection chromatography of ions Fig. 4 c of white glue with vinyl sample; Wherein, 1: vinyl acetate; The 2:2-hexanone; 3:N, dinethylformamide.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment only are used to the present invention is described and are not used in restriction protection scope of the present invention.
1 experimental section
1.1 material, reagent and instrument
Cigarette is with white glue with vinyl sample (being selected from cigarette enterprise); Glyceryl triacetate (AR, chemical reagent Ltd of traditional Chinese medicines group); Cyclohexane, normal hexane (chromatographically pure, Tianjin Da Mao chemical reagent factory); N, dinethylformamide (AR, chemical reagent factory of Chongqing Chuan Dong chemical industry (group) company limited); Methyl-n-butyl ketone (interior mark, IS; 99%) vinyl acetate (99%, U.S. Sigma company); HP6890/5973 type gas chromatography appearance, 7694 automatic head space appearance (U.S. Agilent company); AG104 type electronic analytical balance (sensibility reciprocal: 0.1mg, Switzerland Mettler Toledo Inc.).
1.2 sample preparation and analysis
Accurately take by weighing the 0.25g vinyl acetate in the 25mL volumetric flask, use N, the dinethylformamide constant volume gets 10mg/mL vinyl acetate standard solution.Accurately take by weighing 0.3g methyl-n-butyl ketone (IS) in the 50mL volumetric flask, use N, the dinethylformamide constant volume gets 6mg/mL IS solution; Get 2mL IS solution in the 100mL volumetric flask, use N, the dinethylformamide constant volume, subsequent use as the matrix solvent, its concentration is 120 μ g/mL.Accurately take by weighing the 0.1g sample, place the head space bottle, add the N of 1mL120 μ g/mL IS, dinethylformamide solution compresses bottle cap rapidly, puts into head-space sampler and carries out the GC-MS check and analysis.The check and analysis condition is:
(1) SHS condition.Sample equilibrium temperature: 80 ℃; Sample loop temperature: 100 ℃; Transmission line temperature: 120 ℃; Sample equilibration time: 15min; Sample bottle moulding pressure: 15psi; Nebulizer gas pressure: 15psi; Pressing time: 0.20min; Inflationtime: 0.20min; Sample loop equilibration time: 0.05min; Sample injection time: 0.5min.
(2) GC/MS condition.Chromatographic column: HP-INNOWAX (30m * 0.25mm * 0.25 μ m); Injector temperature: 150 ℃; Carrier gas: high-purity helium, purity>=99.999%; Flow velocity: 1.0mL/min (constant current mode); Split ratio: 10: 1; Heating schedule:
transmission line temperature: 250 ℃; Ion source temperature: 230 ℃; Quadrupole rod temperature: 150 ℃; Solvent delay: 3min; Ionization mode: EI source; Ionizing energy: 70eV; Scan mode: select ion monitoring (SIM).
Retention time is compared in employing, the standard specimen addition method is qualitative, inner mark method ration under the SIM pattern.Retention time and the characteristic ion of vinyl acetate and IS are seen table 1.
Table 1 vinyl acetate and with retention time and the qualitative, quantitative ion of IS
2 results and discussion
2.1 the selection of SHS equilibration time
SHS analyzes the influence that mainly receives sample equilibrium temperature, equilibration time and sample substrate, therefore, adopts the mode of single factor experiment that these influence factors are selected.With concentration is that the vinyl acetate standard solution of 10 μ g/mL places the head space bottle; Under 80 ℃ equilibrium temperature to different equilibration times (5,10,15; 20; Head space gas 30min) is analyzed, and is index with the chromatographic peak area of vinyl acetate, investigates the influence of different equilibration times to vinyl acetate amount in the static headspace gas.(see figure 1) shows as a result, when equilibration time is 10～30min, and basic indifference, the distribution of vinyl acetate has reached dynamic balance state during this explanation 10min.In order to ensure the abundant balance of sample system, selected the SHS equilibration time of 15min as sample.
2.2 the selection of SHS equilibrium temperature
Under identical equilibration time, to different equilibrium temperatures (45 ℃, 50 ℃, 60 ℃, 80 ℃, 90 ℃, 100 ℃) down in the static headspace gas content of vinyl acetate compare.(see figure 2) shows as a result, and along with the raising of equilibrium temperature, the chromatographic peak area of vinyl acetate increases gradually, and under 45～60 ℃, speedup is slower, and in the time of 60～90 ℃, speedup is very fast, eases up subsequently.The high volatile volatile compound is many more more owing to temperature; Impurity peaks increases, and also big more to the ion gun pollution, therefore; Take all factors into consideration the effumability (boiling point is 71.8 ℃) of vinyl acetate and reduce ionogenic pollution and impurity peaks disturbs the factor of two aspects, selecting equilibrium temperature is 80 ℃.
2.3 the selection of SHS matrix correction agent
Each components contents was both relevant with the volatility of itself in the head space gas; Relevant with sample substrate again; Especially the component of those solubleness in sample substrate big (partition factor is big), matrix effect is more obvious, makes analytic sample and standard solution have identical matrix solvent; Can eliminate the matrix effect of sample effectively, thereby improve the accuracy of quantitative test.Therefore, glyceryl triacetate, normal hexane, cyclohexane and N are selected in this experiment respectively, and 4 kinds of organic solvents of dinethylformamide are used for sample determination as the matrix correction agent and investigate (see figure 3).The result shows that therefore normal hexane and cyclohexane are not suitable for the matrix correction agent as vinyl acetate because boiling point is relatively low, and solvent appearance time and vinyl acetate are approaching, and the chromatographic resolution degree is bad, causes quantitative accuracy relatively poor.The glyceryl triacetate boiling point is higher, is difficult for flowing out at short notice, and is more consuming time when being used for lower boiling vinyl acetate and analyzing.N, dinethylformamide have moderate boiling point, are a kind of non-proton preferably polar reagents, can dissolve cigarette and use glue, sample is dispersed in the matrix solvent, thereby makes quantitative result more accurate.In sum, select N, dinethylformamide is as the matrix solvent.
2.4 interior target is selected
When adopting SHS-GC to measure volatile compound, external standard method is adopted in quantitative test usually.Because it is bigger that the head space method is influenced by environment and sample substrate, makes the quantitative accuracy of external standard method receive certain limitation, internal standard method is attempted being used for head space-quantitative analysis by gas chromatography in recent years.The present invention's experiment selects for use methyl-n-butyl ketone to analyze as IS.Result (Fig. 4) shows: under same quality level condition, the mass spectrum response of methyl-n-butyl ketone and vinyl acetate component to be measured is comparatively approaching, and with the degree of separation of component to be measured high (seeing Fig. 4 b), so the selection methyl-n-butyl ketone is internal standard compound IS.
2.5 the detectability of working curve and method, the recovery, precision
Accurately pipette 10mg/mL vinyl acetate standard solution 25 μ L, 50 μ L, 100 μ L, 200 μ L; 400 μ L, 1000 μ L are in 6 25mL volumetric flasks, and adding 500 μ L concentration respectively is 6mg/mL IS solution, and uses N; Dinethylformamide is settled to 25mL, obtains concentration and is respectively 10,20,40; 80,160,400 μ g/mL and IS concentration are the vinyl acetate series standard solution of 6 grades of concentration gradients of 120 μ g/mL.Standard solution to these 6 grades of gradient concentrations carries out the SHS-GC-MS analysis respectively; And be that ordinate, its respective quality concentration X (μ g/mL) are that horizontal ordinate carries out regretional analysis with vinyl acetate chromatographic peak area and interior mark peak area ratio Y, obtain regression equation Y=21.039X+1.6013 (R
2=0.9999), calculates detection and be limited to 0.63mg/kg with 3 times of signal to noise ratio (S/N ratio)s (S/N=3).
In the white glue with vinyl sample of known vinyl acetate content (mean values of 6 mensuration), add high, normal, basic 3 variable concentrations (40 respectively; 20; The standard solution of vinyl acetate 10 μ g/mL); Adopt the SHS-GC-MS method to measure corresponding vinyl acetate content,, calculate the recovery (seeing table 2) of this assay method according to the addition of measuring result and vinyl acetate.Result's (table 2) shows that the recovery of vinyl acetate is 104%～107%, shows that the accuracy of this assay method is higher; The relative standard deviation (RSD) of calculating vinyl acetate according to the mensuration result is 2.5%～4.9%, less than 5%, explains that the repeatability of this assay method is better.
Table 2 cigarette is with the recovery and the precision (n=6) of vinyl acetate in the glue
2.6 actual cigarette is with the mensuration of the vinyl acetate content in the white glue with vinyl sample
The preparation steps of each solution is measured with the residual quantity of vinyl acetate in the white glue with vinyl 6 kinds of cigarettes of cigarette enterprise use with determination step in utilizing 1.2 sample preparation in the said determination method and analyzing; Each sample replicate determination 6 times; Result's (seeing table 3) shows: between 72.27～310.09mg/kg, RSD is 1.6%～4.5% with the residual quantity of vinyl acetate in the white glue with vinyl for 6 kinds of cigarettes.Wherein, 6 kinds of cigarettes that disposed are with the be added with interior target matrix correction agent of cigarette in the white glue with vinyl sample solution with the corresponding 1ml of the every 0.1g of white glue with vinyl, and the concentration that is added with methyl-n-butyl ketone in the interior target matrix correction agent is 120 μ g/mL.
Table 3 cigarette is with the testing result and the precision (n=6) of middle vinyl acetate in the glue sample
3 conclusions
The present invention has set up the static head space-gas chromatography-mass spectrography method of selective determination cigarette with residual acetic acid vinyl acetate content in the white glue with vinyl; This assay method has been avoided loaded down with trivial details solvent extraction, and has quantitatively remedied the not high defective of GC-flame ionization ditector sensitivity through SIM.This assay method has characteristics such as good reproducibility, accuracy height, rapid sensitive, is suitable for the mensuration of cigarette with residual vinyl acetate in the white glue with vinyl.
Claims (9)
1. static head space-gaschromatographic mass spectrometry selective determination cigarette is with the method for remaining vinyl acetate in the white glue with vinyl; It is characterized in that; With the methyl-n-butyl ketone is internal standard compound, adopts static head space balance, gas chromatography-mass spectrum to select ion mode to measure the content of cigarette with remaining vinyl acetate in the white glue with vinyl, wherein; Gas chromatography adopts the HP-INNOWAX chromatographic column, and assay adopts inner mark method ration.
2. static head space as claimed in claim 1-gaschromatographic mass spectrometry selective determination cigarette is characterized in that with the method for remaining vinyl acetate in the white glue with vinyl, specifically comprises the steps:
(1) preparation of vinyl acetate standard solution: accurately take by weighing the pure material of vinyl acetate, use N, dinethylformamide is made into standard solution;
(2) be added with in the preparation of target matrix correction agent: accurately take by weighing the internal standard compound methyl-n-butyl ketone, use N, dinethylformamide is made into the N of methyl-n-butyl ketone, and dinethylformamide solution obtains to be added with interior target matrix correction agent, and subsequent use as the matrix solvent;
(3) drafting of the detection of vinyl acetate standard solution and typical curve: many parts of the standard solution of accurately removing step (1) acquisition; Add the matrix solvent that a certain amount of step (2) obtains respectively; And use N; The dinethylformamide constant volume obtains the vinyl acetate standard solution of a series of variable concentrations gradients, respectively the vinyl acetate standard solution of these a series of variable concentrations gradients is carried out static head space balance after, put into head-space sampler respectively and carry out SHS-GC/MS and detect; Chromatographic peak area and interior mark peak area ratio Y with vinyl acetate are that ordinate, its respective quality concentration X (μ g/mL) are the typical curve that horizontal ordinate is drawn vinyl acetate, calculate the regression equation of vinyl acetate typical curve;
(4) the static head space of sample is handled: cigarette is placed the head space bottle with the white glue with vinyl sample, add institute's matrix prepared solvent, the testing sample solution of acquisition is sealed rapidly, carry out after the static head space balance to be measured;
(5) cigarette is with the assay of remaining vinyl acetate in the white glue with vinyl sample: the testing sample solution after the static head space balance is put into head-space sampler carry out SHS-GC/MS and detect; In the said regression equation of ratio substitution with the peak area of the vinyl acetate that obtains and the peak area of interior mark methyl-n-butyl ketone, obtain the residual content of cigarette with vinyl acetate in the white glue with vinyl sample.
3. static head space as claimed in claim 2-gaschromatographic mass spectrometry selective determination cigarette is characterized in that with the method for remaining vinyl acetate in the white glue with vinyl in the step (1), the concentration of vinyl acetate is 5mg/mL-50mg/mL in the standard solution.
4. static head space as claimed in claim 2-gaschromatographic mass spectrometry selective determination cigarette is characterized in that with the method for remaining vinyl acetate in the white glue with vinyl in the step (2), the concentration of methyl-n-butyl ketone is 100 μ g/mL-500 μ g/mL in the matrix solvent.
5. static head space as claimed in claim 2-gaschromatographic mass spectrometry selective determination cigarette is characterized in that with the method for remaining vinyl acetate in the white glue with vinyl, in the step (3); The umber of the vinyl acetate standard solution that accurately pipettes is 6 parts, and in the vinyl acetate standard solution of a series of variable concentrations gradients that obtain, the concentration of vinyl acetate is respectively 10 μ g/mL; 20 μ g/mL, 40 μ g/mL, 80 μ g/mL; 160 μ g/mL, 400 μ g/mL, the concentration of methyl-n-butyl ketone is 120 μ g/mL.
6. static head space as claimed in claim 2-gaschromatographic mass spectrometry selective determination cigarette is with the method for remaining vinyl acetate in the white glue with vinyl; It is characterized in that; In step (3) neutralization procedure (4), the equilibrium temperature of static head space balance is 80 ℃, and equilibration time is 10-30min.
7. static head space as claimed in claim 2-gaschromatographic mass spectrometry selective determination cigarette is with the method for remaining vinyl acetate in the white glue with vinyl; It is characterized in that; In the step (4), target matrix solvent in every 0.1g cigarette is added with white glue with vinyl adding 1-5ml in the said testing sample solution.
8. it is characterized in that with the method for remaining vinyl acetate in the white glue with vinyl like each described static head space-gaschromatographic mass spectrometry selective determination cigarette among the claim 2-7 that in step (3) neutralization procedure (5), the static head space condition that SHS-GC/MS detects is:
Sample equilibrium temperature: 80 ℃; Sample loop temperature: 100 ℃; Transmission line temperature: 120 ℃; Sample equilibration time: 15min; Sample bottle moulding pressure: 15psi; Nebulizer gas pressure: 15psi; Pressing time: 0.20min; Inflationtime: 0.20min; Sample loop equilibration time: 0.05min; Sample injection time: 0.5min.
9. it is characterized in that with the method for remaining vinyl acetate in the white glue with vinyl like each described static head space-gaschromatographic mass spectrometry selective determination cigarette among the claim 2-7 that in step (3) neutralization procedure (5), the GC/MS condition that SHS-GC/MS detects is:
GC conditions: chromatographic column: HP-INNOWAX; Injector temperature: 150 ℃; Carrier gas: high-purity helium, purity >=99.999%; The constant current mode of flow velocity: 1.0mL/min; Split ratio: 10: 1; Heating schedule: initial temperature keeps 3min for 40 ℃, and the speed with 10 ℃/min rises to 180 ℃ again, and the speed with 20 ℃/min rises to 200 ℃ then, keeps 1min;
Mass spectrum condition: transmission line temperature: 250 ℃; Ion source temperature: 230 ℃; Quadrupole rod temperature: 150 ℃; Solvent delay: 3min; Ionization mode: EI source; Ionizing energy: 70eV; Scan mode: SIM selects ion monitoring.
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| CN104198602A (en) * | 2014-09-01 | 2014-12-10 | 云南中烟工业有限责任公司 | Method for detecting vinyl acetate in hot melt adhesive |
| CN106841442A (en) * | 2017-01-25 | 2017-06-13 | 江苏中烟工业有限责任公司 | Vinyl acetate and six kinds of methods of benzene homologues in water base adhesive are determined simultaneously |
| CN112557531A (en) * | 2020-11-27 | 2021-03-26 | 衢州康鹏化学有限公司 | Method for detecting residual solvent in vinyl sulfate by headspace gas chromatography |
| CN112557531B (en) * | 2020-11-27 | 2023-05-09 | 衢州康鹏化学有限公司 | Method for detecting residual solvent in vinyl sulfate by headspace gas chromatography |
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