CN106596826A - Method for determining benzene and benzene series content in cellulose acetate fiber and cellulose acetate fiber mouth stick - Google Patents

Method for determining benzene and benzene series content in cellulose acetate fiber and cellulose acetate fiber mouth stick Download PDF

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Publication number
CN106596826A
CN106596826A CN201710055395.9A CN201710055395A CN106596826A CN 106596826 A CN106596826 A CN 106596826A CN 201710055395 A CN201710055395 A CN 201710055395A CN 106596826 A CN106596826 A CN 106596826A
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benzene
acetate fiber
solution
standard
sample
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徐光忠
李青
于小红
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China Tobacco Jiangsu Industrial Co Ltd
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China Tobacco Jiangsu Industrial Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N2030/062Preparation extracting sample from raw material
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
    • G01N2030/884Integrated 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

Abstract

The invention discloses a method for determining the benzene and benzene series content in cellulose acetate fiber and a cellulose acetate fiber mouth stick. The determining method comprises the steps of preparation of an internal standard containing extraction solution and a working standard solution, sample processing and calculation of a headspace-gas chromatograph-mass spectrometric analysis and determination result. Quantification is performed by adopting an internal standard method, operation is simple and accurate, errors brought by instrument precision are decreased, adopted chromatographic conditions make chromatographic peaks of six targets and an internal standard substance separated well, the method has good linear correlation, a detection limit is 0.02-0.03 mg/kg, the average relative standard deviation is 0.86%-4.75%, the adding standard recovery rate is 88.1%-98.5%, the repeatability is good, the recovery rate is high, and the method has good practicability.

Description

The method for determining benzene and benzene homologues content in acetate fiber and acetate fiber mouth rod
Technical field
The invention belongs to Medicated cigarette physical and chemical index detection technique field, and in particular to one kind determines acetate fiber and acetate fiber The method of benzene and benzene homologues content in mouth rod.
Background technology
Acetate fiber mouth rod is required a kind of auxiliary material during production of cigarettes, by forming paper and acetate fiber structure Into.Acetate fiber may produce in process of production the benzene homologues such as benzene, toluene, ethylbenzene, dimethylbenzene.Benzene, toluene, ethylbenzene, two The benzene homologues such as toluene have larger toxicity, are likely to result in the diseases such as human body skin, pulmonary, nervous system, benzene therein, with determination Carcinogenesis, can accumulate in nervous system and skeleton, make nervous system and hemopoietic tissue suffer damage, serious harm consumption The health of person.Therefore, the aesthetic quality from cigarette material and the angle of safety, improve acetate fiber and acetate fiber mouth The level of ability that benzene and benzene homologues are determined in rod, it is significant for the security control of smoking material.
The content of the invention
The purpose of the present invention is:A kind of side for determining benzene and benzene homologues content in acetate fiber and acetate fiber mouth rod is provided Method, the method determines benzene and benzene homologues in acetate fiber and acetate fiber mouth rod using HS GC-mass spectrometry combination method Content, quick detection, measurement result accurately, determines interference few.
In order to realize foregoing invention purpose, the technical solution that the present invention is adopted is as follows:The measure acetate fiber and vinegar The method of benzene and benzene homologues content is comprised the following steps in sour fiber mouth rod:
S1. the preparation of containing the internal standard extract:Internal standard substance is weighed, is dissolved in solvent and is configured to extract;
S2. the preparation of Working Standard Solution:The standard substance of benzene and benzene homologues are benzene, toluene, ethylbenzene, xylol, meta-xylene And o-Dimethylbenzene, make solvent with DMF, Jing stepwise dilutions are configured to hybrid working mark storing solution, add step Suddenly(1)Containing the internal standard extract be configured to the Working Standard Solution of five Concentraton gradient;
S3. the preparation of sample solution:A certain amount of acetate fiber is weighed in ml headspace bottle or the acetate fiber mouth rod of forming paper is removed, Containing the internal standard extract is added, it is to be measured after gland sealing;
S4. head space-gaschromatographic mass spectrometric analysises:With head space-gas chromatography mass spectrometer to standard working solution and good seal Sample solution is tested and analyzed;
S5. Specification Curve of Increasing and result are calculated:Benzene, toluene, ethylbenzene, xylol, meta-xylene and neighbour are carried out with internal standard method The quantitative analyses of xylene content, i.e., with benzene, toluene, ethylbenzene, xylol, meta-xylene and o-Dimethylbenzene respectively and internal standard substance Chromatographic peak area compare its respective concentration and carry out regression analyses, obtain standard curve;The sample measured under the same terms is molten The chromatographic peak area of benzene, toluene, ethylbenzene, xylol, meta-xylene and o-Dimethylbenzene and internal standard substance in liquid is than substitution standard Curve, obtains final product the content of benzene and benzene homologues in sample.
Wherein, in step S1, the preparation of the containing the internal standard extract is:Internal standard substance methyl-n-butyl ketone is weighed, with N, N- dimethyl Methanamide is solvent, is configured to the extract that methyl-n-butyl ketone concentration is 0.6mg/L.
Wherein, in step S2, the concentration of the Working Standard Solution of seven Concentraton gradient is:0.002μg/mL、0.006μg/ ML, 0.012 μ g/mL, 0.020 μ g/mL, 0.030 μ g/mL, 0.044 μ g/mL and 0.060 μ g/mL.
Wherein, in step S2, the preparation of Working Standard Solution is:Benzene, toluene, ethylbenzene, the adjacent diformazan of 20mg are weighed respectively Benzene, meta-xylene, xylol use DMF constant volume in 10mL volumetric flasks, are configured to each component concentration and are 2mg/mL hybrid standard storing solutions;Each component concentration is progressively diluted to again for 0.2 μ g/mL hybrid working standard reserving solutions, sealing In 0~4 DEG C, effect duration is 6 months to stored protected from light;Accurately pipette respectively 10.0 μ L, 30.0 μ L, 60.0 μ L, 100.0 μ L, 150.0 μ L, 220.0 μ L, 300.0 μ L hybrid workings standard reserving solutions are in the ml headspace bottle of 20ml, then accurately add 1.0mL containing the internal standards extraction Take solution, rapid gland sealing, that is, obtain object benzene and benzene homologues concentration be respectively 0.002 μ g/mL, 0.006 μ g/mL, The work mark of seven Concentraton gradient of 0.012 μ g/mL, 0.020 μ g/mL, 0.030 μ g/mL, 0.044 μ g/mL and 0.060 μ g/mL Quasi- solution.
Wherein, in step S3, the preparation of the sample solution is:Weigh 0.10~0.15g acetate fibers or go forming paper Acetate fiber mouth rod in 20mL ml headspace bottles, add 1.0mL containing the internal standards extraction solution, it is to be measured after gland sealing.
Wherein, in step S4, the head space condition of described head space-gas phase-chromatograph mass spectrum analysis is:Ml headspace bottle volume 20ml, 80 DEG C of Sample equilibration temperature, 160 DEG C of sample introduction needle temperature, 180 DEG C of transmission line temperature, equilibration time 30.0min, sample bottle Pressing time 1.00min, sample injection time 1.00min, pull out pin time 0.50min;Sample introduction pattern be high pressure sample introduction, chromatograph column pressure For 196.51kPa, sample introduction pressure is 241.33kPa;Chromatographiccondition is:Using Polyethylene Glycol elastic capillary pipe chromatographic column, Carrier gas is helium, 180 DEG C of injector temperature, constant current mode, column flow 1.0ml/min, split ratio 40:1, temperature programming is 40 DEG C, keep 3min;110 DEG C are risen to the speed of 15 DEG C/min, with the speed of 5 DEG C/min 180 DEG C are risen to, kept 3min;Mass spectral analyses condition is:Transmission line temperature is 240 DEG C, and ion source temperature is 230 DEG C, and the solvent delay time is 3.0min, Ionization mode be EI, quadrupole rod temperature be 150 DEG C, scan mode be selectivity ion scan pattern fractional scanning, scanning of the mass spectrum 30~180u of scope, library searching enters line retrieval using NIST storehouses, and with characteristic ion quantitative analyses are carried out.
Wherein, the selection ion of benzene is 78,51, and the selection ion of toluene is 91,51, and the selection ion of methyl-n-butyl ketone is 58, 100, the selection ion of ethylbenzene is 91,106, and the selection ion of xylol is 91,106, and the selection ion of meta-xylene is 91, 106, the selection ion of o-Dimethylbenzene is 91,106;Ethylbenzene, xylol, meta-xylene, o-Dimethylbenzene selection ion it is identical, It is aided with single mark to be distinguish between.
Wherein, in step S5, described Specification Curve of Increasing and result calculates and is:With benzene in working solution and benzene homologues with The ratio of interior target amount is abscissa, and benzene and benzene homologues are carried out linear with the ratio of interior target peak area as vertical coordinate with chromatogram Regression analyses, obtain calibration curve equation;By six kinds of benzene in the sample solution measured under the same terms and benzene homologues and interior target Chromatographic peak area ratio, substitutes into working curve equation, that is, try to achieve the content of benzene and benzene homologues in sample.
It is an advantage of the current invention that:
1. the present invention uses headspace technique, and pre-treatment step is simple, quick, and it is high and reproducible to test accurate, sensitivity;
2. inner mark method ration is utilized, instrument precision problem is offset and is brought the error for determining thing;
3. have good practicality, for cigarette product suck safety evaluatio provides technology by and support, can produce compared with Economic benefit well and social effect.
4. headspace technique adopts Matrix phase, the matrix interference of sample itself is effectively offset, while it has at sample The advantages of simple, easy automatization of reason and few solvent consumption, with reference to the high efficiency separation ability of gas chromatogram, and report is there is no to survey at present Determine the research of the headspace gas chromatography of benzene and benzene homologues in acetate fiber and acetate fiber mouth rod.
Description of the drawings
Fig. 1 is the assay method flow chart of the present invention;
Fig. 2 is that standard solution selects chromatography of ions exemplary plot, wherein:1- benzyl alcohol, 2- toluene, IS-2- hexanones, 3- ethylbenzene, 4- Xylol, 5- meta-xylenes, 6- o-Dimethylbenzenes;
Fig. 3 selects chromatography of ions exemplary plot, wherein 1- ethylbenzene, IS-2- hexanones for the testing sample of embodiment 1.
Specific embodiment
Technical scheme is described further with reference to embodiment.
Instrument and reagent:Benzene, toluene, ethylbenzene, o-Dimethylbenzene, meta-xylene, xylol, analyze pure;Methyl-n-butyl ketone, point Analysis is pure;DMF, analyzes pure;Analytical balance, sensibility reciprocal:0.0001g;HS GC GC-MS (HS/GC/MS).
Embodiment:The content of benzene and benzene homologues in acetate fiber and acetate fiber mouth rod is determined according to following steps
(1) preparation of containing the internal standard extract:Internal standard substance methyl-n-butyl ketone is weighed, with DMF as solvent, 2- is configured to Hexanone concentration is the extract of 0.6mg/L;
(2) prepared by Working Standard Solution:Weigh respectively the benzene of 20mg, toluene, ethylbenzene, o-Dimethylbenzene, meta-xylene, to diformazan Benzene uses DMF constant volume in 10mL volumetric flasks, is configured to each component concentration for 2mg/mL hybrid standard deposits Liquid;Each component concentration is progressively diluted to again for 0.2 μ g/mL hybrid working standard reserving solutions;Accurately pipette respectively 10.0 μ L, 30.0 μ L, 60.0 μ L, 100.0 μ L, 150.0 μ L, 220.0 μ L, 300.0 μ L hybrid workings standard reserving solutions are accurate in the ml headspace bottle of 20ml 1.0mL containing the internal standards extraction solution, rapid gland sealing, that is, the concentration for obtaining object benzene and benzene homologues is really added to be respectively 0.002 μ g/mL, 0.006 μ g/mL, 0.012 μ g/mL, 0.020 μ g/mL, 0.030 μ g/mL, 0.044 μ g/mL and 0.060 μ g/mL Seven Concentraton gradient Working Standard Solution;
(3) prepared by sample solution:Weigh the acetate fiber mouth rod that 0.1g goes forming paper(It is accurate to 0.0001g)In the top of 20ml In empty bottle, 1.0ml containing the internal standard extracts are accurately added, it is to be measured after rapid gland sealing;
(4) HS/GC/MS analyses:
Head space condition is:Ml headspace bottle volume 20ml, 80 DEG C of Sample equilibration temperature, 160 DEG C of sample introduction needle temperature, transmission line temperature 180 DEG C, equilibration time 30.0min, sample bottle pressing time 1.00min, sample injection time 1.00min pull out pin time 0.50min;Sample introduction Pattern is high pressure sample introduction, and chromatograph column pressure is 196.51kPa, and sample introduction pressure is 241.33kPa;
Chromatographiccondition is:Using Polyethylene Glycol elastic capillary pipe chromatographic column, carrier gas is helium, and 180 DEG C of injector temperature is permanent Stream mode, column flow 1.0mL/min, split ratio 40:1, temperature programming is 40 DEG C, keeps 5min;With the speed liter of 15 DEG C/min To 110 DEG C, 180 DEG C are risen to the speed of 5 DEG C/min, keep 3min;
Mass spectral analyses condition is:Transmission line temperature is 240 DEG C, and ion source temperature is 230 DEG C, and the solvent delay time is 3.0min, Ionization mode is EI, and quadrupole rod temperature is 150 DEG C, and scan mode is selectivity ion scan(Ethylbenzene, xylol, a diformazan Benzene, o-Dimethylbenzene selection ion it is identical, be distinguish between with single mark in advance);The selection ion of benzene is 78,51, the selection of toluene Ion is 91,51, and the selection ion of methyl-n-butyl ketone is 58,100, and the selection ion of ethylbenzene is 91,106, the selection of xylol Ion is 91,106, and the selection ion of meta-xylene is 91,106, and the selection ion of o-Dimethylbenzene is 91,106;
(5) Specification Curve of Increasing and result are calculated:By the benzene of the variable concentrations for preparing, toluene, ethylbenzene, o-Dimethylbenzene, two Toluene, xylol Working Standard Solution injection GC/MS, chromatogram is shown in Fig. 2, with benzene, toluene, ethylbenzene, o-Dimethylbenzene, a diformazan Benzene, xylol compare its concentration and carry out regression analyses with the chromatographic peak area of internal standard methyl-n-butyl ketone respectively, obtain standard curve;It is right Sample solution after extraction is measured, and chromatogram is shown in Fig. 3, measure benzene, toluene, ethylbenzene, o-Dimethylbenzene, meta-xylene, to two Toluene respectively with the chromatographic peak area ratio of internal standard methyl-n-butyl ketone, substitute into standard curve, try to achieve the benzene content 0.00mg/ in sample solution Kg, toluene level are 0.00mg/kg, ethyl-benzene level 0.07mg/kg, ortho-xylene content 0.00mg/kg, meta-xylene content 0.00mg/kg, xylol content 0.00mg/kg.
The test limit of the inventive method:By the benzene of variable concentrations, toluene, ethylbenzene, o-Dimethylbenzene, meta-xylene, to diformazan Benzene standard working solution carries out HS/GC/MS analyses, with 3 times of signal to noise ratios(S/N=3)Test limit is calculated, test limit scope is 0.02-0.03mg/kg, correlation coefficient r2>=0.999, the linear equation of standard curve and r2Refer to table 1.
Table 1
The repeatability of the present invention and recovery of standard addition:Without benzene, toluene, ethylbenzene, o-Dimethylbenzene, meta-xylene, xylol Acetate fiber sample in add the benzene of 3 variable concentrations, toluene, ethylbenzene, o-Dimethylbenzene, meta-xylene, xylol it is mixed Working Standard Solution is closed, HS/GC/MS analyses are carried out respectively, each sample replication 6 times calculates recovery of standard addition and average Relative standard deviation RSD, between 88.1%~98.5%, the RSD of repeatability is 0.86%~4.75% for the response rate of six kinds of compositions Between, the results detailed in Table 1, illustrate that the response rate of the inventive method is higher, it is reproducible.
What is finally illustrated is:Above example only to illustrative and not limiting technical scheme, although with reference to upper State embodiment to be described in detail the present invention, it will be understood by those within the art that:Still can be to this It is bright to modify or equivalent, any modification or partial replacement without departing from the spirit and scope of the present invention, it all should Cover in the middle of scope of the presently claimed invention.

Claims (8)

1. the method for determining benzene and benzene homologues content in acetate fiber and acetate fiber mouth rod, is characterized in that:The assay method bag Include following steps:
S1. the preparation of containing the internal standard extract:Internal standard substance is weighed, is dissolved in solvent and is configured to extract;
S2. the preparation of Working Standard Solution:The standard substance of benzene and benzene homologues are benzene, toluene, ethylbenzene, xylol, meta-xylene And o-Dimethylbenzene, make solvent with DMF, Jing stepwise dilutions are configured to hybrid working mark storing solution, add step The containing the internal standard extract of rapid S1 is configured to the Working Standard Solution of five Concentraton gradient;
S3. the preparation of sample solution:A certain amount of acetate fiber is weighed in ml headspace bottle or the acetate fiber mouth rod of forming paper is removed, Containing the internal standard extract is added, it is to be measured after gland sealing;
S4. head space-gaschromatographic mass spectrometric analysises:With head space-gas chromatography mass spectrometer to standard working solution and good seal Sample solution is tested and analyzed;
S5. Specification Curve of Increasing and result are calculated:Benzene, toluene, ethylbenzene, xylol, meta-xylene and neighbour are carried out with internal standard method The quantitative analyses of xylene content, i.e., with benzene, toluene, ethylbenzene, xylol, meta-xylene and o-Dimethylbenzene respectively and internal standard substance Chromatographic peak area compare its respective concentration and carry out regression analyses, obtain standard curve;The sample measured under the same terms is molten The chromatographic peak area of benzene, toluene, ethylbenzene, xylol, meta-xylene and o-Dimethylbenzene and internal standard substance in liquid is than substitution standard Curve, obtains final product the content of benzene and benzene homologues in sample.
2. the method for determining benzene and benzene homologues content in acetate fiber and acetate fiber mouth rod according to claim 1, its It is characterized in that:In step S1, the preparation of the containing the internal standard extract is:Internal standard substance methyl-n-butyl ketone is weighed, with DMF For solvent, the extract that methyl-n-butyl ketone concentration is 0.6mg/L is configured to.
3. the method for determining benzene and benzene homologues content in acetate fiber and acetate fiber mouth rod according to claim 1, its It is characterized in that:In step S2, the concentration of the Working Standard Solution of seven Concentraton gradient is:0.002μg/mL、0.006μg/mL、 0.012 μ g/mL, 0.020 μ g/mL, 0.030 μ g/mL, 0.044 μ g/mL and 0.060 μ g/mL.
4. the method for determining benzene and benzene homologues content in acetate fiber and acetate fiber mouth rod according to claim 3, its It is characterized in that:In step S2, the preparation of Working Standard Solution is:Weigh respectively the benzene of 20mg, toluene, ethylbenzene, o-Dimethylbenzene, two Toluene, xylol use DMF constant volume in 10mL volumetric flasks, are configured to each component concentration for 2mg/mL Hybrid standard storing solution;Each component concentration is progressively diluted to again for 0.2 μ g/mL hybrid working standard reserving solutions, sealing lucifuge storage 0~4 DEG C is stored in, effect duration is 6 months;Accurately pipette respectively 10.0 μ L, 30.0 μ L, 60.0 μ L, 100.0 μ L, 150.0 μ L, 220.0 μ L, 300.0 μ L hybrid workings standard reserving solutions are in the ml headspace bottle of 20ml, then accurately add the extraction of 1.0mL containing the internal standards molten Liquid, the sealing of rapid gland, that is, obtain object benzene and benzene homologues concentration be respectively 0.002 μ g/mL, 0.006 μ g/mL, The work mark of seven Concentraton gradient of 0.012 μ g/mL, 0.020 μ g/mL, 0.030 μ g/mL, 0.044 μ g/mL and 0.060 μ g/mL Quasi- solution.
5. the method for determining benzene and benzene homologues content in acetate fiber and acetate fiber mouth rod according to claim 1, its It is characterized in that:In step S3, the preparation of the sample solution is:Weigh 0.10~0.15g acetate fibers or remove the acetic acid of forming paper Fiber mouth rod adds 1.0mL containing the internal standards extraction solution in 20mL ml headspace bottles, to be measured after gland sealing.
6. the method for determining benzene and benzene homologues content in acetate fiber and acetate fiber mouth rod according to claim 1, its It is characterized in that:In step S4, the head space condition of described head space-gas phase-chromatograph mass spectrum analysis is:Ml headspace bottle volume 20ml, sample 80 DEG C of equilibrium temperature, 160 DEG C of sample introduction needle temperature, 180 DEG C of transmission line temperature, equilibration time 30.0min, sample bottle pressing time 1.00min, sample injection time 1.00min, pull out pin time 0.50min;Sample introduction pattern is high pressure sample introduction, and chromatograph column pressure is 196.51kPa, sample introduction pressure is 241.33kPa;Chromatographiccondition is:Using Polyethylene Glycol elastic capillary pipe chromatographic column, carry Gas is helium, 180 DEG C of injector temperature, constant current mode, column flow 1.0ml/min, split ratio 40:1, temperature programming is 40 DEG C, Keep 3min;110 DEG C are risen to the speed of 15 DEG C/min, with the speed of 5 DEG C/min 180 DEG C are risen to, keep 3min;Matter Analysis of spectrum condition is:Transmission line temperature be 240 DEG C, ion source temperature be 230 DEG C, the solvent delay time be 3.0min, ionization side Formula is EI, and quadrupole rod temperature is 150 DEG C, and scan mode is selectivity ion scan pattern fractional scanning, scanning of the mass spectrum scope 30 ~180u, library searching enters line retrieval using NIST storehouses, and with characteristic ion quantitative analyses are carried out.
7. the method for determining benzene and benzene homologues content in acetate fiber and acetate fiber mouth rod according to claim 6, its It is characterized in that:The selection ion of benzene is 78,51, and the selection ion of toluene is 91,51, and the selection ion of methyl-n-butyl ketone is 58,100, second The selection ion of benzene is 91,106, and the selection ion of xylol is 91,106, and the selection ion of meta-xylene is 91,106, adjacent The selection ion of dimethylbenzene is 91,106;Ethylbenzene, xylol, meta-xylene, o-Dimethylbenzene selection ion it is identical, be aided with list Mark is distinguish between.
8. the method for determining benzene and benzene homologues content in acetate fiber and acetate fiber mouth rod according to claim 1, its It is characterized in that:In step S5, described Specification Curve of Increasing and result calculates and is:With benzene in working solution and benzene homologues and interior target The ratio of amount is abscissa, and benzene and benzene homologues carry out linear regression point with the ratio of interior target peak area as vertical coordinate with chromatogram Analysis, obtains calibration curve equation;By six kinds of benzene in the sample solution measured under the same terms and benzene homologues and interior target chromatographic peak Area ratio, substitutes into working curve equation, that is, try to achieve the content of benzene and benzene homologues in sample.
CN201710055395.9A 2017-01-25 2017-01-25 Method for determining benzene and benzene series content in cellulose acetate fiber and cellulose acetate fiber mouth stick Pending CN106596826A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111812245A (en) * 2020-07-22 2020-10-23 北京印刷学院 Method for detecting content of benzene series in lithographic printing product based on ionic liquid
CN113075332A (en) * 2021-04-08 2021-07-06 乐山市食品药品检验检测中心(乐山市药品不良反应监测中心) Method for determining low-content benzene series
CN115931828A (en) * 2023-02-17 2023-04-07 华谱智能科技(天津)有限公司 Component analysis and prediction method, unit and system suitable for complex soil matrix

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102353742A (en) * 2011-09-29 2012-02-15 贵州中烟工业有限责任公司 Method for selectively measuring 7 benzene series in white latex for cigarette through static headspace-gas chromatograph mass spectrum
CN104316636A (en) * 2014-10-29 2015-01-28 广东中烟工业有限责任公司 Method for internal standard determination of benzene and benzene series in glyceryl triacetate through headspace-gas mass spectrometry
CN104330490A (en) * 2014-10-29 2015-02-04 广东中烟工业有限责任公司 External standard measurement method for benzene and benzene series in glyceryl triacetate by adopting headspace-gas phase mass spectrometry
JP2016200531A (en) * 2015-04-13 2016-12-01 株式会社Jvcケンウッド Analytic method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102353742A (en) * 2011-09-29 2012-02-15 贵州中烟工业有限责任公司 Method for selectively measuring 7 benzene series in white latex for cigarette through static headspace-gas chromatograph mass spectrum
CN104316636A (en) * 2014-10-29 2015-01-28 广东中烟工业有限责任公司 Method for internal standard determination of benzene and benzene series in glyceryl triacetate through headspace-gas mass spectrometry
CN104330490A (en) * 2014-10-29 2015-02-04 广东中烟工业有限责任公司 External standard measurement method for benzene and benzene series in glyceryl triacetate by adopting headspace-gas phase mass spectrometry
JP2016200531A (en) * 2015-04-13 2016-12-01 株式会社Jvcケンウッド Analytic method

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
XIAORONG JI ET AL.: "Quantitative analysis of trace-level benzene,toluene, ethylbenzene, and xylene in cellulose acetate tow using headspace heart-cutting multidimensional gas chromatography with mass spectrometry", 《 J. SEP. SCI.》 *
冯骉: "《食品工程原理》", 31 March 2013 *
周景喜 等: "顶空-气相色谱-质谱法测定烟用水基型乳胶中苯系物", 《质谱学报》 *
姬厚伟 等: "静态顶空-气相色谱质谱选择性测定烟用白乳胶中 7 种苯系物", 《中国烟草学报》 *
鲍峰伟 等: "气相色谱-质谱法测定醋酸纤维滤棒中的苯系物", 《中国测试》 *
黄惠贞 等: "顶空-气质联用法分析水基胶中的苯系物", 《安徽农业科学》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111812245A (en) * 2020-07-22 2020-10-23 北京印刷学院 Method for detecting content of benzene series in lithographic printing product based on ionic liquid
CN113075332A (en) * 2021-04-08 2021-07-06 乐山市食品药品检验检测中心(乐山市药品不良反应监测中心) Method for determining low-content benzene series
CN115931828A (en) * 2023-02-17 2023-04-07 华谱智能科技(天津)有限公司 Component analysis and prediction method, unit and system suitable for complex soil matrix
CN115931828B (en) * 2023-02-17 2023-06-16 华谱智能科技(天津)有限公司 Component analysis and prediction method, unit and system suitable for complex soil matrix

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