CN103472149B - Method for analyzing influence of mentholated cigarette processing process on production environment - Google Patents
Method for analyzing influence of mentholated cigarette processing process on production environment Download PDFInfo
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Abstract
The invention provides a method for analyzing influence of a mentholated cigarette processing process on a production environment, aiming at solving the problem in the prior art that the menthol content in a mentholated cigarette production environment can not be accurately measured. According to the invention, an atmosphere sample during the mentholated cigarette processing process is captured through an on-line capturing device, and the concentration of menthol in the mentholated cigarette production environment is measured by a thermal desorption-gas chromatography-mass spectrography technology. The method is simple to operate and reliable to quantify, an analysis result is accurate and effective, the linear relation of a standard curve is good, the correlation index r<2> equals to 0.9999, a detection limit of the method reaches 0.34 microgram/m <3>, the recovery rate of the menthol in the production environment is 97.92% to 102.38%, and the relative standard deviation (RSD) is 6.57%. The method ensures the reliability and objectivity of an environmental menthol quantifying result in the cigarette processing process, and is of great significance to alleviation of pollution to a production line and a production environment.
Description
Technical field
The present invention relates to a kind of method analyzed mentholated cigarette process and production environment is affected, belong to environment measuring analysis technical field.
Background technology
The production of mentholated cigarette starts from last century two, the '30s, and since appearance, output progressively rises, and only on American market, mentholated cigarette just accounts for about 1/3rd of cigarette total sales volume at present.Here alleged mentholated cigarette refers to that menthol reaches the cigarette of certain content.Tobacco itself is not containing menthol, and the mint flavored in cigarette is added primarily of spices, and by adopting certain slow release method, menthol can be added in cigarette filter rod in right amount, be one of important production ways of mint type cigarette.And menthol is also known as hexahydrothymol, popular name menthol is the extract in plant, can be separated and obtain from natural menthence, also can by citronellal or thymol Prof. Du Yucang.In cigarette, with the addition of the menthol of certain content, refrigerant sense can be produced when sucking, effectively can reduce the burning heat sensation of flue gas, and stimulate nervous centralis, make breathing smooth and easy.
But the fusing point of menthol is lower (42-43 DEG C), volatility is very strong, easily distils, can produce intense stimulus smell, and therefore mentholated cigarette menthol in process has scattering and disappearing to a certain degree, and very easily pollutes production line and production environment; Meanwhile, menthol is easily taint of odour also, produces odor contamination, affect the suction taste of other types cigarette to the other types cigarette processed in Same Site simultaneously.Thus, mentholated cigarette is lost in process to the detection of menthol concentration in production environment, seems particularly important.
At present, in tobacco business, the mensuration to menthol content in finished cigarettes and flue gas is only rested on for the detection of menthol, and not in mentholated cigarette process on the analytical approach of production environment impact, only by the sense organ of people the menthol concentration in production site air judged and evaluate, subjective randomness is comparatively large, lacks the quantitative basis of science.
Thermal desorption technology is a kind of pretreatment technology being highly suitable for volatile matter, and it makes volatile matter from the technology of desorption involatile substance by carrier gas heated sample.It utilizes inert gas to extract the volatile matter in sample hose in solid/liquid matrix as carrier, after the method heated again carries out secondary desorption, transfers in gas chromatograph by the transmission line of heating and thermal insulation, reach highly enriched effect by condensation.
Therefore, the present invention is by the atmospheric sample in online trapping mentholated cigarette process, adopt thermal desorption-Gas chromatographyMass spectrometry, measure the menthol concentration in mentholated cigarette production environment, ensure that reliability and the objectivity of environment menthol quantitative result in Cigarette processing process, provide a kind of simple and convenient, analyze the method that mentholated cigarette process affect production environment accurately and effectively, for the menthol concentration in mensuration mentholated cigarette production environment provides technical support and theoretical reference.
Summary of the invention
The object of the present invention is to provide a kind of method analyzed mentholated cigarette process and production environment is affected, for solving in prior art the problem of the menthol concentration lacked in Accurate Determining mentholated cigarette production environment.The present invention is by the atmospheric sample in online trapping mentholated cigarette process, adopt and thermal desorption technology and gas phase hydrolysis and condensation are combined, a kind of method can analyzed mentholated cigarette process intuitively, accurately and easily and affect production environment is provided.
For achieving the above object, the present invention, by the atmospheric sample in online capturing device trapping mentholated cigarette process, adopts thermal desorption-Gas chromatographyMass spectrometry, measures the menthol concentration in mentholated cigarette production environment.Wherein, gas chromatographic column is Agilent DB-WAX capillary column, quantified by external standard method.
Preferably, the material affecting production environment in described mentholated cigarette process is menthol.
A kind of described method evaluated mentholated cigarette process and affect production environment, mainly comprises the following steps:
1) atmospheric sample is in thermal desorption online trapping before treatment: online capturing device is made up of adsorption sampling pipe and gas collecting pump, is connected on gas collecting pump by adsorption sampling pipe by proofed sleeve.Setting sampling time and sampling flow, start gas collecting pump and trap.In sampling process, gas collecting pump constantly aspirates production environment air by sampling flow, and when air is by being connected to the adsorption sampling pipe on pump, menthol contained in air is by the adsorbent of filling in adsorption tube.Sampling terminate rear sealed copper cap adsorption sampling pipe is taken off seal to be measured.
Preferably, in described step 1), adsorption sampling pipe is the compound adsorption sampling pipe of Carbotrap349 tri-sections.The compound adsorption sampling pipe of described Carbotrap349 tri-sections is commercial adsorption tube, and adsorbent filler is wherein that syllogic meets, and trade name is respectively Carbopack Y, Carbopack B, Carbosieve1003.There is larger specific surface area, namely there is larger safe sampling volume, and good hydrophobic performance, low to the adsorptive power of water, and easy desorption, there is not chemical reaction on the sorbent in the material of analysis.
Preferably, in described step 1), the setting sampling time is t (min), and sampling flow is s (m
3/ min).Be preferably sampling time each 30min, sampling flow 100mL/min(1 × 10
-4m
3/ min).Sampling time and sampling flow are with this understanding, better by the chromatographic peak type of gas chromatography/mass spectrometry, response is comparatively large, and within the adsorption capacity allowed band of adsorption tube.
Preferably, in described step 1), each two adsorption sampling pipes gather simultaneously.
2) preparation of menthol standard solution: accurately take a certain amount of menthol standard items to volumetric flask, be diluting solvent with ethanol, obtain menthol standard solution.
Preferably, described step 2) in the concentration of menthol standard solution be 0.2mg/ml.
3) drafting of menthol standard working curve: the step 2 pipetting a series of different volumes respectively) middle menthol standard solution, by gas-chromatography packed column injection port, use gas chromatographic sample introduction pin, inject adsorption sampling pipe respectively, the adsorption tube being adsorbed with menthol is placed in thermal desorption instrument, thermal desorption instrument is directly connected with GC/MS, menthol is brought GC/MS into by carrier gas and is detected after thermal desorption, obtain the linear relationship of menthol content and peak area, with corresponding its corresponding content (μ g) of menthol chromatographic peak area, draw corresponding standard working curve, calculate the regression equation of standard working curve.
Preferably, in described step 3), inject adsorption sampling pipe step 2) menthol standard solution volume be respectively 1 μ L, 2 μ L, 4 μ L, 8 μ L, 16 μ L.
Preferably, in described step 3), adsorption sampling pipe is connected with gas-chromatography packed column injection port, injector temperature is set: 150 DEG C; Helium gas flow: 90mL/min.
Preferably, in described step 3), the described method mechanism injecting menthol standard solution that is connected with gas-chromatography packed column injection port by adsorption sampling pipe is: be directly connected with screw cap with gas-chromatography packed column injection port by adsorption sampling pipe, when the method is used for production standard curve, by giving certain temperature and pressure (injector temperature 150 DEG C to packed column injection port; Helium gas flow 90mL/min) make menthol standard solution be injected into filled absorption in adsorption sampling pipe according to different volumes.The adsorption sampling pipe injecting menthol obtained is placed on thermal desorption instrument again and carries out desorption, and the menthol after desorption enters gas chromatograph-mass spectrometer analysis.(solution directly can not enter sampling pipe, can destroy the filler of sampling pipe, by gas-chromatography packed column injection port indirect sample introduction)
4) the online mensuration trapping menthol content in atmospheric sample: the sample being sealed in adsorption sampling pipe in step 1) is placed in thermal desorption instrument, thermal desorption instrument is directly connected with GC/MS, menthol is brought GC/MS into by carrier gas and is detected after thermal desorption, by the menthol chromatographic peak area obtained, substitute into the regression equation of step 3) Plays working curve respectively, calculate corresponding menthol content (μ g).
Preferably, in described step 3) and step 4), thermal desorption condition is:
Carrier gas: high-purity helium, carrier gas purity >=99.999%; Nebulizer gas pressure: 15.7psi; The pre-blowing time: 5min; Valve temperature: 200 DEG C; Transmission line temperature: 220 DEG C; One-level desorption temperature: 250 DEG C, keeps 30min; Desorption flow: 50mL/min; Import is shunted: 50mL/min; Secondary desorption temperature: 250 DEG C (heating rate: 20 DEG C/min), keeps 4min; Outlet manifold: 30mL/min.
Preferably, in described step 3) and step 4), GC/MS condition is:
GC conditions is: chromatographic column: Agilent DB-WAX capillary column (60m × 0.32mm i.d. × 0.25 μm df); Carrier gas: high-purity helium, carrier gas purity >=99.999%; Transmission line temperature: 220 DEG C; Heating schedule: initial temperature 40 DEG C keeps 5min, rises to 200 DEG C with the speed of 4 DEG C/min, keep 15min, the bulk analysis time is 60min.
Mass Spectrometry Conditions is: ion source temperature: 230 DEG C; Level Four bar temperature: 150 DEG C; Ionization mode: EI source; Ionizing energy: 70eV; Scan mode: full scan; Mass scan range: 35 ~ 350amu.
Preferably, NIST and Wiley standard spectrum storehouse is used to carry out library searching to data in described step 3) and step 4) qualitative.
5) mensuration of the menthol concentration of atmospheric sample in production environment: the menthol content calculated in the sampling time set in step 1), sampling flow and step 4) (μ g) is substituted into formula C=A/ (s × t), calculates the menthol concentration affecting production environment in process.
Preferably, in the formula of described step 5), C is menthol concentration (the μ g/m in production environment
3); A is that step 4) quantified by external standard method calculates corresponding menthol content (μ g); S is sampling flow (m
3/ min); T is sampling time (min).
As mentioned above, the present invention has following beneficial effect:
The present invention, by atmospheric sample in online capturing device trapping mentholated cigarette process, through thermal desorption-gas chromatograph-mass spectrometer (GCMS) analysis, then by formulae discovery, can measure the menthol concentration in mentholated cigarette production environment more accurately.Have the following advantages:
1. judge to compare with the present situation evaluated to the menthol concentration in production site air with the sense organ by means of only people, this method ensure that reliability and the objectivity of environment menthol quantitative result in Cigarette processing process.
2. the present invention is to production environment air without the need to carrying out pre-service, directly traps sample introduction, and have simple to operate, quantitatively reliable, analysis result feature accurately and effectively, the linear relationship of typical curve is good, correlation coefficient r
2=0.9999, method detects and is limited to 0.34 μ g/m
3, have higher sensitivity, in production environment, the recovery of menthol content is 97.92% ~ 102.38%, relative standard deviation RSD is 6.57%, has good accuracy and precision.
3. can analyse mentholated cigarette process scientifically to production environment influence degree, minimizing production line and production environment be polluted and is extremely important.
Visible, the present invention is that the menthol concentration measured in mentholated cigarette production environment provides a kind of quantitative detecting method reliably, has reality and theory value on mentholated cigarette process to the analysis that production environment affects.
Accompanying drawing explanation
The online capturing device schematic diagram of environment menthol in Fig. 1 mentholated cigarette process, the wherein compound adsorption sampling pipe of 1:Carbotrap349 tri-sections; 2: proofed sleeve; 3: gas collecting pump
Thermal desorption-gas chromatography-mass spectrum the chromatogram of Fig. 2 menthol standard model
Thermal desorption-gas chromatography-mass spectrum the chromatogram of online trapping atmospheric sample in Fig. 3 mentholated cigarette process
Embodiment
Set forth the present invention further below in conjunction with specific embodiment, should be understood that these embodiments are only not used in for illustration of the present invention and limit the scope of the invention.
Embodiment 1
1 material
1.1 instrument
6890GC/5973MS Gc/ms Analyser (Agilent company of the U.S.); TurboMatrix ATD thermal desorption instrument (Perkin Elmer company of the U.S.); Carbotrap349 adsorption sampling pipe, gas collecting pump (Supelco company of the U.S.); Flowmeter (AALBORG company of the U.S.).
1.2 reagent and sample
Cigarette sample (being selected from Shanghai Cigarette Factory); Menthol standard model (purity 99.0%, lark prestige Science and Technology Ltd.); Absolute ethyl alcohol (purity 99.9%, ACS grace section of U.S. chemistry).
2 methods
During for analyzing mentholated cigarette production, on the impact of surrounding environment, investigate the spread condition of menthol in production environment and concentration change situation is tested as follows: at same production site, 1# board produces mentholated cigarette, 2#, 3#, 4# board production other types simultaneously cigarette (with the distance of 1# board: 2#<3#<4#).
The process of 2.1 samples
The compound adsorption sampling pipe 1 of Carbotrap349 tri-sections is adopted to be connected on gas collecting pump 3 by proofed sleeve 2, the online capturing device of menthol in composition production environment air.Setting sampling time each 30min, sampling flow 100mL/min(1 × 10
-4m
3/ min).Online capturing device is positioned over respectively the jack connection place of 2#, 3#, 4# board, the surrounding air of trapping respective regions.Each two sampling pipes trap simultaneously.Start gas collecting pump and carry out sample trapping, continuously trapping 8 times.Gas collecting pump constantly aspirates production environment air by sampling flow, and when air is by being connected to the adsorption sampling pipe on pump, menthol contained in air is by the adsorbent of filling in adsorption tube.Sampling terminate rear sealed copper cap adsorption sampling pipe is taken off seal to be measured.
Accurately take 0.0100g menthol standard items to 50mL volumetric flask, and dilute constant volume with ethanol, obtain menthol standard solution.Be connected with gas-chromatography packed column injection port by adsorption sampling pipe, arranging injector temperature is 150 DEG C; Helium gas flow is 90mL/min.By gas chromatographic sample introduction pin, in sampling pipe, inject 1 μ L, 2 μ L, 4 μ L, 8 μ L, 16 μ L menthol standard solution respectively.With sealed copper cap by be measured for the adsorption sampling seal of tube.
The analysis of 2.2 samples
Menthol standard model in adsorption sampling pipe is carried out thermal desorption-GC/MS respectively detect, obtain the linear relationship of menthol content and peak area, with menthol chromatographic peak area for Y-axis, its corresponding content (μ g) is X-axis, draw corresponding standard working curve, calculate the regression equation of standard working curve.Analysis condition is:
(1) thermal desorption condition.Carrier gas: high-purity helium, carrier gas purity >=99.999%; Nebulizer gas pressure: 15.7psi; ; The pre-blowing time: 5min; Valve temperature: 200 DEG C; Transmission line temperature: 220 DEG C; One-level desorption temperature: 250 DEG C, keeps 30min; Desorption flow: 50mL/min; Import is shunted: 50mL/min; Secondary desorption temperature: 250 DEG C (heating rate: 20 DEG C/min), keeps 4min; Outlet manifold: 30mL/min.
(2) GC/MS condition.Agilent DB-WAX capillary chromatographic column (60m × 0.32mm i.d. × 0.25 μm df); Carrier gas: high-purity helium, carrier gas purity >=99.999%; Transmission line temperature: 220 DEG C; Heating schedule: initial temperature 40 DEG C keeps 5min, rises to 200 DEG C with the speed of 4 DEG C/min, keep 15min, the bulk analysis time is 60min.Ion source temperature: 230 DEG C; Level Four bar temperature: 150 DEG C; Ionization mode: EI source; Ionizing energy: 70eV; Scan mode: full scan; Mass scan range: 35 ~ 350amu.NIST and Wiley standard spectrum storehouse is used to carry out library searching to data qualitative.
The sample being sealed in adsorption sampling pipe is carried out thermal desorption-GC/MS analyze, be Y value by the menthol chromatographic peak area of acquisition, substitute into the regression equation of above-mentioned standard working curve respectively, calculate corresponding menthol content (μ g).
By the sampling time (min) of setting, sampling flow (m
3/ min) and instrument detect the menthol content (μ g) that obtains of quantified by external standard method and substitute into formula C=A/ (s × t), calculate menthol concentration (the μ g/m affecting production environment in process
3).
The regression equation of 2.3 working curves and method, detection limit, the recovery, precision
Accurately take 0.0100g menthol standard items to 50mL volumetric flask, and dilute constant volume with ethanol, obtain menthol standard solution.Adsorption sampling pipe is connected with gas-chromatography packed column injection port.Arranging injector temperature is 150 DEG C; Helium gas flow is 90mL/min.By gas chromatographic sample introduction pin, in sampling pipe, inject 1 μ L, 2 μ L, 4 μ L, 8 μ L, 16 μ L menthol standard solution respectively.The adsorption sampling pipe of the menthol solutions containing different volumes is carried out thermal desorption-GC-MS(gas chromatography-mass spectrography) analysis, obtains the regression equation (see table 1) of the linear relationship of menthol content and peak area, correlation coefficient r
2=0.9999.The analyte concentration corresponding to 3 times of signal to noise ratio (S/N ratio)s (S/N) produced on instrument with component in sample calculates qualitative detecting and is limited to 1.02ng, and substitute into formula C=A/ (s × t), the method for obtaining detects and is limited to 0.34 μ g/m
3.
Table 1 working curve and detection limit
Y: peak area; X: menthol content, μ g
In the adsorption sampling pipe containing known content menthol, inject the menthol of low high 3 different contents respectively, adopt thermal desorption-GC-MS(gas chromatography-mass spectrography) to measure, obtain the determination of recovery rates data of menthol content, the results are shown in Table 2.Simultaneously to same sample replicate determination 5 times (n=5), obtain the precision determination data of menthol content, the results are shown in Table 3.By table 2,3 display, in production environment, the recovery of menthol content is 97.92% ~ 102.38%, relative standard deviation RSD is 6.57%, show the accuracy of this method and precision better.
The recovery of menthol content in table 2 production environment
The precision (n=5) of menthol content in table 3 production environment
3 interpretations of result
Utilize the workstation software record atmospheric sample of thermal desorption-gas chromatograph-mass spectrometer (GCMS) and the spectrogram of menthol standard model, calculated by external standard method, obtain the environment menthol concentration (table 4) in each time period, each board region Cigarette processing process by spectrogram chromatographic peak area.
Table 4 environment menthol concentration measurement result
By relatively can see 2#, 3# and 4# board same time, along with the distance from the 1# board producing mentholated cigarette increases, in environment, menthol concentration presents decline trend.Because 3# and 4# board is all comparatively far away with 1# board, therefore environment menthol concentration is similar to.From the environment menthol concentration near same board, the menthol in environment in continuous production process, in progressively increasing trend.
4 conclusions
The present invention passes through to the online trapping of atmospheric sample in mentholated cigarette process, through thermal desorption-gas chromatograph-mass spectrometer (GCMS) analysis, ensure that reliability and the objectivity of environment menthol quantitative result in Cigarette processing process, provide a kind of simple and convenient, evaluate the method that mentholated cigarette process affects production environment accurately and effectively.From the environment menthol concentration near same board, the menthol in environment in continuous production process, in progressively increasing trend.Visible, the invention provides the quantivative approach of a kind of directly perceived, objective, science of knowing clearly, evaluating mentholated cigarette process affects production environment.
Claims (8)
1. the method analyzed mentholated cigarette process and production environment is affected, it is characterized in that, by the atmospheric sample in online capturing device trapping mentholated cigarette process, adopt thermal desorption-Gas chromatographyMass spectrometry, measure the menthol concentration in mentholated cigarette production environment, mainly comprise the following steps:
1) atmospheric sample is in thermal desorption online trapping before treatment, and the sampling flow set when trapping online and sampling time;
I, adsorption sampling pipe is connected on gas collecting pump by proofed sleeve, the online capturing device of menthol in air in composition production environment;
II, set sampling time and sampling flow, start gas collecting pump and trap;
III, gas collecting pump constantly aspirates production environment air by sampling flow, and when air is by being connected to the adsorption sampling pipe on pump, menthol contained in air is by the adsorbent of filling in adsorption tube;
IV, sampling terminates rear sealed copper cap by be measured for the adsorption sampling seal of tube;
Described adsorption sampling pipe is the compound adsorption sampling pipe of Carbotrap 349 3 sections;
2) preparation of menthol standard solution;
3) drafting of menthol standard working curve;
4) the online mensuration trapping menthol content in atmospheric sample;
Described thermal desorption condition is: carrier gas: high-purity helium, carrier gas purity >=99.999%; Nebulizer gas pressure: 15.7psi; The pre-blowing time: 5min; Valve temperature: 200 DEG C; Transmission line temperature: 220 DEG C; One-level desorption temperature: 250 DEG C, keeps 30min; Desorption flow: 50mL/min; Import is shunted: 50mL/min; Secondary desorption temperature: 250 DEG C, keeps 4min; Heating rate: 20 DEG C/min; Outlet manifold: 30mL/min;
Described GC/MS condition is:
GC conditions is: chromatographic column: Agilent DB-WAX capillary column; Carrier gas: high-purity helium, carrier gas purity >=99.999%; Transmission line temperature: 220 DEG C; Heating schedule: initial temperature 40 DEG C keeps 5min, rises to 200 DEG C with the speed of 4 DEG C/min, keep 15min, the bulk analysis time is 60min;
Mass Spectrometry Conditions is: ion source temperature: 230 DEG C; Level Four bar temperature: 150 DEG C; Ionization mode: EI source; Ionizing energy: 70eV; Scan mode: full scan; Mass scan range: 35 ~ 350amu; NIST and Wiley standard spectrum storehouse is used to carry out library searching to data;
5) mensuration of the menthol concentration of atmospheric sample in production environment.
2. a kind of method analyzed mentholated cigarette process and production environment is affected as claimed in claim 1, it is characterized in that, described step 2) be: accurately take a certain amount of menthol standard model to volumetric flask, be diluting solvent with ethanol, obtain menthol standard solution.
3. a kind of method analyzed mentholated cigarette process and affect production environment as claimed in claim 2, is characterized in that, the concentration of described menthol standard solution is 0.2 mg/ml.
4. a kind of method analyzed mentholated cigarette process and production environment is affected as claimed in claim 1, it is characterized in that, described step 3) be: the step 2 pipetting a series of different volumes respectively) middle menthol standard solution, by gas-chromatography packed column injection port, use gas chromatographic sample introduction pin, inject adsorption sampling pipe respectively, the adsorption tube being adsorbed with menthol is placed in thermal desorption instrument, thermal desorption instrument is directly connected with GC/MS, menthol is brought GC/MS into by carrier gas and is detected after thermal desorption, obtain the linear relationship of menthol content and peak area, with menthol chromatographic peak area its corresponding content corresponding, draw corresponding standard working curve, calculate the regression equation of standard working curve.
5. a kind of method analyzed mentholated cigarette process and affect production environment as claimed in claim 4, is characterized in that, the menthol standard solution volume injecting adsorption sampling pipe is respectively 1 μ L, 2 μ L, 4 μ L, 8 μ L, 16 μ L.
6. a kind of method analyzed mentholated cigarette process and affect production environment as claimed in claim 4, is characterized in that, be connected by adsorption sampling pipe, arrange injector temperature with gas-chromatography packed column injection port: 150 DEG C; Helium gas flow: 90mL/min.
7. a kind of method analyzed mentholated cigarette process and production environment is affected as claimed in claim 1, it is characterized in that, described step 4) be: by step 1) in be sealed in adsorption sampling pipe sample be placed in thermal desorption instrument, thermal desorption instrument is directly connected with GC/MS, menthol is brought GC/MS into by carrier gas and is detected after thermal desorption, by the menthol chromatographic peak area obtained, substitute into step 3 respectively) regression equation of Plays working curve, calculate corresponding menthol content.
8. as a kind of method analyzed mentholated cigarette process and affect production environment as described in arbitrary in claim 1-7, it is characterized in that, described step 5) be: by step 1) in sampling time of setting, sampling flow and step 4) in menthol content substitute into formula C=A/ (s × t), calculate the menthol concentration affecting production environment in process; In described formula, C is the menthol concentration in production environment, and A is step 4) calculate corresponding menthol content, s is sampling flow, and t is the sampling time.
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| CN103808849B (en) * | 2014-03-16 | 2015-01-07 | 国家烟草质量监督检验中心 | Method for measuring content of menthol in electronic cigarette liquid |
| CN103969386B (en) * | 2014-05-08 | 2015-09-02 | 浙江中烟工业有限责任公司 | Matrix Match correction-headspace gas chromatography measures the method for menthol content in the fine filter stick of vinegar |
| CN103954720B (en) * | 2014-05-08 | 2016-08-31 | 浙江中烟工业有限责任公司 | A kind of method of menthol content in rapid automatized mensuration cigarette shreds |
| CN104237428B (en) * | 2014-08-26 | 2015-12-30 | 上海烟草集团有限责任公司 | The assay method of menthol in a kind of smoke-free tobacco product |
| CN104931633B (en) * | 2015-06-05 | 2016-06-01 | 浙江中烟工业有限责任公司 | The measuring method of a kind of tobacco Dry distillated flavor chemical composition |
| CN109900844A (en) * | 2017-12-08 | 2019-06-18 | 南京天成环境科技工程有限公司 | A kind of Thermal desorption module of equilibrium air pressure |
| CN108845060A (en) * | 2018-09-04 | 2018-11-20 | 甘肃出入境检验检疫局检验检疫综合技术中心 | A kind of method of thermal desorption-gas chromatography/mass spectrometry analysis olive oil volatile flavor component |
| CN109557195A (en) * | 2018-09-27 | 2019-04-02 | 谱尼测试集团股份有限公司 | A kind of method of 82 kinds of volatile organic matters in accurate detection gas |
| CN110514760A (en) * | 2019-08-26 | 2019-11-29 | 上海烟草集团有限责任公司 | A kind of evaluation method of the cigarette package leakproofness based on chemical marker |
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