CN105203653A - Cigarette paper quality stability testing method - Google Patents
Cigarette paper quality stability testing method Download PDFInfo
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- CN105203653A CN105203653A CN201510574784.3A CN201510574784A CN105203653A CN 105203653 A CN105203653 A CN 105203653A CN 201510574784 A CN201510574784 A CN 201510574784A CN 105203653 A CN105203653 A CN 105203653A
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Abstract
The invention discloses a cigarette paper quality stability testing method, which comprises the following steps of (1) respectively shearing cigarette paper samples with the same specifications in different batches into fragments, and then performing cracking, wherein the cracking conditions are as follows: the initial temperature is 300+/-20 DEG C, the temperature rise rate is 20+/-5 DEG C/ms, and the cracking temperature is 900+/-20 DEG C; (2) performing GC-MS (gas chromatography-mass spectrometer) analysis on cracking products, and obtaining the quality stability of the cigarette paper samples with the same specifications in different batches according to analysis results of aroma substances in the cracking products. The number of the cigarette paper samples with the same specifications in different batches is 3 to 5. The testing method has the advantages that the thermal cracking GC-MS is used; cigarette paper is subjected to heating cracking at a certain temperature in gas atmosphere; by analyzing the integral area change of ions extracted from aroma components in the cracking products of the cigarette paper with the same specifications in different batches, the test on the cigarette paper quality stability is realized.
Description
Technical field
The present invention relates to cigarette paper analysis technical field, be specifically related to a kind of method of testing of cigarette paper quality stability.
Background technology
Cigarette paper accounts for 5% of cigarette weight, in cigarette smoking process, participate in burning directly, has considerable influence to the burning performance of cigarette, fragrance and suction taste, and therefore, the steady quality controlling cigarette paper has vital role and meaning for maintenance cigarette smoking quality.
At present, produce and use quantitative, air permeability, Smoldering rate, the ash of enterprise to cigarette paper physical index of grading to set standard, simultaneously in conjunction with the measure such as detection, cigarette main stream flue gas index judgement of Combustion Improver in Cigarette Paper content, reach the object controlling cigarette paper quality.
In cigarette paper production run, can impact the compound that cigarette paper produces when participating in burning because of reasons such as the fluctuation of technique, the replacements of raw and auxiliary material, but usually cannot be judged by conventional sense means, therefore, it may be necessary the burning behavior that additive method investigates cigarette paper, and the quality stability of cigarette paper is evaluated.
Thermal cracking gas chromatography mass spectrometer can heat sample under the strict condition controlled, and qualitative and quantitative analysis is carried out to pyrolysis product, have sample size few, can the feature such as fast, the favorable reproducibility of direct injected, analysis speed, this device can by whole sample in moment evenly cracking simultaneously, there is the advantages such as heat time short, secondary reaction is few, be thus widely applied.
During cigarette smoking, the conditions such as the temperature residing for cigarette paper change greatly, and researcher adopts thermal cracking gas chromatography mass spectrometer to simulate the burning condition residing for cigarette paper, and carries out quantitative and semi-quantitative analysis to pyrolysis product.Wherein, by chromatographic peak ion figure and standard spectrum storehouse being compared, the qualitative analysis of pyrolysis product can be realized; When carrying out semi-quantitative analysis to pyrolysis product, then mainly adopting normalization method, is secondly ion peak areas representation.
Normalization method is using the ratio of single chromatographic peak area and total chromatogram peak area as analyzing something ratio shared in pyrolysis product, then can not judge for whether something generation in pyrolysis product is stable.Ion peak areas representation can be investigated the stability of something generation in pyrolysis product, but because cigarette paper pyrolysis product is more, the chromatographic peak of moieties there will be overlap, and prior art cannot be separated completely, interference can be caused to the integral result of pyrolysis product and the stability analysis of generation thereof.
Extracting ion method is carry out integration to a certain specific ion in something fragment ion in chromatogram, select assisting ion to carry out qualitative simultaneously, can reduce because the overlap of chromatographic peak is on the impact caused during integrating peak areas, have not yet to see it and be applied to cigarette paper cracking analysis.
Summary of the invention
The invention provides a kind of method of testing of cigarette paper quality stability, compared with conventional sense means, investigation can be carried out on reasons such as the replacements due to technological fluctuation, raw and auxiliary material on the impact of the compound that cigarette paper produces when participating in burning to analyze, controlling the steady quality of cigarette paper.
A method of testing for cigarette paper quality stability, comprises the following steps:
(1), after the cigarette paper sample of same size, different batches being cut into fragment respectively, carry out cracking, cracking condition is as follows:
Initial temperature: 300 ± 20 DEG C; Heating rate 20 ± 5 DEG C/ms; Cracking temperature: 900 ± 20 DEG C;
(2) GC-MS analysis is carried out to pyrolysis product, according to the analysis result of flavor matter in pyrolysis product, obtain the quality stability of cigarette paper sample of same size, different batches.
Cigarette paper is carried out cracking by the present invention under simulated conditions, chromatographic peak ion figure and standard spectrum storehouse are compared, realize the qualitative of cigarette paper pyrolysis product, the ion high to abundance in the standard mass spectral database in pyrolysis product corresponding to flavor matter carries out extraction integration, select assisting ion to carry out qualitative simultaneously, the relatively change of same size, different batches cigarette paper pyrolysis product extraction ion integral area, thus realize the evaluation to the quality stability of cigarette paper.
As preferably, the atmosphere of cracking is 9%O
2+ 91%N
2.Under this atmosphere, carry out cracking, make cracking process close to the combustion process of cigarette paper.
In order to obtain the characterization result of cigarette paper quality stability accurately, preferably, the quantity of the cigarette paper sample of same size, different batches is 3 ~ 5.
What emphasis of the present invention was weighed is, the quality stability of the cigarette paper sample of same size, different batches, because specification is identical, it is only a batch difference, thus the mass discrepancy of cigarette paper sample is very little, adopt conventional means cannot obtain this species diversity, and the present invention carries out thermal cracking to cigarette paper under suitable conditions, then GC-MS analysis is carried out to thermal cracking products, utilize analysis result can obtain less mass discrepancy.
As preferably, utilize NIST08 standard mass spectral database to retrieve pyrolysis product, carry out qualitative with matching degree >=85%.
As preferably, the ion high to the abundance in pyrolysis product corresponding to flavor matter carries out extraction integration, selects assisting ion qualitative.The flavor matter calculated in same batch of cigarette paper sample dissociation product extracts the mean value of ion integral area, and the relative standard deviation of mean value, if relative standard deviation≤20%, then and steady quality.
Select suitable GC-MS condition, the peak position of each ion in the pyrolysis product of acquisition and intensity are suitable for, and preferably, the Temperature Programmed Processes that described GC-MS analyzes is as follows:
Keep 1 ~ 2min at 40 ± 5 DEG C, then rise to 280 ± 20 DEG C with the heating rate of 5 ± 1 DEG C/min, keep 10 ~ 15min.
As preferably, the condition that described GC-MS analyzes is as follows:
Injector temperature: 280 ± 20 DEG C; Split ratio: 50:1; Carrier gas: He; Constant current mode; Flow velocity 1mL/min; Chromatographic column: DB-5MS; The solvent delay time: 3 ± 1min; Ionization mode: EI; Transmission line temperature: 280 ± 20 DEG C; Ion source temperature: 230 ± 10 DEG C; Level Four bar temperature: 150 ± 10 DEG C; Sweep limit: 35 ~ 500amu; Scan mode: full scan.
The present invention adopts thermal cracking gas chromatography mass spectrometer, heating pyrolyze is carried out under cigarette paper being placed in uniform temperature and atmosphere, extracted the change of ion integral area by the aroma component analyzed in same size, different batches cigarette paper pyrolysis product, realize the test to cigarette paper quality stability.
Embodiment
The present invention will be further described with the following Examples:
Get from cigarette paper stock in specification A, each dish of cigarette paper of two different batches, for each batch, after peelling off outer impaired paper, cuts along overall with and is no less than 20 layers, randomly draw 3 layers, as lysate sample.Two different batches are respectively batch A1 and batch A2, every one deck of each batch is as a lysate sample, i.e. batch A1 corresponding lysate sample A1-1, lysate sample A1-2, lysate sample A1-3, batch A2 corresponding lysate sample A2-1, lysate sample A2-2, lysate sample A2-3.
Proceed as follows for each lysate sample:
(1) lysate sample is cut into 1mm
2the little scraps of paper of left and right, take 2.00 (± 0.03) mg cigarette paper fragment and be placed in quartz ampoule, put into cracking instrument and carry out cracking, cracking condition is as follows:
Atmosphere: 9%O
2+ 91%N
2; Initial temperature (keeping 5s): 300 DEG C; Heating rate: 20 DEG C/ms; Cracking temperature (keeping 5s): 900 DEG C.
(2) carry out GC-MS analysis to pyrolysis product, analysis condition is as follows:
Injector temperature: 280 DEG C; Split ratio: 50:1; Carrier gas: He; Constant current mode; Flow velocity 1mL/min; Chromatographic column: DB-5MS (specification 60m × 0.25mm × 1 μm); Temperature programme: 40 DEG C keep 1min, then rise to 280 DEG C with the heating rate of 5 DEG C/min, keep 10min;
The solvent delay time: 3min; Ionization mode: EI; Transmission line temperature: 280 DEG C; Ion source temperature: 230 DEG C; Level Four bar temperature: 150 DEG C; Sweep limit: 35 ~ 500amu; Scan mode: full scan (SCAN).
(3) adopt the retrieval of NIST08 standard mass spectral database, carry out qualitative with matching degree >=85%.
(4) high to abundance in standard mass spectral database corresponding to flavor matter in pyrolysis product ion carries out extraction integration, selects assisting ion qualitative.
(5) calculate flavor matter in the thermal cracking products of specification A, same batch of 3 lysate sample and extract the mean value of ion integral area; Relatively in specification A, different batches lysate sample thermal cracking products, flavor matter extracts the relative standard deviation (RSD) of ion integration area average, namely obtains the difference of different batches sample, if RSD≤20%, then and steady quality.
The cigarette paper of specification A, in two batches of pyrolysis products, the com-parison and analysis result of flavor matter is as shown in table 1.
Table 1
As can be seen from data each in table 1, be all batch A1 of specification A and the steady quality of batch A2.
Claims (8)
1. a method of testing for cigarette paper quality stability, is characterized in that, comprises the following steps:
(1), after the cigarette paper sample of same size, different batches being cut into fragment respectively, carry out cracking, cracking condition is as follows:
Initial temperature: 300 ± 20 DEG C; Heating rate 20 ± 5 DEG C/ms; Cracking temperature: 900 ± 20 DEG C;
(2) GC-MS analysis is carried out to pyrolysis product, according to the analysis result of flavor matter in pyrolysis product, obtain the quality stability of cigarette paper sample of same size, different batches.
2. the method for testing of cigarette paper quality stability as claimed in claim 1, it is characterized in that, the quantity of the cigarette paper sample of same size, different batches is 3 ~ 5.
3. the method for testing of cigarette paper quality stability as claimed in claim 1, is characterized in that, utilize NIST08 standard mass spectral database to retrieve pyrolysis product, carry out qualitative with matching degree >=85%.
4. the method for testing of cigarette paper quality stability as claimed in claim 3, it is characterized in that, the ion high to the abundance in pyrolysis product corresponding to flavor matter carries out extraction integration, selects assisting ion qualitative.
5. the method for testing of cigarette paper quality stability as claimed in claim 4, it is characterized in that, the flavor matter calculated in same batch of cigarette paper sample dissociation product extracts the mean value of ion integral area, and the relative standard deviation of mean value, if relative standard deviation≤20%, then steady quality.
6. the method for testing of cigarette paper quality stability as claimed in claim 5, it is characterized in that, the atmosphere of cracking is 9%O
2+ 91%N
2.
7. the method for testing of cigarette paper quality stability as claimed in claim 6, is characterized in that, the Temperature Programmed Processes that described GC-MS analyzes is as follows:
Keep 1 ~ 2min at 40 ± 5 DEG C, then rise to 280 ± 20 DEG C with the heating rate of 5 ± 1 DEG C/min, keep 10 ~ 15min.
8. the method for testing of cigarette paper quality stability as claimed in claim 7, is characterized in that, the condition that described GC-MS analyzes is as follows:
Injector temperature: 280 ± 20 DEG C; Split ratio: 50:1; Carrier gas: He; Constant current mode; Flow velocity 1mL/min; Chromatographic column: DB-5MS; The solvent delay time: 3 ± 1min; Ionization mode: EI; Transmission line temperature: 280 ± 20 DEG C; Ion source temperature: 230 ± 10 DEG C; Level Four bar temperature: 150 ± 10 DEG C; Sweep limit: 35 ~ 500amu; Scan mode: full scan.
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Cited By (7)
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| CN106093355A (en) * | 2016-08-26 | 2016-11-09 | 浙江中烟工业有限责任公司 | A kind of evaluation methodology of cigarette paper safety |
| CN106404937A (en) * | 2016-08-26 | 2017-02-15 | 浙江中烟工业有限责任公司 | Cigarette paper type selection method in cigarette product quality maintenance |
| CN106979904A (en) * | 2017-03-30 | 2017-07-25 | 安徽中烟工业有限责任公司 | A kind of method for judging cigarette paper quality stability |
| CN108051521A (en) * | 2017-12-27 | 2018-05-18 | 浙江中烟工业有限责任公司 | A kind of test method of cigarette tipping paper quality stability |
| CN110057953A (en) * | 2019-04-28 | 2019-07-26 | 贵州中烟工业有限责任公司 | A kind of tobacco trademark papery amount control method |
| CN112763613A (en) * | 2020-12-28 | 2021-05-07 | 浙江中烟工业有限责任公司 | Method for determining quality stability of cigarettes |
| CN115575545A (en) * | 2022-10-28 | 2023-01-06 | 湖北中烟工业有限责任公司 | Method for measuring thermal cracking products of cigarette paper |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093355A (en) * | 2016-08-26 | 2016-11-09 | 浙江中烟工业有限责任公司 | A kind of evaluation methodology of cigarette paper safety |
| CN106404937A (en) * | 2016-08-26 | 2017-02-15 | 浙江中烟工业有限责任公司 | Cigarette paper type selection method in cigarette product quality maintenance |
| CN106979904A (en) * | 2017-03-30 | 2017-07-25 | 安徽中烟工业有限责任公司 | A kind of method for judging cigarette paper quality stability |
| CN106979904B (en) * | 2017-03-30 | 2019-11-29 | 安徽中烟工业有限责任公司 | A method of determining cigarette paper quality stability |
| CN108051521A (en) * | 2017-12-27 | 2018-05-18 | 浙江中烟工业有限责任公司 | A kind of test method of cigarette tipping paper quality stability |
| CN110057953A (en) * | 2019-04-28 | 2019-07-26 | 贵州中烟工业有限责任公司 | A kind of tobacco trademark papery amount control method |
| CN112763613A (en) * | 2020-12-28 | 2021-05-07 | 浙江中烟工业有限责任公司 | Method for determining quality stability of cigarettes |
| CN115575545A (en) * | 2022-10-28 | 2023-01-06 | 湖北中烟工业有限责任公司 | Method for measuring thermal cracking products of cigarette paper |
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Application publication date: 20151230 |