CN101334387B - Cigarette filter stick triacetyl glycerine determination method - Google Patents
Cigarette filter stick triacetyl glycerine determination method Download PDFInfo
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- CN101334387B CN101334387B CN 200810071562 CN200810071562A CN101334387B CN 101334387 B CN101334387 B CN 101334387B CN 200810071562 CN200810071562 CN 200810071562 CN 200810071562 A CN200810071562 A CN 200810071562A CN 101334387 B CN101334387 B CN 101334387B
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- triacetyl glycerine
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Abstract
The invention discloses a triacetyl glycerine measuring method of cigarette filtering sticks, which comprises following ordered steps: a sample filtering stick is prepared; triacetyl glycerine content is measured; spectral scanning is implemented so as to obtain a near infrared spectrogram of the sample filtering stick; a model is set up so as to correlate the near infrared spectrogram of the sample filtering stick that is preprocessed with the corresponding triacetyl glycerine content, a spectral region range and an optimal main factor number are chosen, and the partial least square method is adopted for setting up a mathematical model between the near infrared spectrum and the triacetyl glycerine content of the sample filtering stick, and the mathematical model is stored into a storage; the filtering sticks are randomly inspected on the spot so as to obtain the near infrared spectrograms of the filtering sticks, then the comparison with the mathematical model in the storage is carried out, thus obtaining the triacetyl glycerine content in the randomly inspected filtering sticks. The triacetyl glycerine measuring method has the advantages of accurate detecting results, simple and convenient operations, time-saving and labor-saving effects, good detecting result repetitiveness and high sensitivity, and is suitable for being used for measuring and analyzing mass samples in workshops and monitoring the feeding amount of the triacetyl glycerine in the production process of the filtering sticks.
Description
One. technical field
The present invention relates to a kind of assay method of cigarette filter stick triacetyl glycerine.
Two. background technology
Triacetyl glycerine commonly used is as plastifier, hardening agent in the filter stick formation technology, and the target consumption of triacetyl glycerine is generally the 6-10% of filter stick general assembly (TW).Because the content of triacetyl glycerine directly has influence on the hardness, resistance to suction of filter stick etc., even can have influence on the aesthetic quality of cigarette smoke.If its content is low excessively, the hardness of filter stick is just not enough, the tipping operation and the performance of filter stick and Cigarette will directly be influenced, if its content is too high, triacetyl glycerine can be transferred to flue gas more, thereby the aesthetic quality of negative effect cigarette smoke is so the content of the triacetyl glycerine in the filter stick is a leading indicator of filter rod quality, of crucial importance for the quality control of filter stick formation technology.
Triacetyl glycerine Determination on content method in the filter stick mainly contains gravimetric method, saponification method, vapor-phase chromatography, liquid phase chromatography, near infrared spectroscopy at present.Gravimetric method is applicable to the workshop fast-field evaluation, but its degree of accuracy is not high; Saponification method is the triacetyl glycerine content that the method for tobacco business standard YCT144-1998 regulation is measured filter stick, but that it is operated is loaded down with trivial details time-consuming; Vapor-phase chromatography, liquid phase chromatography detect the degree of accuracy height, but its operation is wasted time and energy and difficulty is used for the on-the-spot mensuration in batches in workshop; Near-infrared spectrum technique is a kind of quick, easy assay method, be widely used in agricultural at present, forestry, papermaking, tobacco, tealeaves, food, the kind discriminating of petrochemical industry and Chinese herbal medicine and the quality control of production run, someone attempts near-infrared spectrum technique is used for measuring the triacetyl glycerine content of filter stick, its pre-treatment process often needs the outer field forming paper of filter stick is peeled off, and filter stick is pulverized with comminutor, during in enormous quantities mensuration, also need high-frequency cleaning comminutor, the whole operation process is loaded down with trivial details, waste time and energy, have high input, can not be used for the on-the-spot batch detection in workshop.
Therefore seek a kind of energy and measure the effective ways of the triacetyl glycerine content of filter stick fast, accurately, in batches, have the meaning of outbalance.
Three. summary of the invention
The assay method that the purpose of this invention is to provide a kind of cigarette filter stick triacetyl glycerine can be measured the triacetyl glycerine content in the filter stick fast, accurately, in batches
The assay method of cigarette filter stick triacetyl glycerine, this method comprises following sequential steps:
(1) preparation filter stick, preparation triacetyl glycerine content is the sample filter stick of 1-15%;
(2) measure content, adopt the accurate content of the method working sample filter stick triacetyl glycerine of the gas Chromatographic Determination filter stick triacetyl glycerine content that international tobacco research establishment recommends;
(3) spectral scan after 40～50 filter sticks are tightened, is directly put into rotating cup and is carried out spectral scan with ft-nir spectrometer, obtains the near infrared spectrogram of sample filter stick;
(4) set up model, the near infrared spectrogram of sample filter stick is carried out after the pre-treatment carrying out relatedly with corresponding triacetyl glycerine content, be chosen in 8000.00～7000.00cm
-1And 4800.00～4200.00cm
-1In the spectrum district scope, best main cause subnumber 10 adopts partial least square method to set up near infrared spectrum and the sample filter stick mathematical model between triacetyl glycerine content and deposit in the storer;
(5) filter stick detects, after 40～50 filter sticks of spot sampling check are tightened, also directly put into rotating cup and carry out spectral scan with ft-nir spectrometer, the near infrared spectrogram that obtains the sampling observation filter stick again with storer in mathematical model compare and can obtain the content of triacetyl glycerine in the filter stick.
The assay method of cigarette filter stick triacetyl glycerine further may further comprise the steps:
The technological parameter of spectral scan can be decided to be: spectral range 10000～3800cm
-1, interval 4cm
-1, resolution 8cm
-1, scanning times 69 times.
To the spectrum pre-service:
(1) adopt the multicomponent signal correction to eliminate the inhomogeneous difference of bringing of sample;
(2) the employing segment length is 9, is spaced apart 5 the level and smooth spectrum of Norris's derivative filtering, eliminates the low-frequency information that high frequency noise remains with usefulness;
(3) adopt second-order differential to handle, eliminate the influence of baseline wander, obtain than more high resolving power and the spectral profile variation more clearly of former spectrum.
The near infrared spectrometer market that can be used as the present invention's use is easily purchased.
Advantage of the present invention:
1. testing result is accurate, easy and simple to handle, time saving and energy saving.
2. testing result good reproducibility, highly sensitive.
3. be suitable for the determination and analysis of workshop batch samples, but and the triacetyl glycerine applied amount of filter stick in the monitoring industrial processes.
Four. description of drawings
Fig. 1 is the assay method process flow diagram according to a kind of cigarette filter stick triacetyl glycerine of the present invention's proposition.
Fig. 2 is the actual value of cigarette filter stick triacetyl glycerine and the scatter diagram of model predication value.
Fig. 3 is the actual value of cigarette filter stick triacetyl glycerine and the deviation profile figure of model predication value.
Below in conjunction with accompanying drawing the present invention is done to describe in further detail.
Five. embodiment
As shown in Figure 1, the assay method of cigarette filter stick triacetyl glycerine of the present invention, this method comprises following sequential steps:
(1) preparation filter stick, preparation triacetyl glycerine content is the sample filter stick of 1-15%;
(2) measure content, adopt the accurate content of triacetyl glycerine of the triacetyl glycerine content method working sample filter stick of the gas Chromatographic Determination filter stick that international tobacco research establishment recommends;
(3) spectral scan after 40～50 filter sticks are tightened, is directly put into rotating cup and is carried out spectral scan with ft-nir spectrometer, obtains the near infrared spectrogram of sample filter stick;
(4) set up model, the near infrared spectrogram of sample filter stick is carried out carrying out related with corresponding triacetyl glycerine content after the pre-treatment, select suitable spectrum district scope and optimum number of principal components, adopt partial least square method to set up near infrared spectrum and the sample filter stick mathematical model between triacetyl glycerine content and deposit in the storer;
(5) filter stick detects, after 40～50 filter sticks of spot sampling check are tightened, also directly put into rotating cup and carry out spectral scan with ft-nir spectrometer, the near infrared spectrogram that obtains the sampling observation filter stick again with storer in mathematical model compare and can obtain the content of triacetyl glycerine in the filter stick.
The assay method of cigarette filter stick triacetyl glycerine further may further comprise the steps:
(1) technological parameter of spectral scan can be decided to be: spectral range 10000～3800cm
-1, interval 4cm
-1, resolution 8cm
-1, scanning times 69 times.
(2) to the spectrum pre-service:
A. adopt the multicomponent signal correction to eliminate the inhomogeneous difference of bringing of sample;
B. to adopt the segment length be 9, be spaced apart 5 the level and smooth spectrum of filtering, eliminates the low-frequency information that high frequency noise remains with usefulness;
C. adopt second-order differential to handle, eliminate the influence of baseline wander, obtain than more high resolving power and the spectral profile variation more clearly of former spectrum.
With reference to Fig. 2, the actual value of cigarette filter stick triacetyl glycerine and the scatter diagram of model predication value, wherein the related coefficient of mathematical model is 0.99869, the modeling standard deviation is 0.135.
With reference to Fig. 3, the actual value of cigarette filter stick triacetyl glycerine and the deviation profile figure of model predication value, all deviations satisfy the requirement of actual production process to the cigarette filter stick triacetyl glycerine control accuracy in ± 0.3.
Detect testing result such as following table according to the method for the invention and international tobacco research establishment recommend method respectively to criticizing filter stick triacetyl glycerine content together:
As seen from the table, the mean relative deviation of measurement result of the present invention is 2.69%, correlation analysis shows, two kinds of method acquisition results' related coefficient is 0.99826, correlativity reaches utmost point level of signifiance P＜0.01, carry out the conspicuousness paired t-test and show, the result that two kinds of methods obtain does not have significant difference P=0.53209＞0.05.And this method is measured about 3 minutes of a used time of sample, is less than the international used time of tobacco research establishment recommend method far away.
Claims (2)
1. the assay method of cigarette filter stick triacetyl glycerine, this method comprises following sequential steps:
(1) preparation filter stick, preparation triacetyl glycerine content is the sample filter stick of 1-15%;
(2) measure content, adopt the accurate content of triacetyl glycerine of the triacetyl glycerine content method working sample filter stick of the gas Chromatographic Determination filter stick that international tobacco research establishment recommends;
(3) spectral scan after 40～50 filter sticks are tightened, is directly put into rotating cup and is carried out spectral scan with ft-nir spectrometer, obtains the near infrared spectrogram of sample filter stick;
(4) set up model, the near infrared spectrogram of sample filter stick is carried out the inhomogeneous difference of bringing of (a) employing multicomponent signal correction elimination sample in advance, (b) to adopt the segment length be 9, be spaced apart 5 the level and smooth spectrum of Norris's derivative filtering, eliminate the low-frequency information that high frequency noise remains with usefulness, (c) adopt second-order differential to handle, eliminate the influence of baseline wander, acquisition is more carried out relatedly with triacetyl glycerine content accordingly after high resolving power and the processing that changes of spectral profile more clearly than former spectrum, is chosen in 8000.00～7000.00cm
-1And 4800.00～4200.00cm
-1In the spectrum district scope, best main cause subnumber 10 adopts partial least square method to set up near infrared spectrum and the sample filter stick mathematical model between triacetyl glycerine content and deposit in the storer;
(5) filter stick detects, after 40～50 filter sticks of spot sampling check are tightened, also directly put into rotating cup and carry out spectral scan with ft-nir spectrometer, the near infrared spectrogram that obtains the sampling observation filter stick again with storer in mathematical model compare and can obtain the content of triacetyl glycerine in the filter stick.
2. the assay method of cigarette filter stick triacetyl glycerine according to claim 1, the technological parameter of this method spectral scan can be decided to be: spectral range 10000～3800cm
-1, interval 4cm
-1, resolution 8cm
-1, scanning times 69 times.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101666785B (en) * | 2009-09-09 | 2012-05-09 | 广东中烟工业有限责任公司 | Method for quantitatively detecting components in glycerol triacetate for tobacco |
| CN105891147A (en) * | 2016-03-30 | 2016-08-24 | 浙江中烟工业有限责任公司 | Near infrared spectrum information extraction method based on canonical correlation coefficients |
| CN110006843B (en) * | 2019-04-15 | 2024-02-09 | 深圳烟草工业有限责任公司 | Filter stick forming machine for detecting filter sticks on line in real time |
| CN110174417A (en) * | 2019-05-05 | 2019-08-27 | 贵州中烟工业有限责任公司 | The quantitative detecting method of glyceryl triacetate in a kind of filter stick |
| CN111077103A (en) * | 2019-11-30 | 2020-04-28 | 贵州中烟工业有限责任公司 | Method for measuring content of glyceryl triacetate |
| CN113740290A (en) * | 2021-08-23 | 2021-12-03 | 浙江中烟工业有限责任公司 | Near-infrared rapid analysis method for content of glycerol in heated cigarette tobacco shreds |
| CN114397269B (en) * | 2022-01-25 | 2023-12-08 | 湖北中烟工业有限责任公司 | Method for measuring content of triacetin in cigarette filter stick |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2006092962A1 (en) * | 2005-02-28 | 2006-09-08 | Japan Tobacco Inc. | Multi-filter rod inspection device for cigarettes |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006092962A1 (en) * | 2005-02-28 | 2006-09-08 | Japan Tobacco Inc. | Multi-filter rod inspection device for cigarettes |
Non-Patent Citations (4)
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| 曹建国等.近红外漫反射光谱法测试醋酸纤维滤棒中的三醋酸甘油酯.《烟草科技》.2005,(第3期),第6－9页. * |
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