CN107014768B - Infrared spectrum analysis method for overall quality characteristics of cigarette mainstream smoke - Google Patents
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- 239000000779 smoke Substances 0.000 title claims abstract description 68
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 58
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 22
- 238000004458 analytical method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000001228 spectrum Methods 0.000 claims abstract description 10
- 238000007781 pre-processing Methods 0.000 claims abstract description 8
- 238000000265 homogenisation Methods 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 42
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 9
- 239000003546 flue gas Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000007405 data analysis Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 238000012844 infrared spectroscopy analysis Methods 0.000 claims 1
- 238000011156 evaluation Methods 0.000 abstract description 5
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 238000012827 research and development Methods 0.000 abstract description 3
- 238000004364 calculation method Methods 0.000 abstract description 2
- 238000012854 evaluation process Methods 0.000 abstract description 2
- 241000208125 Nicotiana Species 0.000 description 8
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 235000019505 tobacco product Nutrition 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 3
- 230000000391 smoking effect Effects 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 2
- 238000000668 atmospheric pressure chemical ionisation mass spectrometry Methods 0.000 description 2
- 150000001555 benzenes Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229960002715 nicotine Drugs 0.000 description 2
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000513 principal component analysis Methods 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000001926 trapping method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
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Abstract
The invention discloses an infrared spectrum analysis method for the overall quality characteristics of cigarette mainstream smoke, which completes the overall quality characteristics of the mainstream smoke of a sample cigarette by collecting smoke, starting and preprocessing a vacuum infrared spectrometer, deducting a background, collecting a spectrum and analyzing data. The method is suitable for analyzing and detecting the integral quality characteristics of the cigarette smoke, does not need to place a Cambridge filter to independently capture a grain phase part, can directly collect integral spectrum information of the mainstream smoke, can enhance the sensitivity of instrument analysis by background subtraction and data preprocessing, can conveniently calculate the principal component score of the sample by combining with a metrological calculation method, and the score represents the integral quality characteristics of the mainstream smoke of the sample. The score can be widely applied to classification, true and false smoke discrimination and homogenization evaluation of different samples. The whole evaluation process is rapid and accurate, has high sensitivity, and provides effective technical support for quality improvement and efficiency enhancement of cigarette products and research and development of new products.
Description
Technical Field
The invention relates to an analysis method for the overall quality characteristics of cigarette mainstream smoke, in particular to a method for directly analyzing the overall quality characteristics of the cigarette mainstream smoke by adopting a high-sensitivity vacuum Fourier transform infrared spectrometry.
Background
Cigarettes are a special consumer product which achieves a use effect by smoking, and the use performance of cigarettes depends on the effect of mainstream smoke on the sense organs of consumers. Therefore, only by researching the overall quality characteristics of the mainstream smoke of the cigarettes and establishing a comprehensive evaluation method of the mainstream smoke quality based on the overall quality characteristics, the smoking performance and the technical characteristics of the cigarette products can be reflected more truly and comprehensively, and the improvement of the quality of the cigarette products and the research and development of new products are facilitated.
The mainstream smoke can be divided into a gas phase part and a particle phase part, wherein the content of tar, nicotine and CO in the particle phase part is relatively high, and the tar, nicotine and CO are generally collected and detected by adopting a Cambridge filter. For the gas phase part, because the components are extremely complex and the collection and detection difficulty is high, the existing trapping method can only collect certain stable components in the main stream smoke and is difficult to trap active intermediate gas products. Therefore, the research on the mainstream smoke still stays at the offline detection level at present, and only certain specific components in the smoke can be detected and analyzed, for example, liu jian and the like establish a method for simultaneously and selectively detecting 7 benzene series in the mainstream smoke gas phase substances of cigarettes by adopting a cold trap trapping-gas chromatography-mass spectrometry (GC/MS) method (the cold trap trapping-gas chromatography-mass spectrometry method is used for determining the benzene series [ J ] in the mainstream smoke gas phase substances of the cigarettes [ tobacco science 2014, 4: 74-78 ]); the Maryuping et al connects the smoking machine with APCI-MS ion source by transformation, and after the cigarette mainstream smoke is filtered by Cambridge filter, the gas phase part is directly introduced into the ion source for analysis. A method for online analyzing 7 organic compounds such as acrylonitrile in cigarette mainstream smoke is established (APCI-MS/MS method for online analyzing the gradual release characteristics of the 7 organic compounds in mainstream smoke gas phase substances [ J ] tobacco science and technology, 2014, 1: 40-44.). The basis for evaluating the quality of a gas phase by using a part of components in the gas phase is obviously approximate, and the requirement of accurate evaluation of products is difficult to meet.
The infrared spectrum characteristic spectrum is an effective method for controlling the quality of tobacco and tobacco products, the infrared spectrum can reflect absorption signals of all main functional groups in molecules, the infrared spectrum of any molecule of the tobacco and tobacco products has uniqueness, the overall chemical characteristics of the tobacco and tobacco products can be reflected, and the method becomes an effective method for identifying the authenticity of the tobacco and tobacco products and controlling the quality of the tobacco and tobacco products. However, infrared spectroscopy has been used only for analysis and evaluation of liquid or solid (KBr) samples for a long time, and is rarely applied to direct analysis of gas samples, and particularly, research on direct integral analysis of cigarette mainstream smoke is not reported.
Disclosure of Invention
In order to solve the problem that the characteristics of the mainstream smoke of the cigarettes are difficult to analyze and evaluate directly, the invention provides an infrared spectrum analysis method for the overall quality characteristics of the mainstream smoke of the cigarettes.
The invention is realized by the following technical scheme: an infrared spectrum analysis method for the overall quality characteristics of cigarette mainstream smoke comprises the following steps:
(1) collecting flue gas: collecting the smoke of a cigarette sample to be detected by using a conventional cigarette smoke suction and trapping device, and placing the smoke in a sealed gas collection bag;
(2) starting and preprocessing a vacuum infrared spectrometer: opening a Fourier transform vacuum infrared spectrometer, preheating, purging residual air in an instrument gas pool by using air/nitrogen for 2 min, then closing an air inlet valve, opening a valve connected with a mechanical pump, pumping the vacuum degree of the gas pool to-100.00 KPa by using an external mechanical pump, and closing the mechanical pump and the valve connected with a sample pool;
(3) background subtraction: adopting the operation of the step (1), collecting air in an experimental environment as a background under the condition of not igniting cigarettes, collecting the air for 10 times in total, opening an air inlet valve of a sample cell each time when 100mL of air is collected, and closing the air inlet valve when the sample is fed to a pressure gauge for stable reading; collecting central infrared spectrum signal, using the signal as background signal, and measuring two parallel samples until the signal is stable;
(4) collecting a spectrum: connecting the sealed gas collecting bag in the step (1) with a sample inlet of a gas cell of an infrared spectrometer, opening a valve connected with a mechanical pump and a sample cell, opening the mechanical pump to pump the vacuum degree of the gas cell to-100.00 KPa again, closing the mechanical pump and the valve connected with the gas cell, opening an air inlet valve to enable smoke in the sealed gas collecting bag to enter the gas cell, and closing the air inlet valve to collect the infrared spectrum of the sample after the reading of a pressure gauge of the sample inlet is stable;
(5) and (3) data analysis: preprocessing the infrared spectrum obtained in the step (4) by using a self-adaptive background subtraction algorithm to improve the signal-to-noise ratio of the signal; and conventionally calculating the principal component score (PCA) of the filtered signal, wherein the score is the integral quality characteristic of the mainstream smoke of the sample cigarette.
The cigarette smoke sucking and trapping device has one mouth per time of sucking, the capacity is 100mL, the first mouth of mainstream smoke which is incompletely combusted is not collected, and 2-6 mouths of mainstream smoke is collected for each cigarette, wherein the total number of the 5 mouths of mainstream smoke is 5.
The invention has the advantages and effects that: the method for analyzing the overall quality characteristics of the cigarette smoke, namely the vacuum Fourier transform infrared spectroscopy, is suitable for analyzing and detecting the overall quality characteristics of the cigarette smoke, does not need to place a Cambridge filter to independently capture a grain phase part, can directly collect the overall spectral information of the mainstream smoke, can enhance the sensitivity of instrument analysis through background subtraction and data preprocessing, can conveniently calculate the score of a Principal Component (PCA) of a sample by combining with a metrological calculation method, and the score represents the overall quality characteristics of the mainstream smoke of the sample and evaluates the overall quality characteristics of the sample. The score can be widely applied to classification, true and false smoke discrimination and homogenization evaluation of different samples. The whole evaluation process is rapid and accurate, has high sensitivity, and provides effective technical support for quality improvement and efficiency enhancement of cigarette products and research and development of new products.
Drawings
FIG. 1 is a raw infrared spectrum of a sample of the flue gas of an example;
FIG. 2 is an infrared spectrum of a sample of flue gas from an example after pretreatment;
FIG. 3 is a graph of the principal component scores of the infrared spectra of the smoke samples of the examples.
Detailed Description
The present invention will be further described with reference to the following examples.
1. Reagents and materials:
the reagents used were, unless otherwise specified, analytically pure.
Nitrogen gas: n2 (purity is more than or equal to 99.99%).
100mL medical glass syringe (Tianjin sky wave instrument company)
2. Instruments and devices:
2.1 vacuum type Fourier transform infrared spectrometer (Vertex 80V Germany Bruker)
2.1.1 signal-to-noise ratio: 55000:1.
2.1.2 resolution: 0.06 cm-1。
2.1.3 wavenumber range: 50000-5 cm-1。
2.2 Smoke gas collecting bag (Borgwaldt KC, Germany)
2.2.11L volume gas collection bag
2.3 cigarette holder (Borgwaldt KC, Germany)
The cigarette holder can hold conventional cigarettes and fine cigarettes without placing Cambridge filter sheets inside.
2.4 mechanical pump (D60C Laibao Germany)
Purpose of the experiment: the application potential of the high-sensitivity infrared gas spectrum technology in cigarette mainstream smoke analysis is verified, the experimental reproducibility is discussed, and the application of the high-sensitivity infrared gas spectrum technology in smoke distinguishing of different types of cigarettes is tried.
Experimental materials: yuxi brand cigarette and Yunyan soft treasure cigarette.
The experimental process comprises the following steps:
(1) collecting flue gas: respectively collecting the smoke of a cigarette sample to be tested (Yuxi brand cigarette and Yunyan soft treasure cigarette) by using a conventional cigarette smoke suction and trapping device, and placing the smoke in a sealed gas collection bag; the cigarette smoke sucking and trapping device has one mouth per time of sucking, the capacity is 100mL, the first mouth of mainstream smoke which is incompletely combusted is not collected, and 2-6 mouths of mainstream smoke is collected for each cigarette, wherein the total number of the 5 mouths of mainstream smoke is 5.
5 mainstream smoke samples are collected from Yuxi brand cigarettes and Yunyan soft-treasure cigarettes respectively, the mainstream smoke samples are numbered 1-5 times before numbering, and the mainstream smoke samples are numbered 6-10 times after numbering.
(2) Starting and preprocessing a vacuum infrared spectrometer: opening a Fourier transform vacuum infrared spectrometer, preheating, purging residual air in an instrument gas pool by using air/nitrogen for 2 min, then closing an air inlet valve, opening a valve connected with a mechanical pump, pumping the vacuum degree of the gas pool to-100.00 KPa by using an external mechanical pump, and closing the mechanical pump and the valve connected with a sample pool;
(3) background subtraction: adopting the operation of the step (1), collecting air in an experimental environment as a background under the condition of not igniting cigarettes, collecting the air for 10 times in total, opening an air inlet valve of a sample cell each time when 100mL of air is collected, and closing the air inlet valve when the sample is fed to a pressure gauge for stable reading; collecting central infrared spectrum signal, using the signal as background signal, and measuring two parallel samples until the signal is stable;
(4) collecting a spectrum: connecting the sealed gas collecting bag in the step (1) with a sample inlet of a gas cell of an infrared spectrometer, opening a valve for connecting a mechanical pump and the sample cell, opening the mechanical pump to pump the vacuum degree of the gas cell to-100.00 KPa again, closing the mechanical pump and a valve connected with the gas cell, opening an air inlet valve to enable smoke in the sealed gas collecting bag to enter the gas cell, closing the air inlet valve after the indication of a sample inlet pressure meter is stable, and respectively collecting the infrared spectrum of the sample: the scanning times of the instrument are 24 times (the scanning times can be increased subsequently to improve the signal to noise ratio), and the spectral resolution is 1cm-1(ii) a As shown in fig. 1;
(5) and (3) data analysis: an infrared spectroscopy solution module of chempatern software (kemeien technologies ltd., china) is adopted to preprocess spectral data by an adaptive background subtraction algorithm so as to improve the signal-to-noise ratio of signals, as shown in fig. 2; and calculating the principal component scores (PC 1, PC2 and PC 3) of the filtered signals according to the conventional method, wherein the variance interpretation rates of the three principal component scores to the original variables are respectively as follows: 46.53%, 24.96% and 13.49%. The score is the overall quality characteristic of the mainstream smoke of the sample cigarette, as shown in the following table:
(6) and (3) verification: the discrimination of the two types of tobacco samples can be observed and classified according to the distribution of the three principal component scores (PC 1, PC2 and PC 3) in a mode space enclosed by coordinate axes.
Fig. 1 shows the original infrared spectrum of the flue gas sample, and it can be seen from the graph that the discrimination between the two types of flue gas samples is low, but the high-sensitivity infrared gas spectroscopy technology has good reproducibility in terms of reproducibility. The spectrum of fig. 1 was subjected to an automatic background subtraction operation, as shown in fig. 2, and in order to further verify the nuances of the smoke characteristics in fig. 2, the spectrum of fig. 2 was subjected to a principal component analysis, and the results are shown in fig. 3. As can be seen from FIG. 3, the long-optical-path infrared spectrum technology accurately extracts the subtle feature differences of two different types of flue gas samples, and is expected to be further applied to accurately distinguishing different types of flue gas by virtue of the chemometrics technology.
The samples numbered 1-10 are calculated to obtain respective principal component scores, the principal component scores are positioned at different positions in a mode space defined by coordinate axes, wherein the samples numbered 1-5 are positioned above a red dotted line in the figure, and are grouped into one type, namely Yuxi brand cigarettes; and No. 6-10 samples are positioned below the red dotted line and are also gathered into a category, so that the cigarette is a Yunyan soft treasure cigarette. Therefore, the method is applied to the accurate distinguishing of the overall quality characteristics of the smoke of different types and has good application potential.
Claims (2)
1. An infrared spectrum analysis method for characterizing the integral quality characteristics of cigarette mainstream smoke based on PCA score is characterized by comprising the following steps: the method is used for classifying different samples, judging true and false smoke and evaluating homogenization, and comprises the following steps:
(1) collecting flue gas: collecting the smoke of a cigarette sample to be detected by using a conventional cigarette smoke suction and trapping device, and placing the smoke in a sealed gas collection bag; collecting mainstream smoke of 2 nd to 6 th mouths and 5 mouths in total for each cigarette;
(2) starting and preprocessing a vacuum infrared spectrometer: opening a Fourier transform vacuum infrared spectrometer, preheating, purging residual air in an instrument gas pool by using air nitrogen for 2 min, then closing an air inlet valve, opening a valve connected with a mechanical pump, pumping the vacuum degree of the gas pool to-100.00 KPa by using an external mechanical pump, and closing the mechanical pump and the valve connected with a sample pool;
(3) background subtraction: adopting the operation of the step (1), collecting air in an experimental environment as a background under the condition of not igniting cigarettes, collecting the air for 10 times in total, opening an air inlet valve of a sample cell each time when 100mL of air is collected, and closing the air inlet valve when the sample is fed to a pressure gauge for stable reading; collecting central infrared spectrum signal, using the signal as background signal, and measuring two parallel samples until the signal is stable;
(4) collecting a spectrum: connecting the sealed gas collecting bag in the step (1) with a sample inlet of a gas cell of an infrared spectrometer, opening a valve connected with a mechanical pump and a sample cell, opening the mechanical pump to pump the vacuum degree of the gas cell to-100.00 KPa again, closing the mechanical pump and the valve connected with the gas cell, opening an air inlet valve to enable smoke in the sealed gas collecting bag to enter the gas cell, and closing the air inlet valve to collect the infrared spectrum of the sample after the reading of a pressure gauge of the sample inlet is stable;
(5) and (3) data analysis: preprocessing the infrared spectrum obtained in the step (4) by using a self-adaptive background subtraction algorithm to improve the signal-to-noise ratio of the signal; and conventionally calculating the principal component score of the filtered signal, wherein the score is the integral quality characteristic of the mainstream smoke of the sample cigarette.
2. The infrared spectroscopic analysis method of claim 1, wherein: the cigarette smoke sucking and trapping device has one mouth per time of suction and the capacity of 100 mL.
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| CN107340265B (en) * | 2017-08-09 | 2020-09-22 | 云南中烟工业有限责任公司 | Mainstream smoke authenticity identification and analysis device and analysis method |
| CN107462540B (en) * | 2017-08-09 | 2021-02-02 | 云南中烟工业有限责任公司 | Cigarette tipping paper color difference analysis device and method |
| CN107505286A (en) * | 2017-09-22 | 2017-12-22 | 中国烟草总公司郑州烟草研究院 | Oxygen consumption amount detecting device and detection method during a kind of cigarette is burnt and sucked |
| CN108801968B (en) * | 2018-06-05 | 2021-07-13 | 天津大学 | Cut tobacco overall quality characteristic analysis method based on vacuum infrared spectrum |
| CN109444326A (en) * | 2019-01-10 | 2019-03-08 | 云南中烟工业有限责任公司 | A kind of cigarette mainstream flue gas principal component trapping detection device and its analysis method |
| CN112749906A (en) * | 2021-01-14 | 2021-05-04 | 云南中烟工业有限责任公司 | Sensory evaluation method for spectrum data of cigarette mainstream smoke |
| CN112666086A (en) * | 2021-01-14 | 2021-04-16 | 云南中烟工业有限责任公司 | Coupling method of hollow waveguide infrared spectrometer and smoking machine |
| CN112881323B (en) * | 2021-01-14 | 2022-03-08 | 云南中烟工业有限责任公司 | Quality evaluation method of cigarette mainstream smoke |
| CN113484275B (en) * | 2021-07-08 | 2023-01-31 | 云南中烟工业有限责任公司 | Method for rapidly predicting oil content in fresh tobacco leaves by adopting peak separation analysis technology based on mid-infrared spectrum |
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