CN107014768A - The infrared spectrum analysis of cigarette mainstream flue gas total quality feature - Google Patents
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- CN107014768A CN107014768A CN201710386737.5A CN201710386737A CN107014768A CN 107014768 A CN107014768 A CN 107014768A CN 201710386737 A CN201710386737 A CN 201710386737A CN 107014768 A CN107014768 A CN 107014768A
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 60
- 239000003546 flue gas Substances 0.000 title claims abstract description 41
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 21
- 238000004458 analytical method Methods 0.000 title claims abstract description 20
- 238000001228 spectrum Methods 0.000 claims abstract description 12
- 239000000779 smoke Substances 0.000 claims abstract description 9
- 238000007405 data analysis Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 30
- 238000007789 sealing Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 230000006641 stabilisation Effects 0.000 claims description 6
- 238000011105 stabilization Methods 0.000 claims description 6
- 238000010926 purge Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 230000003044 adaptive effect Effects 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 12
- 238000011156 evaluation Methods 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 238000012356 Product development Methods 0.000 abstract description 2
- 238000000205 computational method Methods 0.000 abstract description 2
- 241000208125 Nicotiana Species 0.000 description 7
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000003595 mist Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 235000019505 tobacco product Nutrition 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000000668 atmospheric pressure chemical ionisation mass spectrometry Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007792 gaseous phase Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 238000000513 principal component analysis Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
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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
- 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
-
- 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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- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The present invention discloses a kind of infrared spectrum analysis of cigarette mainstream flue gas total quality feature, by collecting flue gas, the start of vacuum infrared spectrometer and pretreatment, background deduction, collection spectrum, data analysis, the total quality feature of the main flume of complete paired samples cigarette.The present invention is detected suitable for the analysis of cigarette smoke total quality feature, cambridge filter need not be placed to grain mutually part individually trapping, the overall spectrum information of main flume can directly be collected, pass through background deduction and data prediction, the sensitivity of Instrumental Analysis can be strengthened, the principal component scores of sample can be easily calculated with reference to meterological computational methods, score is the main flume total quality feature for characterizing the sample.The score can be widely applied to classify to different samples, true and false cigarette differentiates and the evaluation that homogenizes.Whole evaluation procedure is quick, accurate, sensitivity is high, and effective technical support is provided to cigarette product upgrading synergy and new-product development.
Description
Technical field
The present invention relates to a kind of analysis method of cigarette mainstream flue gas total quality feature, specially using highly sensitive
The method that vacuum type Fourier transform infrared spectrometry carries out Direct Analysis to the total quality feature of cigarette mainstream flue gas.
Background technology
Cigarette is a kind of special consumer goods that using effect is reached by sucking, and its performance depends on main flume pair
The sensory effect of consumer.Therefore, the total quality feature of cigarette mainstream flue gas is only studied, and main flow is set up based on this
The integrated evaluating method of flue gas quality, more truly could more fully reflect cigarette product sucks performance and technical characteristic,
It is more conducive to the lifting of cigarette product quality and the research and development of new product.
Main flume can be divided into gas phase and grain phase part, wherein, tar in grain phase part, nicotine, CO content it is larger, one
As trapped and detected using cambridge filter.For gas phase portion, because wherein component is extremely complex, detection difficulty is collected again
Larger, existing capture method can only all be collected into the stable component of some of main flume, it is difficult to catch active middle gas
Body product.So, the research to main flume still stays in offline inspection aspect at present, and can only realize some of flue gas spy
Composition detection and analysis are determined, for example, Liu Jian etc. is established using the means of cold trap trapping-gas chromatography-mass spectrography (GC/MS)
The method of 7 kinds of benzene homologues in simultaneous selection detection gaseous phase of main stream smoke of cigarette thing(Cold trap trapping-gas chromatography-mass spectrography is surveyed
Determine benzene homologues [J] the tobaccos science and technology in gaseous phase of main stream smoke of cigarette thing, 2014,4: 74-78.);Horse space equality is by changing
Make and be connected smoking machine with APCI-MS ion guns, after cigarette mainstream flue gas is filtered through cambridge filter, gas phase portion is introduced directly into
Analyzed in ion gun.The method for establishing 7 kinds of organic compounds such as acrylonitrile in on-line analysis cigarette mainstream flue gas
(7 kinds of organic compounds by mouth release characteristic [J] tobaccos section in APCI-MS/MS method on-line analysis main flume gas gas-phase objects
Skill, 2014,1: 40-44.).The foundation for being used as its quality evaluation with constituent part in gas gas-phase objects is clearly to take a part for the whole,
It is difficult to meet the demand that product is precisely assessed.
Infrared spectrum characteristic spectrum is the effective ways for controlling tobacco and tobacco product quality, and infrared spectrum can reflect point
The infrared spectrum of the absorption signal of all major function bases in son, any tobacco and tobacco product molecule all has uniqueness, energy
Reflect the total chemical characteristics of tobacco and tobacco product, one as discriminating tobacco and the tobacco product true and false, and its quality control
Plant effective ways.But infrared spectrum is all only used for liquid or solid for a long time(KBr)Sample is analyzed and evaluated, and is applied to
Carry out that Direct Analysis is also rarely found to gaseous sample, the research of direct global analysis is especially carried out to cigarette mainstream flue gas just not yet
Appear in the newspapers.
The content of the invention
The problem of being difficult to directly be analyzed and evaluated cigarette mainstream flue gas characteristic for solution is above-mentioned, the present invention proposes one
Plant the infrared spectrum analysis of cigarette mainstream flue gas total quality feature.
The present invention is realized by following technical proposal:A kind of infrared spectrum analysis of cigarette mainstream flue gas total quality feature
Method, by following each step:
(1)Collect flue gas:The flue gas that capturing device collects cigarette sample to be measured is aspirated with conventional cigarette flue gas, sealing gas collection is placed in
In bag;
(2)The start and pretreatment of vacuum infrared spectrometer:Fourier transform vacuum infrared spectrometer is opened, and is preheated,
With the air remained in air/nitrogen purging instrument gas cell, purge time is 2 min, is then shut off intake valve, is opened and machine
The valve that tool pump is connected, and the vacuum of gas cell is extracted into -100.00 KPa with external mechanical pump, close mechanical pump and
The valve being connected with sample cell;
(3)Background deduction:Using step(1)Operation, in the case of not lighting cigarette collect experimental situation in air make
For background, collect 10 times altogether, each 100mL air, open sample cell intake valve, during sample introduction to pressure gauge registration stabilization, close
Close intake valve;Mid-infrared light spectrum signal is gathered, and using this signal as background signal, signal can determine two Duplicate Samples, until
Untill signal stabilization;
(4)Gather spectrum:By step(1)Sealing collection airbag be connected with infrared spectrometer gas cell injection port, open machinery
The valve that pump is connected with sample cell, and open mechanical pump gas cell vacuum is evacuated to -100.00 KPa again, close mechanical pump
And its valve being connected with gas cell, intake valve is opened, the flue gas in sealing collection airbag is entered in gas cell, treats sample introduction
After mouth pressure gauge registration is stable, intake valve is closed, the infrared spectrum of sample is gathered;
(5)Data analysis:With adaptive background deduction arithmetic to step(4)Gained infrared spectrum is pre-processed, to lift letter
Number signal to noise ratio;The principal component scores of filtered signal are routinely calculated again(PCA), the score is the main flow of the sample cigarette
The total quality feature of flue gas.
Suction is a bite to the cigarette smoke suction capturing device every time, and capacity is 100mL, does not collect incomplete combustion
First main flume, every cigarette collects the 2nd~6 mouthful, totally 5 mouthfuls of main flume.
Advantage and effect that the present invention possesses:The analysis method for the cigarette smoke total quality feature that the present invention is provided, i.e.,
Vacuum type Fourier transform infrared spectrometry, it is adaptable to the analysis detection of cigarette smoke total quality feature, without placing Cambridge
Filter disc can directly collect the overall spectrum information of main flume to grain mutually part individually trapping, pre- by background deduction and data
Processing, can strengthen the sensitivity of Instrumental Analysis, the principal component of sample can be easily calculated with reference to meterological computational methods
(PCA)Score, score is the main flume total quality feature for characterizing the sample, and its total quality characteristic is evaluated.
The score can be widely applied to classify to different samples, true and false cigarette differentiates and the evaluation that homogenizes.Whole evaluation procedure is fast
Speed, accurate, sensitivity are high, and effective technical support is provided to cigarette product upgrading synergy and new-product development.
Brief description of the drawings
Fig. 1 is the original infrared spectrum of the flue gas sample of embodiment;
Fig. 2 is the flue gas sample infrared spectrum after pretreatment of embodiment;
Fig. 3 is the principal component scores figure of the flue gas sample infrared spectrum of embodiment.
Embodiment
With reference to embodiment, the present invention will be further described.
1st, reagent and material:
Unless otherwise specified, agents useful for same is that analysis is pure.
Nitrogen:N2(Purity >=99.99%).
100 mL medical glass syringes(Tianjin sky wave instrument company)
2nd, instrument and equipment:
2.1 vacuum type Fourier transformation infrared spectrometers(Brooker company of Vertex 80V Germany)
2.1.1 signal to noise ratio:55000:1.
2.1.2 resolution ratio:0.06 cm-1。
2.1.3 wave-number range:50000-5 cm-1。
2.2 flue gas collection airbags(German Borgwaldt KC companies)
2.2.1 the collection airbag of 1L volumes
2.3 cigarette clamping devices(German Borgwaldt KC companies)
Conventional cigarette and ramuscule cigarette are clamped, cambridge filter is not placed in inside.
2.4 mechanical pump(Lai Bao companies of D60C Germany)
Experiment purpose:Application potential of the highly sensitive infrared-gas spectral technique in cigarette mainstream flue gas analysis is verified, it is inquired into
Reappearance is tested, and attempts to be applied to the flue gas of different category cigarette and is distinguished.
Experiment material:The soft treasure cigarette of Yuxi brand cigarette, cloud and mist.
Experimentation:
(1)Collect flue gas:Cigarette sample to be measured is collected with conventional cigarette flue gas suction capturing device respectively(Yuxi brand cigarette,
The soft treasure cigarette of cloud and mist)Flue gas, be placed in sealing collection airbag in;Suction is one to the cigarette smoke suction capturing device every time
Mouthful, capacity is 100mL, does not collect the first main flume of incomplete combustion, every cigarette collects the 2nd~6 mouthful, totally 5 mouthfuls
Main flume.
Yuxi brand cigarette and the soft treasure cigarette of cloud and mist respectively collect 5 main flume samples, and numbering preceding 1~5 is Yuxi product
The main flume sample of board cigarette, numbering 6~10 is the main flume sample of the soft treasure cigarette of cloud and mist.
(2)The start and pretreatment of vacuum infrared spectrometer:Fourier transform vacuum infrared spectrometer is opened, and is carried out pre-
Heat, the air remained in instrument gas cell is purged with air/nitrogen, and purge time is 2 min, is then shut off intake valve, is opened
The valve being connected with mechanical pump, and the vacuum of gas cell is extracted into -100.00 KPa with external mechanical pump, close machinery
Pump and the valve being connected with sample cell;
(3)Background deduction:Using step(1)Operation, in the case of not lighting cigarette collect experimental situation in air make
For background, collect 10 times altogether, each 100mL air, open sample cell intake valve, during sample introduction to pressure gauge registration stabilization, close
Close intake valve;Mid-infrared light spectrum signal is gathered, and using this signal as background signal, signal can determine two Duplicate Samples, until
Untill signal stabilization;
(4)Gather spectrum:By step(1)Sealing collection airbag be connected with infrared spectrometer gas cell injection port, open machinery
The valve that pump is connected with sample cell, and open mechanical pump gas cell vacuum is evacuated to -100.00 KPa again, close mechanical pump
And its valve being connected with gas cell, intake valve is opened, the flue gas in sealing collection airbag is entered in gas cell, treats sample introduction
After mouth pressure gauge registration is stable, intake valve is closed, the infrared spectrum of sample is gathered respectively:Instrument scanning times are 24 times(Subsequently
Scanning times can be increased to lift signal to noise ratio), spectral resolution is 1cm-1;As shown in Figure 1;
(5)Data analysis:Using Chempattern softwares(Ke Maien Science and Technology Ltd.s, China)Infra-red sepectrometry solve
Module, is pre-processed with adaptive background deduction arithmetic to spectroscopic data, with the signal to noise ratio of promotion signal, as shown in Figure 2;Again
Routinely calculate the principal component scores of filtered signal(PC1、PC2、PC3), variance of three principal component scores to original variable
Explanation rate is respectively:46.53%th, 24.96% and 13.49%.It see the table below, the score is the whole of the main flume of the sample cigarette
Constitution measure feature:
(6)Checking:Pass through three principal component scores(PC1、PC2、PC3)Distribution feelings in the model space that reference axis is surrounded
Condition can observe the discrimination of two class tobacco samples, and be classified.
Fig. 1 shows the original infrared spectrum of flue gas sample, as seen from the figure, and the discrimination of two class flue gas samples is relatively low, but
For reappearance, highly sensitive infrared-gas spectral technique possesses good reappearance.Bales catch has been carried out to the spectrum in Fig. 1
Except background operation, as shown in Fig. 2 for the nuance of the smoke transportation in further proof diagram 2, entering to the spectrum in Fig. 2
Principal component analysis is gone, acquired results are as shown in Figure 3.As seen from Figure 3, long light path infrared spectrum technology is accurately extracted two classes not
With the fine feature difference of flue gas sample, by chemometric techniques, it is expected to further apply the standard of different category flue gases
Really distinguish.
The sample of numbering 1~10 obtains respective principal component scores by calculating, and principal component scores are surrounded in reference axis
Different positions is in model space, wherein 1~No. 5 sample is in figure above red dotted line, is polymerized to as a class, is beautiful
Small stream brand cigarette;And 6~No. 10 samples are in below red dotted line, also it is polymerized to as a class, is the soft treasure cigarette of cloud and mist.It can be seen that,
The present invention is accurately distinguished applied to different category flue gas total quality features, possesses good application potential.
Claims (2)
1. a kind of infrared spectrum analysis of cigarette mainstream flue gas total quality feature, it is characterised in that pass through following each step
Suddenly:
(1)Collect flue gas:The flue gas that capturing device collects cigarette sample to be measured is aspirated with conventional cigarette flue gas, sealing gas collection is placed in
In bag;
(2)The start and pretreatment of vacuum infrared spectrometer:Fourier transform vacuum infrared spectrometer is opened, and is preheated,
With the air remained in air/nitrogen purging instrument gas cell, purge time is 2 min, is then shut off intake valve, is opened and machine
The valve that tool pump is connected, and the vacuum of gas cell is extracted into -100.00 KPa with external mechanical pump, close mechanical pump and
The valve being connected with sample cell;
(3)Background deduction:Using step(1)Operation, in the case of not lighting cigarette collect experimental situation in air make
For background, collect 10 times altogether, each 100mL air, open sample cell intake valve, during sample introduction to pressure gauge registration stabilization, close
Close intake valve;Mid-infrared light spectrum signal is gathered, and using this signal as background signal, signal can determine two Duplicate Samples, until
Untill signal stabilization;
(4)Gather spectrum:By step(1)Sealing collection airbag be connected with infrared spectrometer gas cell injection port, open machinery
The valve that pump is connected with sample cell, and open mechanical pump gas cell vacuum is evacuated to -100.00 KPa again, close mechanical pump
And its valve being connected with gas cell, intake valve is opened, the flue gas in sealing collection airbag is entered in gas cell, treats sample introduction
After mouth pressure gauge registration is stable, intake valve is closed, the infrared spectrum of sample is gathered;
(5)Data analysis:With adaptive background deduction arithmetic to step(4)Gained infrared spectrum is pre-processed, to lift letter
Number signal to noise ratio;The principal component scores of filtered signal are routinely calculated again, and the score is the main flume of the sample cigarette
Total quality feature.
2. the infrared spectrum analysis of cigarette mainstream flue gas total quality feature according to claim 1, its feature exists
In:Suction is flatly, capacity is 100mL to the cigarette smoke suction capturing device every time, and every cigarette collects the 2nd~6 mouthful, altogether
5 mouthfuls of main flume.
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CN113484275A (en) * | 2021-07-08 | 2021-10-08 | 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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