CN107340265B - Mainstream smoke authenticity identification and analysis device and analysis method - Google Patents
Mainstream smoke authenticity identification and analysis device and analysis method Download PDFInfo
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Abstract
The invention relates to a mainstream smoke authenticity identification and analysis device and an analysis method, the device comprises a smoking machine, a heating device, a filtering device, an annular optical fiber pool, an infrared light incidence device and a detection device which are connected in sequence, the annular optical fiber pool comprises an annular pool body, a sample inlet arranged at one end of the annular pool body and a sample outlet arranged at the other end of the annular pool body, the infrared incidence device is arranged at one side of the sample outlet, the detection device is arranged at one side of the sample inlet, the outlet of the filtering device is connected with the sample inlet of the annular pool body, a buffer gas supply device is arranged between the smoking machine and the heating device, and the device further comprises a PLC controller connected with the smoking machine, the heating device, the filtering device, the annular optical fiber pool, the infrared light incidence device, the buffer gas. The whole identification process is rapid, accurate and high in 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 device, in particular to a mainstream smoke authenticity identification and analysis device and a method for identifying the authenticity of mainstream smoke by using the device, belonging to the field of instrument analysis.
Background
China is a big cigarette production country, the cigarette yield is high, and the production brands are numerous. Although various measures are taken by the country and the tobacco monopoly management is continuously strengthened, a large amount of counterfeit cigarettes flow into the market, and the benefits of the country, enterprises and consumers are seriously damaged. Therefore, the cigarette counterfeit is one of the important problems discussed and researched by cigarette manufacturing enterprises and tobacco law enforcement supervision departments, and is also a topic which is commonly concerned by vast cigarette consumers.
In the cigarette fake making process, the key point is that the fake can be distinguished and determined immediately, so that lawless persons who make and sell fake cigarettes can be restrained in time. Although, with the continuous development and progress of the cigarette industry, various advanced anti-counterfeiting technologies are used for cigarette products, most of the anti-counterfeiting technologies are often applied to cigarette packages, such as fluorescence technology, laser holograms and the like. However, with the advanced development of modern science and technology, the technology of fake making and fake making is also increasing day by day, and the high-tech of fake and inferior cigarettes appears, so that fake cigarettes and real cigarettes are more and more difficult to distinguish on the outer package, and the degree of fake and genuine cigarettes is achieved. It has become increasingly frustrating to identify the authenticity of a cigarette by conventional means alone, such as by identifying an appearance feature or an anti-counterfeit label. Especially, when counterfeit products with similar external packaging and internal quality are encountered, the identification is only carried out by the appearance anti-counterfeiting technology, so that the method is very important.
Furthermore, instrument identification and inspection methods, smoking identification and inspection methods and sensory identification and inspection methods are used for identification at present, and among the three identification methods, the sensory identification and inspection method is the most commonly used cigarette authenticity identification method, but in the actual identification work, the sensory identification and inspection methods and the smoking identification and inspection methods are influenced by various factors, such as the change of tobacco shred formulas, the occupational level and experience of detection personnel and the like, and the authenticity judgment accuracy of cigarettes can be influenced. Although the instrument identification method is also listed as one of the methods for identifying the authenticity of the cigarette, no specific test items and contents exist. There are also related researches in this field, for example, a qualitative mathematical model is established by using a near infrared spectrum detection technology to discriminate the authenticity of cigarettes, and factor analysis and cluster analysis are performed on mainstream smoke indexes to assist in discriminating the authenticity of cigarettes (near infrared qualitative analysis method [ J ] for cigarette authenticity discrimination, tobacco technology, 2008, 11: 5-8.). However, these methods have respective limitations, for example, the near infrared technology can be well modeled to predict the content of some macroscopic indicators in the cigarette, such as total sugar, total nitrogen, nicotine, chlorine, etc. But due to its sensitivity limitations, it is not ideal for the characterization and prediction of most micro and trace species in tobacco. Meanwhile, due to the fact that the geometric structure and filling of the three threads are not uniform, when near infrared is used for analysis, the three threads are easily interfered and influenced by diffuse reflection light of the tobacco threads, the cut stems and the thin slices, and accuracy of an analysis result is affected.
The main stream smoke indexes are adopted for evaluation, so that the problems can be effectively overcome, but because the components of the main stream smoke are extremely complex, the collection and detection difficulty of a gas phase part is higher, the existing trapping method can only collect certain stable components in the main stream smoke, and active intermediate gas products are difficult to capture.
Therefore, the current research on the mainstream smoke is still in off-line detection, and only certain specific components in the smoke can be detected and analyzed, so that the requirement for accurate evaluation of product identification is difficult to meet. Therefore, research and development of a device and a method for identifying the authenticity of cigarettes with higher accuracy are urgently needed.
Disclosure of Invention
In order to solve the problem that the cigarette is directly analyzed and identified by using the mainstream smoke characteristics of the cigarette, the invention provides a mainstream smoke true-false identification and analysis device, which has the following specific scheme:
the utility model provides a mainstream flue gas true and false authentication analytical equipment, including the smoking machine that connects gradually, heating device, filter equipment, annular optical fiber tank, infrared light incidence device and detection device, annular optical fiber tank includes annular cell body, locate the introduction port of annular cell body one end, locate the appearance mouth of the annular cell body other end, infrared incidence device locates appearance mouth one side, detection device locates introduction port one side, the filter equipment export links to each other with the introduction port of annular cell body, still be equipped with buffer gas air feeder between smoking machine and the heating device, still include and the smoking machine, heating device, filter equipment, annular optical fiber tank, infrared light incidence device, the PLC controller that buffer gas air feeder and detection device are connected.
Further, the annular pool body is an annular hollow capillary column, the inner diameter is 0.2mm, the length is 10m, the inner wall of the annular pool body is coated with an Ag/AgI composite coating, and the quantity ratio of Ag to AgI is 1:1, the coating thickness was 0.15. mu.m.
Furthermore, three-way valves are arranged at two ends of the annular tank body, one end of the three-way valve at the sampling end is connected with the annular tank body, the other end of the three-way valve at the sampling end is connected with the detection device, the rest end of the three-way valve at the sampling end is a sampling port, one end of the three-way valve at the sampling end is connected with the annular tank body, the other end of the three-way valve at the sampling end is connected with the infrared incidence device.
Further, heating device includes the body, locate the flue gas passageway in the body, locate the heat conduction material between flue gas pipeline and the body, locate heating element and a plurality of temperature sensor around the flue gas passageway.
Further, the pipe body is a hollow rectangular plastic body, the smoke channel is a thin copper pipe, the heating elements are heating resistance wires arranged around the smoke channel, the heating resistance wires are rectangular frames surrounding the smoke channel, the heat conduction material is fibrous aluminum silicate wool, the plurality of temperature sensors are arranged nearby the heating resistance wires, and the heating resistance wires and the plurality of temperature sensors are connected with the PLC.
Further, the aperture of the filter disc of the filter device is 2 μm.
Further, the detection device is a diode array detector, and the infrared light incidence device is a two-dimensional correlation infrared spectrometer.
The invention relates to a method for discriminating authenticity of mainstream smoke by using the device, which comprises the following steps:
(1) starting and preprocessing an infrared incidence device: opening an infrared incidence device for preheating, emitting the mid-infrared spectrum in tandem, purging residual air in a heating device, a filtering device and an annular optical fiber pool by using buffer gas, then closing a valve at a sample inlet, closing a buffer gas supply device, opening a valve at a sample outlet, vacuumizing, and then closing the valve at the sample outlet;
(2) background collection: opening a sample inlet valve of the annular optical fiber cell, collecting inert gas in an experimental environment as a background, and closing an air inlet valve when the sample is injected until the reading of a pressure gauge is stable; collecting two-dimensional mid-infrared spectrum signals, taking the signals as background signals, and measuring two parallel samples by the signals until the signals are stable;
(3) flue gas generation and pretreatment: opening a control valve of a high-pressure gas cylinder, adjusting the flow of buffer gas to be 1-10ml/min, respectively sucking the cigarettes to be detected through a smoking machine, sequentially passing the generated smoke through a heating device and a filtering device, and preparing the smoke to enter a gas pool, wherein the volume ratio of the generated smoke to the buffer gas is 1: 5-10;
(4) collecting a spectrum: the smoking machine starts to smoke the cigarettes for about 5s, the valve of the sample outlet is opened, the cigarettes are quickly vacuumized again, the valve of the sample outlet is closed, the valve of the sample inlet is opened, the generated smoke enters the gas cell, after the reading of the pressure gauge of the sample inlet is stable, the gas inlet valve is closed, the infrared spectrum of the sample is collected, and the number of times of drawing is at least 24 times;
(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 characteristic of the mainstream smoke of the sample cigarette.
Further, in the step (1), the purging time is 2min, and the vacuum degree is pumped to-100.00 Kpa; in the step (3), the total collection is carried out for 10 times, and each time is 35 mL; in the step (4), the vacuum degree is pumped to-100.00 Kpa.
Furthermore, the cigarette smoke suction device sucks one mouth of mainstream smoke at each time, the capacity of the cigarette smoke suction device is 35mL, and each cigarette collects 2 nd-7 th mouths of mainstream smoke totally with 6 mouths of mainstream smoke.
Compared with the prior art, the invention has the following advantages and effects:
the annular optical fiber gas cell is of a hollow optical fiber structure, and the inner wall of the annular optical fiber gas cell is coated with the Ag/AgI composite coating, so that an incident light source forms multiple reflections in the hollow optical fiber to prolong the optical path of light and substance interaction, and the infrared absorption intensity of a system to be detected can be improved more efficiently, thereby reducing the detection limit and improving the precision and accuracy of analysis.
The heating device has excellent heat transfer performance, the cubic heating resistance wire is convenient for better heat transfer, and the temperature sensor is arranged to facilitate the adjustment of the heating efficiency of the heating wire.
The invention designs and applies the hollow fiber waveguide two-dimensional infrared spectrum, the infrared incidence device is a two-dimensional related infrared spectrometer with high sensitivity (ppm level), the detection device adopts a diode array detector and is provided with a high-speed diode with 20Hz to ensure that the data acquisition is quicker, so that the narrow peak can be more accurately reproduced; with a 20-bit A/D converter, better baseline noise digital resolution is provided, and quantification errors are reduced; the light beam uses hundreds of diode arrays, has response on the whole spectrum wave band, and the digital resolution can reach 1.2 nm, thereby realizing the dynamic real-time detection and the on-line monitoring of the main stream smoke gas phase object and breaking through the technical bottleneck of the cigarette true and false identification. On the basis of spectrum data accumulation, a mathematical statistical analysis technology is applied to accurately extract the overall characteristic information of the mainstream smoke of the real smoke (the benchmark smoke) from the spectrum data, and an effective, simple and rapid instrument identification method is constructed. The method is suitable for analyzing and detecting the overall characteristics of the mainstream smoke of the cigarettes, 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 Principal Component (PCA) score of a sample by combining a metrological calculation method, represents the overall characteristics of the mainstream smoke of the sample, and can be used for identifying the truth of cigarettes of different brands. The whole identification 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. The method can be popularized and applied to the authenticity identification of cigarette mainstream specifications and brands of Yunyan (soft treasure), Yuxi (soft), Yunyan (nine-great-weight) and other cloud products, and provides effective technical support and leading-edge technical solutions for standardizing the cigarette sale market and protecting the legal rights and interests of consumers.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic structural view of a heating apparatus according to the present invention;
FIG. 3 is a raw infrared spectrum of a sample of the flue gas of the example;
FIG. 4 is an infrared spectrum of a sample of flue gas from an example after pretreatment;
FIG. 5 is a graph of the principal component scores of the infrared spectra of the smoke samples of the examples.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of examples of the present invention, and not all examples. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
As shown in fig. 1, mainstream smoke true and false identification and analysis device of this embodiment, including smoking machine 1 that connects gradually, heating device 2, filter equipment 3, annular optical fiber pool 4, infrared light incidence device 5 and detection device 6, annular optical fiber pool 4 includes annular cell body 4.1, locate the introduction port of annular cell body 4.2 one end, locate the appearance mouth of the 4.2 other end of annular cell body, infrared incidence device 5 is located appearance mouth one side, detection device 6 locates introduction port one side, the 3 exports of filter equipment link to each other with the introduction port of annular cell body 4, still include with smoking machine 1, heating device 2, filter equipment 3, annular optical fiber pool 4, the PLC controller that infrared light incidence device 5 and detection device 6 are connected. Still be equipped with the high-pressure gas cylinder 8 that provides buffer gas between smoking machine 1 and heating device 2, 8 mouths of high-pressure gas cylinder are equipped with the control valve, and the control valve is connected with the PLC controller. The sample outlet is connected with a vacuum pump.
The annular pool body 4.1 is an annular hollow capillary column with the inner diameter of 0.2mm and the length of 10m, the inner wall of the annular pool body is coated with an Ag/AgI composite coating, and the quantity ratio of Ag to AgI is 1:1, the coating thickness was 0.15. mu.m.
Annular cell body both ends are equipped with the three-way valve, the three-way valve 4.2 one end and the annular cell body of introduction end are connected, the other end is connected with detection device, surplus one end is the introduction port, be equipped with first valve 4.3 on the introduction port, the detection device connector is equipped with second valve 4.4, the three-way valve 4.7 one end and the annular cell body 4.1 of appearance end are connected, the other end is connected with infrared incidence device 5, this connector is equipped with third valve 4.5, surplus one end is appearance mouth, be equipped with the fourth valve on the appearance mouth, it links to each other with the vacuum pump to go out the appearance mouth, first, two, three, four valves are controlled by the PLC controller, the three-way valve is the.
The heating device 2 comprises a pipe body 2.2, a flue gas channel 2.1 arranged in the pipe body 2.2, a heat conduction material 2.5 arranged between the flue gas channel 2.1 and the pipe body 2.2, a heating element 2.3 arranged around the flue gas channel 2.1 and a plurality of temperature sensors 2.4. Preferably, the pipe body 2.2 is a hollow rectangular plastic body, the smoke channel 2.1 is a thin copper pipe, the heating element 2.3 is a heating resistance wire arranged around the smoke channel 2.1, the heating resistance wire is a rectangular frame surrounding the smoke channel, the heat conduction material 2.5 is fibrous aluminum silicate wool, the plurality of temperature sensors 2.4 are arranged near the heating resistance wire, and the heating resistance wire and the plurality of temperature sensors are connected with the PLC. The material of the pipe body 2.2 is thermoplastic polyester PBT/PET engineering plastic which has excellent heat resistance and wear resistance and moderate market price. The heating resistance wire is made of Cr/Ni alloy, and the outer layer is wrapped by alkali-free glass fiber insulating material.
The filter device is a cigarette holder device specially used for SM450 (Cerulin company, UK) smoking machine, wherein a special filter disc with the aperture of 2 μm is arranged in the cigarette holder device, and impurities with larger particle size such as carbon particles can be filtered when the mainstream smoke passes through the filter disc of the holder device.
The detection device can adopt a Model 6000 (Super Systems Inc., USA) diode array detector, the infrared light incidence device can adopt a Spectrum 100 two-dimensional correlation infrared spectrometer and Spectrum v 6.3.5 operating software (Perkin Elmer, USA), the spectrometer can emit two infrared spectrums with different speeds, and the measuring range of the infrared spectrums is 3500-400 cm-1The inter-spectrum phase difference ranges from (-pi, pi). Smoking machine 1, heating device 2, filtering device 3 and annular optical fiber pool4 are communicated through copper pipes with excellent toughness and certain pressure resistance.
The smoking machine adopts RM1/Puls single-hole smoking machine (Borgwaldt KC company, Germany); for smoking cigarettes and generating mainstream smoke.
The buffer gas is an inert gas with stable properties, such as N2And He and the like, wherein gas is supplied by a high-pressure gas bottle, the gas flow is controlled within 1-10mL/min, and the gas can play a role in buffering and stabilizing the mainstream smoke and prevent high-activity molecules in the mainstream smoke from generating elastic collision and quenching. The vacuum pump may be a mechanical pump from leber, D60C, germany. The volume ratio of the flue gas to the inert gas is always 1: 5-10.
Example 2
The apparatus of example 1 was used to perform discrimination and analysis of the authenticity of mainstream smoke.
1. Reagents and materials:
the reagents used were, unless otherwise specified, analytically pure.
Nitrogen gas: n is a radical of2(the purity is more than or equal to 99.99%).
Materials: yuxi brand genuine cigarettes and Yuxi brand fake cigarettes.
The method for identifying the authenticity of the mainstream smoke comprises the following steps:
(1) starting and preprocessing a two-dimensional infrared spectrum: opening a two-dimensional infrared spectrum, wherein two-dimensional spectrum signals are mid-infrared spectra emitted in tandem, setting the difference between the two spectra for 5 seconds, preheating, purging residual air in a heating device, a filtering device and an annular optical fiber pool by using inert gas, wherein the inert gas is nitrogen, the purging time is 2min, then closing an air inlet valve at a sample inlet, closing a high-pressure gas cylinder control valve, opening an air outlet valve at an optical fiber outlet 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 a valve connected with a sample pool;
(2) background collection: opening a sample inlet valve and a high-pressure gas cylinder control valve of the annular optical fiber cell, introducing nitrogen, collecting inert gas in an experimental environment as a background, closing an air inlet valve when sample introduction is stable in a pressure gauge, and collecting 35mL of air for 10 times in total each time; the detection device collects a central infrared spectrum signal, and the signal is used as a background signal, so that the signal can measure two parallel samples until the signal is stable;
(3) flue gas generation and pretreatment: respectively sucking cigarettes to be detected (Yuxi brand certified cigarettes and Yuxi brand fake cigarettes) through a single-channel smoking machine, enabling the generated smoke to sequentially pass through a heating device and a filtering device and be ready to enter a gas pool, opening a high-pressure gas cylinder control valve, and adjusting the flow of inert gas to be 10ml/min so that the volume ratio of the generated smoke to the inert gas is 1: 10; and (3) not collecting the first mouth of main stream smoke which is incompletely combusted, and collecting 2-7 mouths of main stream smoke of each cigarette for 6 mouths. Yuxi brand genuine cigarettes and Yuxi brand counterfeit cigarettes respectively generate 5 mainstream smoke samples, the mainstream smoke samples of the Yuxi brand genuine cigarettes are 1-5 before numbering, and the mainstream smoke samples of the Yuxi brand counterfeit cigarettes are 6-10 after numbering.
(4) Collecting a spectrum: and (4) starting to suck the cigarettes for about 5 seconds by the single-channel smoking machine in the step (3), opening a valve at the sample outlet, opening a mechanical pump to quickly pump the vacuum degree of the gas pool to-100.00 KPa again, closing the mechanical pump and a valve connected with the gas pool, opening the valve at the sample inlet to enable the smoke generated in the step (3) to enter the gas pool, and closing an air inlet valve after the reading of a pressure gauge at the sample inlet is stable to respectively collect the infrared spectrums of the samples. The scanning frequency of the instrument is 25 times, the scanning frequency is increased to improve the signal-to-noise ratio, and the spectral resolution is 1cm-1(ii) a As shown in fig. 3;
(5) and (3) data analysis: an infrared spectroscopy solution module of chempatern software (kemeien technologies ltd., china) is adopted to preprocess the spectral data by an adaptive background subtraction algorithm so as to improve the signal-to-noise ratio of the signal, as shown in fig. 4; and calculating the principal component scores (PC 1 and PC 2) of the filtered signals according to the conventional method, wherein the interpretation rates of the two principal component scores to the variance of the original variable are respectively as follows: 81.74% and 16.45%. See table 1 below, where the score is the overall characteristic of mainstream smoke for that sample cigarette:
TABLE 1 principal Components scores for different samples
(6) And (3) verification: the discrimination of the two types of tobacco samples can be observed and classified according to the distribution of the two principal component scores (PC 1 and PC 2) in a mode space enclosed by coordinate axes.
Fig. 3 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. 3 was subjected to an automatic background subtraction operation, as shown in fig. 4, and to further verify the nuances of the smoke features of fig. 4, the spectrum of fig. 4 was subjected to a principal component analysis, and the results are shown in fig. 5. As can be seen from FIG. 5, the method of the present invention accurately extracts the subtle feature differences of two different types of flue gas samples, and is expected to be further applied to the accurate distinction of different types of flue gas by means of the chemometrics technology.
The samples numbered 1-10 are calculated to obtain respective principal component scores, the principal component scores are located at different positions in a mode space defined by coordinate axes, wherein the samples numbered 1-5 are spherical and located in a third quadrant of a mode plane to form a circle, and the sample is a Yuxi brand certified cigarette; and No. 6-10 samples are in one quadrant and four quadrants, are green squares, are also gathered into one class, and are Yuxi brand counterfeit cigarettes. Therefore, the method is applied to the identification of the true and false cigarette mainstream smoke and has good application potential.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A mainstream smoke true and false distinguishing and analyzing device based on hollow fiber waveguide two-dimensional infrared spectroscopy is characterized in that: the device comprises a smoking machine, a heating device, a filtering device, an annular optical fiber pool, an infrared light incidence device and a detection device which are sequentially connected, wherein the annular optical fiber pool comprises an annular pool body, a sample inlet arranged at one end of the annular pool body and a sample outlet arranged at the other end of the annular pool body; the annular optical fiber gas pool is of a hollow optical fiber structure, the inner wall of the annular optical fiber gas pool is coated with an Ag/AgI composite coating, and the quantity ratio of Ag to AgI is 1:1, the thickness of the coating is 0.15 mu m; the incident light source forms multiple reflections in the hollow optical fiber to prolong the optical path of the interaction between the light and the substance; the infrared incidence device is a two-dimensional correlation infrared spectrometer, and the detection device adopts a diode array detector and is provided with a 20Hz high-speed diode and a 20-bit A/D converter; the beam uses hundreds of diode arrays and is responsive across the entire spectral band; the two-dimensional spectral signal is a mid-infrared spectrum emitted in tandem.
2. The mainstream smoke authenticity discriminating and analyzing apparatus according to claim 1, wherein: the annular pool body is an annular hollow capillary column, the inner diameter is 0.2mm, and the length is 10 m.
3. The mainstream smoke authenticity discriminating and analyzing apparatus according to claim 1, wherein: annular cell body both ends are equipped with the three-way valve, and the three-way valve one end of appearance end is connected with annular cell body, and the other end is connected with detection device, and surplus one end is the introduction port, and the three-way valve one end of appearance end is connected with annular cell body, and the other end is connected with infrared incidence device, and surplus one end is the appearance mouth, and the appearance mouth links to each other with the vacuum pump.
4. The mainstream smoke authenticity discriminating and analyzing apparatus according to claim 1, wherein: the heating device comprises a pipe body, a flue gas channel arranged in the pipe body, a heat conduction material arranged between the flue gas channel and the pipe body, a heating element arranged around the flue gas channel and a plurality of temperature sensors.
5. The mainstream smoke authenticity identification and analysis device according to claim 4, wherein: the heating device is characterized in that the pipe body is a hollow rectangular plastic body, the smoke channel is a thin copper pipe, the heating elements are heating resistance wires arranged around the smoke channel, the heating resistance wires are rectangular frames surrounding the smoke channel, the heat conduction material is fibrous aluminum silicate cotton, the plurality of temperature sensors are arranged nearby the heating resistance wires, and the heating resistance wires and the plurality of temperature sensors are connected with the PLC.
6. The mainstream smoke authenticity identification and analysis device according to claim 4, wherein: the aperture of the filter disc of the filter device is 2 μm.
7. A method of discriminating between mainstream smoke and counterfeit using the apparatus of any one of claims 1 to 6, wherein: the method comprises the following steps:
(1) starting and preprocessing an infrared incidence device: opening an infrared incidence device for preheating, emitting the mid-infrared spectrum in tandem, purging residual air in a heating device, a filtering device and an annular optical fiber pool by using buffer gas, then closing a valve at a sample inlet, closing a buffer gas supply device, opening a valve at a sample outlet, vacuumizing, and then closing the valve at the sample outlet;
(2) background collection: opening a sample inlet valve of the annular optical fiber cell, collecting inert gas in an experimental environment as a background, and closing an air inlet valve when the sample is injected until the reading of a pressure gauge is stable; collecting two-dimensional mid-infrared spectrum signals, taking the signals as background signals, and measuring two parallel samples by the signals until the signals are stable;
(3) flue gas generation and pretreatment: opening a control valve of a high-pressure gas cylinder, adjusting the flow of buffer gas to be 1-10ml/min, respectively sucking the cigarettes to be detected through a smoking machine, sequentially passing the generated smoke through a heating device and a filtering device, and preparing the smoke to enter a gas pool, wherein the volume ratio of the generated smoke to the buffer gas is 1: 5-10;
(4) collecting a spectrum: the smoking machine starts to smoke the cigarettes for 5s, opens the valve of the sample outlet, quickly vacuumizes the cigarettes again, closes the valve of the sample outlet, opens the valve of the sample inlet, enables the generated smoke to enter the gas cell, closes the air inlet valve after the reading of the pressure gauge of the sample inlet is stable, and collects the infrared spectrum of the sample for at least 24 times;
(5) and (3) data analysis: preprocessing the infrared spectrum obtained in the step (4) by using a self-adaptive background subtraction algorithm; and conventionally calculating the principal component score of the filtered signal, wherein the score is the integral characteristic of the mainstream smoke of the sample cigarette.
8. The mainstream smoke authenticity identification method of cigarettes according to claim 7, wherein: in the step (1), the purging time is 2min, and the vacuum degree is pumped to-100.00 Kpa; in the step (2), the total collection is carried out for 10 times, and each time is 35 mL; in the step (4), the vacuum degree is pumped to-100.00 Kpa.
9. The mainstream smoke authenticity identification method of cigarettes according to claim 7, wherein: the cigarette smoke suction device sucks one mouth of mainstream smoke with the volume of 35mL every time, and each cigarette collects 2 nd-7 th mouth of mainstream smoke with 6 mouths.
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| 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 |
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