CN105699239A - Method for analyzing moisture retention ability of tobaccos and tobacco products by aid of near-infrared spectral models - Google Patents

Method for analyzing moisture retention ability of tobaccos and tobacco products by aid of near-infrared spectral models Download PDF

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CN105699239A
CN105699239A CN201610100394.7A CN201610100394A CN105699239A CN 105699239 A CN105699239 A CN 105699239A CN 201610100394 A CN201610100394 A CN 201610100394A CN 105699239 A CN105699239 A CN 105699239A
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sample
tobacco
infrared
keeping performance
tobacco product
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庄亚东
张华�
朱龙杰
曹毅
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China Tobacco Jiangsu Industrial Co Ltd
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China Tobacco Jiangsu Industrial Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/02Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light

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  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The invention provides a method for analyzing moisture retention ability of tobaccos and tobacco products by the aid of near-infrared spectral models. The method includes measuring variable quantities of the weights of tobacco samples in dynamic temperature and humidity environments along with the humidity and computing moisture retention numerical values; acquiring near-infrared spectral patterns of corresponding tobacco samples by the aid of a near-infrared spectrometer; establishing mathematical models of the moisture retention numerical values of the tobacco samples and near-infrared spectral patterns of the corresponding samples by the aid of mathematical statistics and spectral pre-processing techniques; quickly predicting and analyzing the moisture retention ability of unknown tobacco products and tobacco humectants by the aid of the near-infrared data models. The method has the advantages that problems of complicated operation and long periods of existing methods for evaluating moisture retention ability of existing tobaccos and existing tobacco products can be solved by the aid of the method, the method is simple, feasible, convenient and speedy, and the moisture retention ability of the tobaccos and the tobacco products can be effectively measured.

Description

Adopt the method that near-infrared spectroscopy analyzes Nicotiana tabacum L., tobacco product humid keeping performance
Technical field
The present invention relates to a kind of method adopting near-infrared spectroscopy to analyze Nicotiana tabacum L., tobacco product humid keeping performance。
Background technology
The quality of Medicated cigarette humid keeping performance is the important indicator affecting cigarette quality, has carried out a series of research about humid keeping performance method of testing and evaluation in recent years。Medicated cigarette humid keeping performance being measured with the main method evaluated at present is that tobacco sample is put into adjustable constant temperature and humidity system, regularly weighs quality, is that moisture content the mathematical model setting up moisture content and time are to evaluate humid keeping performance by weighing the mass transitions drawn。
This type of method can the humid keeping performance of accurate evaluation tobacco sample, but the generally complete humectation effect testing a sample needs tens even tens hours, complex operation, length consuming time。When sample size is bigger, the data feedback cycle is long, it is difficult to meet industrialization production requirements。For these reasons, a set of quick and precisely effective humid keeping performance of tobacco test new method is set up extremely urgent。
Summary of the invention
The problem that there is complex operation, cycle length when the invention aims to solve existing evaluation Nicotiana tabacum L. and tobacco product humid keeping performance, it is provided that a kind of method conveniently adopting near-infrared data model to evaluate Nicotiana tabacum L. and tobacco product humid keeping performance。
For realizing the purpose of foregoing invention, the present invention takes following technical proposals:
A kind of method adopting near-infrared spectroscopy to analyze Nicotiana tabacum L., tobacco product humid keeping performance, including:
Step one, measure tobacco sample humectation data: tobacco product is balanced in climatic chamber standby;Accurately weigh a certain amount of sample, measure tobacco sample its quality in dynamic humiture environment and, with the changing value of humidity, by deducting the butt quality of sample, calculate the humectation numerical value of sample;
Step 2, spectra collection: take tobacco sample, apply near-infrared spectrometers multi collect sample spectral data, it is thus achieved that the meansigma methods of sample spectral data, obtain the near infrared light spectrogram of tobacco sample;
Step 3, set up Nicotiana tabacum L. and tobacco product humid keeping performance near-infrared analysis data model: combined with tobacco product humid keeping performance result by the near infrared light spectrogram of gained sample, after mathematical statistics and preprocessing procedures computing, set up data model, form the near-infrared data model for analyzing Nicotiana tabacum L. and tobacco product humid keeping performance;
Step 4, the quick of unknown tobacco sample humid keeping performance measure: by the unknown tobacco sample through pretreatment, the method adopting step 2 gathers the near infrared spectrum of unknown tobacco sample, near infrared spectrum value is brought in the near-infrared forecast model that step 3 is set up through pretreatment by spectrum again, through model calculation, the humid keeping performance of unknown sample can be obtained。
Further, in step one, tobacco product adopts tobacco shred, stem, thin slice or with the addition of the tobacco product of humectant, and standby after balance 10h~48h in climatic chamber。
Further, weighing sample size in step one is 0.1g~1.0g。
Further, step one measures tobacco sample its quality in dynamic humiture environment and have dynamic water adsorption instrument method, oven for drying method or sulphuric acid desiccator method with the method for the changing value of humidity。
Further, step one measures the concretely comprising the following steps of humectation data of tobacco sample:
Tobacco shred is placed in weighing plate, weighs the quality that sample is initial;
At interval of 1-10min automatic weighing sample mass Mi, until constant mass constant reach balance after, envionmental humidity is set and reduces to 20% from 60%, a sample mass is measured at interval of regular time, treat that its mass change is less than 0.02%, automatically into next envionmental humidity, terminate until measuring;
After test terminates, the dry basis M of measuring samples0
Calculate each sample humectation data under equilibrium humidity environmentWherein, M60%For at envionmental humidity being the sample mass under 60%, M20%For at envionmental humidity being the sample mass under 20%。
Further, in step one, humiture environment refers to humidity range 10%-85%, temperature range 10 DEG C-40 DEG C。
Further, in step 2, near infrared light spectral condition is: test sample mode is diffuse-reflectance, and spectral scan ranges for 4000-12000nm-1, resolution 8nm-1, ambient temperature 22 DEG C-25 DEG C, ambient humidity 20%-70%, each tobacco sample repeats dress sample 3 times scanning 3 times, using 3 meansigma methodss as sample spectra。
Further, in step 3, mathematical statistics and preprocessing procedures are: at least one in variance analysis, cluster analysis, principal component analysis, artificial neural network analysis, partial least square method, straight line minusing, vector normalization method, min-max normalization method, multiplicative scatter correction method, Wavelet Transform, standard normal variable correction method, First derivative spectrograply and second derivative method。
The invention has the beneficial effects as follows: this kind adopts the method that near-infrared spectroscopy analyzes Nicotiana tabacum L., tobacco product humid keeping performance, it may be achieved the fast qualitative of Nicotiana tabacum L. and tobacco product humid keeping performance is with quantitative。Compared with conventional method easily tens hours consuming time, the present invention evaluates humid keeping performance of tobacco and only needs a few minutes, and advantage is clearly, and simple to operate, accurate quick。The invention solves existing Nicotiana tabacum L. and the problem of tobacco product humid keeping performance evaluation methodology complex operation, cycle length, have simple, convenient and swift, the advantage that can effectively measure Nicotiana tabacum L. and tobacco product humid keeping performance。The method is applicable not only to the evaluation of the humid keeping performance of the dissimilar tobacco products such as Nicotiana tabacum L., tobacco shred, expanded cut tobacco, stem, leaf group, finished cigarettes, and may be used for the humid keeping performance evaluation of humectant。
Accompanying drawing explanation
Fig. 1 is the process description schematic diagram that the embodiment of the present invention adopts the method for near-infrared spectroscopy analysis Nicotiana tabacum L., tobacco product humid keeping performance。
Fig. 2 be in embodiment nearly infrared spectrogram and sample humectation data acquisition with deducting straight line method and the near-infrared data model of best tobacco product humid keeping performance that crosscheck method is determined。
Fig. 3 is the cross validation results schematic diagram of near-infrared data model in embodiment。
Detailed description of the invention
The preferred embodiments of the present invention are described in detail below in conjunction with accompanying drawing。
Embodiment solves existing Nicotiana tabacum L. and the problem of tobacco product humid keeping performance evaluation methodology complex operation, cycle length, has simple, convenient and swift, the advantage that can effectively measure Nicotiana tabacum L. and tobacco product humid keeping performance。Mainly comprising the following steps of embodiment method: a. measures tobacco sample quality in dynamic humiture environment and with the variable quantity of humidity and calculates humectation numerical value;B. near infrared spectrometer is utilized to obtain the near infrared light spectrogram of corresponding tobacco sample;C. adopt mathematical statistics and preprocessing procedures by the near infrared light spectrogram founding mathematical models of tobacco sample humectation numerical value Yu counter sample;D. utilize this near-infrared data model that the humid keeping performance of unknown tobacco sample and tobacco humectant is carried out fast prediction analysis。
Sample pre-treatments: needed for embodiment 1-3, tobacco shred, stem are in climatic chamber, temperature is 22 ± 2 DEG C, and relative humidity is 60 ± 2%, and 10h-48h is as a child standby for balance。
Three below embodiment illustrates from tobacco shred, stem, three application examples of humectant respectively。
Embodiment 1
(1) the ambient temperature and humidity condition of dynamic water absorption is set as follows: the temperature first regulating dynamic water adsorption instrument is 22 DEG C, and relative humidity is 60%, and after reaching balance, relative humidity directly reduces to 20% from 60%;
(2) in dynamic water instrument, put into the weighing plate of dress sample, separately put into an identical weighing plate as blank, then weigh the tare weight of plate;
(3) 1.0g tobacco shred is placed in the dynamic water adsorption instrument aluminum matter weighing plate having surveyed tare weight, weighs the quality that sample is initial;
(4) at interval of 1-10min automatic weighing sample mass Mi, until constant mass constant reach balance after, envionmental humidity is set and reduces to 20% from 60%, a sample mass is measured at interval of regular time, treat that its mass change is less than 0.02%, automatically into next envionmental humidity, terminate until measuring;
(5) after test terminates, the dry basis M of measuring samples0
(6) mass change according to sample, calculates each sample humectation data under equilibrium humidity environment Y = ( M 60 % - M 20 % ) ( M 60 % - M 0 ) * 100 % , Basic data as modeling;
(7) adopt near infrared spectrometer that above-mentioned modeling sample collects the spectrogram of sample。
(8) by Bruker company MATRIX-1 near infrared spectroscopy instrument OPUS software by sample near infrared light spectrogram and corresponding humectation data acquisition with deducting straight line method and crosscheck method simulates best modeled model, the coefficient of determination (R of model2) value is closer to 100, it was shown that predictive value is closer to true value。The R of this tobacco sample2Value is 90.59, and what absolutely prove this model predicts the outcome close to true value, as shown in Figure 2;
(9) stability and the predictive ability of model is verified by relation analysis error (RPD), as RPD > 3 time, model stability and predictability are good, cross validation root-mean-square (RMSECV) represents the departure degree between predictive value and standard value in cross validation situation, quality for judgment models, its value is more little, and model is more good。RPD=3.26, the RMSECV=0.221 of this model, illustrates that this model is better, and stability and predictability are good, illustrate as shown in Figure 3;
(10) when model stability and predictability are good, by model, sample spectra is carried out pretreatment;
(11) adopt prediction to adopt analytical model in addition assay to through pretreated sample spectra, obtain the humectation numerical value of testing sample, it is possible to evaluate the humid keeping performance of tobacco shred quickly and easily。
(12) the near-infrared spectrogram of unknown tobacco sample is gathered, substitute into the near-infrared humectation model built up in OPUS software, adopt and deduct straight line method to calculate the humectation numerical value of this sample be 9.52%, recording actual humectation value with dynamic water adsorption instrument again is 9.68%, both are closer to result, illustrate that the prediction effect of this near-infrared data model is ideal。
Embodiment 2
(1) 1g testing sample stem A is accurately weighed, it is accurate to 0.001g, it is placed in the dynamic water adsorption instrument aluminum matter weighing plate having surveyed tare weight, first temperature: 22 DEG C, relative humidity: 60% balance, after reaching balance, directly reduces to 30% by ambient humidity, measure after its balance and terminate, and the humectation numerical value calculating stem is standby。
(2) adopt near infrared spectrometer that above-mentioned modeling sample collects the spectrogram of sample。
(3) humectation data acquisition method of least square and crosscheck method by OPUS software infrared spectrogram nearly and sample determine best modeled model, the coefficient of determination (R of this model2) value is 95.59, relation analysis error (RPD)=3.85, cross validation root-mean-square (RMSECV)=0.140, illustrates that this model stability and predictive ability are good。
(4) choosing the stem sample of the unknown, gather after spectrogram through near infrared spectrometer, the employing of stem humid keeping performance is deducted straight line method and is calculated by the near-infrared data model that substitution OPUS software is set up, and its result is 8.35%;Adopting dynamic water instrument that stem humid keeping performance is measured, measured value is 8.22%, and both results are closely。
Embodiment 3
(1) a certain amount of humectant is sprayed respectively in tobacco sample, such as xylitol, then puts into sample balance 48h in climatic chamber, accurately weighs the 1.0g testing sample tobacco shred balanced, it is accurate to 0.001g, measures the humectation numerical value of sample by the method in embodiment 1 respectively。
(2) adopt near infrared spectrometer that above-mentioned modeling sample collects the spectrogram of sample。
(3) First derivative spectrograply and crosscheck method is adopted to determine best modeled model by the humectation numerical value of OPUS Software of Data Statistics infrared spectrogram nearly and sample, the R of this model2Value is 98.40, RPD=4.25, RMSECV=0.150, illustrates that this model stability and predictive ability are relatively good, it is possible to evaluate the humid keeping performance of humectant better。
(4) choosing a kind of humectant, be uniformly sprayed on tobacco shred, gather near infrared light spectrogram after balance, substitution OPUS software utilizes the employing of near-infrared data model to deduct straight line method and is calculated, and result is 12.30%;Adopting dynamic water instrument to be analyzed, actual measurement humectation value is 12.45%, illustrates that predicting the outcome of this model is comparatively accurate。
Embodiment 4
(1) 1.0g tobacco sample is weighed, it is placed in climatic chamber and balances, climatic chamber is respectively provided with temperature 10 DEG C-40 DEG C, humidity 10%-60%, take out sample after balance 48h and weigh quality, then be placed in 40 DEG C of baking ovens and dry, again weigh quality, after deduction sample butt quality, calculate the humectation value of tobacco sample。
(2) near infrared spectrometer is adopted to gather the near infrared light spectrogram of tobacco sample。
(3) adopting the near-infrared data model set up in embodiment 1 that the humectation value employing of this tobacco sample is deducted straight line method to be calculated, result is 9.67%, and compared with Oven Method result of calculation 9.83%, both results are suitable。
Embodiment 5
(1) 1g stem is weighed, be placed in temperature 22 DEG C, humidity respectively 20%, 40%, 60% sulphuric acid desiccator in, and sulphuric acid desiccator is positioned in the climatic chamber of same environment to keep temperature constant, a few days ago sample every day 2 times and weigh stem quality, sample no less than 1 time every day afterwards, until constant mass, calculate the humectation value of stem。
(2) near infrared spectrometer is adopted to gather the near infrared light spectrogram of stem sample。
(3) utilizing the stem near-infrared data model set up in embodiment 2 that the employing of stem humid keeping performance is deducted straight line method to be calculated, its result is 8.41%, and compared with sulphuric acid desiccator method measurement result 8.35%, both results are closely。
Integrated comparative embodiment 1, embodiment 2, embodiment 3 and embodiment 4, embodiment 5, adopt near-infrared data model that the humid keeping performance of tobacco product is predicted the outcome the measured result with Oven Method and sulphuric acid desiccator method all closely, illustrates that the humid keeping performance of tobacco product effectively can be predicted analysis by near-infrared data model。But, no matter it is Oven Method or sulphuric acid desiccator method, its humectation numerical value analyzing tobacco product is both needed to more than 48h, and adopts near-infrared data model to be predicted only needing about ten minutes。Therefore, adopt method therefor of the present invention can significantly reduce the time evaluating tobacco product humid keeping performance, improve data feedback efficiency, meet industrialized production needs。
Embodiment utilizes near-infrared means to gather the near infrared light spectrogram of Nicotiana tabacum L. and tobacco product, in conjunction with dynamic water analysis-e/or determining sample humectation data at different conditions, set up the near-infrared data model about Nicotiana tabacum L. humectation, the evaluation cycle of sample humid keeping performance can be greatly shortened, improve and evaluate efficiency, and expand Nicotiana tabacum L. and tobacco product application in physics moisture content, for the technical support that the further investigation offer of Medicated cigarette " flavouring humectation " is certain。
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, but not is the restriction to embodiments of the present invention。For those of ordinary skill in the field, other multi-form change or variations can also be made on the basis of the above description, cannot all of embodiment be given exhaustive here。Every belong to apparent change that technical scheme amplified out or the variation row still in protection scope of the present invention。

Claims (8)

1. one kind adopts the method that near-infrared spectroscopy analyzes Nicotiana tabacum L., tobacco product humid keeping performance, it is characterised in that including:
Step one, measure tobacco sample humectation data: tobacco product is balanced in climatic chamber standby;Accurately weigh a certain amount of sample, measure tobacco sample its quality in dynamic humiture environment and, with the changing value of humidity, by deducting the butt quality of sample, calculate the humectation numerical value of sample;
Step 2, spectra collection: take tobacco sample, apply near-infrared spectrometers multi collect sample spectral data, it is thus achieved that the meansigma methods of sample spectral data, obtain the near infrared light spectrogram of tobacco sample;
Step 3, set up Nicotiana tabacum L. and tobacco product humid keeping performance near-infrared analysis data model: combined with tobacco product humid keeping performance result by the near infrared light spectrogram of gained sample, after mathematical statistics and preprocessing procedures computing, set up data model, form the near-infrared data model for analyzing Nicotiana tabacum L. and tobacco product humid keeping performance;
Step 4, the quick of unknown tobacco sample humid keeping performance measure: by the unknown tobacco sample through pretreatment, the method adopting step 2 gathers the near infrared spectrum of unknown tobacco sample, near infrared spectrum value is brought in the near-infrared forecast model that step 3 is set up through pretreatment by spectrum again, through model calculation, the humid keeping performance of unknown sample can be obtained。
2. the method adopting near-infrared spectroscopy to analyze Nicotiana tabacum L., tobacco product humid keeping performance as claimed in claim 1, it is characterized in that: in step one, tobacco product adopts tobacco shred, stem, thin slice or with the addition of the tobacco product of humectant, and standby after balance 10h~48h in climatic chamber。
3. the method adopting near-infrared spectroscopy to analyze Nicotiana tabacum L., tobacco product humid keeping performance as claimed in claim 1, it is characterised in that: weighing sample size in step one is 0.1g~1.0g。
4. the method adopting near-infrared spectroscopy analysis Nicotiana tabacum L., tobacco product humid keeping performance as described in any one of claim 1-3, it is characterised in that: measuring tobacco sample its quality in dynamic humiture environment in step one has dynamic water adsorption instrument method, oven for drying method or sulphuric acid desiccator method with the method for the changing value of humidity。
5. adopt, as described in any one of claim 1-3, the method that near-infrared spectroscopy analyzes Nicotiana tabacum L., tobacco product humid keeping performance, it is characterised in that: step one measures the concretely comprising the following steps of humectation data of tobacco sample:
Tobacco shred is placed in weighing plate, weighs the quality that sample is initial;
At interval of 1-10min automatic weighing sample mass Mi, until constant mass constant reach balance after, envionmental humidity is set and reduces to 20% from 60%, a sample mass is measured at interval of regular time, treat that its mass change is less than 0.02%, automatically into next envionmental humidity, terminate until measuring;
After test terminates, the dry basis M of measuring samples0
Calculate each sample humectation data under equilibrium humidity environmentWherein, M60%For at envionmental humidity being the sample mass under 60%, M20%For at envionmental humidity being the sample mass under 20%。
6. the method adopting near-infrared spectroscopy to analyze Nicotiana tabacum L., tobacco product humid keeping performance as claimed in claim 5, it is characterised in that: in step one, humiture environment refers to humidity range 10%-85%, temperature range 10 DEG C-40 DEG C。
7. the method adopting near-infrared spectroscopy to analyze Nicotiana tabacum L., tobacco product humid keeping performance as claimed in claim 6, it is characterised in that: in step 2, near infrared light spectral condition is: test sample mode is diffuse-reflectance, and spectral scan ranges for 4000-12000nm-1, resolution 8nm-1, ambient temperature 22 DEG C-25 DEG C, ambient humidity 20%-70%, each tobacco sample repeats dress sample 3 times scanning 3 times, using 3 meansigma methodss as sample spectra。
8. adopt, as described in any one of claim 1-3, the method that near-infrared spectroscopy analyzes Nicotiana tabacum L., tobacco product humid keeping performance, it is characterised in that: in step 3, mathematical statistics and preprocessing procedures are: variance analysis, cluster analysis, principal component analysis, artificial neural network analysis, partial least square method, straight line minusing, at least one that deducts in straight line method, vector normalization method, min-max normalization method, multiplicative scatter correction method, Wavelet Transform, standard normal variable correction method, First derivative spectrograply and second derivative method。
CN201610100394.7A 2016-02-23 2016-02-23 Method for analyzing moisture retention ability of tobaccos and tobacco products by aid of near-infrared spectral models Pending CN105699239A (en)

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CN107490658A (en) * 2017-09-11 2017-12-19 云南中烟工业有限责任公司 A kind of evaluation method of cigarette humid keeping performance
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CN112666038A (en) * 2021-01-22 2021-04-16 山东大学 Method for representing moisture absorption process based on near infrared spectrum
CN112666038B (en) * 2021-01-22 2023-02-28 山东大学 Method for representing moisture absorption process based on near infrared spectrum

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