CN104596979A - Method for measuring cellulose of reconstituted tobacco by virtue of near infrared reflectance spectroscopy technique - Google Patents
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Abstract
The invention discloses a method for measuring cellulose of a reconstituted tobacco by virtue of a near infrared reflectance spectroscopy technique. The method comprises the following steps: (1) collecting and preparing a representative sample; (2) collecting an original spectrum; (3) selecting a correcting sample set and a verifying sample set; (4) measuring a reference value of the sample; (5) carrying out pretreatment on spectrum; (6) establishing a PLC model; (7) verifying the model; and (8) measuring cellulose. The method disclosed by the invention is simple, feasible and fast. By adopting a near infrared spectrum nondestructive detection technology, not only can the analytical efficiency be enhanced and the cost be lowered, but the method also has obvious practicality for accurately measuring the cellulose of the reconstituted tobacco, improving the detection efficiency and objectively reflecting the product quality. The method disclosed by the invention has the advantages of high detection speed, no pollution, greenness and environmental protection, high accuracy, good repeatability and the like, and is suitable for on-site analysis and fast detection of the cellulose of a reconstituted tobacco product as well as online monitoring of fluctuation of product quality.
Description
Technical field
The present invention relates to near-infrared diffuse reflection spectrum technology and measure the cellulosic method of papermaking-method reconstituted tobaccos, belong to papermaking-method reconstituted tobaccos field.
Background technology
Cellulose is one of important component part of tobacco cell wall.Cell wall substance content is higher, and the quality of tobacco leaf is poorer, and particularly in discarded tobacco leaf, the cell wall substance content such as cellulose is higher, its flue gas can produce strong impulse, choke cough, puckery mouth, withered and burnt smell.Reconstituted tobacco utilizes discarded offal, tobacco leaf fragment, offal etc. to be raw material, to be processed into through a series of, content of cellulose is also the key factor affecting reconstituted tobacco quality, therefore measures the cellulose in reconstituted tobacco, significant for evaluation reconstituted tobacco quality.
At present, in reconstituted tobacco, the mensuration of content of lignin is mainly measured by tobacco business mark YC/T347-2010 " mensuration-Detergent method of tobacco and tobacco product neutral detergent fiber, acid detergent fiber, pickling lignin ", the method mainly adopts diluted acid, diluted alkaline and sample to boil rear organic solvent process successively altogether, weigh after drying again, this method complex operation, time-consuming effort; Chinese patent CN200810098885 " cellulose in flowing analysis technique for determining tobacco " also provides an assay method growing tobacco middle content of cellulose in addition, the method is according to character glucogenic after cellulose hydrolysis, after utilizing the cellulose in cellulase degradation tobacco to obtain glucose, content of reducing sugar is detected with Flow Analyzer, cellulosic content is with glucose meter, though this method is easy compared with YC/T347-2010, cellulosic enzymolysis is still very consuming time.Given this, be necessary to develop a kind of content of cellulose of mensuration fast method newly, the content of cellulose for assay reconstituted tobacco provides certain reference.
After near infrared light to material, can absorb, transmission, total reflection, several interaction type such as diffuse reflection.The acquisition mode of near infrared spectrum mainly contains three kinds: transmission-type, diffuse reflection type, thoroughly diffuse type.
For the good fluid sample of light penetrability, near infrared light can penetrate whole sample, and the transmission mode that adopts carries out spectral scan more, and measured data are comparatively accurate.Near infrared light can not penetrate papermaking-method reconstituted tobaccos completely, therefore adopts diffuse reflectance to carry out spectral scan.After near-infrared diffuse reflection enters sample interior, occur to reflect many times, reflect, diffraction, after absorption, return the light of the plane of incidence, the structure of this analysis light load sample and composition information, it is quick, an environment amenable detection technique, current application near infrared reflectance spectroscopy measures the aspects such as tobacco routine chemical components, style, homogeneity and has been reported, but has no report for the method for measuring of papermaking-method reconstituted tobaccos content of cellulose.
Summary of the invention
For simple, easy, Fast Measurement reconstituted tobacco cellulose, the invention provides a kind of near-infrared diffuse reflection spectrum and measure the cellulosic method of papermaking-method reconstituted tobaccos, near infrared spectrum Dynamic Non-Destruction Measurement is adopted to improve analysis efficiency, cost-saving, for Accurate Determining reconstituted tobacco cellulose, improve detection efficiency, objective reactor product quality, has obvious practicality.
The present invention is realized by following technical proposal: a kind of near-infrared diffuse reflection spectrum technology measures the cellulosic method of papermaking-method reconstituted tobaccos, comprises the steps:
Step (1), the collection of sample: collect a collection of representative papermaking-method reconstituted tobaccos product;
Step (2), gathers original spectrum: adopt the irreflexive mode of near infrared spectrum to carry out spectral scan one by one to the papermaking-method reconstituted tobaccos product that step (1) is collected, obtain original spectrum;
Step (3), selects Calibration and verification sample collection: in step (2) gained original spectrum, adopt the method for standard GB/T 29858-2013 to select Calibration and verification sample collection;
Step (4), working sample reference value: at the standard conditions, utilizes standard method to carry out cellulosic mensuration one by one to the papermaking-method reconstituted tobaccos product that step (1) is collected, obtains samples Reference value;
Step (5), pre-processed spectrum: pre-service is carried out, the impact of stress release treatment and baseline wander to the spectrum of the Calibration selected in step (3) and verification sample collection;
Step (6), set up PLS model: step (5) pretreated Calibration and step (4) gained samples Reference value are carried out one_to_one corresponding, application partial least square method carries out matching cellulose determination data corresponding with it for spectroscopic data, set up quantitative model, carry out in modeling process detecting and rejecting abnormalities value, remaining spectra values is worth to rejecting abnormalities, again carry out one_to_one corresponding with step (4) gained samples Reference value, application partial least square method carries out matching cellulose determination data corresponding with it for spectroscopic data, set up the quantitative model obtaining cellulose index,
Step (7), modelling verification: the quantitative model of the cellulose index that the verification sample set pair step (6) after utilizing step (5) to process is set up carries out external prediction;
Step (8), measures cellulose: by the quantitative model of the cellulose index that the original spectrum input step (6) of papermaking-method reconstituted tobaccos sample to be measured is set up, and namely measures and obtains cellulose.
Further, the spectra collection condition of described step (2) is: sweep limit is 4000 ~ 10000cm
-1, resolution is 8cm
-1, scanning times is not less than 72 times.
Further, the original spectrum of described step (2) is obtained by following method: papermaking-method reconstituted tobaccos product step (1) collected, each product gets three Duplicate Samples, the pressed powder of each Duplicate Samples mixing puts into sample cup, gently flatten, thickness >=10mm, be put on spectrometer universal stage, near infrared spectrum is utilized to adopt irreflexive mode to carry out scanning and gathering spectrum, each Duplicate Samples sweeps a spectrum, corresponding 3 the parallel spectrum of each product, again 3 parallel spectrum (with near infrared spectroscopy instrument carry software) are carried out being averaging and obtain an original spectrum, identical method is adopted to scan and gather spectrum to each product successively, obtain the original spectrum that each product is corresponding.
Further, the standard conditions of described step (4) are GB/T 16447 " atmospheric environment that tobacco and tobacco product regulate and test " defined terms; Described standard method refers to be tested by industry standard YC/T 347-2010 " the mensuration Detergent method of tobacco and tobacco product neutral detergent fiber, acid detergent fiber, pickling lignin ".
Further, the pre-service of described step (5) refers to and carries out SNV+ first order derivative+Norris pre-service to original spectrum.
Further, in described step (6), detection and rejecting abnormalities value adopt the method detecting lever value, especially by the following step:
By following formulae discovery sample lever value:
Wherein,
h i for sample lever value,
t i for sample
ibecause of subvector,
t t tfor the factor score matrix of modeling collection,
t t i for
t i transposition;
When sample lever value is greater than 3k/n, wherein k is number of principal components, and n is sample number, and its spectrum has significant impact to recurrence, should reject.
Further, the modelling verification of described step (7) adopts the predicted value of the quantitative model gained of t method of inspection determination verification sample collection input step (6) and corresponding step 4 gained samples Reference value whether to have deviation in statistical significance: namely, the predicted value of the quantitative model of cellulose index step (6) set up and the samples Reference value t value of step (4) and degree of freedom d
v-1critical value t
(a, dv-1)compare, get level of signifiance a=0.05, when | t| < t
(a, dv-1), during probability P >0.05, illustrate that the testing result of two kinds of methods does not exist significant difference, modelling verification success, this model can be used for the cellulose measuring papermaking-method reconstituted tobaccos.
PLS model is the development of principal component regression bearing calibration (PCR).In principle component regression, by certain main cause subnumber, spectrum matrix is decomposed.To reach the object that Data Dimensionality Reduction eliminates garbage (noise).And in PLS regretional analysis, except spectrum matrix is decomposed, also decomposition dimensionality reduction is carried out to concentration matrix, and introduce mutual information simultaneously.Its principle is as follows:
(1) model of matrix decomposition is:
Am×p=Tm×kPk×p+EA
Cm×n=Um×kQk×n+EC
Wherein, A is spectrum matrix; C is concentration or character matrix; T is the score matrix of spectrum matrix; U is the score matrix of concentration matrix; P is the loading matrix-major component matrix of spectrum matrix; Q is the loading matrix-major component matrix of concentration matrix; EA is the spectral error matrix of application PLS introducing when carrying out regretional analysis; EC is the concentration error matrix of application PLS introducing when carrying out regretional analysis; M is sample number; P is number of wavelengths; K is number of principal components.
(2) regretional analysis of score matrix T, U, obtains correlation matrix B
Um×k=Tm×fBk×k
(3) when forecast analysis, the loading matrix P obtained by the unknown Sum decomposition of the spectrum matrix A of sample by Am × p=Tm × kPk × p+EA, the score matrix T obtaining sample is unknown, is obtaining the concentration of unknown sample according to the unknown BQ of C the unknown=T.
The present invention compared with prior art, its beneficial effect is: the invention provides near-infrared diffuse reflection spectrum technology and measure the cellulosic method of papermaking-method reconstituted tobaccos, simply, easy, quick, near infrared spectrum Dynamic Non-Destruction Measurement is adopted to improve analysis efficiency, cost-saving, for Accurate Determining reconstituted tobacco cellulose, improve detection efficiency, objective reactor product quality, has obvious practicality.It is fast that the inventive method has detection speed, pollution-free, environmental protection, and accuracy is high, high repeatability and other advantages, is applicable to the cellulosic on-line monitoring realizing on-the site analysis, fast detection and products thereof quality fluctuation of reconstituted tobacco product.For stability contorting papermaking-method reconstituted tobaccos product interior quality, play papermaking-method reconstituted tobaccos stable roll smoke product quality and mould cigarette style there is obvious beneficial effect.
A. analysis speed is fast: measure in a sample 3min and complete, can the cellulose of rapid test reconstituted tobacco product by the cellulose model set up, and the fluctuation situation of preliminary judgement sample quality;
B. analysis cost is low, pollution-free: in sample analysis process, do not consume sample itself, need not any chemical reagent, and cost reduces, and does not cause any pollution to environment;
C. test favorable reproducibility: spectroscopic assay is less by interference from human factor, measure and there is stability;
D. be convenient to realize on-line analysis: near infrared spectrum has good transport property in a fiber, on-line analysis and remote monitoring can be realized.
Accompanying drawing explanation
Fig. 1 sets up by step (6) the data fitting figure of the quantitative model of cellulose index.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.It will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting scope of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by buying the conventional products obtained.
Step (1), the collection of sample: collect a collection of representative papermaking-method reconstituted tobaccos product 150 ~ 200;
Step (2), gather original spectrum: papermaking-method reconstituted tobaccos product step (1) collected, each product gets three Duplicate Samples, the pressed powder of each Duplicate Samples mixing puts into sample cup, gently flatten, thickness>=10mm, is put on spectrometer universal stage, utilizes near infrared spectrum to adopt irreflexive mode to carry out scanning and gathering spectrum under following spectral conditions: sweep limit is 4000 ~ 10000cm
-1, resolution is 8cm
-1, scanning times is not less than 72 times; Each Duplicate Samples sweeps a spectrum, corresponding 3 the parallel spectrum of each product, again 3 parallel spectrum (with near infrared spectroscopy instrument carry software) are carried out being averaging and obtain an original spectrum, adopt identical method scan and gather spectrum to each product successively, obtain the original spectrum that each product is corresponding;
Step (3), selects Calibration and verification sample collection: in step (2) gained original spectrum, adopt the method for standard GB/T 29858-2013 to select Calibration and verification sample collection;
Step (4), working sample reference value: under standard conditions (GB/T 16447 " atmospheric environment that tobacco and tobacco product regulate and test " defined terms), utilize standard method (industry standard YC/T 347-2010 " the mensuration Detergent method of tobacco and tobacco product neutral detergent fiber, acid detergent fiber, pickling lignin ") to carry out cellulosic mensuration one by one to the papermaking-method reconstituted tobaccos product that step (1) is collected, obtain samples Reference value;
Step (5), pre-processed spectrum: SNV+ first order derivative+Norris pre-service is carried out, the impact of stress release treatment and baseline wander to the spectrum of Calibration in step (3) and verification sample collection;
Step (6), set up PLS model: select, in full spectral range, PLS is carried out to calibration set sample and return and full cross validation, when the number of principal components of model reaches 5, the root mean square cross validation error RMSECV of model is minimum, and the optimum number of principal components of preference pattern is 5.Step (5) pretreated Calibration and step (4) gained samples Reference value are carried out one_to_one corresponding, application partial least square method carries out matching cellulose determination data corresponding with it for spectroscopic data, set up quantitative model, in modeling process, adopt the method detecting lever value to carry out detecting and rejecting abnormalities value:
By following formulae discovery sample lever value:
Wherein,
h i for sample lever value,
t i for sample
ibecause of subvector,
t t tfor the factor score matrix of modeling collection,
t t i for
t i transposition;
When sample lever value is greater than 3k/n, wherein k is number of principal components, and n is sample number, and its spectrum has significant impact to recurrence, should reject; By calculate in steps in (3) the spectrum lever value of Calibration and verification sample collection be all less than 3k/n, do not have abnormal sample to need to reject;
Remaining spectra values is worth to rejecting abnormalities, again carry out one_to_one corresponding with step (4) gained samples Reference value, application partial least square method carries out matching cellulose determination data corresponding with it for spectroscopic data, set up the quantitative model (see figure 1) obtaining cellulose index, the related coefficient of quantitative model is 0.9778, RMSECV is 1.40, have significant linear relationship between visible spectrum data and the index quantification of sample, the near infrared spectrum of interpret sample includes the closely-related information with index quantification;
Step (7), modelling verification: the quantitative model of 50 products to the cellulose index that step (6) is set up that the verification sample after utilizing step (5) to process is concentrated carries out external prediction: by following formulae discovery root-mean-square prediction error RMSEP:
Wherein,
d i f i =x
i-y
ibe i-th sample near infrared measured value x
iwith as this sample reference value y analyzing benchmark
idifference, utilizing formulae discovery to obtain root-mean-square prediction error RMSEP is 1.8075, table 1 predicts the outcome for PLS model prediction collection, the predicted value of quantitative model gained of t method of inspection determination verification sample collection input step (6) and corresponding step 4 gained samples Reference value is adopted whether to have deviation in statistical significance: namely, the predicted value of the quantitative model of cellulose index step (6) set up and the samples Reference value t value of step (4) and degree of freedom d
v-1critical value t
(a, dv-1)compare, get level of signifiance a=0.05, t value is found according to 95% fiducial interval, t
0.05,49=2.009, then | t| < t
0.05,49, during probability P >0.05, illustrate that the testing result of two kinds of methods does not exist significant difference, modelling verification success, this model can be used for the cellulose measuring papermaking-method reconstituted tobaccos, reliable results:
Table 1 PLS model prediction collection predicts the outcome
Step (8), measures cellulose: by the quantitative model of the cellulose index that the original spectrum input step (6) of 10, papermaking-method reconstituted tobaccos sample to be measured is set up, and namely measures and obtains cellulose; Each sample predicts 5 times, the standard method of applying step (4) simultaneously measures sample fiber element, its measurement result is as shown in table 2 below, and it is feasible in production practices, applying near-infrared diffuse reflection spectrum as seen from Table 2 to the detection of reconstituted tobacco weight per unit length.
Table 2 actual sample measurement result
In sum, utilize this model can measure the cellulose of reconstituted tobacco finished product fast and accurately, to the fluctuation situation realizing on-the site analysis, monitoring reconstituted tobacco constant product quality and quality, significant.
In addition, why the pre-service of step (5) adopts SNV+ first order derivative+Norris pre-service, as following table 3 by the PLS model result of Calibration under different Pretreated spectra, visible, different preprocessing procedures has different impacts to PLS modeling result, SNV+ first order derivative+Norris effect is better, final employing SNV+ first order derivative+Norris pre-service:
PLS model result under the different Pretreated spectra of table 3
Note: k is number of principal components, and RMSECV is root mean square cross validation error, and RMSEC is root mean square correction error, MSC is multiplicative scatter correction, SNV is vector normalization, Norris(a, b) be Norris Derivative filtering, a is segment length, b is certain distance, Savitzky-Golay(a, b) be moving-polynomial smoother method, a is level and smooth number of data points, and b is polynomial expression time number formulary.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.Those skilled in the art should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and instructions just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (5)
1. near-infrared diffuse reflection spectrum technology measures the cellulosic method of papermaking-method reconstituted tobaccos, it is characterized in that comprising the steps:
Step (1), the collection of sample: collect a collection of representative papermaking-method reconstituted tobaccos product;
Step (2), gathers original spectrum: adopt the irreflexive mode of near infrared spectrum to carry out spectral scan one by one to the papermaking-method reconstituted tobaccos product that step (1) is collected, obtain original spectrum;
Step (3), selects Calibration and verification sample collection: in step (2) gained original spectrum, adopt the method for standard GB/T 29858-2013 to select Calibration and verification sample collection;
Step (4), working sample reference value: at the standard conditions, utilizes standard method to carry out cellulosic mensuration one by one to the papermaking-method reconstituted tobaccos product that step (1) is collected, obtains samples Reference value; Above-mentioned standard conditions are GB/T 16447 " atmospheric environment that tobacco and tobacco product regulate and test " defined terms; Standard method refers to be tested by industry standard YC/T 347-2010 " the mensuration Detergent method of tobacco and tobacco product neutral detergent fiber, acid detergent fiber, pickling lignin ";
Step (5), pre-processed spectrum: SNV+ first order derivative+Norris pre-service is carried out, the impact of stress release treatment and baseline wander to the spectrum of the Calibration selected in step (3) and verification sample collection;
Step (6), set up PLS model: step (5) pretreated Calibration and step (4) gained samples Reference value are carried out one_to_one corresponding, application partial least square method carries out matching cellulose determination data corresponding with it for spectroscopic data, set up quantitative model, carry out in modeling process detecting and rejecting abnormalities value, remaining spectra values is worth to rejecting abnormalities, again carry out one_to_one corresponding with step (4) gained samples Reference value, application partial least square method carries out matching cellulose determination data corresponding with it for spectroscopic data, set up the quantitative model obtaining cellulose index,
Step (7), modelling verification: the quantitative model of the cellulose index that the verification sample set pair step (6) after utilizing step (5) to process is set up carries out external prediction;
Step (8), measures cellulose: by the quantitative model of the cellulose index that the original spectrum input step (6) of papermaking-method reconstituted tobaccos sample to be measured is set up, and namely measures and obtains cellulose.
2. method according to claim 1, is characterized in that: the spectra collection condition of described step (2) is: sweep limit is 4000 ~ 10000cm
-1, resolution is 8cm
-1, scanning times is not less than 72 times.
3. method according to claim 1, it is characterized in that: the original spectrum of described step (2) is obtained by following method: papermaking-method reconstituted tobaccos product step (1) collected, each product gets three Duplicate Samples, the pressed powder of each Duplicate Samples mixing puts into sample cup, gently flatten, thickness >=10mm, be put on spectrometer universal stage, near infrared spectrum is utilized to adopt irreflexive mode to carry out scanning and gathering spectrum, each Duplicate Samples sweeps a spectrum, corresponding 3 the parallel spectrum of each product, again 3 parallel spectrum are carried out being averaging and obtain an original spectrum, identical method is adopted to scan and gather spectrum to each product successively, obtain the original spectrum that each product is corresponding.
4. method according to claim 1, is characterized in that: in described step (6), detection and rejecting abnormalities value adopt the method detecting lever value, especially by the following step:
By following formulae discovery sample lever value:
Wherein,
h i for sample lever value,
t i for sample
ibecause of subvector,
t t tfor the factor score matrix of modeling collection,
t t i for
t i transposition;
When sample lever value is greater than 3k/n, wherein k is number of principal components, and n is sample number, and its spectrum has significant impact to recurrence, should reject.
5. method according to claim 1, it is characterized in that: the modelling verification of described step (7) adopts the predicted value of the quantitative model gained of t method of inspection determination verification sample collection input step (6) and corresponding step 4 gained samples Reference value whether to have deviation in statistical significance: namely, the predicted value of the quantitative model of the cellulose index that step (6) is set up and the samples Reference value t value of step (4) and degree of freedom d
v-1critical value t
(a, dv-1)compare, get level of signifiance a=0.05, when | t| < t
(a, dv-1), during probability P >0.05, illustrate that the testing result of two kinds of methods does not exist significant difference, modelling verification success, this model can be used for the cellulose measuring papermaking-method reconstituted tobaccos.
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| CN108267414A (en) * | 2017-12-26 | 2018-07-10 | 中山出入境检验检疫局检验检疫技术中心 | The near-infrared spectral analytical method of textile fiber content |
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