CN107367483A - A kind of online throwing of cigarette mixes the method for determination and evaluation of silk uniformity - Google Patents
A kind of online throwing of cigarette mixes the method for determination and evaluation of silk uniformity Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 60
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 31
- 238000011156 evaluation Methods 0.000 title claims abstract description 23
- 241000208125 Nicotiana Species 0.000 claims abstract description 92
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 92
- 235000000346 sugar Nutrition 0.000 claims abstract description 45
- 229930013930 alkaloid Natural products 0.000 claims abstract description 37
- 150000003797 alkaloid derivatives Chemical class 0.000 claims abstract description 35
- 239000003513 alkali Substances 0.000 claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000012544 monitoring process Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 20
- 238000002329 infrared spectrum Methods 0.000 claims description 18
- 238000004088 simulation Methods 0.000 claims description 9
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims description 8
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims description 8
- 229960002715 nicotine Drugs 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000005259 measurement Methods 0.000 claims description 6
- 238000010986 on-line near-infrared spectroscopy Methods 0.000 claims description 5
- 238000003556 assay Methods 0.000 claims description 3
- 238000010276 construction Methods 0.000 claims 1
- 230000006641 stabilisation Effects 0.000 abstract description 6
- 238000011105 stabilization Methods 0.000 abstract description 6
- 238000012545 processing Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 77
- 238000005070 sampling Methods 0.000 description 16
- 238000001228 spectrum Methods 0.000 description 16
- 239000007788 liquid Substances 0.000 description 12
- 238000007689 inspection Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 238000007781 pre-processing Methods 0.000 description 6
- 230000003595 spectral effect Effects 0.000 description 6
- 238000009825 accumulation Methods 0.000 description 4
- QPJDMGCKMHUXFD-UHFFFAOYSA-N cyanogen chloride Chemical compound ClC#N QPJDMGCKMHUXFD-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000011017 operating method Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Natural products OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 229960003742 phenol Drugs 0.000 description 2
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 description 2
- 229950000244 sulfanilic acid Drugs 0.000 description 2
- 235000019505 tobacco product Nutrition 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/04—Humidifying or drying tobacco bunches or cut tobacco
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B5/00—Stripping tobacco; Treatment of stems or ribs
- A24B5/16—Other treatment of stems or ribs, e.g. bending, chopping, incising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/12—Circuits of general importance; Signal processing
- G01N2201/129—Using chemometrical methods
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The invention belongs to technical field of tobacco processing, and in particular to a kind of online throwing of cigarette mixes the patent application matters of the method for determination and evaluation of silk uniformity.This method according to the principle of interior quality of the sugared alkali in the online pipe tobacco of cigarette than can preferably reflect tobacco, using online pipe tobacco sugar alkali than otherness establish online uniform evaluation method；Major technique thinking is：Total alkaloid in tobacco sample is established in the preparation of modeling sample → utilizing the content of total alkaloid and total reducing sugar in continuous flow method determination sample →（Total reducing sugar）The forecast model of content → according to model prediction line pipe tobacco mixing after total alkaloid（Total reducing sugar）Content, and throwing mixing property is evaluated accordingly.The application more can accurately realize online, mixed silk uniformity in real time monitoring and evaluation, so as to be laid the foundation for the stabilization of cigarette quality；This method is utilized simultaneously, can be that the improvement of related process and the Precise control of production of cigarettes are offered reference and referred to, thus there is preferable practical value and popularization and application meaning.
Description
Technical field
The invention belongs to technical field of tobacco processing, and in particular to the detection that a kind of online throwing of cigarette mixes silk uniformity is commented
The patent application matters of valency method.
Background technology
Cigarette become more meticulous production be the research of current tobacco business emphasis, and the research of the uniformity of mixed silk is that cigarette is fine
One of concrete embodiment of metaplasia production.The existing cut tobacco used in raw material of cigarette tobacco leaf formulation, also there is a stem and expansion thread, pipe tobacco with
The mixture uniformity of stem has important supporting role to the stability of cigarette product quality.Raw material of cigarette tobacco shred blending uniformity
The stabilization of cigarette product inherent quality will be directly affected, that is to say, that：It only ensure that mixed silk uniformity just can guarantee that often
The sucking quality of branch cigarette is identical.Therefore analysis is monitored to mixed silk uniformity, establishes mixed silk uniformity monitoring method,
Strong technical support can be provided for the production control that homogenizes.
At present, prediction and the mixed silk uniformity of evaluating cigarette throwing mainly have two methods in tobacco leaf production.The first side
Method is tracer labelling method；It is main from sugared, this kind of chemical composition directly related with aesthetic quality of alkali in second method
Uniformity coefficient reflects the mixed effect being entirely formulated.For both approaches, there is researcher to carry out different emphasis
Research.But in general, because tobacco leaf production enterprise in the prior art is mainly monitored and controlled to raw material proportioning precision,
And to mixed silk is horizontal, mixed silk uniformity still lacks and more clearly required online, still fall within basic theory plus existing research and grind
Study carefully, certain distance be present with production application situation, thus it is uniform that preferably online mixed silk is still a lack of in actual production
The detection of property and evaluation method.
The content of the invention
Present invention aims at the method for determination and evaluation for providing a kind of mixed silk uniformity of online throwing of cigarette, so as to be cigarette
Precise control and the process evaluation of production provide a kind of reference means of science, while are alternatively cigarette quality stabilization and technique
Improvement is offered reference and referred to.
Details are as follows for the technical scheme that the application is taken.
A kind of online throwing of cigarette mixes the method for determination and evaluation of silk uniformity, and this method is according to sugared alkali in the online pipe tobacco of cigarette
Than the principle for the interior quality that can preferably reflect tobacco, using online pipe tobacco sugar alkali than otherness establish and uniformly comment online
Valency method；Major technique thinking is：
Pipe tobacco sample is established in the preparation of modeling sample → utilizing the content of total alkaloid and total reducing sugar in continuous flow method determination sample →
Total alkaloid in product（Total reducing sugar）The forecast model of content → according to model prediction line pipe tobacco mixing after total alkaloid（Total reducing sugar）Contain
Amount, and throwing mixing property is evaluated accordingly；Specifically include following operating procedure：
（1）Prepare modeling sample
Required according to tobacco blend, obtain counter sample online, so that pipe tobacco and stem are cigarette formula material as an example, dried to online
Pipe tobacco and expanded cut stem are separately sampled after silk, and prepared by pipe tobacco and expanded cut stem gradient proportioning into simulation pipe tobacco, in this, as building
Sample needed for mould；Specifically, mode of operation is with reference to as follows：
The pipe tobacco sampling method after line dries silk：Start to sample after drying process normal operation is no less than 10min, at interval of 5min
A sample is taken, each sampling amount is 1.5Kg, accumulation sampling at least 20kg；
Expanded cut stem sampling method：Online addition expanded cut stem is taken, is started after expanded cut stem normal operation is no less than 10min
Sampling, a sample is taken at interval of 5min, and each sampling amount is 1Kg, accumulation sampling at least 15kg；
Pipe tobacco is simulated to prepare：Pipe tobacco and expanded cut stem after sampling, such as by 2% gradient proportion（Until pipe tobacco ratio is 100%）,
It is configured to model required sample；
It should be noted that to ensure to prepare uniformity, the amount of preparation of each modeling sample should typically be no less than 500g；
（2）To step（1）In it is prepared simulation tobacco sample carry out near infrared spectrum scanning,
It should be noted that to ensure that modeling specimen in use is consistent with the moisture content of on-line sample, modeling sample should be first in constant temperature
It is balanced in constant humidity cabinet to ensure the uniformity of moisture, carries out near infrared spectrum scanning again after balance.
（3）To step（1）Total alkaloid and total sugar content are measured in prepared simulation tobacco sample, during measure, are adopted
It is measured with continuous flow method；
The measure of total alkaloid in sample：
Specifically can be according to《The preparation of YC/T 31-1996 tobaccos and tobacco product sample and determination of moisture Oven Method》In will
Ask, sample is determined into moisture and is prepared into sample, is measured with reference to following steps：
0.25 g sample materials are weighed in 50 mL ground triangular flasks, are accurate to 0.0001 g, add 25 mL distilled water, lid
Upper plug, the on the oscillator min of oscillation extraction 30；
Filtered with qualitative filter paper, discard former milliliters of filtrates, subsequent filtrate, which performs an analysis, after collection is used；
Total alkaloid (in terms of nicotine) in extract is reacted with p-aminobenzene sulfonic acid and cyanogen chloride, and cyanogen chloride is by potassium cyanide
React generation online with toluene-sodium-sulfonchloramide；Reaction product colorimeter determines in 460 nm；Upper machine operation working stamndard liquid and sample liquid,
As sample liquid concentration exceed working stamndard liquid concentration range, then should dilute；
The calculating of total alkaloid：
The content of total alkaloid in terms of butt, is calculated as follows and draws：
Total alkaloid (%)=c ×（V/m）× (1-w) × 100%,
In formula：The instrument of c-sample liquid total alkaloid sees side value, and unit is every milliliter of milligram (mg/mL)；
The volume of V-extract, unit are milliliter (mL)；
The quality of m-sample material, unit are milligram (mg)；
The moisture of W-sample material；
The measure of total reducing sugar in sample：
With specific reference to following operating procedure：With 5% acetic acid aqueous solution extracted tobacco sample, the sugar in extract (survey by Water-soluble Total Sugar
Timing should hydrolyze) reacted with para hydroxybenzene formyl trap, the azo-compound of a yellow is produced in 85 DEG C of alkaline medium, it is most
Big absorbing wavelength is 410 nm, is determined with colorimeter；
The calculating of water-soluble sugar：
The content that water solubility in terms of butt is warded off, with glucose meter, it is calculated as follows and draws：
；
In formula：The Instrument observation value of C --- sample liquid total (reduction) sugar, unit is every milliliter of milligram (mg/mL)；
The volume of V --- extract, unit are milliliter (mL)；
The quality of M --- sample material, unit are milligram (mg)；
The moisture of W --- sample material.
（4）The forecast model and total sugar content forecast model of total alkaloid content are established respectively, by step（3）In total plant
Alkaloids assay result and total sugar content measurement result respectively with step（2）In near infrared spectrum corresponded, with
Build forecast model；Specifically：
The forecast model of total alkaloid content
Nicotine is assumed to be a kind of composition, operation analysis software is by step（3）In nicotine content measured value and step（2）In
Spectral scan result is corresponded, to build mathematical forecasting model；
During concrete operations, such as using the supporting data analyzing and processing software of near-infrared spectrometers（Dbase：《It is red
Outer processing software》(Bruker OPUS)6.5）, 17 points of spectrum of setting is smooth, and maximal dimension is set as 15, using vector normalizing
Change, first derivative, subtract the preprocessing procedures such as straight line, multiplicative scatter correction and combinations thereof spectrum is located in advance
Reason, and tentatively optimized；
According to the root-mean-square error of preliminary optimum results（RMSECV）And spectrum range, in the situation that root-mean-square error is basically identical
Under, reference spectra section selects larger spectrum range, is so advantageous to ensureing in the less situation of model root-mean-square error
Under, establishing model includes more spectral informations；
On this basis, internal chiasma inspection is carried out, optimal main composition dimension is determined according to the result of inspection, and it is progressively excellent
Change, rejecting abnormalities value, until establishing the coefficient of determination（R2）The larger and smaller preferably near-infrared forecast model of root-mean-square error；
Total sugar content forecast model
Total reducing sugar is assumed to be a kind of composition, operation analysis software is by step（3）In total sugar content measured value and step（2）In
Spectral scan result is corresponded, to build mathematical forecasting model；
Specific operation process, refer to the forecast model building process of above-mentioned total alkaloid content；
（5）Actually detected and evaluation, using the multi-functional Moisture Meter of On-line near infrared analyzer, moisture is carried out to cut tobacco storing cabinet outlet pipe tobacco
Monitoring and infrared diaphanoscopy；
Prejudged and whether met the requirements first according to moisture result, do not meet production requirement such as, show that pipe tobacco mixing degree is not inconsistent
Close and require；
If moisture result meets the requirements, then according to infrared diaphanoscopy result, with reference to step（4）In constructed prediction mould
Type, export the total alkaloid content of pipe tobacco for cut tobacco storing cabinet and total sugar content is predicted；According to this prediction result, sugared alkali is calculated
Than, and evaluate pipe tobacco accordingly and mix the silk uniformity.
It should be noted that sugared alkali is than not fixed value, during for different tobacco blends, sugared alkali is than numerical value and differs.
Before application method of determination and evaluation provided herein, the sugared alkali that is accordingly formulated can be obtained by measure and calculation early stage than numerical value,
When carrying out on-line checking and evaluation, when testing result and known sugars alkali than it is consistent when, you can think that mixed silk is uniform, when result differs
During cause, you can judge that mixed silk is not uniform enough.
In general, the application more can accurately realize online, mixed silk uniformity in real time monitoring and evaluation, so as to
Laid the foundation for the stabilization of cigarette quality；This method is utilized simultaneously, can be the improvement of related process and becoming more meticulous for production of cigarettes
Control is offered reference and referred to, thus has preferable practical value and popularization and application meaning.
Brief description of the drawings
Fig. 1 is that different water cut blade near infrared spectrum amplifies comparison diagram；
Fig. 2 is that on-line sample scans 3 near-infrared spectrograms；
Fig. 3 is 460 modeling sample atlas of near infrared spectra summary views；
Fig. 4 is mixed silk uniformity controlling figure before technique adjustment；
Fig. 5 is mixed silk uniformity controlling figure after technique adjustment.
Embodiment
Explanation is further explained to the application with reference to embodiment.
Embodiment
The online throwing of cigarette provided herein mixes the method for determination and evaluation of silk uniformity, and this method is online according to cigarette
The principle of interior quality of the sugared alkali than can preferably reflect tobacco in pipe tobacco, using online pipe tobacco sugar alkali than otherness establish exist
The uniform evaluation method of line；Details are as follows for concrete operation step.
（1）Prepare modeling sample
To line dry silk after pipe tobacco and expanded cut stem it is separately sampled, and by pipe tobacco and expanded cut stem gradient proportioning prepare simulation cigarette
Silk, in this, as sample needed for modeling；Specifically, mode of operation is with reference to as follows：
The pipe tobacco sampling method after line dries silk：Start to sample after drying process normal operation is no less than 10min, at interval of 5min
A sample is taken, each sampling amount is 1.5Kg, accumulation sampling at least 20kg；
Expanded cut stem sampling method：Online addition expanded cut stem is taken, is started after expanded cut stem normal operation is no less than 10min
Sampling, a sample is taken at interval of 5min, and each sampling amount is 1Kg, accumulation sampling at least 15kg；
Pipe tobacco is simulated to prepare：Pipe tobacco and expanded cut stem after sampling, such as by 2% gradient proportion（Until pipe tobacco or stem ratio are
100%）, it is configured to model required sample；
It should be noted that to ensure to prepare uniformity, the amount of preparation of each modeling sample should be no less than 500g；
It is final in the present embodiment to amount to 46 tobacco leaf formulation samples of preparation（It is to be understood that when following embodiments prepare sample,
Not fully according to 2% ratio, when mainly pipe tobacco ratio is too low, lack practical significance in strict accordance with 2% gradient, and easily increase
Add workload, but for theory, sample is more, and subsequent result is more accurate）, specific configuration proportion such as following table, then by each sample
10 are uniformly divided into, is prepared for 460 modeling samples altogether.
The mixed ratio design of specific pipe tobacco and stem is as follows：
。
（2）To step（1）In it is prepared simulation tobacco sample carry out near infrared spectrum scanning,
Concrete operation step is with reference to described below（Near infrared spectrometer, MATRIX-1, German BRUKER companies）：
Take step（1）Prepared simulation tobacco sample, it is placed in a diameter of 97mm quartz measuring cup, it is 500g's to be put into quality
" seal " shape sample-pressing device is gently flattened in cup after sample, and background is done with gold-plated diffuse reflector, is put into turntable and is scanned；
During scanning, it is desirable to which every 10 samples sweep a background；Finally data acquisition is carried out by spectra collection requirement.
In scanning process, partial parameters facilities consider as follows：
1st, the setting of nir instrument scanning times：In scanning process, the scanning times of each tobacco sample are set as 64 times；
2nd, the setting of nir instrument resolution ratio：The resolution ratio of instrument influences the quality of collection of illustrative plates, typically requires that instrumental resolution should
Equivalent to the 1/10 of sample collection of illustrative plates half-peak breadth, the half-peak breadth of tobacco sample near-infrared spectra area reflection absorption spectrum is about 200-
400cm-1, therefore resolution setting is 20cm-1Resolution ratio selects 8cm when can meet needs, and analyze-1；
3rd, during spectra collection in environment temperature and instrument environment control：Before spectra collection is carried out, to make spectrometer at least pre-
Hot 1.5h, while instrument drying tube will be in drying regime all the time, to ensure that spectrometer has dry interior environment.
It should be noted that due in water the stretching vibration of O-H keys cause moisture to have stronger absorption near infrared spectrum
Peak, it is the main interference factors of Near-Infrared Quantitative Analysis feeding homogeneity, therefore is preparing modeling sample and near infrared spectrum is swept
Before retouching, inventor has taken into full account influence of the moisture to near-infrared wave spectrum in sample.
By changing the shadow near infrared spectrum to influence of the pipe tobacco different water cut near infrared spectrum, tobacco leaf formulation
Sound, different batches, the near infrared spectrum of different sample time pipe tobaccos are analyzed, and contrast the difference of their near infrared spectrums, hair
Difference is mainly in 4000-7000 cm caused by a person of good sense has found moisture content-1Between（Partial results are as shown in Figure 1, 2）；And with
The increase of moisture, spectrogram baseline translates up, therefore moisture content of cut tobaccos has a great influence to spectrogram.
Amid all these factors, to ensure that modeling specimen in use is consistent with the moisture content of on-line sample, modeling sample Ying Heng
It is balanced in constant temperature and humidity case（The present embodiment balances 48h under the conditions of 22 DEG C, relative humidity 60%）To ensure the consistent of moisture
Property, carry out after balance and then again near infrared spectrum scanning.
It is emphasized that due to different process, different manufacturing enterprises in process of production, for moisture requirement not
Modeling sample that is identical to the greatest extent, thus when being based on different in moisture content requirement, being established（Simulate pipe tobacco）Situation also can difference,
And then cause final IR spectrum scanning result difference；In other words it is specific to prepare modeling, it is necessary to reference to produce reality situation
Sample, preferably prediction and evaluation result could be obtained.
Finally, 460 modeling samples are scanned using near infrared spectrometer, 460 near infrared lights is obtained
Spectrogram（As shown in Figure 3）.
（3）To step（1）Total alkaloid and total sugar content are measured in prepared simulation tobacco sample, during measure, are adopted
It is measured with continuous flow method；
The measure of total alkaloid in sample：
Specifically can be according to《The preparation of YC/T 31-1996 tobaccos and tobacco product sample and determination of moisture Oven Method》In will
Ask, sample is determined into moisture and is prepared into sample, is measured with reference to following steps：
0.25 g sample materials are weighed in 50 mL ground triangular flasks, are accurate to 0.0001 g, add 25 mL distilled water, lid
Upper plug, the on the oscillator min of oscillation extraction 30；
Filtered with qualitative filter paper, discard former milliliters of filtrates, subsequent filtrate, which performs an analysis, after collection is used；
Total alkaloid (in terms of nicotine) in extract is reacted with p-aminobenzene sulfonic acid and cyanogen chloride, and cyanogen chloride is by potassium cyanide
React generation online with toluene-sodium-sulfonchloramide；Reaction product colorimeter determines in 460 nm；Upper machine operation working stamndard liquid and sample liquid,
As sample liquid concentration exceed working stamndard liquid concentration range, then should dilute；
The calculating of total alkaloid：
The content of total alkaloid in terms of butt, is calculated as follows and draws：
Total alkaloid (%)=c ×（V/m）× (1-w) × 100%,
In formula：The instrument of c-sample liquid total alkaloid sees side value, and unit is every milliliter of milligram (mg/mL)；
The volume of V-extract, unit are milliliter (mL)；
The quality of m-sample material, unit are milligram (mg)；
The moisture of W-sample material；
Total alkaloid in 460 modeling samples is measured, and records the measurement result of total alkaloid in modeling sample.
The measure of total reducing sugar in sample：
With specific reference to following operating procedure：With 5% acetic acid aqueous solution extracted tobacco sample, the sugar in extract (survey by Water-soluble Total Sugar
Timing should hydrolyze) reacted with para hydroxybenzene formyl trap, the azo-compound of a yellow is produced in 85 DEG C of alkaline medium, it is most
Big absorbing wavelength is 410 nm, is determined with colorimeter；
The calculating of water-soluble sugar：
The content that water solubility in terms of butt is warded off, with glucose meter, it is calculated as follows and draws：
；
In formula：The Instrument observation value of C --- sample liquid total (reduction) sugar, unit is every milliliter of milligram (mg/mL)；
The volume of V --- extract, unit are milliliter (mL)；
The quality of M --- sample material, unit are milligram (mg)；
The moisture of W --- sample material.
Total sugar content in 460 modeling samples is measured, and records the measurement result of modeling sample.
（4）The forecast model and total sugar content forecast model of total alkaloid content are established respectively, by step（3）In total plant
Alkaloids assay result and total sugar content measurement result respectively with step（2）In near infrared spectrum corresponded, with
Build forecast model；Specifically：
The forecast model of total alkaloid content
Nicotine is assumed to be a kind of composition, with the analysis software that near-infrared spectrometers are supporting（Dbase：《It is infrared
Handle software》(Bruker OPUS)6.5）, by step（3）In nicotine content measured value and step（2）In spectral scan knot
Fruit is corresponded, to build mathematical forecasting model；
During concrete operations, application《Infrared processing software》(Bruker OPUS) 6.5 data processing softwares, 17 points of spectrum of setting are put down
Sliding, maximal dimension is set as 15, is normalized using vector, first derivative, subtracts straight line, multiplicative scatter correction and combinations thereof
Spectrum is pre-processed Deng preprocessing procedures, and tentatively optimized；
According to the root-mean-square error of preliminary optimum results（RMSECV）And spectrum range, in the situation that root-mean-square error is basically identical
Under, reference spectra section selects larger spectrum range, is so advantageous to ensureing in the less situation of model root-mean-square error
Under, establishing model includes more spectral informations；
On this basis, internal chiasma inspection is carried out, optimal main composition dimension is determined according to the result of inspection, and it is progressively excellent
Change, rejecting abnormalities value, until establishing the coefficient of determination（R2）The larger and smaller preferably near-infrared forecast model of root-mean-square error.
Finally, by different preprocessing procedures to tobacco sample collection（Sample sets set constituent as " nicotine "）Enter
Row pretreatment and optimization after, it is determined that preprocessing procedures be：First derivative+MSC, spectrum range are：11202.2~
4246.7；On this basis, then internal chiasma inspection is carried out, and rejects part exceptional value, obtain final near-infrared prediction mould
Type.
Total sugar content forecast model
Total reducing sugar is assumed to be a kind of composition, with the analysis software that near-infrared spectrometers are supporting（Dbase：《It is infrared
Handle software》(Bruker OPUS)6.5）, by step（3）In total sugar content measured value and step（2）In spectral scan knot
Fruit is corresponded, to build mathematical forecasting model；
Building process of the specific operation process with the forecast model of above-mentioned total alkaloid content.It should be noted that building process
In, with the increase of main composition dimension, the coefficient of determination（R2）Incrementally increase, while root-mean-square error progressively reduces, when being tieed up to 13,
The two finally determines that main composition dimension is 13 there is no significant change.
Finally, by different preprocessing procedures to tobacco sample collection（Sample sets set constituent as " total reducing sugar "）Enter
Row pretreatment and optimization after, it is determined that preprocessing procedures be：First derivative+MSC, spectrum range are：11202.2~
4246.7 cm -1；On this basis, then internal chiasma inspection is carried out, and rejects part exceptional value, finally establish root-mean-square error
It is smaller, the coefficient of determination（R2）Larger preferable near-infrared forecast model.
（5）Actually detected and evaluation, using the multi-functional Moisture Meter of On-line near infrared analyzer, the moisture that pipe tobacco is exported to cut tobacco storing cabinet contains
Whether amount is monitored, prejudged and met the requirements first according to moisture result, do not meet production requirement such as, shows that pipe tobacco mixes
Spend undesirable；
If moisture result meets the requirements, show that the application is based on step（2）Infrared scan result and step（3）Inspection
Survey the step constructed by result（4）Forecast model can apply, then according to infrared scan result, and combine step（4）In
Constructed forecast model, export the total alkaloid content of pipe tobacco for cut tobacco storing cabinet and total sugar content is predicted；It is pre- according to this
Result is surveyed, calculates sugared alkali ratio, and evaluates pipe tobacco accordingly and mixes the silk uniformity, shows mixed silk when sugared alkali ratio is consistent with formula design load
Uniformly.
It should be noted that partial results are based on certain manufacturing enterprise's actual conditions acquired results, profit in the above method
With above-mentioned model prediction result, actual experiment has been carried out to the production line of certain batch of the enterprise.
It should be noted that detected and calculated by early stage, for this formula tobacco leaf, when sugared alkali ratio is located at 6.50 ~ 7.10
Between when（During actual motion, according to tobacco formulation, this reasonable interval value can be formulated first as evaluation basic standard）, you can table
Bright pipe tobacco mixing property is preferable；In other words, when carrying out on-line checking assessment, the sugared alkali ratio that material is obtained when detection is located at this scope
When, you can show that the mixing of this batch production material is preferable, but this scope area is broken through again and again when detection obtains material sugar alkali ratio
Between when, show that mixed silk uniformity is to be improved, certain mass be present.
Cut tobacco storing cabinet outlet pipe tobacco is monitored using On-line near infrared analyzer multi-functional Moisture Meter, and according to above-mentioned model result
Calculated, as a result as shown in following table and Fig. 1：
Sugared alkali when mixes the measurement result of the silk uniformity：
。
It can be seen from the results above that the batch pipe tobacco uniformity is only 93.63%（Figure 4, it is seen that online inspection
Survey result break through again and again sugared alkali than reasonable interval）；Further aesthetic quality's smoking result shows, the inherent quality of this batch of pipe tobacco
Stability can not meet requirement, it is necessary to be readjusted to associated production technique.
Through recalibrating main title and respectively mixing the precision matched, and specific aim adjustment correlative belt conveyor and stone belt
Frequency and after the series such as each fixed height of photocell for claiming blanking port improves, re-use the multi-functional Moisture Meter pair of On-line near infrared analyzer
Cut tobacco storing cabinet outlet pipe tobacco is monitored, and testing result is as shown in Fig. 5 and following table：
。
Can be seen that its mixed silk uniformity from upper table data is 97.75%（From figure 5 it can be seen that after being adjusted, sugar
Alkali fluctuates than in normal range (NR) section）, further after aesthetic quality smokes panel test, the inherent quality stability of this batch of pipe tobacco can
Preferably meet to require.
It should be noted that in actual production, preferably throwing mixing degree can be entered using method provided herein
Row on-line real time monitoring, generally, when finding that the mixed silk uniformity is less than 95%, should stop immediately production check and
Concerned process steps are overhauled and improved, and to ensure the stabilization of pipe tobacco mixings degree and reliably, and then ensure the stabilization of cigarette quality.
Claims (4)
1. a kind of online throwing of cigarette mixes the method for determination and evaluation of silk uniformity, it is characterised in that specifically includes following operation step
Suddenly：
（1）Modeling sample is prepared, is required according to tobacco blend, obtains the sample of corresponding formula material respectively online；Then according to
Gradient proportion, be configured to series modeling needed for sample, that is, simulate pipe tobacco；
（2）To step（1）In it is prepared simulation tobacco sample carry out near infrared spectrum scanning,
（3）To step（1）Total alkaloid and total sugar content are measured in prepared simulation tobacco sample,
（4）The forecast model and total sugar content forecast model of total alkaloid content are established respectively, by step（3）In total alkaloid
Assay result and total sugar content measurement result respectively with step（2）In near infrared spectrum corresponded, with structure
Forecast model；
（5）Actually detected and evaluation, using the multi-functional Moisture Meter of On-line near infrared analyzer, moisture is carried out to cut tobacco storing cabinet outlet pipe tobacco
Monitoring and infrared diaphanoscopy；
If moisture monitoring does not meet production requirement, show that pipe tobacco mixing degree is undesirable；
If moisture monitoring result meets the requirements, according to infrared diaphanoscopy result, with reference to step（4）In constructed prediction
Model, export the total alkaloid content of pipe tobacco for cut tobacco storing cabinet and total sugar content is predicted；According to this prediction result, sugar is calculated
Alkali ratio, and evaluate pipe tobacco accordingly and mix the silk uniformity.
2. the online throwing of cigarette as claimed in claim 1 mixes the method for determination and evaluation of silk uniformity, it is characterised in that step（3）
In, total alkaloid and total sugar content are measured respectively using continuous flow method.
3. the online throwing of cigarette as claimed in claim 1 mixes the method for determination and evaluation of silk uniformity, it is characterised in that step（1）
In, the amount of preparation of each modeling sample is no less than 500g.
4. the online throwing of cigarette as claimed in claim 1 mixes the method for determination and evaluation of silk uniformity, it is characterised in that step（4）
In, when building forecast model, nicotine, total reducing sugar are assumed to be a kind of composition respectively and carry out model construction.
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