CN106932365A - A kind of method that maize straw composition is detected near infrared spectrometer - Google Patents
A kind of method that maize straw composition is detected near infrared spectrometer Download PDFInfo
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- CN106932365A CN106932365A CN201511023790.6A CN201511023790A CN106932365A CN 106932365 A CN106932365 A CN 106932365A CN 201511023790 A CN201511023790 A CN 201511023790A CN 106932365 A CN106932365 A CN 106932365A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/47—Scattering, i.e. diffuse reflection
- G01N21/49—Scattering, i.e. diffuse reflection within a body or fluid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
- G01N5/045—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder for determining moisture content
Abstract
The invention discloses a kind of method that maize straw composition is detected near infrared spectrometer, comprise the following steps：Step one, maize straw sample pretreatment；Step 2, the analysis of maize straw sample composition；Step 3, the collection of maize straw sample near infrared spectrum；And step 4, the qualitative, quantitative calibrating mathematical model set up between the Components Chemical value of maize straw and its near infrared spectrum data.The component of one straw sample of near-infrared method for quick measure of the present invention is completed by only needing to 5 minutes~10 minutes, and simple to operate, without reagent chemicals consumption.In a large amount of sample analysis, considerable artificial and analysis cost will be saved out for enterprise.
Description
Technical field
The invention belongs to components of biomass analysis field, more particularly to a kind of method of use near infrared spectrometer quick detection maize straw composition.
Background technology
Maize straw is a kind of main biomass resource, with stock number is big, renewable, sulfur content is low and used as using energy source CO2The advantages of zero-emission.But because its harvest season property is strong, distribution disperses, bulk density is small, memory space is big, in long term storage, the composition such as its cellulose and hemicellulose can all change, and the component content such as the cellulose of different sources different cultivars maize straw also has different.Currently, the relevant criterion of the method for quick and quality evaluation with specification corn stalk raw material is not set up also both at home and abroad, although in maize straw constituent analysis, standard method and the technology of a series of biomass material composition analysis and Quality Identification have been set up using chemical method, but these method generally existings waste time and energy, it is with high costs the shortcomings of, the quick means for dividing material quality grade can not be provided for biomass energy enterprise, to formulate reasonable purchasing price.
In order to set up biomass material method for evaluating quality, carry out a series of researchs both at home and abroad and achieve constructive progress, especially using near-infrared spectrum technique (Near infrared reflectance spectroscopy, abbreviation NIRS) qualitative and quantitative analysis biomass composition aspect, have been achieved for considerable progress.At present, near-infrared spectrum technique has been achieved for preferable achievement in the research of the qualitative, quantitatives such as wheat stalk composition, straw chemical composition, the moisture content of various energy resources crop and the ash content of coal, is the developing direction of future biological matter raw material fast qualitative quantitative study.The relevant criterion that near-infrared spectrum technique carries out quick measure to maize straw main chemical compositions then has no report.
Near-infrared spectrum technique has the characteristics that：(1) it is simple, sample is not consumed without cumbersome pre-treatment and, Direct Analysis solid sample can be used；(2) quick, determining a sample generally only needs 1~2 minute；(3) sample detection low cost；(4) efficiently, the detection of multiple sample difference chemical index can simultaneously be completed；(5) environmental protection, detection process is pollution-free；(6) with database expansion and perfect, can correction model, improve accuracy of detection.(7) it is capable of achieving on-line checking etc..
The content of the invention
It is an object of the invention to provide a kind of method that maize straw composition is detected near infrared spectrometer.
To achieve the above object, the invention provides a kind of method that maize straw composition is detected near infrared spectrometer, comprise the following steps：
Step one, maize straw sample pretreatment；
Step 2, the analysis of maize straw sample composition；
Step 3, the collection of maize straw sample near infrared spectrum；
Step 4, the qualitative, quantitative calibrating mathematical model set up between the Components Chemical value of maize straw and its near infrared spectrum data.
Wherein, the detailed process of maize straw sample pretreatment is that the moisture of maize straw sample is dropped into 6%~12% in step one, crushed and sieved, granularity is determined in 40 mesh~60 mesh samples for chemical score, sample of the granularity more than 60 mesh is used near infrared spectrum scanning.
Wherein, the composition that maize straw sample composition analysis is carried out in step 2 includes holocellulose, cellulose, hemicellulose, lignin, extract, ash content and moisture.
Wherein, the collection process of maize straw sample near infrared spectrum is in step 3：It is that more than 60 mesh maize straw sample is put into sample analysis disk by granularity, analysis panel surface is struck off, in wave number 6061cm-1~1053cm-1It is interior that near infrared spectrum collection is carried out to maize straw sample.
Wherein, near infrared spectrum collection is carried out to maize straw sample using the diode array holography fixed grating continuous spectrum mode of Bo Tong companies of Sweden DA7250 near infrared spectrometers.
Wherein, it is 100 times/second, wavelength accuracy 2nm~5nm, multiple scanning sample 1 time~2 times to carry out spectrum collection rate when near infrared spectrum is collected.
Wherein, in step 4 qualitative, quantitative calibrating mathematical model set up process be carry out that convolution is smooth to the diffusing reflection original spectrum of maize straw and standard normalization pretreatment after, recycle PLS and complete intersection verification mode to set up the near infrared spectrum linear model of maize straw holocellulose, cellulose, hemicellulose, lignin, extract, ash content and moisture.
Wherein, qualitative, quantitative calibrating mathematical model is set up using the multivariate data analysis softwares of The Unscrambler 9.8 of CAMO companies of Norway.
Wherein, the coefficient of determination of holocellulose, cellulose, hemicellulose, lignin, extract, ash content and moisture is respectively 0.8432,0.8383,0.9026,0.8616,0.9187,0.9134 and 0.8805 in qualitative, quantitative calibrating mathematical model；Factor of influence is respectively 7,12,14,3,5,11 and 4；Root-mean-square-deviation RMSECV is respectively 2.02%, 1.86%, 1.27%, 1.16%, 1.50%, 0.63% and 0.53%.
Beneficial effects of the present invention：
The component of one straw sample of near-infrared method for quick measure of the present invention is completed by only needing to 5 minutes~10 minutes, and simple to operate, without reagent chemicals consumption.In a large amount of sample analysis, considerable artificial and analysis cost will be saved out for enterprise.
Brief description of the drawings
Fig. 1 diffuses spectrogram for the near-infrared of maize straw；
Fig. 2 is through convolution is smooth and standard normalizes the near-infrared of pretreated maize straw and diffuses spectrogram；
Fig. 3 is holocellulose predicted value figure related to measured value；
Fig. 4 is cellulose predicted value figure related to measured value；
Fig. 5 is hemicellulose predicted value figure related to measured value；
Fig. 6 is lignin predicted value figure related to measured value；
Fig. 7 is extract predicted value figure related to measured value；
Fig. 8 is ash content predicting value figure related to measured value；
Fig. 9 is moisture predicted value figure related to measured value.
Specific embodiment
Be combined for near-infrared spectrum technique and chemometrics method by the present invention, and the qualitative, quantitative calibrating mathematical model set up between the main component chemical score of maize straw and its near infrared spectrum data using multivariate data analysis software, so as to set up the method for quick of maize straw main component.
Technical solution of the present invention is as follows：
(1) maize straw sample pretreatment：The moisture of maize straw sample is dropped to 10%, is crushed and is sieved, granularity is determined in 40 mesh~60 mesh samples for chemical score, sample of the granularity more than 60 mesh is used near infrared spectrum scanning；
(2) maize straw sample composition analysis：Holocellulose determines the assay method with reference to GB/T 2677.10-1995 paper making raw material holocellulose contents；Cellulose is determined and determined with reference to NREL (National Renewable Energy laboratory) method, and maize straw hydrolysis sugar is analyzed using Japanese Shimadzu Corporation LC-20A plus liquid chromatographs；It is difference of the holocellulose content with content of cellulose that hemicellulose is determined；Lignin determines the assay method with reference to the insoluble lignin content of GB/T 2677.8-94 paper making raw materials；Extract determines the assay method and NREL (National Renewable Energy laboratory) method with reference to GB/T 2677.4-93 paper making raw material water extract contents；The assay method of ash determination reference GB/T 742-2008 paper making raw materials, paper pulp, paper and cardboard ash content, and ash analysis is carried out to maize straw analysis sample using the extensive and profound in meaning Science and Technology Ltd. TL0910 Muffle furnaces in BeiJing ZhongKe；The assay method of the insoluble moisture of determination of moisture reference GB/T 2677.2-2011 paper making raw materials, and water analysis is carried out to maize straw analysis sample using Japanese AND companies MX-70 fast tester for water content；
(3) collection of maize straw sample near infrared spectrum：It is that more than 60 mesh maize straw sample is put into a diameter of 7.5cm by granularity, depth is in the sample analysis disk of 1.0cm~2.8cm, struck off panel surface is analyzed using leveling ruler, using the diode array holography fixed grating continuous spectrum mode of Bo Tong companies of Sweden DA7250 near infrared spectrometers in wave number 6061cm-1~1053cm-1Near infrared spectrum collection is carried out to maize straw sample in (950nm~1650nm), spectral collection speed reaches 100 times/second, wavelength accuracy 5nm, multiple scanning sample 2 times；
(4) foundation of the qualitative, quantitative calibrating mathematical model between the main component chemical score and its near infrared spectrum data of maize straw：After convolution smooth (S Golay) and standard normalization (SNV) pretreatment are carried out to the diffusing reflection original spectrum of maize straw using the multivariate data analysis softwares of The Unscrambler 9.8 of CAMO companies of Norway, PLS (PLS) and complete intersection verification mode is recycled to establish the near infrared spectrum linear model of maize straw holocellulose, cellulose, hemicellulose, lignin, extract, ash content and moisture.The coefficient of determination (the R of model2) it is respectively 0.8432,0.8383,0.9026,0.8616,0.9187,0.9134 and 0.8805；Factor of influence is respectively 7,12,14,3,5,11 and 4；Root-mean-square-deviation RMSECV is respectively 2.02%, 1.86%, 1.27%, 1.16%, 1.50%, 0.63% and 0.53%.
The present invention have collected the chemical analysis Value Data and its near infrared spectrum data of 213 holocellulose of maize straw sample, cellulose, hemicellulose, lignin, extract, ash content and moisture with the maize straw of the representational maize straw in Jilin Area and packing storage as research object, altogether.And using CAMO companies of Norway the multivariate data analysis softwares of The Unscrambler 9.8 convolution smooth (S Golay) and standard normalization (SNV) pretreatment are carried out to diffusing reflection original spectrum after, the near infrared spectrum linear model of maize straw holocellulose, cellulose, hemicellulose, lignin, extract, ash content and moisture is established using PLS (PLS) and complete intersection verification mode.
Embodiment 1 analyzes maize straw main component using chemical analysis
1.1 sample pretreatments
Stalk is put into heated-air circulation oven, moisture is dried in 50 DEG C of baking ovens and is reduced to 10% or so, then using high speed disintegrator by crushed stalk, then the stalk that drying is sieved with sub-sieve, the stalk taken between 40 mesh~60 mesh is stored in valve bag, and equilibrium water conten carries out subsequent step after 24 hours.
The measure of 1.2 extracts
Testing sample accurately is weighed, its dry biomass m0It is 0.9023g (being accurate to 0.0001g), is wrapped with filter paper and marked, it is with degreasing cotton thread that filter paper looping is good, prevent raw material from spilling.It is then placed in placing into boiling water bath laser heating in the beaker equipped with water, beaker reclaimed water need to change clear water untill clarification of water in beaker when turning yellow, washing terminates natural air drying in holding chamber, it is then placed in apparatus,Soxhlet's, is stripped with absolute ethyl alcohol, it is ensured that reflow's cycle is no less than 4 times per hour, filter paper bag is taken out after extracting 6h, standby after ethanol volatilizees, remaining solid dries two hours in 105 DEG C of baking ovens, and determines its quality m with fast tester for water content1It is 0.7840g.It is 13.00% to calculate extract content by formula (1).
1.3 content of cellulose are determined
Testing sample accurately is weighed, its dry biomass m0It is 0.9023g (being accurate to 0.0001g), wrapped with filter paper and marked, after passing it through water extracting and ethanolic extraction, it is put into the beaker of 50mL and adds the 72% of 15mL sulfuric acid, stir in hydrolyzing 2.5h at 20 DEG C, then hydrolyzate is transferred in the triangular flask of 1L and the distilled water of 545mL is added thereto to, triangular flask is placed in autoclave and is hydrolyzed 1h at 121 DEG C.Hydrolysis filters hydrolyzate gained solid as lignin after terminating with G2 crucible types filter, and after filtering gained filtrate is neutralized to neutrality with barium hydroxide, the content that glucose in filtrate is determined with HPLC is 0.615g.The content for calculating cellulose by formula (2) is 34.35%.
1.4 holocellulose contents are determined
Testing sample accurately is weighed, its dry biomass m0It is 0.9023g (being accurate to 0.0001g), is wrapped with filter paper and marked, testing sample is entered into water-filling and ethanolic extraction first.The filter paper bag after extracting and air-drying is opened, by whole samples immigration 250mL triangular flasks.55mL distilled water, 0.5mL glacial acetic acids, 0.55g sodium chlorites are added, is shaken up, buckle 25mL conical flasks, 1h is reacted in 75 DEG C of waters bath with thermostatic control, in heating process, should often rotate and shake conical flask.After time reaches, to 0.5mL glacial acetic acids and 0.55g sodium chlorites is added in conical flask again, shake up, 1h is heated in continuation in 75 DEG C of water-baths, is so repeated 3 times, untill sample bleaches.Taken out from water-bath during conical flask is put into ice-water bath and cooled down, be filtered by suction with the glass filter of constant weight, with distilled water cyclic washing to neutrality, dried to constant weight in 105 DEG C of baking ovens, and record its quality m1It is 0.6930g.Content in sand core crucible is transferred in porcelain crucible, 6h is ashed in 800 DEG C of Muffle furnaces, after ashing terminates, the quality m of precise porcelain crucible content2It is 0.0567g.The content for calculating holocellulose by formula (3) is 70.52%.
1.5 hemicellulose levels are determined
Determine the content of cellulose and holocellulose respectively according to formula (2) and (3) methods described, the content for calculating hemicellulose by formula (4) is 36.17%
Hemicellulose level=holocellulose content-content of cellulose (4)
1.6 content of lignin are determined
Content of lignin in stalk is determined using two-step method sour water solution, as holocellulose is determined, testing sample should be accurately weighed first, its dry biomass m0It is 0.9023g (being accurate to 0.0001g), is wrapped with filter paper and marked, then enters water-filling and ethanolic extraction.
By in the sample immigration 100mL beakers after extracting, the sulfuric acid for adding 15mL mass fractions to be 72% makes sample be all impregnated with by acid solution.Then beaker is placed in 20 DEG C of water-baths, reacts 2.5h.Then above-mentioned beaker contents are all moved into 1000mL conical flasks, adds distilled water, then conical flask is placed in autoclave, 1h is hydrolyzed under the conditions of 121 DEG C, be naturally cooling to less than 100 DEG C, take out conical flask.Filtered with G2 crucible types filter, and solid to neutrality is washed with hot distilled water, dried in 105 DEG C of baking ovens, weighed, and record its quality m1It is 0.1616g.The content of sand core crucible is transferred in porcelain crucible, 6h is ashed in 800 DEG C of Muffle furnaces, after ashing terminates, the quality m of precise porcelain crucible content2It is 0.0181g.The content for calculating lignin by formula (5) is 15.90%.
1.7 ash content tests
0.5235g testing samples are weighed, its dry biomass m0=0.4724g (is accurate to 0.0001g), is put into porcelain crucible.Porcelain crucible is ashed 6h in 800 DEG C of Muffle furnaces, after being cooled to room temperature, the sample quality m after being ashed with assay balance accurate weighing1It is 0.0307g.The content for calculating ash content in sample by formula (6) is 6.50%.
1.8 determinations of moisture
Weigh the straw sample m between 40 mesh~60 mesh0=0.609g, is put into MX-70 fast tester for water content pallets, and temperature is set as 120 DEG C of drying 20min, after sample quality is unchanged, reads sample quality m1=0.569g.The content for calculating moisture in sample by formula (7) is 6.57%.
The distribution of 1.9 maize straw each component contents
Constituent analysis work has been carried out to 213 collected maize straw samples using standard chemical analysis method, 1 has been shown in Table.
Maize straw each component content (mass fraction %) of table 1
| Holocellulose | Cellulose | Hemicellulose | Lignin | Extract | Ash content | Moisture | |
| Maximum | 73% | 46% | 36% | 20% | 22% | 12% | 12% |
| Minimum value | 51% | 24% | 19% | 10% | 11% | 1% | 6% |
| Average value | 66% | 37% | 29% | 15% | 15% | 5% | 8% |
The near infrared light spectrum signature of the maize straw composition of embodiment 2
It is the macromolecule organics such as cellulose, hemicellulose and lignin that maize straw is mainly constituted, and these compositions have stronger absorption near infrared region.As shown in figure 1, the main component of maize straw has stronger absworption peak at 1450nm.The bands of a spectrum of near infrared spectrum are wider, and peak overlap is serious, therefore, near infrared spectrum can not clearly determine the ownership of bands of a spectrum as middle infrared spectrum.
The present invention is as shown in Figure 2 through the spectrogram that convolution smooth (S Golay) and standard normalization (SNV) are pre-processed.Figure it is seen that spectrum after pretreatment can be accurately found to the contributive region of model accuracy in 1300nm~1600nm.
The qualitative, quantitative calibrating mathematical model that embodiment 3 is set up between the main component chemical score of maize straw and its near infrared spectrum data
The present invention chooses 213 samples altogether, calibration model is set up using the PLS and complete intersection verification mode of the softwares of The Unscrambler 9.8, as shown in Fig. 3~Fig. 9.The preprocessing procedures of modeling, factor of influence, model correct result and model relative deviation is as shown in table 2.
The Model Parameter Optimization of table 2 and correction result
Embodiment 4 verifies the accuracy of maize straw near infrared spectrum Mathematical Modeling：
The sample of measured value known to a group is predicted using model, predicted value and measured value are carried out into statistical comparison, partial analysis result is as shown in table 3, table 4.Wherein, using the partial results of standard method analysis maize straw sample component as shown in table 5, table 6.
The comparing (mass fraction %) of the maize straw holocellulose of table 3, cellulose and hemicellulose model to the predicted value and measured value of sample
The comparing (mass fraction %) of the Spruce lignin of table 4, extract, ash content and water model to the predicted value and measured value of sample
The chemical analysis results (mass fraction %) of the maize straw holocellulose of table 5, cellulose and hemicellulose sample
The chemical analysis results (mass fraction %) of the Spruce lignin of table 6, extract, ash content and moisture sample
Be can be seen that from the data of 3~table of table 6, holocellulose is -3%~2%, -12%~3% with the relative deviation scope of measured value with the predicted value of fiber prime model, in the range of standard method -3%~4%, -12%~9% relative deviation, illustrate that forecast result of model is preferable；The predicted value of hemicellulose, lignin, extract, ash content and water model and the relative deviation scope of measured value are -13%~4%, -7%~17%, -8%~13%, -25%~40%, -27%~17%, the forecast result of model bigger than normal but above-mentioned than standard method -9%~9%, -6%~6%, -11%~5%, -20%~0%, 0%~17% relative deviation scope is within the acceptable range.
Certainly; the present invention can also have other various embodiments; in the case of without departing substantially from spirit of the invention and its essence, those of ordinary skill in the art can make various corresponding changes and deformation according to the present invention, but these corresponding changes and deformation should all belong to the protection domain of the claims in the present invention.
Claims (9)
1. a kind of method that maize straw composition is detected near infrared spectrometer, it is characterised in that including following step
Suddenly：
Step one, maize straw sample pretreatment；
Step 2, the analysis of maize straw sample composition；
Step 3, the collection of maize straw sample near infrared spectrum；
Step 4, the qualitative, quantitative set up between the Components Chemical value of maize straw and its near infrared spectrum data
Calibrating mathematical model.
2. it is according to claim 1 near infrared spectrometer detect maize straw composition method, its feature
It is that the detailed process of maize straw sample pretreatment is to drop to the moisture of maize straw sample in step one
6%~12%, to be crushed and sieved, granularity is determined in 40 mesh~60 mesh samples for chemical score, grain
The sample spent more than 60 mesh is used near infrared spectrum scanning.
3. it is according to claim 1 near infrared spectrometer detect maize straw composition method, its feature
It is that the composition that maize straw sample composition analysis is carried out in step 2 includes holocellulose, cellulose, half
Cellulose, lignin, extract, ash content and moisture.
4. it is according to claim 1 near infrared spectrometer detect maize straw composition method, its feature
It is that the collection process of maize straw sample near infrared spectrum is in step 3：It is more than 60 mesh by granularity
Maize straw sample be put into sample analysis disk, will analysis panel surface strike off, in wave number 6061cm-1~
1053cm-1It is interior that near infrared spectrum collection is carried out to maize straw sample.
5. it is according to claim 4 near infrared spectrometer detect maize straw composition method, its feature
It is that the diode array holography fixed grating using Bo Tong companies of Sweden DA7250 near infrared spectrometers connects
Continuous spectroscopy mode carries out near infrared spectrum collection to maize straw sample.
6. it is according to claim 5 near infrared spectrometer detect maize straw composition method, its feature
It is that spectrum collection rate is 100 times/second, wavelength accuracy 2nm~5 when carrying out near infrared spectrum collection
Nm, multiple scanning sample 1 time~2 times.
7. it is according to claim 1 near infrared spectrometer detect maize straw composition method, its feature
It is that the process of setting up of qualitative, quantitative calibrating mathematical model is original to the diffusing reflection of maize straw in step 4
Spectrum carry out that convolution is smooth and standard normalization pretreatment after, recycle PLS and complete intersection test
Card mode set up maize straw holocellulose, cellulose, hemicellulose, lignin, extract, ash content and
The near infrared spectrum linear model of moisture.
8. it is according to claim 7 near infrared spectrometer detect maize straw composition method, its feature
It is to set up fixed using the multivariate data analysis softwares of The Unscrambler 9.8 of CAMO companies of Norway
Property quantitative calibration Mathematical Modeling.
9. it is according to claim 8 near infrared spectrometer detect maize straw composition method, its feature
It is, holocellulose, cellulose, hemicellulose, lignin, extraction in qualitative, quantitative calibrating mathematical model
The coefficient of determination of thing, ash content and moisture is respectively 0.8432,0.8383,0.9026,0.8616,0.9187,
0.9134 and 0.8805；Factor of influence is respectively 7,12,14,3,5,11 and 4；Root-mean-square-deviation
RMSECV is respectively 2.02%, 1.86%, 1.27%, 1.16%, 1.50%, 0.63% and 0.53%.
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| CN112666122A (en) * | 2020-12-30 | 2021-04-16 | 华南理工大学 | Method for rapidly detecting glucose and moisture content after corn straw blasting pretreatment |
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