CN107290244A - A kind of quantitative analysis method of low cellulosic plant chemical composition - Google Patents
A kind of quantitative analysis method of low cellulosic plant chemical composition Download PDFInfo
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Abstract
The invention provides a kind of quantitative analysis method of low cellulosic plant chemical composition, it is characterised in that including:Low cellulosic plant raw material is carried out after wax content measure, pectin content measure, water solubles content measure successively, content of lignin measure is carried out, obtains adipocere matter, pectin, the hydrotrope and content of lignin.The present invention is capable of the chemical composition content of the low cellulosic plant raw material of quantitative test comprehensively, and important evidence is provided for its comprehensive utilization.
Description
Technical field
The present invention relates to a kind of quantitative analysis method of low cellulosic plant chemical composition, belong to textile technology field.
Background technology
With developing rapidly for textile technology, a large amount of plant resourceses are widely used in field of textiles, quantitative determine plant
The chemical composition content of raw material comprehensively utilizes significant to it.The method master of plant material chemical composition content is determined at present
There are " quantitative analysis method of ramie chemical composition ", " Van Soest methods " and " paper making raw material chemical constituents determination standard law ", three
Planting measure analytic approach respectively has feature, while there is also drawback." quantitative analysis method of ramie chemical composition " can more comprehensively
Cellulose, lignin, hemicellulose in quantitative analysis plant material, adipocere matter, the hydrotrope, pectin, the content of ash content, are mesh
Preceding field of textiles determines the standard method of the chemical composition of ramie, flax, hemp, jute etc., but for low cellulosic plant, such as
Akund, agricultural crop straw, weeds etc., practical measurement find there is larger error, and such as adipocere matter measurement result is unstable,
There is weightening phenomenon, in view of content of cellulose is the content that total fiber mass subtracts other compositions, therefore determine accuracy by shadow
Ring." Van Soest methods " is only capable of the content of quantitative analysis hemicellulose, cellulose, lignin and ash content, and suction filtration occurs
When foam is more, lignin and the problems such as content of ashes less than normal." paper making raw material chemical constituents determination standard law " can determine organic molten
Agent extract, holocellulose, pentosan, sour insoluble lignin, the content of ash content, but can not accurately measure content of cellulose.Cause
This, the present invention is based on " quantitative analysis method of ramie chemical composition ", with reference to " Van Soest methods " and " paper making raw material chemistry
Composition measurement standard law ", proposes a kind of method for quantitatively determining for low cellulosic plant chemical composition, is this kind of plant resources
Comprehensive utilization provide guidance.
The content of the invention
It is an object of the invention to provide a kind of quantitative analysis method of low cellulosic plant chemical composition, can comprehensively, it is accurate
The chemical composition content of the low cellulosic plant raw material of true ground quantitative analysis.
In order to achieve the above object, the invention provides a kind of quantitative analysis method of low cellulosic plant chemical composition,
It is characterised in that it includes:Low cellulosic plant raw material is subjected to wax content measure, pectin content measure, the hydrotrope successively
After assay, content of lignin measure is carried out, adipocere matter, pectin, the hydrotrope and content of lignin is obtained.
Preferably, the quantitative analysis method of described low cellulosic plant chemical composition also includes:Separately take same quality
Low cellulosic plant raw material, is carried out after wax content measure, pectin content measure, water solubles content measure, then carry out successively
Content of cellulose is determined, hemicellulose level is determined and ash content test, obtains containing for cellulose, hemicellulose and ash content
Amount.
Preferably, described wax content is determined and included:Low cellulosic plant raw material is cleaned up, drying to perseverance
Weight, weighs sample, obtains sample and extracts the dry weight G before adipocere matter0, it is put into after sample is wrapped up in extraction equipment for fat, extract solution
For the benzene and alcohol mixeding liquid of volume ratio 2: 0.8-1.2, sample extracts the dry weight before adipocere matter and the ratio of extracting liquid volume is
3-5g:100-200mL, is extracted under 85-90 DEG C of constant temperature, and it is 4~6 times/h to control back-flow velocity, extracts 5-8h, takes out examination
Sample air-dries 24-36h, dries to constant weight, places into and is weighed after cooling down 30-50min in drier, obtains sample and extracts after adipocere matter
Dry weight G1, sample wax content is calculated, calculation formula is as follows:
In formula:W1For sample wax content, %;G0The dry weight before adipocere matter is extracted for sample, unit is g;G1For sample
Dry weight after adipocere matter is extracted, unit is g.
Preferably, described pectin content is determined to determine with water solubles content and included:The sample for having extracted adipocere matter is put
Enter in ammonium oxalate solution, sample extracts the dry weight G before adipocere matter0It is 3-5g with the ratio between ammonium oxalate solution volume:200-400ml,
Ammonium formiate concentration is 3-8g/l, and bath temperature is 85 ± 5 DEG C, extraction time 4-8h;The extraction stoste of gained is taken out, measurement is carried
The volume V of stoste is taken, is diluted with water that (determination of extract solution extension rate is according to being galacturonic acid standard curve according to making
In, corresponding galacturonic acid concentration range is 0~70ug/ml, generally 3-5 times) after, using ultraviolet specrophotometer to carrying
The concentration c of galacturonic acid in liquid is taken to be detected, ultraviolet specrophotometer wavelength is 530nm, calculates the quality of sample pectin
G2, calculation formula is as follows:
In formula:G2For the quality of sample pectin, unit is g;C is galacturonic acid concentration in extract solution, and unit is μ g/
mL;V is extracts stoste cumulative volume, and unit is mL;K is extraction stoste extension rate;
By the mass conversion of the pectin measured into pectin content, calculation formula is as follows:
In formula:W2For pectin content, %;
Sample after being determined through pectin content takes out, and dries to constant weight, is then placed in drier and cools down 30-40min
Weigh afterwards and obtain the sample mass G for having determined adipocere matter, pectin and the hydrotrope4, calculate the gross mass G of pectin and the hydrotrope3, meter
Calculate formula as follows:
G3=G1-G4,
In formula:G1Dry weight after adipocere matter is extracted for sample, unit is g;
Water solubles content is calculated, calculation formula is as follows:
In formula:W3For sample water solubles content, %;G3For the gross mass of pectin in sample and the hydrotrope, unit is g.
Preferably, described content of lignin is determined and included:Taken in the sample for having determined adipocere matter, pectin and the hydrotrope
Mass is G5=0.5-1.5g part is put into the sulfuric acid solution that 20-40ml concentration is 70%-75% as experimental sample
In, 20-36h is soaked at room temperature, then is diluted to 300-400ml and boils 1-1.5h, residue is lignin, takes out drying to perseverance
It is re-weighed again, obtains the quality G of lignin6, content of lignin is calculated, calculation formula is as follows:
In formula:W4For sample content of lignin, %;G6The quality of-lignin, g;G5- determine adipocere matter, pectin and water
The experimental sample quality of molten thing, g.
Preferably, described content of cellulose is determined and included:The sample for having determined adipocere matter, pectin and the hydrotrope is claimed
Weight, obtains having determined the quality G of the sample of adipocere matter, pectin and the hydrotrope7, it is put into the NaOH solution that concentration is 15-25g/l
2-6h is boiled, sample extracts the dry weight G before adipocere matter0Ratio with NaOH solution volume is 3-5g: 100-200mL, takes out and claims
Weight, obtained quality is cellulose lignin quality insoluble with alkali and G9, then by sample be put into concentration be 70-75% sulfuric acid it is molten
12-36h in liquid, sample extracts the dry weight G before adipocere matter0Ratio with NaOH solution volume is 3-5g: 25-35ml, then will
The sulfuric acid solution dilutes 8-12 times, boils 0.5-1.5h, filters, and the quality for weighing remaining residue is the insoluble wooden quality of alkali
Measure G8, sample fiber cellulose content is calculated, calculation formula is as follows:
In formula:W5For sample fiber cellulose content, %;G9For cellulose lignin quality insoluble with alkali and, unit is g;G8For
The insoluble lignin quality of alkali, unit is g.
Include it is highly preferred that described hemicellulose level is determined:
Calculate hemicellulose and alkali soluble content of lignin summation G10, calculation formula is:
G10=G7-G9
In formula, G9For cellulose lignin quality insoluble with alkali and, unit is g;G7To have determined adipocere matter, pectin and water
The quality of the sample of molten thing, unit is g;
Sample hemicellulose level is calculated, calculation formula is as follows:
In formula:W6For sample hemicellulose level, %;G10For hemicellulose and alkali soluble content of lignin summation, g, W4For
Sample content of lignin, %.
Preferably, described ash content test includes:The undressed original samples of 1g are taken to be put into ceramic whiteware crucible,
Dried to constant weight in baking oven, be put into after taking-up in drier and cool down and weigh;Temperature is then placed in up in 575 ± 25 DEG C of Muffle furnace
Calcination, until white or light gray is presented in the ashes of sample, when muffle furnace is reduced to below 250 DEG C, takes out cold by crucible
But 2-3min, is then placed in after cooling down 30-40min in drier and weighs, calculate content of ashes, calculation formula is as follows:
In formula:W7For sample content of ashes, %;G " is the gross dry weight of sample ash content and crucible, and unit is g;G ' is sample
With the gross dry weight of crucible, unit is g;G′0For crucible dry weight, unit is g.
Preferably, the quantitative analysis method of described low cellulosic plant chemical composition also includes:Repeat adipocere matter
Assay, pectin content are determined, water solubles content is determined, content of lignin is determined twice;Take three average values as it is each into
Divide content.
It is highly preferred that the quantitative analysis method of described low cellulosic plant chemical composition also includes:Repeat fiber
Cellulose content measure, hemicellulose level measure and ash content test twice, take three average values as each component content.
Preferably, described low cellulosic plant raw material be akund, rice straw, wheat stalk, bracteal leaf of corn,
At least one of herbaceous plant such as the agricultural waste materials such as cotton stalk skins and sedge.
Preferably, the content of cellulose of described low cellulosic plant raw material is 15.00%-50.00%.
Preferably, described drying is completed in an oven, and drying temperature is 80 DEG C~100 DEG C;Constant weight refer to before and after twice
The difference weighed is in 0.2mg/g.
Preferably, the specific steps of the quantitative analysis method of described low cellulosic plant chemical composition include:
The first step:Wax content is determined:Low cellulosic plant raw material is cleaned up, constant weight is arrived in drying, weighs 3~5g
Sample, obtains sample and extracts the dry weight G before adipocere matter0, it is put into after sample is wrapped up with woven dacron in extraction equipment for fat, extract solution
For the benzene and alcohol mixeding liquid of 150ml volume ratios 2: 1, extracted under 85-90 DEG C of constant temperature, it is 4~6 to control back-flow velocity
Secondary/h, extracts 5h, takes out sample and air-dries 24h, dry to constant weight, places into and weighed after cooling down 30min in drier, obtain sample
Extract dry weight G after adipocere matter1, sample wax content is calculated, calculation formula is as follows:
In formula:W1For sample wax content, %;G0The dry weight before adipocere matter is extracted for sample, unit is g;G1For sample
Dry weight after adipocere matter is extracted, unit is g;
Second step:Pectin content is determined:The sample for having extracted adipocere matter is put into 300ml ammonium oxalate solutions, ammonium oxalate
Concentration is 5g/l, and bath temperature is 85 ± 5 DEG C, extraction time 6h;The extraction stoste of gained is taken out, the body of stoste is extracted in measurement
Product V, after being diluted with water, is detected, ultraviolet spectrometry using ultraviolet specrophotometer to the concentration c of galacturonic acid in extract solution
Spectrometer wavelength is 530nm, calculates the quality G of sample pectin2, calculation formula is as follows:
In formula:G2For the quality of sample pectin, unit is g;C is galacturonic acid concentration in extract solution, and unit is μ g/
mL;V is extracts stoste cumulative volume, and unit is mL;K is extraction stoste extension rate;
By the mass conversion of the pectin measured into pectin content, calculation formula is as follows:
In formula:W2For pectin content, %;
3rd step:Water solubles content is determined:
Sample after being determined through pectin content takes out, and dries to constant weight, is then placed in drier and cools down title after 30min
Restore the sample mass G for having determined adipocere matter, pectin and the hydrotrope4, calculate the gross mass G of pectin and the hydrotrope3, calculate public
Formula is as follows:
G3=G1-G4,
In formula:G1Dry weight after adipocere matter is extracted for sample, unit is g;
Water solubles content is calculated, calculation formula is as follows:
In formula:W3For sample water solubles content, %;G3For the gross mass of pectin in sample and the hydrotrope, unit is g.
4th step:Content of lignin is determined:It is G that quality is taken out in the sample for having determined adipocere matter, pectin and the hydrotrope5
=1g part is put into the sulfuric acid solution that 30ml concentration is 72% as experimental sample, 24h is soaked at room temperature, then dilute
Release to 300ml and boil 1h, residue is lignin, take out drying and be re-weighed to constant weight, obtain the quality G of lignin6, calculate wood
Lignin content, calculation formula is as follows:
In formula:W4For sample content of lignin, %;G6The quality of-lignin, g;G5- determine adipocere matter, pectin and water
The experimental sample quality of molten thing, g;
5th step:Content of cellulose is determined:The low cellulosic plant raw material of phase homogenous quantities is taken, repeats the first step to
Three steps, the sample for having determined adipocere matter, pectin and the hydrotrope of gained is weighed, and obtains having determined adipocere matter, pectin and water-soluble
The quality G of the sample of thing7, it is put into the NaOH solution that 150ml concentration is 20g/l and boils 4h, taking-up is weighed, and obtained quality is
Cellulose lignin quality insoluble with alkali and G9, then it is 24h in 72% sulfuric acid solution that sample is put into 30ml concentration, it is then dilute
Release to 300ml and boil 1h, filter, the quality for weighing remaining residue is the insoluble lignin quality G of alkali8, calculate sample fiber element
Content, calculation formula is as follows:
In formula:W5For sample fiber cellulose content, %;G9For cellulose lignin quality insoluble with alkali and, unit is g;G8For
The insoluble lignin quality of alkali, unit is g;
6th step:Hemicellulose level is determined:
Calculate hemicellulose and alkali soluble content of lignin summation G10, calculation formula is:
G10=G7-G9
In formula, G9For cellulose lignin quality insoluble with alkali and, unit is g;G7To have determined adipocere matter, pectin and water
The quality of the sample of molten thing, unit is g;
Sample hemicellulose level is calculated, calculation formula is as follows:
In formula:W6For sample hemicellulose level, %;G10For hemicellulose and alkali soluble content of lignin summation, g, W4For
Sample content of lignin, %;
7th step:Ash content test:Take the undressed original samples of 1g to be put into ceramic whiteware crucible, be dried in an oven
It is put into after constant weight, taking-up in drier and cools down and weigh;Temperature is then placed in up to calcination in 575 ± 25 DEG C of Muffle furnace, until
White or light gray is presented in the ashes of sample, when muffle furnace is reduced to below 250 DEG C, crucible is taken out into cooling 2min, so
After be put into cool down 30min in drier after weigh, calculate content of ashes, calculation formula is as follows:
In formula:W7For sample content of ashes, %;G " is the gross dry weight of sample ash content and crucible, and unit is g;G ' is sample
With the gross dry weight of crucible, unit is g;G′0For crucible dry weight, unit is g.
8th step:Repeat the step of the first step~the 7th twice, take three average values as each component content.
Preferably, described woven dacron is 200 mesh.
Compared with prior art, the beneficial effects of the invention are as follows:
1st, the present invention can detect adipocere matter, the hydrotrope and pectin, lignin, cellulose, hemicellulose and ash content successively
Content, it is adaptable to the relatively low akund of content of cellulose and herbaceous plant etc., can its chemical composition of quantitative analysis comprehensively
Content, the comprehensive utilization for this kind of plant resources provides guidance.
2nd, the present invention makes detection wax content result accurately steady using the extraction time of adipocere matter, air-dry time is extended
It is fixed;
3rd, the present invention merges the hydrotrope and pectin detecting step, and optimization is adapted to the extraction water of low cellulosic plant raw material
Bath temperature, it is ensured that hemicellulose will not be hydrolyzed in this step, adds the reliability of testing result;
4th, the present invention quantitatively divides in the step of detecting lignin, cellulose, hemicellulose compared to ramie chemical composition
Analysis method, add the sample after being handled through NaOH solution placing into the step for being handled in sulfuric acid solution, it is to avoid ramie
The alkali soluble when influence factor of content of cellulose is calculated in chemical composition quantitative analysis method, and avoiding detection hemicellulose level
The influence of lignin, further improves the degree of accuracy to hemicellulose, content of cellulose measurement.
Embodiment
The invention will be further described with reference to embodiments:The bracteal leaf of corn place of production used in following examples is mountain
Eastern Binzhou;The used rice straw place of production is Shanghai Songjiang;Used benzene is Tianjin Fu Yu Fine Chemical Co., Ltd
Production, is analyzed pure;Used ethanol produces for Laiyang City Kant Chemical Co., Ltd., analyzes pure;Used ammonium oxalate is
Tianjin Bo Di chemical inc is produced, and is analyzed pure;Used sulfuric acid is Laiyang economic and technological development zone fine chemistry industry
Factory produces, and analyzes pure;Used NaOH produces for Laiyang City Kant Chemical Co., Ltd., analyzes pure.
Used electric-heated thermostatic water bath is Beijing's bright Medical Instruments factory production, DZKW-S-6 types forever;Used
Ultraviolet-uisible spectrophotometer be Beijing Puxi General Instrument Co., Ltd production, TU-1810 types;Used water-bath
Oscillator produces for Nantong Hongda Experiment Instruments Co., Ltd., HD500B-16 types;Used adjustable temperature control electric jacket is Shandong
Zhen Cheng Hua Lu electric heating Instrument Ltd. produces, KDM types;Used Muffle furnace is given birth to for Yuyao City Jin electricity finite instruments company
Production.
Dry and complete in an oven in various embodiments of the present invention, drying temperature is 105 DEG C;Constant weight is weighed twice before and after referring to
Difference in 0.2mg/g.
Embodiment 1
A kind of quantitative analysis method of low cellulosic plant chemical composition, is concretely comprised the following steps:
The first step:Wax content is determined.Using bracteal leaf of corn as raw material, clean up, constant weight is arrived in drying, is weighed
2.7048g extracts the dry weight G before adipocere matter as sample, sample0=2.7048g, is cut into about 4mm × 4mm fragment, uses
It is put into after the wrapping of 200 mesh woven dacrons in extraction equipment for fat, extract solution is the benzene and alcohol mixeding liquid of 150ml volume ratios 2: 1,85
Extracted under DEG C constant temperature, it is 4~6 times/h to control back-flow velocity, extracts 5h, take out sample and air-dry 24h, drying to constant weight, so
It is put into rapidly after cooling down 30min in drier and weighs afterwards, obtains sample and extract dry weight G after adipocere matter1, the matter of sample before and after extracting
Amount difference is wax content, and the electric-heated thermostatic water bath used is Beijing's bright Medical Instruments factory production, DZKW-S-6 forever
Type;
Sample wax content is calculated, calculation formula is as follows:
In formula:W1For sample wax content, %;G0The dry weight before adipocere matter is extracted for sample, is 2.7048g;G1For examination
Sample extracts dry weight after adipocere matter, is 2.6401g.
Second step:Pectin content is determined:The bracteal leaf of corn for having extracted adipocere matter is put into 300ml ammonium oxalate solutions and carried out
Extract, ammonium formiate concentration is 5g/l, bath temperature is 80 DEG C, and extraction time is 6h;Stoste will be extracted to take out, stoste is extracted in measurement
Volume V, after being diluted with water, the concentration c of galacturonic acid in extract solution is detected using ultraviolet specrophotometer, it is purple
Outer spectrophotometer wavelength is 530nm, and the galacturonic acid measured can be converted into pectin content, the UV, visible light light splitting light used
Degree is calculated as Beijing Puxi General Instrument Co., Ltd's production, and TU-1810 types, water bath chader is the grand laboratory apparatus in Nantong
Co., Ltd produces, HD500B-16 types, and frequency is 150 times/min;
The quality of sample pectin is calculated, calculation formula is as follows:
In formula:G2It is 0.0527g for the quality of sample pectin;C is galacturonic acid concentration, is 42.78 μ g/mL;V is
Stoste cumulative volume is extracted, is 300ml;K is extract solution extension rate, and the present embodiment is 3 times;
By the mass conversion of the pectin measured into pectin content, calculation formula is as follows:
In formula:W2For pectin content, %.
3rd step:Water solubles content is determined:Sample after being determined through pectin content takes out, drying to constant weight, Ran Houxun
Speed, which is put into drier to cool down to weigh after 30min, obtains the sample mass G for having determined adipocere matter, pectin and the hydrotrope4, calculate fruit
The gross mass G of glue and the hydrotrope3, calculation formula is as follows:
G3=G1-G4,
In formula:G1Dry weight after adipocere matter is extracted for sample, unit is g;
Water solubles content is calculated, calculation formula is as follows:
In formula:W3For sample water solubles content, %;G3It is 0.1774g for the gross mass of pectin in sample and the hydrotrope.
4th step:Content of lignin is determined:Quality is taken out in the bracteal leaf of corn for having determined adipocere matter, pectin and the hydrotrope
For G5=1g part is put into the sulfuric acid solution that 30ml concentration is 72% as experimental sample, 24h is soaked at room temperature,
300ml is diluted to again and boils 1h, residue is lignin, is taken out drying and is re-weighed to constant weight, obtains the quality G of lignin6, make
Adjustable temperature control electric jacket is the production of Shandong Zhen Cheng Hua Lu electric heating Instrument Ltd., KDM types.Calculate content of lignin, meter
Calculate formula as follows:
In formula:W4For sample content of lignin, %;G6The quality of-lignin, unit is g, is 0.1651g;G5- determined
The experimental sample quality of adipocere matter, pectin and the hydrotrope, unit is g, is 1g.
5th step:Content of cellulose is determined:Take phase homogenous quantities (G0=2.7048g) bracteal leaf of corn, repeat first
Walk to the 3rd step, the sample for having determined adipocere matter, pectin and the hydrotrope of gained is weighed, obtain having determined adipocere matter, pectin
With the quality G of the sample of the hydrotrope7=2.6940g, is put into the NaOH solution that 150ml concentration is 20g/l and boils 4h, take out and claim
Weight, obtained quality is cellulose lignin quality insoluble with alkali and G9, be 1.2314g, then sample be put into 30ml concentration be
24h in 72% sulfuric acid solution, is then diluted with water to 300ml and boils 1h, filtering, weighs the quality of remaining residue for alkali not
Molten lignin quality G8, the adjustable temperature control electric jacket used be Shandong Zhen Cheng Hua Lu electric heating Instrument Ltd. production, KDM types,
Sample fiber cellulose content is calculated, calculation formula is as follows:
In formula:W5For sample fiber cellulose content, %;G9For cellulose lignin quality insoluble with alkali and, be 1.2314g;G8
It is 0.1872g for the insoluble lignin quality of alkali.
6th step:Hemicellulose level is determined:Calculate hemicellulose and alkali soluble content of lignin summation G10, calculation formula
For:
G10=G7-G9
In formula, G9For cellulose lignin quality insoluble with alkali and, unit is g;G7To have determined adipocere matter, pectin and water
The quality of the sample of molten thing, unit is g;
Sample hemicellulose level is calculated, calculation formula is as follows:
In formula:W6For sample hemicellulose level, %;G10For hemicellulose and alkali soluble content of lignin summation, it is
1.3036g, W4For sample content of lignin, %;
7th step:Ash content test:Take the undressed original samples of 1g to be put into ceramic whiteware crucible, be dried in an oven
Constant weight, places into drier and cools down and weigh;Temperature is then placed in up to calcination in 575 ± 25 DEG C of Muffle furnace, until sample
Ashes white or light gray is presented, this process generally lasts for 4h.When muffle furnace is reduced to below 250 DEG C, crucible is taken
Go out and cool down 2min, then be put into rapidly cool down 30min in drier after weigh, used Muffle furnace is the electric instrument of Yuyao City gold
Co., Ltd produces.Content of ashes is calculated, calculation formula is as follows:
In formula:W7For sample content of ashes, %;G " is the gross dry weight of sample ash content and crucible, is 53.9874g;G ' is examination
The gross dry weight of sample and crucible, is 54.8718g;G′0It is 53.9738g for crucible dry weight.
8th step:Repeat the step of the first step~the 7th twice, take three average values as each component content.
The chemical composition content measurement result of bracteal leaf of corn is as follows:
Embodiment 2
A kind of quantitative analysis method of low cellulosic plant chemical composition, is concretely comprised the following steps:
The first step:Wax content is determined:Using rice straw as raw material, clean up, constant weight is arrived in drying, is weighed
4.5670g extracts the dry weight G before adipocere matter as sample, sample0=4.5670g, is shredded, and is put after being wrapped up with 200 mesh woven dacrons
Enter in extraction equipment for fat, extract solution is the benzene and alcohol mixeding liquid of 150ml volume ratios 2: 1, is extracted under 85 DEG C of constant temperature, control
Back-flow velocity processed is 4~6 times/h, extracts 5h, takes out sample and air-dries 24h, dries to constant weight, be then put into rapidly cold in drier
But weighed after 30min, obtain sample and extract dry weight G after adipocere matter1, the of poor quality of sample is wax content before and after extracting,
The electric-heated thermostatic water bath used is Beijing's bright Medical Instruments factory production, DZKW-S-6 types forever;
Sample wax content is calculated, calculation formula is as follows:
In formula:W1For sample wax content, %;G0The dry weight before adipocere matter is extracted for sample, is 4.5670g;G1For examination
Sample extracts dry weight after adipocere matter, is 4.4277g.
Second step:Pectin content is determined:The rice straw for having extracted adipocere matter is put into 300ml ammonium oxalate solutions and carried out
Extract, ammonium formiate concentration is 5g/l, bath temperature is 90 DEG C, and extraction time is 6h;The extraction stoste of gained is taken out, measurement is carried
Take the volume V of stoste, after being diluted with water, examined using ultraviolet specrophotometer to the concentration c of galacturonic acid in extract solution
Survey, ultraviolet specrophotometer wavelength is 530nm, the galacturonic acid measured can be converted into pectin content, the UV, visible light used
Spectrophotometric is calculated as Beijing Puxi General Instrument Co., Ltd's production, and TU-1810 types, water bath chader is the grand reality in Nantong
Instrument Ltd.'s production is tested, HD500B-16 types, frequency is 150 times/min;
The quality of sample pectin is calculated, calculation formula is as follows:
In formula:G2It is 0.1251g for the quality of sample pectin;C is galacturonic acid concentration, is 60.89 μ g/mL;V is
Stoste cumulative volume is extracted, is 300ml;K is extract solution extension rate, and the present embodiment is 5 times;
By the mass conversion of the pectin measured into pectin content, calculation formula is as follows:
In formula:W2For pectin content, %.
3rd step:Water solubles content is determined:Sample after being determined through pectin content takes out, drying to constant weight, Ran Houxun
Speed, which is put into drier to cool down to weigh after 30min, obtains the sample mass G for having determined adipocere matter, pectin and the hydrotrope4, calculate fruit
The gross mass G of glue and the hydrotrope3, calculation formula is as follows:
G3=G1-G4,
In formula:G1Dry weight after adipocere matter is extracted for sample, unit is g;
Water solubles content is calculated, calculation formula is as follows:
In formula:W3For sample water solubles content, %;G3It is 0.7298g for the gross mass of pectin in sample and the hydrotrope.
4th step:Content of lignin is determined:Quality is taken out in the rice straw for having determined adipocere matter, pectin and the hydrotrope
For G5=1g part is put into the sulfuric acid solution that 30ml concentration is 72% as experimental sample, 24h is soaked at room temperature,
300ml is diluted to again and boils 1h, residue is lignin, is taken out drying and is re-weighed to constant weight, obtains the quality G of lignin6, make
Adjustable temperature control electric jacket is the production of Shandong Zhen Cheng Hua Lu electric heating Instrument Ltd., KDM types.Calculate content of lignin, meter
Calculate formula as follows:
In formula:W4For sample content of lignin, %;G6The quality of-lignin, unit is 0.3160g, is g;G5- determined
The experimental sample quality of adipocere matter, pectin and the hydrotrope, unit is g, is 1g.
5th step:Content of cellulose is determined:Take phase homogenous quantities (G0=4.5670g) rice straw, repeat first
Walk to the 3rd step, the sample for having determined adipocere matter, pectin and the hydrotrope of gained is weighed, obtain having determined adipocere matter, pectin
With the quality G of the sample of the hydrotrope7=4.5454g, is put into the NaOH solution that 150ml concentration is 20g/l and boils 4h, take out and claim
Weight, obtained quality is cellulose lignin quality insoluble with alkali and G9, be 2.3409g, then sample be put into 30ml concentration be
24h in 72% sulfuric acid solution, is then diluted with water to 300ml and boils 1h, filtering, weighs the quality of remaining residue for alkali not
Molten lignin quality G8, the adjustable temperature control electric jacket used be Shandong Zhen Cheng Hua Lu electric heating Instrument Ltd. production, KDM types,
Sample fiber cellulose content is calculated, calculation formula is as follows:
In formula:W5For sample fiber cellulose content, %;G9For cellulose lignin quality insoluble with alkali and, be 2.3409g;G8
It is 0.6932g for the insoluble lignin quality of alkali.
6th step:Hemicellulose level is determined:
Calculate hemicellulose and alkali soluble content of lignin summation G10, calculation formula is:
G10=G7-G9
In formula, G9For cellulose lignin quality insoluble with alkali and, unit is g;G7To have determined adipocere matter, pectin and water
The quality of the sample of molten thing, unit is g;
Sample hemicellulose level is calculated, calculation formula is as follows:
In formula:W6For sample hemicellulose level, %;G10For hemicellulose and alkali soluble content of lignin summation, it is
1.4123g, W4For sample content of lignin, %;
7th step:Ash content test:Take the undressed original samples of 1g to be put into ceramic whiteware crucible, be dried in an oven
Constant weight, places into drier and cools down and weigh;Temperature is then placed in up to calcination in 575 ± 25 DEG C of Muffle furnace, until sample
Ashes white or light gray is presented, this process generally lasts for 4h.When muffle furnace is reduced to below 250 DEG C, crucible is taken
Go out and cool down 2min, then be put into rapidly cool down 30min in drier after weigh, used Muffle furnace is that the electric instrument of Yuyao City gold has
Limit company produces.Content of ashes is calculated, calculation formula is as follows:
In formula:W7For sample content of ashes, %;G " is the gross dry weight of sample ash content and crucible, is 60.3596g;G ' is examination
The gross dry weight of sample and crucible, is 61.1713g;G′0It is 60.2622g for crucible dry weight.
8th step:Repeat the step of the first step~the 7th twice, take three average values as each component content.
The chemical composition content measurement result of rice straw is as follows:
Above-mentioned used experimental temperature, extraction time parameter, testing process etc. be only presently preferred embodiments of the present invention and
, not for limit the present invention practical range.The equivalence changes that i.e. all contents according to scope of the present invention patent are made
With modification, the technology category of the present invention all should be.
Claims (10)
1. a kind of quantitative analysis method of low cellulosic plant chemical composition, it is characterised in that including:Low cellulosic plant is former
Material is carried out after wax content measure, pectin content measure, water solubles content measure successively, is carried out content of lignin measure, is obtained
To adipocere matter, pectin, the hydrotrope and content of lignin.
2. the quantitative analysis method of low cellulosic plant chemical composition as claimed in claim 1, it is characterised in that described is low
The quantitative analysis method of cellulosic plant chemical composition also includes:The low cellulosic plant raw material of same quality is separately taken, is entered successively
After row wax content measure, pectin content measure, water solubles content are determined, then carry out content of cellulose measure, hemicellulose
Assay and ash content test, obtain the content of cellulose, hemicellulose and ash content.
3. the quantitative analysis method of low cellulosic plant chemical composition as claimed in claim 1 or 2, it is characterised in that described
Wax content determine include:Low cellulosic plant raw material is cleaned up, constant weight is arrived in drying, is weighed sample, is obtained sample
Extract the dry weight G before adipocere matter0, it is put into after sample is wrapped up in extraction equipment for fat, extract solution is the benzene of volume ratio 2: 0.8-1.2
And alcohol mixeding liquid, it is 3-5g: 100-200mL that sample, which extracts the dry weight before adipocere matter and the ratio of extracting liquid volume, in 85-90
Extracted under DEG C constant temperature, it is 4~6 times/h to control back-flow velocity, extracts 5-8h, take out sample and air-dry 24-36h, drying to perseverance
Weight, places into and is weighed after cooling down 30-50min in drier, obtains sample and extracts dry weight G after adipocere matter1, calculate sample adipocere matter
Content, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>1</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
<mo>-</mo>
<msub>
<mi>G</mi>
<mn>1</mn>
</msub>
</mrow>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>1</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W1For sample wax content, %;G0The dry weight before adipocere matter is extracted for sample, unit is g;G1Extracted for sample
Dry weight after adipocere matter, unit is g.
4. the quantitative analysis method of low cellulosic plant chemical composition as claimed in claim 1 or 2, it is characterised in that described
Pectin and water solubles content determine and include:The sample for having extracted adipocere matter is put into ammonium oxalate solution, sample extracts adipocere
Dry weight G before matter0It is 3-5g: 200-400ml with the ratio between ammonium oxalate solution volume, ammonium formiate concentration is 3-8g/l, bath temperature
For 85 ± 5 DEG C, extraction time 4-8h;The extraction stoste of gained is taken out, the volume V of stoste is extracted in measurement, be diluted with water and (extract
The determination of liquid extension rate is according in being the galacturonic acid standard curve according to making, corresponding galacturonic acid concentration range
It is 0~70ug/ml, generally 3-5 times) after, the concentration c of galacturonic acid in extract solution is carried out using ultraviolet specrophotometer
Detection, ultraviolet specrophotometer wavelength is 530nm, calculates the quality G of sample pectin2, calculation formula is as follows:
<mrow>
<msub>
<mi>G</mi>
<mn>2</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<mi>c</mi>
<mo>&times;</mo>
<mi>V</mi>
<mo>&times;</mo>
<mi>K</mi>
</mrow>
<msup>
<mn>10</mn>
<mn>6</mn>
</msup>
</mfrac>
<mo>&times;</mo>
<mn>1.37</mn>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>2</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:G2For the quality of sample pectin, unit is g;C is galacturonic acid concentration in extract solution, and unit is μ g/mL;V is
Stoste cumulative volume is extracted, unit is mL;K is extraction stoste extension rate;
By the mass conversion of the pectin measured into pectin content, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>2</mn>
</msub>
<mo>=</mo>
<mfrac>
<msub>
<mi>G</mi>
<mn>2</mn>
</msub>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>3</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W2For pectin content, %;
Sample after being determined through pectin content takes out, and dries to constant weight, is then placed in drier and cools down title after 30-40min
Restore the sample mass G for having determined adipocere matter, pectin and the hydrotrope4, calculate the gross mass G of pectin and the hydrotrope3, calculate public
Formula is as follows:
G3=G1-G4,
In formula:G1Dry weight after adipocere matter is extracted for sample, unit is g;
Water solubles content is calculated, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>3</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>G</mi>
<mn>3</mn>
</msub>
<mo>-</mo>
<msub>
<mi>G</mi>
<mn>2</mn>
</msub>
</mrow>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>4</mn>
<mo>)</mo>
</mrow>
</mrow>
1
In formula:W3For sample water solubles content, %;G3For the gross mass of pectin in sample and the hydrotrope, unit is g.
5. the quantitative analysis method of low cellulosic plant chemical composition as claimed in claim 1 or 2, it is characterised in that described
Content of lignin determine include:It is G that quality is taken out in the sample for having determined adipocere matter, pectin and the hydrotrope5=0.5-
A 1.5g part is put into the sulfuric acid solution that 20-40ml concentration is 70%-75%, soaked at room temperature as experimental sample
20-36h, then be diluted to 300-400ml and boil 1-1.5h, residue is lignin, takes out drying and is re-weighed to constant weight, obtains wood
The quality G of quality6, content of lignin is calculated, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>4</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<mo>(</mo>
<mn>1</mn>
<mo>-</mo>
<msub>
<mi>W</mi>
<mn>1</mn>
</msub>
<mo>-</mo>
<msub>
<mi>W</mi>
<mn>2</mn>
</msub>
<mo>-</mo>
<msub>
<mi>W</mi>
<mn>3</mn>
</msub>
<mo>)</mo>
<msub>
<mi>G</mi>
<mn>6</mn>
</msub>
</mrow>
<msub>
<mi>G</mi>
<mn>5</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>5</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W4For sample content of lignin, %;G6The quality of-lignin, g;G5- determine adipocere matter, pectin and the hydrotrope
Experimental sample quality, g.
6. the quantitative analysis method of low cellulosic plant chemical composition as claimed in claim 2, it is characterised in that described fibre
Dimension cellulose content, which is determined, to be included:The sample for having determined adipocere matter, pectin and the hydrotrope is weighed, obtains having determined adipocere matter, pectin
With the quality G of the sample of the hydrotrope7, it is put into the NaOH solution that concentration is 15-25g/l and boils 2-6h, sample extracts adipocere matter
Preceding dry weight G0Be 3-5g: 100-200mL with the ratio of NaOH solution volume, taking-up is weighed, obtained quality be cellulose with
The insoluble lignin quality of alkali and G9, then it is 12-36h in 70-75% sulfuric acid solution that sample is put into concentration, sample extracts adipocere
Dry weight G before matter0Ratio with NaOH solution volume is 3-5g: 25-35ml, and the sulfuric acid solution then is diluted into 8-12 times,
0.5-1.5h is boiled, is filtered, the quality for weighing remaining residue is the insoluble lignin quality G of alkali8, calculate sample fiber element and contain
Amount, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>5</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>G</mi>
<mn>9</mn>
</msub>
<mo>-</mo>
<msub>
<mi>G</mi>
<mn>8</mn>
</msub>
</mrow>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>6</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W5For sample fiber cellulose content, %;G9For cellulose lignin quality insoluble with alkali and, unit is g;G8For alkali not
Molten lignin quality, unit is g.
7. the quantitative analysis method of low cellulosic plant chemical composition as claimed in claim 2, it is characterised in that described half
Content of cellulose, which is determined, to be included:
Calculate hemicellulose and alkali soluble content of lignin summation G10, calculation formula is:
G10=G7-G9
In formula, G9For cellulose lignin quality insoluble with alkali and, unit is g;G9To have determined adipocere matter, pectin and the hydrotrope
Sample quality, unit is g;
Sample hemicellulose level is calculated, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>6</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>G</mi>
<mn>10</mn>
</msub>
<mo>-</mo>
<mrow>
<mo>(</mo>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
<mo>&times;</mo>
<msub>
<mi>W</mi>
<mn>4</mn>
</msub>
<mo>-</mo>
<msub>
<mi>G</mi>
<mn>8</mn>
</msub>
<mo>)</mo>
</mrow>
</mrow>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>7</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W6For sample hemicellulose level, %;G10For hemicellulose and alkali soluble content of lignin summation, g, W4For sample wood
Lignin content, %.
8. the quantitative analysis method of low cellulosic plant chemical composition as claimed in claim 2, it is characterised in that described ash
Assay is divided to include:Take the undressed original samples of 1g to be put into ceramic whiteware crucible, dry to constant weight, put after taking-up in an oven
Enter and cool down and weigh in drier;Temperature is then placed in up to calcination in 575 ± 25 DEG C of Muffle furnace, until the ashes of sample are presented
White or light gray, when muffle furnace is reduced to below 250 DEG C, takes out cooling 2-3min by crucible, are then placed in drier
Weighed after middle cooling 30-40min, calculate content of ashes, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>7</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<msup>
<mi>G</mi>
<mrow>
<mo>&prime;</mo>
<mo>&prime;</mo>
</mrow>
</msup>
<mo>-</mo>
<msubsup>
<mi>G</mi>
<mn>0</mn>
<mo>&prime;</mo>
</msubsup>
</mrow>
<mrow>
<msup>
<mi>G</mi>
<mo>&prime;</mo>
</msup>
<mo>-</mo>
<msubsup>
<mi>G</mi>
<mn>0</mn>
<mo>&prime;</mo>
</msubsup>
</mrow>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>8</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W7For sample content of ashes, %;G " is the gross dry weight of sample ash content and crucible, and unit is g;G ' is sample and crucible
Gross dry weight, unit is g;G′0For crucible dry weight, unit is g.
9. the quantitative analysis method of low cellulosic plant chemical composition as claimed in claim 1, it is characterised in that described is low
Cellulosic plant raw material is akund, in rice straw, wheat stalk, bracteal leaf of corn, cotton stalk skins and sedge extremely
Few one kind.
10. the quantitative analysis method of low cellulosic plant chemical composition as claimed in claim 1, it is characterised in that specific step
Suddenly include:
The first step:Wax content is determined:Low cellulosic plant raw material is cleaned up, constant weight is arrived in drying, weigh 3~5g examinations
Sample, obtains sample and extracts the dry weight G before adipocere matter0, it is put into after sample is wrapped up with woven dacron in extraction equipment for fat, extract solution is
The benzene and alcohol mixeding liquid of 150ml volume ratios 2: 1, are extracted under 85-90 DEG C of constant temperature, control back-flow velocity for 4~6 times/
H, extracts 5h, takes out sample and air-dries 24h, dry to constant weight, places into and weighed after cooling down 30min in drier, obtain sample and carry
Take dry weight G after adipocere matter1, sample wax content is calculated, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>1</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
<mo>-</mo>
<msub>
<mi>G</mi>
<mn>1</mn>
</msub>
</mrow>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>1</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W1For sample wax content, %;G0The dry weight before adipocere matter is extracted for sample, unit is g;G1Extracted for sample
Dry weight after adipocere matter, unit is g;
Second step:Pectin content is determined:The sample for having extracted adipocere matter is put into 300ml ammonium oxalate solutions, ammonium formiate concentration
For 5g/l, bath temperature is 85 ± 5 DEG C, extraction time 6h;The extraction stoste of gained is taken out, the volume V of stoste is extracted in measurement,
After being diluted with water, the concentration c of galacturonic acid in extract solution is detected using ultraviolet specrophotometer, uv-spectrophotometric
Meter wavelength is 530nm, calculates the quality G of sample pectin2, calculation formula is as follows:
<mrow>
<msub>
<mi>G</mi>
<mn>2</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<mi>c</mi>
<mo>&times;</mo>
<mi>V</mi>
<mo>&times;</mo>
<mi>K</mi>
</mrow>
<msup>
<mn>10</mn>
<mn>6</mn>
</msup>
</mfrac>
<mo>&times;</mo>
<mn>1.37</mn>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>2</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:G2For the quality of sample pectin, unit is g;C is galacturonic acid concentration in extract solution, and unit is μ g/mL;V is
Stoste cumulative volume is extracted, unit is mL;K is extraction stoste extension rate;
By the mass conversion of the pectin measured into pectin content, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>2</mn>
</msub>
<mo>=</mo>
<mfrac>
<msub>
<mi>G</mi>
<mn>2</mn>
</msub>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>3</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W2For pectin content, %;
3rd step:Water solubles content is determined:Sample after being determined through pectin content takes out, and dries to constant weight, is then placed in dry
Cool down to weigh after 30min in dry device and obtain the sample mass G for having determined adipocere matter, pectin and the hydrotrope4, calculate pectin with it is water-soluble
The gross mass G of thing3, calculation formula is as follows:
G3=G1-G4,
In formula:G1Dry weight after adipocere matter is extracted for sample, unit is g;
Water solubles content is calculated, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>3</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>G</mi>
<mn>3</mn>
</msub>
<mo>-</mo>
<msub>
<mi>G</mi>
<mn>2</mn>
</msub>
</mrow>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>4</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W3For sample water solubles content, %;G3For the gross mass of pectin in sample and the hydrotrope, unit is g.
4th step:Content of lignin is determined:It is G that quality is taken out in the sample for having determined adipocere matter, pectin and the hydrotrope5=1g
A part as experimental sample, be put into the sulfuric acid solution that 30ml concentration is 72%, 24h soaked at room temperature, then be diluted to
300ml boils 1h, and residue is lignin, takes out drying and is re-weighed to constant weight, obtains the quality G of lignin6, calculate lignin
Content, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>4</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<mo>(</mo>
<mn>1</mn>
<mo>-</mo>
<msub>
<mi>W</mi>
<mn>1</mn>
</msub>
<mo>-</mo>
<msub>
<mi>W</mi>
<mn>2</mn>
</msub>
<mo>-</mo>
<msub>
<mi>W</mi>
<mn>3</mn>
</msub>
<mo>)</mo>
<msub>
<mi>G</mi>
<mn>6</mn>
</msub>
</mrow>
<msub>
<mi>G</mi>
<mn>5</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>5</mn>
<mo>)</mo>
</mrow>
</mrow>
3
In formula:W4For sample content of lignin, %;G6The quality of-lignin, g;G5- determine adipocere matter, pectin and the hydrotrope
Experimental sample quality, g;
5th step:Content of cellulose is determined:The low cellulosic plant raw material of phase homogenous quantities is taken, repeats the first step to the 3rd
Step, the sample for having determined adipocere matter, pectin and the hydrotrope of gained is weighed, obtains having determined adipocere matter, pectin and the hydrotrope
Sample quality G7, it is put into the NaOH solution that 150ml concentration is 20g/l and boils 4h, taking-up is weighed, obtained quality is fibre
Dimension element lignin quality insoluble with alkali and G9, then sample is put into 24h in the sulfuric acid solution that 30ml concentration is 72%, then dilute
1h is boiled to 300ml, is filtered, the quality for weighing remaining residue is the insoluble lignin quality G of alkali8, calculate sample fiber element and contain
Amount, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>5</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>G</mi>
<mn>9</mn>
</msub>
<mo>-</mo>
<msub>
<mi>G</mi>
<mn>8</mn>
</msub>
</mrow>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>6</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W5For sample fiber cellulose content, %;G9For cellulose lignin quality insoluble with alkali and, unit is g;G8For alkali not
Molten lignin quality, unit is g;
6th step:Hemicellulose level is determined:
Calculate hemicellulose and alkali soluble content of lignin summation G10, calculation formula is:
G10=G7-G9
In formula, G9For cellulose lignin quality insoluble with alkali and, unit is g;G7To have determined adipocere matter, pectin and the hydrotrope
Sample quality, unit is g;
Sample hemicellulose level is calculated, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>6</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>G</mi>
<mn>10</mn>
</msub>
<mo>-</mo>
<mrow>
<mo>(</mo>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
<mo>&times;</mo>
<msub>
<mi>W</mi>
<mn>4</mn>
</msub>
<mo>-</mo>
<msub>
<mi>G</mi>
<mn>8</mn>
</msub>
<mo>)</mo>
</mrow>
</mrow>
<msub>
<mi>G</mi>
<mn>0</mn>
</msub>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>7</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W6For sample hemicellulose level, %;G10For hemicellulose and alkali soluble content of lignin summation, g, W4For sample wood
Lignin content, %;
7th step:Ash content test:Take the undressed original samples of 1g to be put into ceramic whiteware crucible, perseverance is dried in an oven
Weight, is put into drier after taking-up and cools down and weigh;Temperature is then placed in up to calcination in 575 ± 25 DEG C of Muffle furnace, until examination
White or light gray is presented in the ashes of sample, when muffle furnace is reduced to below 250 DEG C, crucible is taken out into cooling 2min, then
It is put into after cooling down 30min in drier and weighs, calculate content of ashes, calculation formula is as follows:
<mrow>
<msub>
<mi>W</mi>
<mn>7</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<msup>
<mi>G</mi>
<mrow>
<mo>&prime;</mo>
<mo>&prime;</mo>
</mrow>
</msup>
<mo>-</mo>
<msubsup>
<mi>G</mi>
<mn>0</mn>
<mo>&prime;</mo>
</msubsup>
</mrow>
<mrow>
<msup>
<mi>G</mi>
<mo>&prime;</mo>
</msup>
<mo>-</mo>
<msubsup>
<mi>G</mi>
<mn>0</mn>
<mo>&prime;</mo>
</msubsup>
</mrow>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mn>8</mn>
<mo>)</mo>
</mrow>
</mrow>
In formula:W7For sample content of ashes, %;G " is the gross dry weight of sample ash content and crucible, and unit is g;G ' is sample and crucible
Gross dry weight, unit is g;G′0For crucible dry weight, unit is g.
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