CN101105444A - Detection and analysis method for cotton fiber lignin content - Google Patents
Detection and analysis method for cotton fiber lignin content Download PDFInfo
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- CN101105444A CN101105444A CNA2007101005587A CN200710100558A CN101105444A CN 101105444 A CN101105444 A CN 101105444A CN A2007101005587 A CNA2007101005587 A CN A2007101005587A CN 200710100558 A CN200710100558 A CN 200710100558A CN 101105444 A CN101105444 A CN 101105444A
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Abstract
The invention relates to a detecting and analyzing method for detecting and analyzing the lignin content in cotton fiber. The invention is characterized in that the impurity in the cotton fiber is firstly put away and the soluble substance is washed, and then the cotton fiber is digested and hydrolyzed and the lignin is dissolved, the liquor digested and hydrolyzed is diluted, sodium hydroxide and oxammonium hydrochloride are added to eliminate the background influence the liquor, the constant volume and the stewing are taken, then the absorbance is determined at the place 280nm by an ultraviolet spectrophotometer. The invention has the adventages that (1) a detecting and analyzing method for detecting and analyzing the lignin content in cotton fiber is provided; (2) the lignin which has less content in cotton fiber is provided with a good analyzing method that the analyzing result is correct, the analyzing speed is quick, the operation is simple, the sensitivity is high and the reproduction quality is good. The researcher and the processor are provided with a new appraisal method of cotton fiber structure and the quality formed.
Description
Technical field
The present invention relates to the check and analysis method of content of lignin in a kind of cotton fiber.
Background technology
Lignin is the main composition composition of plant cell wall and forms cross-linked structure with the polysaccharide of cell membrane that its function is to strengthen the brute force and the elasticity of plant cell wall.Ripe cotton fiber is the plant monocyte cell membrane.For a long time, because the restriction that is subjected to analytical technology and continues to use idea, think that the cell membrane of ripe cotton fiber mainly is made of cellulose, and do not contain lignin or lignin and cellulosic composite structure (Basra AS and Malik CP, Development of the cotton fiber.International Review of Cytology, V89:65-113,1984).Seriously hindered understanding, at present the international and domestic method that does not also have content of lignin in a kind of check and analysis cotton fiber to cotton fiber structure and quality formation.Therefore, need a kind of method correct, that be fit to and detect content of lignin in the cotton fiber.
The content of lignin is relatively low in the cotton fiber, and it is difficult finding suitable analytical approach.The analytical approach of existing content of lignin is mainly used in the analysis of woody or herbaceous plant stem, leaf material, and its content of lignin is higher, is not suitable for being directly used in the analysis of content of lignin in the cotton fiber.
Summary of the invention
The purpose of this invention is to provide a kind of check and analysis method that is suitable for content of lignin in the cotton fiber.Help cotton researcher and processer understanding to cotton fiber structure and quality formation.The present invention is to provide acidifying acetyl bromide method, its principle is: under the condition that glacial acetic acid and heating are arranged, bromine has replaced in the lignin hydroxyl of α-C to be made lignin form acetyl derivative to be dissolved in the acetate, can to realize measuring the absorbance analysis.
Before analyzing the cotton sample, need choose the blade of sneaking in the cotton fiber earlier and plant impurity such as shell fragment, clean cotton fiber.Centrifugation method reject cleaning liquid is all adopted in the cleaning of general plant sample, can not realize because the cotton fiber hydroscopicity is strong, so extrude liquid residual in the cotton fiber with metal clip garlic device.
Experiment showed, that classical Klason method is not suitable for the check and analysis of the low material of content of lignin; The mercaptoacetic acid method detects confirmation through residue can not be complete with the lignin extraction in the cotton fiber, and testing process is long, expense is higher.After the analysis relatively to detection method, first-selected acidifying acetyl bromide method.
What the first step of realization acidifying acetyl bromide method need solve is the temperature and time of reagent dosage, reaction, and whether this is related to can make lignin dissolution by catapepsis hydrolysis cotton fiber.Having compared 2,3,4, behind the reagent dosage of 5ml, having determined to handle the 0.1g cotton fiber, has a reappearance preferably with the acidifying acetyl bromide of 5ml.Comparing in 30min to 5h, behind 50 ℃, 60 ℃, 70 ℃ the bath temperature, determining to be used under 1 hour 45 minutes conditions of 70 ℃ of water-baths, can 0.1g cotton sample digestion hydrolysis is complete with the acidifying acetyl bromide solution of 5ml, also being unlikely to excessively, digestion reddens solution.
Cotton fiber is difficult to grind to form powdery, and the time of catapepsis hydrolysis cotton fiber is long than other sample, and sample room is also slightly variant, in case the digestion excessive hydrolysis, digestive juice can present red interference detection results.In addition, the bromine in the solution and many bromines also can interference detection results, therefore, eliminate the influence of solution background, and it is extremely important correctly to present the result.NaOH and oxammonium hydrochloride can be eliminated the influence of these two kinds of backgrounds.In order to determine the correct NaOH and the reagent dosage of oxammonium hydrochloride, we have carried out two kinds of reagent, 24 groups of different proportioning tests, i.e. 4M NaOH 1.0,2.0,2.5,3.0,3.5,4.0,4.5,8 gradients of 5.0ml and 5M oxammonium hydrochloride 1.0,1.5, three gradients of 2.0ml.After the digestion hydrolyzate ice-water bath cooling with 25 identical cotton samples of 0.100g, whole digestive juices are concentrated mixing, distinguish packing 5ml then in 24 volumetric flasks, add the 10ml glacial acetic acid, press treatment combination then respectively and add NaOH and oxammonium hydrochloride, constant volume, leave standstill, measure absorbance.Repeatedly repeated experiments proof 4M NaOH 4.5ml and 5M oxammonium hydrochloride 1.5ml are the best treatment combination of eliminating the solution background with different cotton fiber samples.Its reason is: (1) can obtain the solution with the same colour system of standard solution; (2) content difference of sample room can show; (3) in the test of the time under the fixed temperature condition, in the best digestion hydrolysis time ± 15min, all can obtain very close absorbance, for example: absorbance=0.7247 ± 0.01709.
The preparation of general alkali lignin standard solution and blank basic background solution is to use glacial acetic acid, makes the basic background of standard solution and the basic background of actual detected solution differ bigger, and the content of lignin that records is higher.The content of cellulose of cotton fiber is more than 90%, and experimental study confirms can form higher background value after the cotton fiber digestion hydrolysis.The invention reside in and not only contain in blank basic background solution and the alkali lignin series standard solution and detect the identical reagent treatment of solution, and contain the pure cellulose that digests hydrolysis, making blank base soln, alkali lignin series standard solution and detecting solution has identical background.Owing to defined suitable blank base soln, both effectively eliminated systematic error like this, and also eliminated effectively and digested cellulolytic influence in the cotton sample.What deserves to be explained is: the typical curve that (1) is obtained in this way meets Beer-Lambert law, and promptly chromophoric beam absorption degree is linear change along with the variation of chromophore concentration in transparent solvent, related coefficient 〉=0.995, favorable reproducibility (Fig. 1); (2) be that the corresponding alkali lignin solution of basic background scans can obtain extremely similar absorbance scanning curve with containing or do not contain cellulosic blank solution; (3) the cotton fiber sample also can obtain the absorbance scanning curve (Fig. 2) similar to the alkali lignin standard solution, is similar at 280 ± 10nm place particularly.
The present invention has been for the relatively low lignin of content in the cotton fiber provides that a kind of analysis result is correct, analysis speed is fast, the analytical approach of simple to operate, highly sensitive, favorable reproducibility, the method that provides a kind of new evaluation cotton fiber structure and quality to form for cotton researcher and processer.
Description of drawings
Fig. 1: the typical curve of alkali lignin
Fig. 2: the absorbance scanning curve of standard solution of alkali lignin (50 μ g/ml) and cotton fiber sample solution.
Embodiment
1. instrument and reagent
GBC Cintra 20 ultraviolets/visible spectrophotometer (Australia), DKZ-2 type electric heating constant temperature concussion tank (it is grand to go up the Nereid), EYELA NDO-700 constant temperature thermostatic drying chamber (Shanghai).
Tris-HCl (Beijing is glad through section); Triton x-100 is analyzed pure (Beijing is glad through section); NaCl is for analyzing pure (Xi'an chemical reagent factory); Acetone pure for analyzing (the many chemical reagent of Zhengzhou City's moral factory); NaOH is for analyzing pure (Xi'an chemical reagent factory); Oxammonium hydrochloride is for analyzing pure (Shishewei Chemical Co., Ltd., Shanghai); Acetyl bromide (Sigma-Aldrich), alkali lignin (Sigma-Aldrich), pure cellulose (Sigma-Aldrich).
Even matter damping fluid (50mM Tris-HCl, 1% (v/v) triton x-100,1M sodium chloride, pH8.3).
Acidifying acetyl bromide (acetyl bromide: glacial acetic acid=1: 3 (v/v)).
2. the preparation of cotton sample
Choose the blade of sneaking into non-cotton fiber impurity in the cotton fiber earlier and plant shell fragment impurity, take by weighing the 1.0g cotton sample, with homogenization buffer solution for cleaning cotton fiber twice, clean once to avoid the interference of soluble substance with twice of 80% acetone cleaning and pure acetone respectively again analyzing.Clean all vortex, extruding repeatedly at every turn, cotton fiber be placed in the metal clip garlic device and extrude residual liquid, 45 ℃ of dry for standby at last.
3. the drafting of typical curve
With acidifying acetyl bromide solution preparation alkali lignin content is the storage liquid of 2.5mg/ml.
Make digestion hydrolysis bottle with serum vial with teflon seal closure, take by weighing the 0.090g cellulose in every bottle, in every bottle, add 0,0.2,0.3,0.4,0.5 respectively, the alkali lignin storage liquid of 0.6ml, in every bottle, add 5,4.8,4.7,4.6,4.5 then respectively, the acidifying acetyl bromide of 4.4ml, the acidifying acetyl bromide that 5ml is finally all arranged in making every bottle, and the content difference of lignin.Water-bath is until the pure cellulose catapepsis under 70 ℃ condition.After the ice-water bath cooling, solution is changed in the 25ml volumetric flask, add 10ml glacial acetic acid, 4N NaOH 4.5ml, 5M oxammonium hydrochloride 1.5ml, mixing behind each liquid feeding.Be settled to 25ml with glacial acetic acid at last, form and to contain that the lignin concentration of digest cellulose, identical background is the series standard liquid of 0,20,30,40,50,60 μ g/ml, leave standstill 30min.With the solution that does not contain lignin is the blank background basis, measures absorbance at the 280nm place with ultraviolet spectrophotometer, obtains the linear relationship between absorbance and the solution content of lignin, related coefficient=0.9996 (Fig. 1).
4. the analysis of sample
The cotton fiber sample that takes by weighing the abundant mixing that 0.100g cleaned places the serum bottle with teflon seal closure, adds 5ml acidifying acetyl bromide, with bottle cap screwing.Place preset temperature in 70 ℃ and slight vibration (about 60 times/min) electric heating constant temperature shaking bath groove tepidarium 1 hour 45 minutes, ice-water bath cessation reaction immediately.Solution is changed in the 25ml volumetric flask, add 10ml glacial acetic acid, 4N NaOH 4.5ml, 5M oxammonium hydrochloride 1.5ml, mixing behind each liquid feeding.Be settled to 25ml with glacial acetic acid.Leave standstill 30min.Based on aforementioned blank background solution, measure absorbance at the 280nm place with ultraviolet spectrophotometer.Table 1 is a cotton fiber sample detection example as a result, totally two samples, and every sample repeats 5 times.
The calculating of content of lignin:
(1) calculates the concentration of solution according to typical curve and absorbance
The concentration of solution (μ g/ml)=55.422 * absorbance-4.4993
(2) according to the concentration of solution, the volume and the example weight calculated weight degree of sample constant volume
Weight percent content=((volume of solution concentration * sample constant volume)/example weight) * 100%
Table 1. cotton fiber sample content of lignin testing result example
| Sample sequence number | Light absorption value | Weight percent content |
| 1-1 1-2 1-3 1-4 1-5 | 0.4423 0.4503 0.4571 0.4741 0.4629 | 0.5003 0.5114 0.5209 0.5444 0.5289 |
| 2-1 2-2 2-3 2-4 2-5 | 0.6297 0.6299 0.6392 0.6355 0.6210 | 0.7610 0.7603 0.7732 0.7680 0.7480 |
Claims (6)
1. the present invention relates to the check and analysis method of content of lignin in a kind of cotton fiber.It is characterized in that at first the impurity picking with cotton fiber is clean, clean soluble substance.Digest hydrolysis cotton fiber dissolved lignin then, the solution dilution with after the digestion hydrolysis adds the influence that NaOH and oxammonium hydrochloride are eliminated the solution background, and constant volume leaves standstill, and measures absorbance at the 280nm place with ultraviolet spectrophotometer.
2. the check and analysis method of content of lignin in a kind of cotton fiber according to claim 1.It is characterized in that at first cleaning cotton fiber, pure cotton fiber with even matter buffer solution for cleaning twice, is cleaned once to avoid the interference of soluble substance to analyzing with twice of 80% acetone cleaning and 100% acetone respectively again.Clean all vortex, extruding repeatedly at every turn, cotton fiber be placed in the metal clip garlic device and extrude residual liquid, 45 ℃ of dry for standby at last.
3. the check and analysis method of content of lignin in a kind of cotton fiber according to claim 1.It is characterized in that need be with the digestion of the cotton fiber after cleaning hydrolysis with the lignin in the dissolving cotton fiber.The method of digestion hydrolysis cotton fiber has sulfuric acid process (Klason method), acidifying acetyl bromide method, mercaptoacetic acid method etc., first-selected acidifying acetyl bromide method.
4. the check and analysis method of content of lignin in a kind of cotton fiber according to claim 1.When it is characterized in that with acidifying acetyl bromide digestion hydrolysis cotton fiber, the optimum reagent consumption is that 5ml, best bath temperature are that 70 ℃, best digestion hydrolysis time are 1 hour 45 minutes.
5. the check and analysis method of content of lignin in a kind of cotton fiber according to claim 1.It is characterized in that the solution dilution after the digestion hydrolysis is added 4M NaOH 4.5ml and 5M oxammonium hydrochloride 1.5ml and can remove the interference of solution background to the lignin absorbance.
6. contain the pure cellulose that has digested in the blank base soln that is provided with when measuring absorbance with ultraviolet spectrophotometer, also contain the pure cellulose that has digested in the series standard solution, make blank base soln with test sample solution identical background be arranged with series standard solution.Can eliminate and digest the influence of hydrocellulose in the cotton fiber sample solution to be detected testing result.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101799389A (en) * | 2010-03-03 | 2010-08-11 | 新疆农业科学院核技术生物技术研究所 | Method for determining correlationship of lignin content and fiber quality in cotton fiber |
| CN101957315A (en) * | 2010-09-11 | 2011-01-26 | 大连工业大学 | Method for measuring lignin content in black liquor |
| CN103335974A (en) * | 2013-06-08 | 2013-10-02 | 广东中烟工业有限责任公司 | Measuring method of content of lignin in tobacco |
| CN103364516A (en) * | 2013-06-28 | 2013-10-23 | 新疆农业科学院核技术生物技术研究所 | Detection method of phenylpropane structure monomer contained in cotton fiber |
| CN104089912A (en) * | 2014-06-30 | 2014-10-08 | 浙江天能电池(江苏)有限公司 | Method for determining dissolved quantity of lignin |
| CN104655580A (en) * | 2015-02-10 | 2015-05-27 | 华南理工大学 | Method for quickly determining content of alpha-cellulose in dissolving pulp |
| CN104819948A (en) * | 2015-05-19 | 2015-08-05 | 山东大学 | Method for measuring content of dissoluble lignin by utilizing Coomassie brilliant blue G-250 |
| CN104849166A (en) * | 2015-05-26 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Method for detecting content of alpha cellulose in alkali cellulose |
| CN105717073A (en) * | 2015-09-30 | 2016-06-29 | 广东工业大学 | Cotton fiber maturity measuring method based on densitometry |
| CN103868778B (en) * | 2014-04-02 | 2016-07-06 | 兰州大学 | The measuring method of herbaceous plant content of lignin |
| CN108872118A (en) * | 2017-10-13 | 2018-11-23 | 济宁明升新材料有限公司 | A kind of detection method of papermaking pre-cooked liquid content of lignin |
| CN108872119A (en) * | 2017-10-13 | 2018-11-23 | 济宁明升新材料有限公司 | The detection method of Lignin in Wastewater from Paper-Making Mill content |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| FI69132C (en) * | 1982-10-19 | 1985-12-10 | Advanced Forest Automation Ab | PROCESSING OF SULFIT CELLULOSE CONCRETE PROCESSES |
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2007
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| CN101799389A (en) * | 2010-03-03 | 2010-08-11 | 新疆农业科学院核技术生物技术研究所 | Method for determining correlationship of lignin content and fiber quality in cotton fiber |
| CN101957315A (en) * | 2010-09-11 | 2011-01-26 | 大连工业大学 | Method for measuring lignin content in black liquor |
| CN101957315B (en) * | 2010-09-11 | 2012-02-15 | 大连工业大学 | Method for measuring lignin content in black liquor |
| CN103335974A (en) * | 2013-06-08 | 2013-10-02 | 广东中烟工业有限责任公司 | Measuring method of content of lignin in tobacco |
| CN103335974B (en) * | 2013-06-08 | 2015-06-03 | 广东中烟工业有限责任公司 | Measuring method of content of lignin in tobacco |
| CN103364516A (en) * | 2013-06-28 | 2013-10-23 | 新疆农业科学院核技术生物技术研究所 | Detection method of phenylpropane structure monomer contained in cotton fiber |
| CN103868778B (en) * | 2014-04-02 | 2016-07-06 | 兰州大学 | The measuring method of herbaceous plant content of lignin |
| CN104089912A (en) * | 2014-06-30 | 2014-10-08 | 浙江天能电池(江苏)有限公司 | Method for determining dissolved quantity of lignin |
| CN104655580A (en) * | 2015-02-10 | 2015-05-27 | 华南理工大学 | Method for quickly determining content of alpha-cellulose in dissolving pulp |
| CN104655580B (en) * | 2015-02-10 | 2017-06-06 | 华南理工大学 | A kind of method of the chemical cellulose content in quick measure dissolving pulp |
| CN104819948A (en) * | 2015-05-19 | 2015-08-05 | 山东大学 | Method for measuring content of dissoluble lignin by utilizing Coomassie brilliant blue G-250 |
| CN104819948B (en) * | 2015-05-19 | 2017-04-26 | 山东大学 | Method for measuring content of dissoluble lignin by utilizing Coomassie brilliant blue G-250 |
| CN104849166A (en) * | 2015-05-26 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Method for detecting content of alpha cellulose in alkali cellulose |
| CN104849166B (en) * | 2015-05-26 | 2018-02-23 | 宜宾丝丽雅集团有限公司 | The detection method of first fibre content in a kind of alkali fibre |
| CN105717073A (en) * | 2015-09-30 | 2016-06-29 | 广东工业大学 | Cotton fiber maturity measuring method based on densitometry |
| CN108872118A (en) * | 2017-10-13 | 2018-11-23 | 济宁明升新材料有限公司 | A kind of detection method of papermaking pre-cooked liquid content of lignin |
| CN108872119A (en) * | 2017-10-13 | 2018-11-23 | 济宁明升新材料有限公司 | The detection method of Lignin in Wastewater from Paper-Making Mill content |
| CN108872118B (en) * | 2017-10-13 | 2021-01-22 | 济宁明升新材料有限公司 | Method for detecting lignin content of papermaking pre-cooking liquid |
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