CN104458611A - Method for determining degree of substitution of water soluble food grade sodium carboxymethylcellulose - Google Patents
Method for determining degree of substitution of water soluble food grade sodium carboxymethylcellulose Download PDFInfo
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Abstract
The invention provides a method for determining degree of substitution of water soluble food grade sodium carboxymethylcellulose. The method comprises the following steps: accurately weighing a sample and dissolving the sample in high purity water, wherein the use ratio of the sample and the high purity water is 1g: (100-500)ml; diluting the obtained uniform solution to a certain concentration in a volumetric flask to obtain a to-be-determined solution; testing the sodium ion concentration of the to-be-determined solution by using a modern tester to obtain the sodium ion percentage composition C of the sample, and calculating the degree of substitution (DS) of the sample according to a formula: DS=162*C/(23-80*C). The method provided by the invention has the characteristics that time is saved, the operation is simple and convenient, the determining range is wide, and the data error is small.
Description
Technical field
The present invention relates to a kind of assay method of degree of substitution, be specifically related to a kind of method measuring water-soluble food level sodium carboxymethylcellulose degree of substitution.
Background technology
Ethyloic sodium carboxymethyl cellulose (CMC) is a kind of important fine chemical product that cellulose and chloroacetic acid etherification reaction occurs in the basic conditions obtain.Standard GB/T 2760-2007 is classified as: can, by the adjuvant list (A3,53) that need of production uses in right amount in varieties of food items, be nutrition, safe, healthy food additives.Use as adjuvant in food, there is the several functions such as thickening, suspension, emulsification, stable, conformal, film forming, expanded, anti-corrosive fresh-keeping, acidproof and health care, simultaneously due to the price of CMC, comparatively the foodstuff glue such as gelatin, agar, sodium alginate is cheap, is therefore widely used in the food such as the beverage of modern food industry, dairy produce, ice cream, soy sauce, jelly, jam, instant noodles.
The technical indicator of CMC mainly contains the viscosity, pH etc. of degree of substitution, purity, water cut and aqueous solution thereof.Wherein degree of substitution is the index of most critical, determines the performance and application scope of CMC.The degree of substitution (DS) of CMC refer to hydrogen on the hydroxyl on each cellulose macromolecule glucose residue ring the average number that replaces by ethyloic.
The assay method of existing CMC degree of substitution (DS) mainly contains ashing method, acid wash, spectrophotometric method, the mantoquita precipitation method, gas-liquid chromatography.
Ash purification determining CMC degree of substitution is: by pure sample, slowly heat, and is warming up to 700 DEG C gradually, calcination 3 h, makes the complete ashing of sample, is converted into Na
2o.Dissolve calcination with quantitative HCl standard solution, then use the hydrochloric acid of standard solution of sodium hydroxide overtitration, methyl red is indicator.Heating rate wants slow, and the time is long, and whether accurately method is classical, be various references of improving one's methods.
Nonaqueous titration determination CMC degree of substitution is: add 50-100 glacial acetic acid doubly at pure sample product, 10-20 times of acetic anhydride, 100 DEG C, 45 minutes, perchloric acid standard solution is used in cooling, and methyl violet is given instruction agent.Need not now.
Acid wash measures CMC degree of substitution: the ethanol adding 3-5 times 95% at the pure sample product of drying, add 1-1.5 times of nitric acid, stir 2 minutes, heating boils 5 minutes, stop heating, stir 10-15 minute, with the alcohol settling of 10-30 times 95%, ethanol washing precipitation with 60 DEG C 80% 4-8 time, until nitrate-free exists.By methanol wash, air-dry except methyl alcohol, 105 DEG C of dryings 3 hours, take 0.5 gram and measure sulfated ash, the repetitive operation when being greater than 0.5%, until ash content is less than 0.5%, is got 1-1.5 gram of sample and is dissolved in standard solution of sodium hydroxide, to give instruction agent with phenolphthalein, use standard salt acidometric titration, calculate degree of substitution DS; The method theoretical end point pH value is about 8. 2, and when adopting phenolphthalein indicator, the variable color that solution becomes colorless from lightpink is sharp not, and titration end-point is not easy to grasp.Improve one's methods: potentiometric titration and infra-red sepectrometry.By potentiometric titration, be indicator electrode with glass electrode, contrast electrode made by mercurous chloride electrode, measured the pH value of solution, second-time derivative determination titration end-point by acidometer, then more accurate than indicator method, can improve precision and the accuracy of experiment; Carry out mensuration DS with infra-red sepectrometry, than titrimetry, there is consumption few (falling 3-5 milligram from 1-1.5 gram), the feature that the time is short.
Spectrophotometry CMC degree of substitution is: at the dense H of 100 DEG C
2sO
4in can release formaldehyde quantitatively, formaldehyde and J acid act ons and generate developing dye, the absorbance obedience lambert-Beer law of its solution.According to the assay method of formaldehyde, use chromotropic acid (4,5-dihydroxy-2,7-naphthalenedisulfonic acid) to replace J acid as developer, measure absorbance at 570 nm wavelength places, same experimental result can be obtained.The determination step of chromotropic acid method is substantially identical with J acid system, and just the heat time reduces to 0. 5 h, and after colour developing, solution is aubergine.The advantage of chromotropic acid method is that comparatively J acid system is stable for the colored dyes formed, and analysis time is shorter.
Mantoquita Precipitation Determination CMC degree of substitution is: in CM C solution, add quantitative CuSO
4solution, reaction generates carboxymethyl cellulose copper precipitation, filters, and removing precipitation, copper EDTA standard solution titration excessive in filtrate, uses the CuSO of EDTA standard solution titration certain volume simultaneously
4solution.By titration CuSO
4the difference of the EDT A volume that solution and filtrate consume, can obtain the copper content reacted with CMS, and then obtain degree of substitution DS.
Gas-liquid chromatography is that CMC first fully reacts, then with NaBH with 1-ethyl-3-(3-dimethylamine propyl)-carbodiimides (EDC)
4be obtained by reacting hydroxyethylation reduzate HCMC, HCMC is in 100 DEG C with formic acid hydrolysis, and residue is dissolved in trifluoroacetic acid, then uses NaBH
4reduction; through acetylation reagent, (acetic anhydride: pyridine=1: the derivant 1) being obtained by reacting serial monose, is dissolved in chloroform reducing solution, uses flame ionization ditector; vapour liquid chromatography is carried out, to determine the degree of substitution DS of CMC with temperature programme.
A kind of method measuring water-soluble food level sodium carboxymethylcellulose degree of substitution of the present invention, have reduce reagent, save time, simple, convenient, the feature that data have preci-sion and accuracy high, stable.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide that a kind of cost is low, efficiency is high, simple, convenient, the method for the mensuration water-soluble food level sodium carboxymethylcellulose degree of substitution that data preci-sion and accuracy is high, stable.
Technical solution of the present invention is as follows.
Measure a method for water-soluble food level sodium carboxymethylcellulose degree of substitution, comprise the steps:
The first step: accurately sample product, is dissolved in high purity water, and the amount ratio of sample and high purity water is 1 gram: 100-500 milliliter, by the homogeneous solution constant volume in volumetric flask obtained, obtains solution to be measured;
Second step: get the solution to be measured that the first step obtains, uses modern testing equipment to test the Na ion concentration of solution to be measured, obtains sample sodion percentage composition C, according to formula:
DS=162* C/(23-80*C) ，
The degree of substitution (DS) of calculation sample.
In said method, described sample is water-soluble food level sodium carboxymethylcellulose, its ashing method degree of substitution: 0.80-1.10, purity is greater than 99.5%, the Testing index of described high purity water reaches or higher than 1 grade of water index in China national lab analysis water supply standard (GB6682-92) " water for analytical laboratory use specification and experimental technique ", and institute's use container is for through cleaned and without the vessel of sodium and potassium stripping.
In said method, second step modern testing equipment is flame atomic absorption spectrophotometer, and the method for the Na ion concentration of test solution is carried out according to GB GB11904.
The present invention compared with prior art tool has the following advantages:
1, sodium carboxymethyl cellulose degree of substitution data preci-sion and accuracy is high, stable;
2, only with high purity water, there is no other reagent, save time, simple, convenient;
3, in the same time, only with high purity water, do not have other reagent, other method completes degree of substitution and measures;
4, plant maintenance and simple, convenient.
Embodiment
Below in conjunction with embodiment, do describe in detail further specific embodiment of the invention, but enforcement of the present invention and protection domain are not limited thereto, if there is the technological parameter do not indicated especially below, those skilled in the art can refer to routine techniques and carry out.
Inventor, to invention has been in depth creative research and test, enumerates five embodiments below.Following instance is raw materials used and testing standard is consistent with foregoing summary.
embodiment 1
The first step accurately takes sodium carboxymethyl cellulose sample (DS:0.80-1.10, purity is greater than 99.5%, food grade products), 1.0000 grams, is dissolved in 450 milliliters of high purity waters, stirring and dissolving, and solution constant volume is in 500 milliliters of volumetric flasks;
The mass percentage content C of the solution sodion that the second step flame atomic absorption spectrophotometer test first step obtains, three times mean value is 8.14%, according to formulae discovery:
DS=162* C/ (23-80*C)=0.80, (standard deviation S is 0.024, variance S
2be 0.0004)
Ashing method records average DS=0.80 simultaneously, and standard deviation S is 0.044, variance S
2be 0.0020.This method and ashing method there was no significant difference.
In the same time, only with high purity water, do not have other reagent, other method completes degree of substitution and measures.
embodiment 2
The first step accurately takes sodium carboxymethyl cellulose sample (DS:0.80-1.10, purity is greater than 99.5%, food grade products), 0.2000 gram, is dissolved in 90 grams of high purity waters, stirring and dissolving, and solution constant volume is in the volumetric flask of 100 milliliters;
The mass percentage content C of the solution sodion that the second step flame atomic absorption spectrophotometer test first step obtains, three times mean value is 10.12%, according to formulae discovery:
DS=162* C/ (23-80*C)=1.10, (standard deviation S is 0.028, variance S
2be 0.0006)
Ashing method records average DS=1. 09 simultaneously, and standard deviation S is 0.046, variance S
2be 0.0028, this method and ashing method there was no significant difference.
In the same time, only with high purity water, do not have other reagent, other method completes degree of substitution and measures.
embodiment 3
The first step accurately takes 0.4500 gram, sodium carboxymethyl cellulose sample (DS:0.80-1.10, purity is greater than 99.5%, food grade products), is dissolved in 90 grams of high purity waters, stirring and dissolving, and solution constant volume is in the volumetric flask of 100 milliliters;
The mass percentage content C of the solution sodion that the second step flame atomic absorption spectrophotometer test first step obtains, three times mean value is 8.57%, according to formulae discovery:
DS=162* C/ (23-80*C)=0.86, (standard deviation S is 0.020, variance S
2be 0.0001)
Ashing method records average DS=0. 85 simultaneously, and standard deviation S is 0.044, variance S
2be 0.0028, this method and ashing method there was no significant difference.
In the same time, only with high purity water, do not have other reagent, other method completes degree of substitution and measures.
embodiment 4
The first step accurately takes 0.3000 gram, sodium carboxymethyl cellulose sample (DS:0.80-1.10, purity is greater than 99.5%, food grade products), is dissolved in 90 grams of high purity waters, stirring and dissolving, and solution constant volume is in the volumetric flask of 100 milliliters;
The mass percentage content C of the solution sodion that the second step flame atomic absorption spectrophotometer test first step obtains, three times mean value is 8.85%, according to formulae discovery:
DS=162* C/ (23-80*C)=0.90, (standard deviation S is 0.028, variance S
2be 0.0006)
Ashing method records average DS=0. 90 simultaneously, and standard deviation S is 0.066, variance S
2be 0.0038, this method and ashing method there was no significant difference.
In the same time, only with high purity water, do not have other reagent, other method completes degree of substitution and measures.
embodiment 5
The first step accurately takes sodium carboxymethyl cellulose sample (DS:0.80-1.10, purity is greater than 99.5%, food grade products), 0.4000 gram, is dissolved in 140 grams of high purity waters, stirring and dissolving, and solution constant volume is in the volumetric flask of 150 milliliters;
The percentage concentration C of the solution sodion that the second step flame atomic absorption spectrophotometer test first step obtains, three times mean value is 8.98%, according to formulae discovery:
DS=162* C/ (23-80*C)=0.92, (standard deviation S is 0.020, variance S
2be 0.0003)
Ashing method records average DS=0. 89 simultaneously, and standard deviation S is 0.064, variance S
2be 0.0032, this method and ashing method there was no significant difference.
In the same time, only with high purity water, do not have other reagent, other method completes degree of substitution and measures.
The above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Exhaustive without the need to also giving all embodiments herein.All any amendments done within the spirit and principles in the present invention, equivalent to replace and improvement etc., within the protection domain that all should be included in the claims in the present invention.
Claims (3)
1. measure a method for water-soluble food level sodium carboxymethylcellulose degree of substitution, it is characterized in that, comprise the steps:
The first step: accurately sample product, is dissolved in high purity water, and the amount ratio of sample and high purity water is 1 gram: 100-500 milliliter, by the homogeneous solution constant volume in a reservoir obtained, obtains solution to be measured;
Second step: get the solution to be measured that the first step obtains, uses modern testing equipment to test the Na ion concentration of solution to be measured, obtains sample sodion mass percentage content C, according to formula:
DS=162* C/(23-80*C)，
The degree of substitution DS of calculation sample.
2. method according to claim 1, it is characterized in that, described sample is water-soluble food level sodium carboxymethylcellulose, its ashing method degree of substitution: 0.80-1.10, purity is greater than 99.5%, the Testing index of described high purity water reaches or higher than 1 grade of water index in China national lab analysis water supply standard (GB6682-92) " water for analytical laboratory use specification and experimental technique ", and institute's use container is for through cleaned and without the vessel of sodium and potassium stripping.
3. method according to claim 1 and 2, is characterized in that, second step modern testing equipment is flame atomic absorption spectrophotometer, and the method for the Na ion concentration of test solution is carried out according to GB GB11904.
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Cited By (7)
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|---|---|---|---|---|
| CN105136710A (en) * | 2015-09-11 | 2015-12-09 | 青岛科技大学 | Determination method of hydroxypropyl chitosan substitution degree |
| CN105203493A (en) * | 2015-09-11 | 2015-12-30 | 青岛科技大学 | Method for determining substitution degree of hydroxypropyl chitosan |
| CN105277507A (en) * | 2015-09-11 | 2016-01-27 | 青岛科技大学 | Hydroxypropyl chitosan substitution degree determination method |
| CN105300916A (en) * | 2015-09-11 | 2016-02-03 | 青岛科技大学 | Determination method of hydroxypropyl chitosan substitution degree |
| CN107543895A (en) * | 2017-08-31 | 2018-01-05 | 泸州北方化学工业有限公司 | The analysis method of carboxymethyl cellulose ammonium substitution value |
| CN108593573A (en) * | 2018-04-03 | 2018-09-28 | 泸州北方化学工业有限公司 | A method of measuring the lithium content and degree of substitution of carboxymethyl cellulose lithium |
| CN108776111A (en) * | 2018-04-24 | 2018-11-09 | 合肥国轩高科动力能源有限公司 | A kind of test method of lithium ion battery sodium carboxymethylcellulose degree of substitution |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105136710A (en) * | 2015-09-11 | 2015-12-09 | 青岛科技大学 | Determination method of hydroxypropyl chitosan substitution degree |
| CN105203493A (en) * | 2015-09-11 | 2015-12-30 | 青岛科技大学 | Method for determining substitution degree of hydroxypropyl chitosan |
| CN105277507A (en) * | 2015-09-11 | 2016-01-27 | 青岛科技大学 | Hydroxypropyl chitosan substitution degree determination method |
| CN105300916A (en) * | 2015-09-11 | 2016-02-03 | 青岛科技大学 | Determination method of hydroxypropyl chitosan substitution degree |
| CN105300916B (en) * | 2015-09-11 | 2021-07-09 | 青岛科技大学 | Method for measuring substitution degree of hydroxypropyl chitosan |
| CN105203493B (en) * | 2015-09-11 | 2021-07-09 | 青岛科技大学 | Method for measuring substitution degree of hydroxypropyl chitosan |
| CN105277507B (en) * | 2015-09-11 | 2021-07-09 | 青岛科技大学 | Method for measuring substitution degree of hydroxypropyl chitosan |
| CN107543895A (en) * | 2017-08-31 | 2018-01-05 | 泸州北方化学工业有限公司 | The analysis method of carboxymethyl cellulose ammonium substitution value |
| CN108593573A (en) * | 2018-04-03 | 2018-09-28 | 泸州北方化学工业有限公司 | A method of measuring the lithium content and degree of substitution of carboxymethyl cellulose lithium |
| CN108776111A (en) * | 2018-04-24 | 2018-11-09 | 合肥国轩高科动力能源有限公司 | A kind of test method of lithium ion battery sodium carboxymethylcellulose degree of substitution |
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Application publication date: 20150325 |