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Method for auxiliary determination of substitution degree of water-soluble food-grade sodium carboxymethylcellulose by microwaves

A sodium carboxymethyl cellulose, microwave-assisted technology, applied in the field of determination of the degree of substitution of water-soluble food-grade sodium carboxymethyl cellulose, can solve the problems of difficult to grasp the titration end point, the color change is not sensitive enough, etc., to improve the dissolution rate and Dissolution uniformity, shortened test time, and the effect of fewer reagents

Inactive Publication Date: 2015-03-25
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wash with methanol, air-dry to remove methanol, dry at 105°C for 3 hours, weigh 0.5 g to determine the sulfate ash content, repeat the operation until the ash content is less than 0.5% when it is greater than 0.5%, take 1-1.5 g sample and dissolve it in sodium hydroxide standard solution , use phenolphthalein as indicator, titrate with standard hydrochloric acid, and calculate the degree of substitution DS; the theoretical end point pH value of this method is about 8.2. The end is not easy to grasp

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The first step is to accurately weigh 0.5000 grams of sodium carboxymethyl cellulose sample (food grade, the degree of substitution by ashing method is 0.70, and the purity is greater than 99.5%), dissolved in 220 grams of high-purity water, and used in oxygen with a concentration of not less than 30ppm ozone Saturate the solution and microwave for 5 minutes at a power density of 0.1 kW / m 3 , and the solution was adjusted to a volume of 250 ml in a volumetric flask;

[0035] In the second step, the mass percentage content C of sodium ions in the solution obtained in the first step was tested with a flame, atomic absorption, spectrophotometer, and a spectrophotometer. The average value of the three times was 7.39%, which was calculated according to the formula :

[0036] DS=162*C / (23-80*C)=0.70,

[0037] The degree of substitution (DS) of sodium carboxymethyl cellulose was not significantly different from the ashing method. Under the same conditions, the test time can...

Embodiment 2

[0039] The first step is to accurately weigh 0.2000 grams of sodium carboxymethyl cellulose sample (food grade, the degree of substitution by ashing method is 1.10, and the purity is greater than 99.5%), dissolved in 90 grams of high-purity water, and used in oxygen with a concentration of not less than 55ppm ozone Saturate the solution and microwave for 4 minutes at a power density of 0.15 kW / m 3 ; Make up the solution to a 100 ml volumetric flask;

[0040] In the second step, the mass percentage content C of sodium ions in the solution obtained in the first step was tested with a flame, atomic absorption, spectrophotometer, and a spectrophotometer. The average value of the three times was 10.12%, which was calculated according to the formula :

[0041] DS=162*C / (23-80*C)=1.10,

[0042] The degree of substitution (DS) of sodium carboxymethyl cellulose was not significantly different from the ashing method. Likewise, the test time can be shortened by 1 / 3 compared to just usin...

Embodiment 3

[0044] The first step is to accurately weigh 0.4500 grams of sodium carboxymethyl cellulose sample (food grade, the degree of substitution by ashing method is 0.85, and the purity is greater than 99.5%), dissolved in 90 grams of high-purity water, and used in oxygen with a concentration of not less than 40ppm ozone Saturate the solution and microwave for 1 min at a power density of 0.5 kW / m 3 ; Make up the solution to a 100 ml volumetric flask;

[0045] In the second step, the mass percentage content C of sodium ions in the solution obtained in the first step was tested with a flame, atomic absorption, spectrophotometer, and a spectrophotometer. The average value of the three times was 8.57%, which was calculated according to the formula :

[0046] DS=162*C / (23-80*C)=0.86,

[0047] The degree of substitution (DS) of sodium carboxymethyl cellulose was not significantly different from the ashing method. Likewise, the test time can be shortened by 1 / 3 compared to just using mi...

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Abstract

The invention discloses a method for auxiliary determination of the substitution degree of water-soluble food-grade sodium carboxymethylcellulose by microwaves. The method comprises the following steps: weighing a certain amount of sample; saturating high-purity water by ozone gas; dissolving the sample to prepare a solution with the assist of the microwaves; testing the concentration of sodium ions by utilizing a modern determination and test instrument; calculating the substitution degree. According to the method, the substitution degree of the water-soluble food-grade sodium carboxymethylcellulose can be determined. With the assist of the microwaves, the method has the characteristics of time conservation, high simplicity and convenience in operation, wide determination range, and small data error.

Description

technical field [0001] The invention relates to a method for measuring the degree of substitution of water-soluble food-grade sodium carboxymethyl cellulose, in particular to a method for determining the degree of substitution of water-soluble food-grade sodium carboxymethyl cellulose with microwave assistance. Background technique [0002] Sodium carboxymethyl carboxymethyl cellulose (CMC) is an important fine chemical product obtained by the etherification reaction of cellulose and chloroacetic acid under alkaline conditions. The national standard GB2760-2007 lists it as a list of additives that can be used in various foods according to production needs (A3, 53). It is a nutritious, safe and healthy food additive. Used as an additive in food, it has multiple functions such as thickening, suspension, emulsification, stabilization, shape retention, film formation, puffing, antiseptic preservation, acid resistance and health care. Food glue is cheap, so it is widely used in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N1/44
Inventor 叶君熊犍
Owner SOUTH CHINA UNIV OF TECH
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