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Method for testing substitution degree of sodium carboxymethylcellulose

A sodium carboxymethyl cellulose, weighing technology, applied in the preparation of test samples, thermal excitation analysis, material excitation analysis, etc. Simple, shortened detection time, high accuracy

Inactive Publication Date: 2020-01-17
HUIZHOU LIWINON NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The object of the present invention is: aiming at the deficiencies of the prior art, the present invention solves the cumbersome sample pretreatment process, input error, and test operation that still exist in the prior art by providing a method for testing the degree of substitution of sodium carboxymethyl cellulose. Complexity, large experimental error, low precision, etc., aims to provide a simple sample pretreatment, less sample consumption, high accuracy and efficient test method for the degree of substitution, and provide an excellent technical solution for the degree of substitution test

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  • Method for testing substitution degree of sodium carboxymethylcellulose
  • Method for testing substitution degree of sodium carboxymethylcellulose
  • Method for testing substitution degree of sodium carboxymethylcellulose

Examples

Experimental program
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Embodiment 1

[0039] A method for testing the degree of substitution of sodium carboxymethyl cellulose, comprising the following steps:

[0040] S1, weigh about 0.5g sample on the filter membrane of the suction filtration device; pour absolute ethanol into the funnel for washing, stir the sample evenly and then suction filter, repeat washing three times until the sample does not contain chloride ions. It is desirable to add 1 drop of silver nitrate solution and 1 drop of potassium chromate solution to the filtrate to detect chloride ions. Since the solubility of silver chloride is less than that of silver chromate, potassium chromate is used as an indicator. Chloride ions first react with silver nitrate A white precipitate is formed, and after the chloride ion reaction is completed, silver nitrate reacts with potassium chromate to form a brick red precipitate of silver chromate. That is, if there is a brick red precipitate, it means that there is no chloride ion in the CMC, and the sample h...

Embodiment 2

[0054] The difference from Example 1 is that the samples weighed in step S3 and the digestion time are different.

[0055] S3, Accurately weigh 0.7000g of the dried sample, which must be accurate to 0.0001g, put it into a polytetrafluoroethylene digestion tank, then take 10ml of concentrated nitric acid and add it to the digestion tank, after assembling the digestion tank, put it Put it into the cavity of the microwave digestion instrument, select the microwave digestion program to run, and it will automatically cool down after the digestion program is finished. There is no need to add other operation steps in the middle, the operation is simple, and the digestion duration is about 2.5h. Wherein, the sodium element content C tested by the ICP spectrometer is 2.5mg / L.

[0056] The rest are the same as in Embodiment 1, and will not be repeated here.

Embodiment 3

[0058] The difference from Example 1 is that the samples weighed in step S3 and the digestion time are different.

[0059] S3, accurately weigh 0.0500g of the dried sample, accurate to 0.0001g, put it into the polytetrafluoroethylene digestion tank, then take 10ml of concentrated nitric acid and add it to the digestion tank, after assembling the digestion tank, put it Put it into the cavity of the microwave digestion instrument, select the microwave digestion program to run, and it will automatically cool down after the digestion program is finished. There is no need to add other operation steps in the middle, the operation is simple, and the digestion duration is about 0.8h. Wherein, the sodium element content C tested by the ICP spectrometer is 2.5mg / L.

[0060] The rest are the same as in Embodiment 1, and will not be repeated here.

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Abstract

The invention provides a method for testing substitution degree of sodium carboxymethylcellulose. The method comprises the following steps: S1, weighing a sample, putting the sample into a microwave digestion instrument for digestion, and after digestion is completed, transferring the sample into a volumetric flask for constant volume; S2, starting an ICP emission spectrometer, drawing a standardcurve, starting testing when the instrument is in a normal working state, and recording the content C of Na element; and S3, calculating the substitution degree DS of sodium carboxymethylcellulose according to the Na element content obtained by testing in the step S2, wherein DS is equal to 0.162B / (1-0.08B), and B is equal to (C-C0) * V / (m * MNa). Compared with the prior art, the method has the advantages that the sample is pretreated by adopting the microwave digestion instrument, the number of required samples is small, the sample treatment is simple, the digestion time is short, and the sample treatment time is shortened; and in addition, the content of sodium in CMC is detected by adopting the ICP emission spectrometer, the detected limit can be analyzed to be at the ppb level, and theaccuracy is high.

Description

technical field [0001] The invention relates to the field of testing methods for the degree of substitution, in particular to a method for testing the degree of substitution of sodium carboxymethyl cellulose. Background technique [0002] Carboxymethyl cellulose (CMC) is a derivative with an ether structure obtained by chemically modifying natural cellulose. It is also called sodium carboxymethyl cellulose because it usually exists in the form of sodium salt. It has the functions of thickening, bonding, promoting, emulsifying, slow-release, etc. It has been widely used in various industrial categories such as food, medicine, papermaking, building materials, ceramics, daily chemicals, textile printing and dyeing, oil drilling, new energy, etc. Known as "MSG", it has become one of the most important water-soluble cellulose derivatives. Because of the wide application of CMC, the research on its quality evaluation index is also particularly important. At present, the quality ...

Claims

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Application Information

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IPC IPC(8): G01N21/73G01N1/44G01N1/34
CPCG01N1/34G01N1/44G01N21/73
Inventor 徐梦张旋林嘉惠王怀兴唐荣军陈杰杨山李载波
Owner HUIZHOU LIWINON NEW ENERGY TECH CO LTD
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