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Detection method of substitution degree of guar hydroxypropyltrimonium chloride

A technology of guar gum hydroxypropyltrimethylammonium chloride and a detection method, which is applied in the field of analysis and detection, can solve the problems of large test error, poor detection limit, poor repeatability, etc., and achieve small sample size, strong response, good peak effect

Active Publication Date: 2018-06-22
GUANGZHOU TINCI MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

That is, the Kjeldahl method is used to convert all the organic nitrogen into inorganic ammonium salts, and then convert the degree of substitution of the sample according to the ammonia gas decomposed by titration. This method is cumbersome to operate, takes a long time, and has poor repeatability; there are also reports Using an elemental analyzer to measure the nitrogen content to convert the degree of substitution, the detection limit of this method is poor, and the test error of the low degree of substitution is relatively large; in addition, there is also the use of ultraviolet analysis to obtain the degree of substitution, but the ultraviolet method is only applicable to modified groups. Samples with UV absorption
Some of the above methods have large errors, some are cumbersome to operate, and some have strong selectivity. There is no detection method suitable for the degree of substitution of guar gum hydroxypropyltrimethylammonium chloride

Method used

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  • Detection method of substitution degree of guar hydroxypropyltrimonium chloride
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  • Detection method of substitution degree of guar hydroxypropyltrimonium chloride

Examples

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Embodiment 1

[0043] The present embodiment provides a kind of detection method of guar gum hydroxypropyl trimethyl ammonium chloride degree of substitution, comprising the following steps:

[0044] (1) Sample pretreatment:

[0045] Take by weighing 5g guar gum hydroxypropyl trimethyl ammonium chloride sample, place in the ethanol solvent of 300ml, wash in Soxhlet extractor, after drying, get 0.5g drying sample and place 10ml of 1: 20(V 酸 / V 水 ) sulfuric acid solution, and then, the above-mentioned sulfuric acid solution containing the sample was hydrolyzed in a water bath at 80° C. for 1.5 h, and the viscosity was reduced to 31 mpa.s to obtain a sample solution.

[0046] (2) Prepare the solution to be tested:

[0047] Take 0.3g of the reduced-viscosity sample and 0.3ml of deuterated water into a 5mm nuclear magnetic tube, and mix for testing.

[0048] (3) Determination:

[0049] Put the liquid to be tested into the nuclear magnetic resonance instrument for testing, set the carbon spec...

Embodiment 2

[0064] The present embodiment provides a kind of detection method of guar gum hydroxypropyl trimethyl ammonium chloride degree of substitution, comprising the following steps:

[0065] (1) Sample pretreatment:

[0066] Accurately weigh 5g of guar gum hydroxypropyltrimethylammonium chloride sample, place in 300ml of chloroform solvent, wash in a Soxhlet extractor, after drying, take 0.1g of dried sample and place in 10ml of 1 :10(V 酸 / V 水 ) hydrochloric acid solution, and then, the above-mentioned hydrochloric acid solution containing the sample was hydrolyzed in a water bath at 80° C. for 1.5 h, and the viscosity was reduced to 31 mpa.s to obtain a sample solution.

[0067] (2) Prepare the solution to be tested:

[0068] Take 0.3g of the reduced-viscosity sample and 0.3ml of deuterated water into a 5mm nuclear magnetic tube, and mix for testing.

[0069] (3) Determination:

[0070] Put the liquid to be tested into the nuclear magnetic resonance instrument for testing, set...

Embodiment 3

[0072] The present embodiment provides a kind of detection method of guar gum hydroxypropyl trimethyl ammonium chloride degree of substitution, comprising the following steps:

[0073] (1) Sample pretreatment:

[0074] Take by weighing 5g guar gum hydroxypropyl trimethyl ammonium chloride sample, place in the acetone solvent of 300ml, wash in ultrasonic instrument, after drying, get 0.5g oven dry sample and place 1:30 ( V 酸 / V 水 ) trifluoroacetic acid solution, and then, the above-mentioned trifluoroacetic acid solution containing the sample was hydrolyzed in a water bath at 70° C. for 1.5 h, and the viscosity was reduced to 31 mpa.s to obtain a sample solution.

[0075] (2) Prepare the solution to be tested:

[0076] Take 0.3g of the reduced-viscosity sample and 0.3ml of deuterated water into a 5mm nuclear magnetic tube, and mix for testing.

[0077] (3) Determination:

[0078] Put the liquid to be tested into the nuclear magnetic resonance instrument for testing, set th...

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Abstract

The invention relates to a detection method of substitution degree of guar hydroxypropyltrimonium chloride. The method comprises the steps as follows: (1) sample pretreatment: a guar hydroxypropyltrimonium chloride sample is placed in a solvent to be washed and then placed in an acidic reagent for hydrolysis and viscosity reduction, and a sample solution is obtained; (2) the sample solution is mixed with a deuterated reagent, and a to-be-detected solution is obtained; (3) detection: an nuclear magnetic resonance test is conducted on the to-be-detected solution, a carbon spectrogram is obtained, and the substitution degree of guar hydroxypropyltrimonium chloride is calculated according to the carbon spectrogram, wherein the carbon spectrum detection conditions of the nuclear magnetic resonance test are as follows: NS is 20,000, the field width is -20-220 ppm and the pulse sequence is zgig30. The detection method has higher accuracy, better repeatability and higher sensitivity than traditional methods, and interference of nitrogen-containing substances to detection results can be avoided.

Description

technical field [0001] The invention relates to the field of analysis and detection, in particular to a detection method for the degree of substitution of guar gum hydroxypropyltrimethylammonium chloride. Background technique [0002] Guar gum is a natural galactomannan, which can be used as an adhesive, thickener, stabilizer, etc. in food, medicine, water treatment and other fields. However, due to the slow dissolution rate of natural guar gum in water, the high content of insolubles, and the difficulty in controlling the viscosity, it is difficult to meet the requirements of industrial production, and the modification of natural guar gum can greatly improve its processing and application performance. For example: by reacting natural guar gum with dehydrated glycyl ether trimethyl ammonium chloride, guar gum hydroxypropyl trimethyl ammonium chloride can be obtained, which is a kind of cationic guar gum. It can be used as an excellent surfactant to improve the thickening an...

Claims

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Application Information

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IPC IPC(8): G01N24/08
CPCG01N24/08
Inventor 罗海英孙伏恩赵经纬郭娟
Owner GUANGZHOU TINCI MATERIALS TECH
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