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Quick detecting method for guanidine nitrate content

A detection method, the technology of guanidine nitrate, applied in the field of analytical chemistry, can solve the problems of long standing time and unfavorable production process control of the drying method, and achieve the effects of simple operation, shortened test and analysis time, and accurate test results

Active Publication Date: 2013-12-11
NANTONG TENDENCI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is only applicable to the guanidine nitrate produced by the dicyandiamide method, and the guanidine nitrate produced by the urea method is obviously higher by 1% to 1.5%. The method is not conducive to the production process control

Method used

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  • Quick detecting method for guanidine nitrate content
  • Quick detecting method for guanidine nitrate content
  • Quick detecting method for guanidine nitrate content

Examples

Experimental program
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Effect test

Embodiment 2

[0027] 1) Reagent solution and equipment preparation: the reagent is 10% sodium hydroxide solution; picric acid solution 12.0-12.4g / l; the equipment is glass sand core crucible 4 # (5 ~ 15um);

[0028] 2) Sample measurement and analysis: Accurately weigh 2.0g of the sample, dissolve it in a 250ml volumetric flask for dilution, and filter it with filter paper; take 25ml of the filtrate, first add 2ml of liquid caustic soda, then add 60ml of picric acid, and stir slightly; put it in the freezer for refrigeration , 0~-3°C, set aside for 20min; wash the beaker and filter residue 3 times with the original filtrate. Bake at 140°C for 30 minutes in a fast moisture analyzer.

[0029] 3) Result calculation:

[0030] The content of described guanidine nitrate is calculated with following formula:

[0031]

[0032] In the formula, m1——mass of filter residue, g;

[0033] m - the mass of the sample, g;

[0034] 424——The relative molecular weight ratio of guanidine nitr...

Embodiment 3

[0037] 1) Reagent solution and equipment preparation: the reagent is 10% sodium hydroxide solution; picric acid solution 12.0-12.4g / l; the equipment is glass sand core crucible 4 # (5 ~ 15um);

[0038] 2) Sample measurement and analysis: Accurately weigh 2.0g of the sample, dissolve it in a 250ml volumetric flask for dilution, and filter it with filter paper; take 25ml of the filtrate, first add 2ml of liquid caustic soda, then add 70ml of picric acid, and stir slightly; put it in the freezer for refrigeration , 0~-3°C, set aside for 20min; wash the beaker and filter residue 3 times with the original filtrate. Bake at 140°C for 30 minutes in a fast moisture analyzer.

[0039] 3) Result calculation:

[0040] The content of described guanidine nitrate is calculated with following formula:

[0041]

[0042] In the formula, m1——mass of filter residue, g;

[0043] m - the mass of the sample, g;

[0044] 424——The relative molecular weight ratio of guanidine nitr...

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Abstract

The invention discloses a quick detecting method for guanidine nitrate content. The quick detecting method comprises the following steps: (1) preparing a reagent solution and a device; (2) measuring and analyzing a test sample; (3) calculating the result, wherein the detecting and analyzing steps are as follows: precisely weighing the sample, dissolving and diluting, filtering by using filter paper; getting filtrate, firstly adding liquid caustic soda and then adding picric acid and stirring slightly; placing into a refrigerating chamber for refrigeration, precipitating and placing aside; washing a beaker and filter residues by using the original filtrate, and thermally drying with a quick moisture meter. The quick detecting method for the guanidine nitrate content disclosed by the invention is not only suitable for guanidine nitrate produced by a dicyandiamide process, but also suitable for guanidine nitrate produced by a urea process. Moreover, the operation is simple, the test analysis time is shortened and the test result is precise.

Description

technical field [0001] The invention relates to a rapid detection method for guanidine nitrate content, which belongs to the field of analytical chemistry. Background technique [0002] Guanidine nitrate is a pharmaceutical raw material, widely used in the synthesis of sulfa drugs and antibacterial synergist TMP, its molecular formula is [0003] [0004] At present, the determination of guanidine nitrate content adopts the picric acid gravimetric method, which is a method of utilizing ammonia water to adjust the pH value, making guanidine nitrate and picric acid generate guanidine picric acid precipitate, and weighing the precipitate to calculate its content. This method is only applicable to the guanidine nitrate produced by the dicyandiamide method, and the guanidine nitrate produced by the urea method is obviously higher by 1% to 1.5%. The method is not conducive to the production process control. Contents of the invention [0005] In order to solve the above tech...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/04
Inventor 徐平谭建平周喜英奚一平
Owner NANTONG TENDENCI CHEM
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