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Detection method for phosphate ester content in powdery anti-caking agent

A determination method and technology of anti-caking agent, which are applied in the direction of material analysis by observing the effect of chemical indicators, and analysis by chemical reaction of materials, etc., can solve the problem of affecting the anti-caking agent's effect on fertilizer prevention and analysis results Inaccurate, incomplete powder digestion and other problems, to ensure reliability, improve analysis efficiency, and shorten the time

Active Publication Date: 2012-11-28
HUBEI FORBON NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] As far as the current analysis methods for paste and liquid anti-caking agents are concerned, there are large errors in the incomplete digestion of powders, resulting in inaccurate analysis results and affecting the anti-caking effect of the anti-caking agent on fertilizers.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Weigh 3.3045 grams of powder anti-caking agent whose phosphate ester mass percentage is known and place it in a 250 ml conical flask, add 5 ml of concentrated sulfuric acid with a mass concentration of 98%, and let it stand for about ten minutes. Heat it to be completely digested into black. After the substance is completely cooled, add 10 ml of concentrated nitric acid with a mass concentration of 68%, 4 ml of concentrated sulfuric acid with a mass concentration of 98% and 4 ml of perchloric acid with a mass concentration of 65%. After further heating until the substance in the Erlenmeyer flask has completely turned white, place it to cool, add 50 ml of precipitant and boil and leave to cool. A yellow precipitate appears in the solution. Filter the solution with a suction filter. Take the upper layer of precipitate in a 250 ml beaker. Titrate the precipitate with 0.5mol / L standard sodium hydroxide solution until the yellow color disappears and become colorless...

Embodiment 2

[0015] Example 2: Weigh 4.0768 grams of the powder anticaking agent whose phosphate ester mass percentage is known and place it in a 250 ml conical flask, add 8 ml of concentrated sulfuric acid with a mass concentration of 98%, and let it stand for about ten minutes. Heat it to be completely digested into black. After the substance is completely cooled, add 6 ml of 68% concentrated nitric acid, 4 ml of 98% concentrated sulfuric acid and 2 ml of 65% perchloric acid, and heat it further After the substance in the Erlenmeyer flask is completely white, place it to cool, add 60 ml of precipitant and boil and let it cool. A yellow precipitate appears in the solution. Filter the solution with a suction filter. Take the upper layer of the precipitate in a 250 ml beaker and use 0.5 mol. Titrate the precipitate with a standard sodium hydroxide solution of 1 / L until the yellow color disappears and become colorless. Record the consumption volume of sodium hydroxide as 42.06ml. Add 3 drops o...

Embodiment 3

[0016] Example 3: Weigh 3.5468 grams of powder anti-caking agent whose phosphate ester mass percentage is known, put it in a 250 ml conical flask, add 10 ml of concentrated sulfuric acid with a mass concentration of 98%, and let it stand for about ten minutes Heat it to be completely digested into black. After the substance is completely cooled, add 8 ml of 68% concentrated nitric acid, 4 ml of 98% concentrated sulfuric acid and 3 ml of 65% perchloric acid. Heat until the substance in the Erlenmeyer flask is completely white, then place it to cool, add 70 ml of precipitant and boil and let it cool. A yellow precipitate appears in the solution. Filter the solution with a suction filter. Take the upper layer of precipitate in a 250 ml beaker. Use 0.5 Titrate the precipitate with mol / L standard sodium hydroxide solution until the yellow color disappears and become colorless. Record the consumption volume of sodium hydroxide as 28.17 ml. Add 3 drops of 10g / L phenolphthalein to the a...

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Abstract

The invention relates to a detection method for phosphate ester content in a powdery anti-caking agent. The method comprises the following concrete steps of: weighing m g of the powdery anti-caking agent, and placing the powdery anti-caking agent in a conical flask, adding concentrated sulfuric acid, then standing for 10 minutes, followed by heating until the powdery anti-caking agent is dissolved completely, adding concentrated nitric acid, the concentrated sulfuric acid and perchloric acid after the resulting solution is cooled, then carrying out heating until the solution presents white, followed by standing and cooling, adding a precipitation agent and standing for cooling, filtering the resulting solution through a sucking filtration apparatus, placing upper precipitation in a beaker, titrating the precipitation through a standard sodium hydroxide solution until the color of the precipitation turns from yellow to colorless, recording consumed volume of the sodium hydroxide solution, adding three drops of 10 g / L of phenolphthalein to the resulting solution, carrying out back titration through a standard hydrochloric acid solution until red color of the solution disappears, recording the consumed volume of the hydrochloric acid solution, calculating the phosphate ester content in the powdery anti-caking agent according to the consumed volume of the sodium hydroxide solutionand the consumed volume of the hydrochloric acid solution. The method provided by the present invention is applicable for analysis of the phosphate ester content in various powdery anti-caking agents. In addition, the method has the following characteristics that: color error, calculating error, experiment error and the like are reduced.

Description

Technical field [0001] The invention relates to a method for determining the phosphate content of a powder anticaking agent. Background technique [0002] As the demand for fertilizer anti-caking agents increases, the types of anti-caking agents are gradually increasing. At present, there are mainly three types of anti-caking agents in the form of paste, oil and powder. According to market demand and the improvement of fertilizer production technology, the use of powder anti-caking agents is increasing. However, the optimal powder anti-caking agent dosage for different fertilizers requires certain technical indicators for guidance. Among them, phosphoric acid The ester content is an indispensable indicator. [0003] As for the current analysis methods for paste and liquid anticaking agents, there are large errors due to the incomplete digestion of the powder, which leads to inaccurate analysis results and affects the anticaking effect of the anticaking agent on fertilizers. Summa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/83G01N21/79
Inventor 王仁宗孙金艳
Owner HUBEI FORBON NEW MATERIAL CO LTD
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