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

A measurement method and anti-caking agent technology, which are applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions, can solve the problem of affecting the effect of anti-caking agents on fertilizer anti-caking, powder Eliminate incomplete and inaccurate analysis results, etc., to achieve the effect of ensuring reliability, short time, and improving analysis efficiency

Active Publication Date: 2011-11-16
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] Embodiment 1: take by weighing 3.3045 grams of known powder anticaking agent of its phosphate ester mass percentage content and place in 250 milliliters Erlenmeyer flask, add 5 milliliters of concentrated sulfuric acid that mass concentration is 98%, leave standstill after about ten minutes Heating makes it be digested into black completely, treat that after this material cools down completely, add 10 milliliters of mass concentrations and be 68% concentrated nitric acid, 4 milliliters of mass concentrations be the vitriol oil of 98% and 4 milliliters of mass concentrations be the perchloric acid of 65%, Further heat until the substance in the Erlenmeyer flask turns white completely and place it for cooling, add 50 milliliters of precipitating agent to boil and place it for cooling, a yellow precipitate appears in the solution, filter the solution with a suction filter, take the upper layer and deposit it in a 250 milliliter beaker, use The standard sodium hydroxide solu...

Embodiment 2

[0015] Embodiment 2: Take by weighing 4.0768 grams of powder anti-caking agents whose phosphate ester mass percentages are known and place them in a 250 milliliter conical flask, add 8 milliliters of concentrated sulfuric acid with a mass concentration of 98%, and let stand for about ten minutes Heating makes it completely disintegrated into black, and after the substance is completely cooled, add 6 milliliters of mass concentration as 68% concentrated nitric acid, 4 milliliters of mass concentration as 98% concentrated sulfuric acid and 2 milliliters of mass concentration as 65% perchloric acid, and further heat After the substance in the Erlenmeyer flask turns white completely, place it for cooling, add 60 milliliters of precipitating agent, boil it and place it for cooling, a yellow precipitate appears in the solution, filter the solution with a suction filter, take the upper precipitate in a 250 milliliter beaker, and use 0.5 mol The standard sodium hydroxide solution of / L...

Embodiment 3

[0016] Embodiment 3: take by weighing 3.5468 grams of known powder anticaking agent of its phosphate ester mass percentage content and place in 250 milliliters Erlenmeyer flask, add 10 milliliters of mass concentration and be the concentrated sulfuric acid of 98%, leave standstill after about ten minutes Heating makes it be disintegrated into black completely, treat that adding 8 milliliters of mass concentrations after this material cools completely is that the concentrated nitric acid of 4 milliliters of mass concentrations is the vitriol oil of 98% and 3 milliliters of mass concentrations is the perchloric acid of 65%, further Heat until the substance in the Erlenmeyer flask turns white completely, then place it for cooling, add 70 ml of precipitant, boil it and place it for cooling, a yellow precipitate appears in the solution, filter the solution with a suction filter, take the upper precipitate in a 250 ml beaker, and use 0.5 The standard sodium hydroxide solution of mol / ...

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PUM

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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 solution and 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 measuring the phosphate content of a powder anticaking agent. Background technique [0002] With the increasing demand for fertilizer anti-caking agents, the types of anti-caking agents are also gradually increasing. The currently used anti-caking agents mainly include paste, oil and powder. According to the market demand and the improvement of fertilizer production technology, the use of powder anti-caking agent is increasing, but the optimal amount of powder anti-caking agent for different fertilizers needs certain technical indicators to guide, of which phosphoric acid Ester content is an indispensable indicator. [0003] As far as the current analysis methods for paste and liquid anti-caking agents are concerned, there are large errors due to incomplete digestion of the powder, resulting in inaccurate analysis results and affecting the anti-caking effect of the anti-caking agent on fertilizers. Contents of t...

Claims

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Application Information

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IPC IPC(8): G01N21/83G01N21/79
Inventor 王仁宗孙金艳
Owner HUBEI FORBON NEW MATERIAL CO LTD
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