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Assay method for hydrocyanic acid content in glycolonitrile product

A technology of hydroxyacetonitrile and hydrocyanic acid, which is applied in chemical analysis by titration, material analysis by observing the influence on chemical indicators, and analysis by making materials undergo chemical reactions, etc., which can solve problems such as large measurement errors , to achieve the effect of simple operation, short analysis time and fast response

Inactive Publication Date: 2017-03-15
CHONGQING UNISPLENDOUR CHEM
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Problems solved by technology

In the petrochemical industry standard "Method for Determination of Formaldehyde and Hydrocyanic Acid Content in Hydroxyacetonitrile", the Volhard method is used to measure hydrocyanic acid. This method does not interfere with hydroxyacetonitrile, but it needs to accurately add standard solution twice in the operation (back titration method ), for samples with low hydrocyanic acid content, the measurement error is too large

Method used

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  • Assay method for hydrocyanic acid content in glycolonitrile product
  • Assay method for hydrocyanic acid content in glycolonitrile product
  • Assay method for hydrocyanic acid content in glycolonitrile product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1 Actual Sample Measurement

[0023] Weigh 5.1180g of the hydroxyacetonitrile sample numbered 201612029, weigh to an accuracy of 0.0002g, place it in a 100mL measuring bottle, add water to the mark, shake well, and use it as the test solution. Accurately draw 5mL of this solution, put it in a 250mL Erlenmeyer flask, add about 50mL of water, add 10mL of sodium acetate buffer solution (pH=6), shake well; add 3-5 drops of thio-Michler's ketone indicator solution, and Titrate the mercury nitrate standard titration solution until the solution turns from orange yellow to blue, and do a blank test at the same time. Titration sample consumption standard titration solution 2.35mL, blank: 0.00mL.

[0024] The mass fraction w of hydrocyanic acid (HCN) in the sample is calculated according to the following formula:

[0025]

Embodiment 2

[0027] Weigh 5.1380 g of the hydroxyacetonitrile sample numbered 201612033, operate according to the method of Example 1, consume 1.45 mL of the standard titration solution with a concentration of 0.02001 mol / L, and blank: 0.00 mL. Mass fraction of hydrocyanic acid in the sample:

[0028]

Embodiment 3

[0030] Weigh 5.1852 g of the hydroxyacetonitrile sample numbered 201612040, operate according to the method in Example 1, consume 1.75 mL of the standard titration solution with a concentration of 0.02001 mol / L, and blank: 0.00 mL. The mass fraction of hydrocyanic acid in the sample was measured: 0.365%.

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Abstract

The invention provides an assay method for hydrocyanic acid content in a glycolonitrile product. While pH is equal to 6, cyanide (CN-) reacts with mercuric nitrate (Hg(NO3)2) to generate mercury cyanide (HG(CN)2), thiomichler ketone (4,4'-bi(dimethylamino)thiobenzophenone) is used as an indicator, mercuric nitrate standard titration solution is used for titration, and the hydrocyanic acid mass fraction in the glycolonitrile product is measured. The reaction speed is fast, the analysis time is short, and the process is not interfered by the glycolonitrile. The assay method has the characteristics of higher accuracy, simple and rapid operation, and better repeatability, and can be used as the quality control method of the hydrocyanic acid content index in the glycolonitrile product.

Description

technical field [0001] The invention relates to the determination of hydrocyanic acid content, in particular to a method for determining the content of hydrocyanic acid in hydroxyacetonitrile products. Background technique [0002] Hydroxyacetonitrile, also known as glycolonitrile, is a derivative of formaldehyde and the simplest cyanohydrin. It is used in the synthesis of amino acids, glyphosate, indigo dyes and malononitrile, and is also used in the production of chelating agents and flotation Agents, high-efficiency cleaning agents, etc. Hydroxyacetonitrile is unstable to heat and alkali, and is easily decomposed into formaldehyde and hydrocyanic acid. It is reductive and easy to polymerize. At present, it is mainly produced by the reaction of hydrocyanic acid and formaldehyde in China. At the same time, hydroxyacetonitrile is decomposed to produce formaldehyde and hydrocyanic acid, so hydroxyacetonitrile products usually contain impurity hydrocyanic acid. Hydrocyanic a...

Claims

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Application Information

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IPC IPC(8): G01N21/78G01N31/16
CPCG01N21/78G01N31/16
Inventor 罗延谷何咏梅姜曾珍陈依柔刘文枚
Owner CHONGQING UNISPLENDOUR CHEM
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