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A kind of assay method of hydrocyanic acid and chloride ion content in sample

A technology of chloride ion content and determination method, which is applied in the field of determination of hydrocyanic acid and chloride ion content in samples, can solve the problems of low boiling point of hydrogen cyanide, easy volatility, lack of in-depth research, and difficulty in content determination, and achieve rapid Measured effect

Inactive Publication Date: 2016-01-20
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above analysis methods are all aimed at the analysis of the mass fraction of cyanide or chloride ion when they exist alone, but for the system where hydrogen cyanide and chloride ion exist simultaneously, such as using benzoyl chloride and hydrogen cyanide as raw materials to synthesize benzoyl nitrile A certain amount of experimental wastewater produced in the process of the experimental wastewater, hydrogen cyanide and chloride ions exist in the experimental wastewater, the content of the two is more difficult to measure, so far no report
If it is determined by ion chromatography, it needs to be compared and analyzed with cyanide standard substance, and cyanide is mainly hydrocyanic acid, sodium cyanide, potassium cyanide, etc., which are highly toxic and not easy to obtain.
Secondly, ion chromatography is relatively expensive and is not used in general laboratories or production
The above method also has the following problems in analysis: 1) hydrocyanic acid has a low boiling point and is easily volatile, and overcoming this difficulty becomes the key to accurate analysis
2) Under acidic conditions, the method of back titration is used to simultaneously measure hydrogen cyanide and chloride ions. Whether the two are completely determined has not been studied in depth.

Method used

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  • A kind of assay method of hydrocyanic acid and chloride ion content in sample
  • A kind of assay method of hydrocyanic acid and chloride ion content in sample
  • A kind of assay method of hydrocyanic acid and chloride ion content in sample

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Embodiment 1

[0046] A method for measuring hydrocyanic acid and chloride ion content in a sample, wherein, the sample adopts a certain amount of experimental waste water produced in the process of synthesizing benzoyl nitrile with benzoyl chloride and hydrocyanic acid as raw materials, and specifically Follow the steps below to measure:

[0047] (1) Determination of hydrocyanic acid content in the sample

[0048] Add 25mL of sodium hydroxide solution with a concentration of 1mol / L into a 150mL iodine measuring bottle, accurately weigh it, and place it in an ice-water bath to cool for 5 minutes. Put the cork on the bottle, shake it well, let it stand for 2 minutes, weigh until the measured sample amount is 0.5182g, add deionized carbon dioxide-free distilled water to 100mL, then add 10 drops of potassium iodide solution indicator with a concentration of 100g / L, And use 0.1005mol / L silver nitrate standard titration solution to drip until the solution is turbid, record the volume of the cons...

Embodiment 2

[0069] A method for measuring hydrocyanic acid and chloride ion content in a sample, wherein the sample uses benzyl chloride and hydrocyanic acid as raw materials, a certain amount of experimental waste water produced in the process of synthesizing benzyl nitrile, and specifically according to the following steps To measure:

[0070] (1) Determination of hydrocyanic acid content in the sample

[0071] Add 25mL of sodium hydroxide solution with a concentration of 1mol / L into a 150mL iodine measuring bottle, accurately weigh it, and place it in an ice-water bath to cool for 5 minutes. Put the cork on the bottle, shake it well, let it stand for 2 minutes, weigh until the measured sample amount is 0.5324g, add deionized carbon dioxide-free distilled water to 100mL, then add 10 drops of potassium iodide solution indicator with a concentration of 100g / L, And use the silver nitrate standard titration solution of 0.1005mol / L to drop to the solution turbidity, record the volume of the...

Embodiment 3

[0075] A kind of assay method of cyanide and chloride ion content in the sample, wherein, contain hydrocyanic acid and chloride ion simultaneously in the sample, and also contain carboxylate, carbonate, specifically measure according to the following steps:

[0076] (1) Determination of cyanide content in the sample

[0077] Add 25mL of sodium hydroxide solution with a concentration of 1mol / L into a 150mL iodine measuring bottle, accurately weigh it, and place it in an ice-water bath to cool for 5 minutes. Put the cork on the bottle, shake it well, let it stand for 2 minutes, weigh until the measured sample amount is 0.5150g, add deionized distilled water to 100mL, then add 10 drops of potassium iodide solution indicator with a concentration of 100g / L, and use 0.1005 The silver nitrate standard titration solution of mol / L is dripped until the solution is turbid, and the volume of the silver nitrate standard solution consumed is recorded as 1.50mL, and the content of hydrocyani...

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Abstract

The invention relates to a method of detecting hydrocyanic acid and chloride ion content in a sample. According to the sample, industrial wastewater or experimental wastewater containing hydrocyanic acid and chloride ions produced by adopting cyanide to replace of chloride ions of chlorinated organic substances, or a sample containing the hydrocyanic acid, the chloride ions and weak acid affecting the content detection of the hydrocyanic acid and the chloride ions rarely is adopted, the content detection of the hydrocyanic acid is performed firstly, then the content detection of the chloride ions is performed, and accordingly the contents of the cyanide and the chloride ions are detected timely, accurately and rapidly. According to the method, the standard deviation of the hydrocyanic acid ranges from 0.030 to 0.053, the coefficient of variation ranges from 0.73% to 1.40%, and the average recovery rate is 99.89%; the standard deviation of the chloride ions ranges from 0.043 to 0.072, the the coefficient of variation ranges from 0.36% to 0.57%, and the average recovery rate is 99.34%.

Description

technical field [0001] The invention relates to a chemical analysis for simultaneously measuring cyanide and chloride ions in experimental wastewater, in particular to a method for determining the content of hydrocyanic acid and chloride ions in a sample. Background technique [0002] Hydrogen cyanide, also known as hydrogen cyanide, is a colorless, highly toxic, low-boiling, volatile gas with a bitter almond smell. Hydrogen cyanide is often used in electroplating and mining industries, and is also an important raw material for the synthesis of intermediates such as pharmaceuticals, pesticides, and dyes. Common analytical methods for hydrocyanic acid include spectrophotometry, silver nitrate complexometric titration, and ion chromatography. Chloride ion is the most common type of halide ion. Its analytical methods are widely studied, and there are typical research fields, such as Mohr's method, Volhard's method, and Fayon justice in precipitation titration; potentiometric ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/82G01N21/78
Inventor 何咏梅罗延谷徐洪吴传隆胡欣李文艳
Owner CHONGQING UNISPLENDOUR CHEM
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