Method for removing hypochlorite and ferric iron interference in thiocyanate measurement

A technology of thiocyanate and hypochlorite, which is used in the measurement of color/spectral characteristics, material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions, etc., can solve the problem of thiocyanate Solve problems such as inaccurate determination of salt, achieve the effect of shortening the decomposition time and increasing the catalytic efficiency

Pending Publication Date: 2020-12-29
CHANGCHUN GOLD RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The invention provides a method for removing the interference of hypochlorite and ferric iron in the determination of thiocyanate to solve the problem that thiocyanate cannot be accurately measured in water containing hypochlorite and ferric iron

Method used

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  • Method for removing hypochlorite and ferric iron interference in thiocyanate measurement
  • Method for removing hypochlorite and ferric iron interference in thiocyanate measurement
  • Method for removing hypochlorite and ferric iron interference in thiocyanate measurement

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] (1) Take a 50mL sample and place it in a 250mL beaker, and add 1mL of Na to the sample 2 CO 3 solution;

[0052] (2) Add 30% hydrogen peroxide solution dropwise until the solution no longer produces bubbles, and an excess of 0.5 mL;

[0053] (3) Heat 0.4g of manganese dioxide powder and 0.5mL of copper chloride solution, cover with a watch glass, heat on an electric hob at a heating temperature of 150°C, heat for 20 minutes, remove the beaker, and cool slightly;

[0054] (4) Filter the solution into a 250mL beaker, wash the precipitate and the filter paper twice, add hydrochloric acid to adjust the pH value of the solution, and adjust it to neutral;

[0055] (5) After adjusting the pH value, the filtrate is settled in a 200mL volumetric flask;

[0056](6) measure the content of ferric iron in the volumetric flask in step (5), measure according to the mensuration o-phenanthroline spectrophotometry of standard HJ / T 345─2007 water quality iron, measure the content of to...

Embodiment 2

[0071] (1) Take a 50mL sample and put it in a 250mL beaker. The sample is strongly alkaline. Add hydrochloric acid to adjust the pH value to 8-8.5. Add 1mL Na 2 CO 3 solution;

[0072] (2) Add 30% hydrogen peroxide solution dropwise until the solution no longer produces bubbles, and an excess of 0.5 mL;

[0073] (3) Heat 0.4g of manganese dioxide powder and 0.5mL of copper chloride solution, cover with a watch glass, heat on an electric stove, the heating temperature is between 160°C, heat for 20 minutes, remove the beaker, and cool slightly;

[0074] (4) Filter the solution into a 250mL beaker, wash the precipitate and the filter paper twice, add hydrochloric acid to adjust the pH value of the solution, and adjust it to neutral;

[0075] (5) After adjusting the pH value, the filtrate is settled in a 200mL volumetric flask;

[0076] (6) measure the content of ferric iron in the volumetric flask in step (5), measure according to standard HJ / T 345─2007 water quality, the mens...

Embodiment 3

[0091] Proceed as follows:

[0092] (1) Take a 50mL sample and place it in a 250mL beaker. If the sample is weakly acidic, add 1mL Na 2 CO 3 solution;

[0093] (2) Add 30% hydrogen peroxide solution dropwise until the solution no longer produces bubbles, and an excess of 0.5 mL;

[0094] (3) Heat 0.4g of manganese dioxide powder and 0.5mL of copper chloride solution, cover with a watch glass, heat on an electric hob at a heating temperature of 170°C, heat for 20 minutes, remove the beaker, and cool slightly;

[0095] (4) Filter the solution into a 250mL beaker, wash the precipitate and the filter paper twice, add hydrochloric acid to adjust the pH value of the solution, and adjust it to neutral;

[0096] (5) After adjusting the pH value, the filtrate is settled in a 200mL volumetric flask;

[0097] (6) measure the content of ferric iron in the volumetric flask in step (5), measure according to the mensuration o-phenanthroline spectrophotometry of standard HJ / T 345─2007 wat...

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Abstract

The invention relates to a method for removing hypochlorite and ferric iron interference in thiocyanate measurement, and belongs to a method for measuring thiocyanate in water. The method has the following beneficial effects that the reducibility of excessive hydrogen peroxide is utilized to react with pypocholoride in a sample so as to eliminate interference of pypocholoride; excessive hydrogen peroxide reacts with thiocyanate under an acidic condition, so that the excessive hydrogen peroxide needs to be eliminated, hydrogen peroxide does not react with thiocyanic acid under an alkaline condition, under the catalytic action of manganese dioxide, hydrogen peroxide is promoted to be rapidly decomposed, and when the pH value is adjusted to 10-12, the catalytic efficiency of manganese dioxideis the highest; manganese dioxide is insoluble under the alkaline condition, and the catalyst can be repeatedly used; copper chloride is adopted as a catalyst promoter, so that the catalytic efficiency of manganese dioxide is improved, the decomposition time of hydrogen peroxide is shortened, hydrogen peroxide is thoroughly destroyed, and the influence of ferric iron is masked by utilizing ascorbic acid; and the problem that thiocyanate in water containing pypocholoride and ferric iron cannot be accurately determined is solved.

Description

technical field [0001] The invention relates to a method for determining thiocyanate in water quality, and is particularly suitable for the method for accurately determining thiocyanate interfered by hypochlorite and ferric iron. Background technique [0002] Thiocyanate is an important chemical raw material. In the process of preparing industrial products, its dosing ratio is often excessive and cannot be completely reacted, resulting in a large amount of thiocyanate entering the wastewater system and affecting the ecological environment. At the same time, thiocyanate itself is toxic. Excessive intake of thiocyanate will hinder the use of iodine by the body and cause acute poisoning of the human body. It is very important to accurately determine thiocyanate in water quality. The current determination methods include gas chromatography , liquid chromatography, ion chromatography, spectrophotometry and electrochemical methods. Spectrophotometry should be used for samples wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N21/78
CPCG01N21/31G01N21/78
Inventor 葛仲义陈永红芦新根
Owner CHANGCHUN GOLD RES INST
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