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A method for measuring selenium content in crude selenium

A crude selenium and content technology, which is applied in the direction of removing certain components and weighing, can solve the problems of cumbersome determination process, etc., and achieves the effects of cheap and easy-to-obtain reagents, easy-to-master, and simple methods.

Active Publication Date: 2020-03-24
YANGGU XIANGGUANG COPPER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The measurement process is more cumbersome

Method used

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  • A method for measuring selenium content in crude selenium
  • A method for measuring selenium content in crude selenium
  • A method for measuring selenium content in crude selenium

Examples

Experimental program
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Effect test

Embodiment 1

[0063] Weigh 0.5022g (m 0 ), placed in a 250mL conical flask. Add about 100 mL of water, heat it to a slight boil, and add 4 g of hydroxylamine hydrochloride. Low temperature heating. Filter with slow quantitative filter paper. Wash the sediment and the beaker 3 times with water. Transfer the precipitate to the original beaker, add 19mL HNO 3 , Heat at low temperature on a hot plate, wait until the brown smoke is exhausted, remove and cool. Add 4.5mL hydrogen peroxide and 4mL perchloric acid, and heat at low temperature until the reaction is complete. Remove, slowly add about 40mL of sodium hydroxide (200g / L), adjust the solution to weak acid, heat at low temperature, and cool slightly. Slowly add about 21 mL of barium nitrate solution (150 g / L), heat at low temperature until the reaction is complete, and cool. Filter with a slow quantitative filter paper and rinse the precipitate with dilute nitric acid. The precipitate is dried in an electric thermostatic drying oven at...

Embodiment 2

[0066] Weigh 0.4981g (m 0 ), placed in a 250mL conical flask. Add about 110mL of water, heat to a slight boil, and add 3.5g of hydroxylamine hydrochloride. Low temperature heating. Filter with slow quantitative filter paper. Wash the sediment and the beaker 3 times with water. Transfer the precipitate to the original beaker, add 22 mL of hydrochloric acid, and heat it at low temperature on a hot plate. When the brown smoke is exhausted, remove it and cool. Add 5mL hydrogen peroxide and 5mL perchloric acid, and heat at low temperature until the reaction is complete. Remove, slowly add about 45mL of potassium hydroxide (220g / L), adjust the solution to weak acid, heat at low temperature, and cool slightly. Slowly add about 23mL barium nitrate solution (150g / L), heat at low temperature until the reaction is complete, and cool. Filter with a slow quantitative filter paper and rinse the precipitate with dilute nitric acid. The precipitate is dried in an electric thermostatic dr...

Embodiment 3

[0069] Weigh 0.5009g (m 0 ), placed in a 250mL conical flask. Add about 100mL of water, heat to a slight boil, and add 5g of hydrazine hydrate. Low temperature heating. Filter with slow quantitative filter paper. Wash the sediment and the beaker 3 times with water. Transfer the precipitate to the original beaker, add 20mL HNO 3 , Heat at low temperature on a hot plate, wait until the brown smoke is exhausted, remove and cool. Add 6g potassium permanganate and heat at low temperature until the reaction is complete. Remove, slowly add about 42mL of sodium hydroxide (200g / L), adjust the solution to weak acidity, heat at low temperature and cool slightly. Slowly add about 20mL barium chloride solution (170g / L), heat at low temperature until the reaction is complete, and cool. Filter with a slow quantitative filter paper and rinse the precipitate with dilute nitric acid. The precipitate is dried in an electric thermostatic drying oven at 105℃±5℃ for about 2 hours, and weighed ...

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Abstract

The invention provides a method for determining selenium content in coarse selenium. The method comprises the following steps of: A) mixing and heating coarse selenium with water, and then adding a reducer to react to obtain a precipitate; B) after dissolving the precipitate with an acid, adding an oxidant to perform an oxidizing reaction, wherein the oxidant is selected from a compound oxidant, potassium permanganate or potassium dichromate formed by perchloric acid and hydrogen peroxide; and C), after salinizing an oxidized product obtained in the step B, adding a precipitant to react to obtain a precipitate, and calculating the selenium content in the coarse selenium according to mass of the precipitate, wherein the precipitant is barium nitrate or barium chloride. The method of determining selenium content in coarse selenium provided by the invention is simple, short in flow, accurate in result and easy to master by an operator. A reagent used in the method is cheap and easily available, and multi-method instruments such as an ICP spectrograph are avoided, so that the test analytical cost is lowered. The method can be suitable for detecting and analyzing coarse selenium production, so that production is favorably guided. The method is also suitable for trade settlement analysis.

Description

Technical field [0001] The invention belongs to the technical field of non-ferrous metal smelting, and specifically relates to a method for determining the selenium content in crude selenium. Background technique [0002] Selenium is a non-metallic chemical element, and its chemical symbol is Se. Selenium is an important industrial raw material, which can be used as photosensitive material and catalyst in electrolytic manganese industry. The use is very wide. [0003] At present, 90% of primary selenium is mainly produced in the anode slime of copper electrolysis, and the crude product is crude selenium. In the process of producing cathode copper by electrolysis, the copper anode slime produced is smelted by fire method to produce selenium-containing flue gas. The flue gas is processed by a purification system and reduced with a reducing agent such as sodium sulfite to produce crude selenium. The selenium content is roughly 80-99%. [0004] Crude selenium is an important by-produ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N5/04
CPCG01N5/04
Inventor 万双李先和赵九柯姜泓戚月花
Owner YANGGU XIANGGUANG COPPER
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