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An analytical method for measuring tellurium in high-selenium tellurium slag

An analysis method and a tellurium slag technology, applied in the field of chemical analysis, can solve the problems of difficult analysis results, long time, difficult to accurately measure the tellurium content, etc., to ensure accuracy, acceleration rate and completeness, and avoid the impact on the test. Effect

Active Publication Date: 2018-12-28
NORTHWEST RES INST OF MINING & METALLURGY INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Tellurium slag, an intermediate product of smelting, mainly comes from the copper smelting process, which mainly contains tellurium with a general content of several percent to tens of percent, selenium with a general content of several percent to more than ten percent, and copper with a general content of 100 percent. The silver content is generally a few percent; because the general tellurium slag contains selenium as an impurity element, and its chemical properties are similar to tellurium, it is difficult to accurately determine the tellurium content in the tellurium slag; the traditional method uses heavy chromium The method of potassium acid potassium oxidation takes a long time, and it is difficult to quickly obtain analysis results to guide industrial production

Method used

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Embodiment 1

[0020] (1) Accurately weigh 0.5000g of a tellurium slag sample into a 400mL beaker, rinse the sample with a small amount of water, add 15mL of 15mol / L concentrated nitric acid, heat and boil until the sample is completely dissolved, add 15mL of sulfuric acid (1+1) and heat to Sulfuric acid fumes, remove and cool, dilute with a small amount of water, add 6.8mol / L hydrobromic acid 10mL, continue heating until sulfuric acid fumes are exhausted, remove, add 12mol / L hydrochloric acid 10mL, heat to boil until the solution is evaporated to nearly dry, Add 20mL of hydrochloric acid (1+1) to flush water to about 150mL, heat the solution to near boiling to dissolve salts, add dropwise 50g / L silver sulfate solution until no silver chloride precipitates in the solution, filter with medium-speed filter paper, and keep the filtrate ;

[0021] (2) Add 0.01mol / L potassium permanganate standard solution to the above filtrate until the color of the solution is a stable purple red and does not f...

Embodiment 2

[0025] (1) Accurately weigh 0.4000g of a tellurium slag sample into a 400mL beaker, rinse the sample with a small amount of water, add 15mL of 15mol / L concentrated nitric acid, heat and boil until the sample is completely dissolved, add 15mL of sulfuric acid (1+1) and heat to Sulfuric acid fumes, remove and cool, dilute with a small amount of water, add 10mL of 6.8mol / L hydrobromic acid, continue heating until sulfuric acid fumes are exhausted, remove, add 12mol / L hydrochloric acid, heat and boil until the solution is evaporated to nearly dry Finally, add 20mL of hydrochloric acid (1+1) to flush water to about 150mL, heat the solution to near boiling to dissolve salts, add dropwise 50g / L silver sulfate solution until no silver chloride precipitates in the solution, and filter with medium-speed filter paper , keep the filtrate;

[0026] (2) Add 0.01mol / L potassium permanganate standard solution to the above filtrate until the color of the solution is stable purple red and does ...

Embodiment 3

[0030] (1) Accurately weigh 0.3000g of a tellurium slag sample into a 400mL beaker, rinse the sample with a small amount of water, add 10mL of 15mol / L concentrated nitric acid, heat and boil until the sample is completely dissolved, add 10mL of sulfuric acid (1+1) and heat to Sulfuric acid fumes, remove and cool, dilute with a small amount of water, add 10mL of 6.8mol / L hydrobromic acid, continue heating until sulfuric acid fumes are exhausted, remove, add 10mL of 12mol / L hydrochloric acid, heat to boil until the solution is evaporated to nearly dry Finally, add 20mL of hydrochloric acid (1+1) to flush the water to about 150mL, heat the solution to near boiling to dissolve the salts, add dropwise 50g / L silver sulfate solution until no silver chloride precipitates in the solution, filter with medium-speed filter paper, keep the filtrate;

[0031] (2) Add 0.01mol / L potassium permanganate standard solution to the above filtrate until the color of the solution is stable purple red...

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Abstract

The invention provides an analytical method for determining tellurium in high-selenium tellurium slag. According to the analytical method, a sample is dissolved in nitric acid and sulfuric acid, sulfuric acid smokes to volatilize and remove selenium in a bromide form, high-valence tellurium (VI) is quantitatively reduced into low-valence tellurium (IV) in a hydrochloric acid medium with the concentration higher than 10mol / L, the interference of chloride ions is eliminated by silver sulfate in a silver chloride precipitate form, low-valence tellurium (IV) is quantitatively oxidized into high-valence tellurium (VI) by potassium hypermanganate, excessive potassium hypermanganate is reduced by ferrous sulfate, and therefore, the content of tellurium in a sample is indirectly determined; tellurium in the high-selenium tellurium slag is analyzed and determined by carrying out indirect titration on ferrous sulfate through taking hydrochloric acid as a reducing agent and a complexing agent and potassium hypermanganate as an oxidizing agent, so that the predicament that tellurium in the high-selenium tellurium slag is difficultly and accurately determined in a recovery process is solved. The method has the advantages of good separation effect, high recovery rate, high accuracy, and the like.

Description

technical field [0001] The invention belongs to the field of chemical analysis, in particular to an analysis method for measuring tellurium in high-selenium tellurium slag. Background technique [0002] Tellurium is a rare metalloid element, and tellurium has both associated ore and independent deposits in nature. It is mainly used as a catalyst for petroleum cracking, a brightener for electroplating solutions, and a coloring material for glass. It is added to steel to increase its ductility, and added to lead to increase its strength and corrosion resistance. Tellurium and its compounds are another semiconductor material. By consulting the literature, there are many methods for the determination of tellurium in tellurium dioxide products, and there are even relevant national standards. There are few relevant literatures on the chemical analysis methods of tellurium in tellurium slag, an intermediate product of smelting, especially those containing high selenium. There are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/79
CPCG01N21/79
Inventor 郑省政余江鸿王同敏王红燕方彦霞路军兵张彦翠齐白羽赵海军展之旺谷雅楠
Owner NORTHWEST RES INST OF MINING & METALLURGY INST
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