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Analysis method for silver in copper anode mud

An analysis method, copper anode slime technology, applied in the field of chemical analysis, can solve problems such as low results, unsuitable silver, poor specificity, etc.

Inactive Publication Date: 2007-03-21
GUANGZHOU RES INST OF NON FERROUS METALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Potassium thiocyanate titration is a classic method for the determination of silver. The main disadvantage of this method is poor specificity. Before titration, it is required to separate silver from other interfering elements.
The above method needs to transfer the AgCl precipitation, which will cause the result to be low, and the AgCl in the copper anode slime cannot be absorbed by HNO 3 Soluble, so not suitable for determination of silver in copper anode slime

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] Weigh 0.2000g sample and place it in a 250ml Erlenmeyer flask, add 30ml 1:1 HNO 3 : Water, after heating for 10 minutes, add 15ml of ρ1.19g / ml hydrochloric acid, then evaporate to 4ml, add 100ml of water, heat and boil for 20 minutes, remove, cool, filter with medium-speed quantitative filter paper, wash the beaker and Precipitate 5 times, transfer the precipitate together with the filter paper to the original beaker, add 14ml ρ1.84g / ml H 2 SO 4 , after carbonization, add ρ1.42g / ml HNO 3 Until the solution is colorless, heat until thick white smoke is emitted, cool, add water to dilute to 40ml, cool, add 1ml ferric ammonium sulfate indicator, and titrate with potassium thiocyanate standard solution until light red is the end point.

Embodiment 2

[0009] Weigh 0.1000g sample and place it in a 250ml Erlenmeyer flask, add 30ml 1:1 HNO 3 : Water, add 25ml of hydrochloric acid ρ1.19g / mL after heating for 20 minutes, then evaporate to 2ml, add 80ml of water, heat and boil for 10 minutes, remove, cool, filter with medium-speed quantitative filter paper, wash the beaker and Precipitate 5 times, transfer the precipitate together with the filter paper to the original beaker, add 10ml ρ1.84g / ml H 2 SO 4 , after carbonization, add ρ1.42g / ml HNO 3 Until the solution is colorless, heat until thick white smoke is emitted, cool, add water to dilute to 50ml, cool, add 1ml ferric ammonium sulfate indicator, and titrate with potassium thiocyanate standard solution to light red, which is the end point.

Embodiment 3

[0011] Weigh 0.5000g sample and place it in a 250ml Erlenmeyer flask, add 30ml 1:1 HNO 3 : Water, after heating for 20 minutes, add 35ml of ρ1.19g / ml hydrochloric acid, then evaporate to 1ml, add 50ml of water, heat and boil for 30 minutes, remove, cool, filter with medium-speed quantitative filter paper, wash the beaker and Precipitate 5 times, transfer the precipitate together with the filter paper to the original beaker, add 6ml ρ1.84g / ml H 2 SO 4 , after carbonization, add ρ1.42g / ml HNO 3 Until the solution is colorless, heat until thick white smoke is emitted, cool, add water to dilute to 60ml, cool, add 1ml ferric ammonium sulfate indicator, and titrate with potassium thiocyanate standard solution to light red, which is the end point.

[0012] Table 1 is the comparison of the results of measuring silver in copper anode slime with the method of the present invention, the fire assay gold method and the method of "Determination of silver and copper in lead anode slime". ...

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PUM

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Abstract

The analysis process of silver in copper anode slime includes adding HNO3 into sample and heating to decompose, adding HCl, heating to evaporate, cooling, adding water, heating to boil, cooling, filtering with quantitative filter paper, washing container and deposit, setting the deposit together with the filter paper into the container, adding H2SO4, carbonizing, adding HNO3 until the solution become colorless, heating to smoke with dense white smoke, cooling, diluting with water, adding ferric ammonium sulfate as indicator, and titrating with standard potassium thiocyanate solution to light red as the terminal. The method is simple, fast, accurate, and suitable for the analysis of silver in copper anode slime.

Description

technical field [0001] The invention relates to a chemical analysis method, in particular to a metal element chemical analysis method. Background technique [0002] Anode slime is an important precious metal material, and the market is active. It is very necessary to accurately and quickly determine the silver content in copper anode slime. Copper anode slime is the product of blister copper electrolysis, which contains not only precious metals, but also a large amount of impurities such as As, Bi, Pb, Sb, Se, Te, etc. The occurrence states of silver in copper anode slime are various, mainly including Ag, Ag 2 Se, Ag 2 Te, AgCl, etc. At present, the chemical analysis method for determining silver in copper anode slime is carried out according to the industry standard YS / T88-1995, which is called fire assay gold method. However, the fire test gold consumes a lot of energy, the equipment is expensive, the lead vapor pollutes the environment and is harmful to human health, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/16G01N21/78
Inventor 戴凤英林海山陈小兰李小玲
Owner GUANGZHOU RES INST OF NON FERROUS METALS