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Separation and enrichment determination method for Ir, Rh, Pt, Pd and Au in secondary resource material

A secondary resource material, separation and enrichment technology, applied in the direction of material stimulation analysis, thermal stimulation analysis, preparation of test samples, etc., can solve the problems of salt interference, acid-soluble insoluble, etc., the method is simple and easy, The effect of addressing demand gaps

Inactive Publication Date: 2016-02-03
GUIYAN DETECTION TECH YUNNAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) Sample dissolution problem: Due to the strong corrosion resistance of precious metals, it is difficult to dissolve them completely with general acid and alkali, especially materials containing iridium, rhodium, and ruthenium
[0005] (2) Separation and enrichment problem: acid dissolution cannot be completely dissolved, while alkali fusion can be completely dissolved, but a large amount of salt interference must be eliminated by separation
[0006] (3) Selection of measurement means: There are many means for the determination of precious metals, but most of them have certain limitations
[0009] Therefore, considering various factors, to solve the measurement problem of noble metal content in secondary resource materials containing rhodium, iridium and ruthenium, we can only choose alkali fusion to become a solution, and then take other separation and enrichment methods to mix iridium, rhodium, platinum, Accurate determination is possible only when palladium and gold are separated from complex matrix components and salts at the same time

Method used

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  • Separation and enrichment determination method for Ir, Rh, Pt, Pd and Au in secondary resource material
  • Separation and enrichment determination method for Ir, Rh, Pt, Pd and Au in secondary resource material
  • Separation and enrichment determination method for Ir, Rh, Pt, Pd and Au in secondary resource material

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Simultaneous determination of low content Ir, Rh, Pt, Pd, Au in aqua regia insoluble slag

[0030] This kind of aqua regia insoluble slag is formed in the hydrometallurgical recycling process of precious metal secondary resource waste. Its composition is relatively complex, containing a large amount of Fe, Al, Si and a small amount of Pt, Mg, Rh, Pd, Ir, Ag, and the sample is homogenized by a disc mill before sampling and analysis. Weigh 5 portions of 0.2 g dried samples in parallel, put them into a 30 mL nickel crucible, place them in a muffle furnace, raise the temperature to 750°C and burn for 1 hour, then cool. Join Na 2 o 2 : NaCO 3 = 3: 1 mixed flux 3g, then covered with 3gNa 2 o 2 , put it into a muffle furnace and raise the temperature to 750°C for 20 minutes, take it out and cool it, put the nickel crucible into a 200mL beaker, heat water to leach the molten salt, and then neutralize it with hydrochloric acid until the solution is clear. Slowly add 5mL of...

Embodiment 2

[0036] Determination of Ir, Rh, Pt, Pd content in catalyst recovery waste residue.

[0037] This kind of catalyst recovery waste residue is acid-insoluble residue in the process of recycling automobile catalysts, petrochemical catalysts, etc., which contains a large amount of Al, Si and sodium salts. The sample was homogenized by a disc mill before sampling and analysis. Weigh 5 portions of 0.5 g dried samples in parallel, put them into a 30 mL nickel crucible, place them in a muffle furnace, raise the temperature to 750°C and burn for 1 hour, then cool. Join Na 2 o 2 : NaCO 3 = 3: 1 mixed flux 5g, then covered with 2gNa 2 o 2 , put it into a muffle furnace and raise the temperature to 750°C to melt for 25 minutes, take it out and cool it, put the nickel crucible into a 200mL beaker, heat water to leach the molten salt, and then neutralize it with hydrochloric acid until the solution is clear. Slowly add 2mL30% sodium chlorate solution and boil for about 45min. Adjust t...

Embodiment 3

[0041] Determination of Pt, Pd, Au content in anode slime

[0042] Anode slime mainly contains a large amount of Cu, Pb, Sn, Sb, Mg, Bi, Ag, Al, Ni, Si, S, P and other elements, and also contains a small amount of precious metals. However, there are serious interferences in direct determination of extremely low content of Pt, Pd, and Au. Generally, lead fire assay is used to enrich Pt, Pd and Au to separate other interfering components for determination. However, the three elements of Pt, Pd, and Au need to be enriched and measured in two batches, so the operation is cumbersome and time-consuming.

[0043] Five samples of 2.00 g were weighed in parallel, put into a nickel crucible with a volume of 30 mL, placed in a muffle furnace, heated to 750° C. for igniting and kept for 1 h, and cooled. Join Na 2 o 2 : NaCO 3 = 3: 1 mixed flux 6g, then covered with 2gNa 2 o 2 , put it into a muffle furnace and raise the temperature to 750°C for 20 minutes, take it out and cool it, ...

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Abstract

The invention discloses a separation and enrichment determination method for Ir, Rh, Pt, Pd and Au in a secondary resource material. The method includes the following steps that 1, samples are dissolved, and after high-temperature firing carbon removal, a Na2O2+NaCO3 mixed fluxing agent is adopted for fusion in a muffle furnace of 750 DEG C; 2, a test solution is oxidized, an appropriate quantity of sodium chlorate solution is added in a dissolving solution, boiling is performed, and Ir in the solution is oxidized so that the valence state can be made stable; the solution is adjusted to be at the appropriate volume, and the volume concentration of hydrochloric acid reaches 50%; 3, tellurium coprecipitation separation is carried out; 4, determination is carried out, an inductively coupled plasma optical emission spectrometry (ICP-AES) is used for determining the content of the Ir, Rh, Pt, Pd and Au in the solution obtained in the third step at the same time. The accurate and fast separation and enrichment determination method is specifically used for the Ir, Rh, Pt, Pd and Au with the content scope being 0.001%-5% in the secondary resource material such as waste and metallurgical middle materials formed in the using process of various precious metal products. The method is also suitable for separation and enrichment determination of Ir, Rh, Pt, Pd and Au single elements in the secondary resource material.

Description

technical field [0001] The invention relates to the field of precious metal analytical chemistry, in particular to a separation and enrichment measurement method for secondary resource materials such as waste materials formed during the use of various precious metal products and intermediate materials formed in metallurgical recovery processes. Background technique [0002] Due to the special physical and chemical properties of precious metals, such as excellent electrical conductivity, catalytic performance, super corrosion resistance and beautiful color, etc., they have been widely used in the electronics industry, petrochemical industry, environmental protection, aerospace and jewelry industries. Applications. Precious metals are expensive due to their relatively small content on the earth. As a scarce resource, many countries have listed it as an important strategic resource. With the continuous development of my country's economy, precious metals have been more and mo...

Claims

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Application Information

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IPC IPC(8): G01N21/71G01N1/34G01N1/40
Inventor 方卫马媛赵云昆李青杨晓滔任传婷罗雁波
Owner GUIYAN DETECTION TECH YUNNAN CO LTD
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