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 deter

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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Example Embodiment

[0028] Example 1

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

[0030] This kind of aqua regia insoluble slag is formed in the hydrometallurgical recovery process of precious metal secondary resource waste. Its composition is relatively complicated, containing a large amount of Fe, Al, Si and a small amount of Pt, Mg, Rh, Pd, Ir, Ag, and sampling and analysis after homogenizing the sample through the disc grinding mechanism. Weigh 5 parts of 0.2 g dried samples in parallel, put them in a nickel crucible with a volume of 30 mL, place them in a muffle furnace, heat up to 750°C, burn and keep them for 1 hour, and cool. Join Na 2 O 2 : NaCO 3 =3:1 Mix 3g of flux, then cover 3g of Na 2 O 2 Put it in a muffle furnace and heat it up to 750℃ to melt for 20min, take it out and cool it, put the nickel crucible into a 200mL beaker, heat the water to extract the molten salt, and then neutralize it with hydrochloric acid until the sol...

Example Embodiment

[0035] Example 2

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

[0037] This type of catalyst recycling waste is the acid insoluble residue in the process of recycling and processing automobile catalysts, petrochemical catalysts, etc., and it contains a large amount of Al, Si and sodium salts. After the sample is homogenized by the disc grinding machine, sampling and analysis are performed. Weigh 5 parts of 0.5 g dried samples in parallel, put them into a nickel crucible with a volume of 30 mL, place them in a muffle furnace, heat up to 750°C, burn and keep them for 1 hour, and cool. Join Na 2 O 2 : NaCO 3 =3:1 Mix 5g of flux, and then cover 2gNa 2 O 2 Put it in a muffle furnace and heat it up to 750℃ to melt for 25min, take it out and cool it, put the nickel crucible into a 200mL beaker, heat the water to extract the molten salt, and then neutralize it with hydrochloric acid until the solution is clear. Slowly add 2 mL of 30...

Example Embodiment

[0040] Example 3

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

[0042] The 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, the direct measurement of extremely low content of Pt, Pd, Au has serious interference. Generally, lead fire assay is used to enrich Pt, Pd, Au to separate other interference components for determination. However, the three elements of Pt, Pd, and Au need to be enriched and determined in two batches, so the operation is troublesome and time-consuming.

[0043] Weigh five 2.00g samples in parallel, put them into a nickel crucible with a volume of 30mL, place them in a muffle furnace, heat up to 750°C, burn and keep them for 1h, and cool. Join Na 2 O 2 : NaCO 3 =3:1 mixed flux 6g, then cover 2gNa 2 O 2 Put it in a muffle furnace and heat it up to 750℃ to melt for 20min, take it out and cool it, put the nickel crucible int...

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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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