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Method of separating, gathering and measuring platinum, palladium and rhodium in automotive catalyst

An auto catalyst, separation and enrichment technology, used in thermal excitation analysis, material excitation analysis, preparation of test samples, etc., can solve the problems of slow analysis speed, inability to meet rapid measurement, interference, etc., and achieve the effect of easy purchase

Active Publication Date: 2010-03-10
GUIYAN DETECTION TECH YUNNAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The domestically established spectrophotometric method for the simultaneous determination of Pt and Pd with the dual-wavelength spectrophotometric method of dibenzyldithiooxalamide-potassium iodide-ascorbic acid and the determination of Rh with the extraction spectrophotometric method of 2-mercaptobenzothiazole-stannous bromide has been established. It is a relatively mature method. Since Pt, Pd, and Rh need to be extracted and separated separately during the determination process, the analysis speed is relatively slow. It usually takes 2 days to get the result after the sample is dissolved, which cannot meet the requirements of rapid determination.
Although the ICP-AES method has the advantages of low detection limit, high precision, wide linear range, and fast speed, there are also a large number of interference problems in the direct determination of Pt, Pd, and Rh in autocatalysts. Some related research work has been published, but it is still weak and lacks systematic work

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: the mensuration of Pt, Pd and Rh in the spent automobile catalyst

[0018] Such catalysts are collected step by step through different channels, and traded when a certain amount is reached, and the samples are relatively complicated. Before trading, the catalyst needs to be crushed mechanically, and after repeated grinding to a certain mesh size, it is homogenized for analysis. Follow the steps below:

[0019] ①Dissolution: Weigh 1g of prepared homogeneous catalyst sample (≤150 mesh), put it into a PTFE digestion tank with a volume of 30mL, add 15mLHCl+3~5mL H 2 o 2, screw on the cap. Dissolve in an oven at a constant temperature of 150°C for 12 hours, take it out, open the can after cooling to room temperature, transfer all the contents into a 200mL beaker with distilled water, evaporate to about 20mL volume under infrared light, filter into a 100mL volumetric flask In, constant volume, mix well.

[0020] ② Separation: tellurium co-precipitation sepa...

Embodiment 2

[0025] Embodiment 2: the mensuration of Pt, Pd and Rh in the washing coating material

[0026] This material is a waste material generated during the catalyst production process, without the carrier cordierite component, the main composition is Al 2 o 3 (52.6%), CeO 2 (30.1%), ZrO 2 (10.2%), La 2 o 3 (4.2%) and NiO (3.0%). Weigh 0.5 g of the dried sample and put it into a polytetrafluoroethylene digestion tank with a volume of 30 mL, and operate according to the dissolution, separation and determination steps in Example 1.

[0027] The calculated contents of Pt, Pd and Rh in this sample are 9141g / t, 3258g / t and 2106g / t respectively.

Embodiment 3

[0028] Embodiment 3: the mensuration of Pd and Rh in the automobile catalyst product

[0029] The catalyst samples sampled by automobile companies for quality control have not yet been installed and used on complete vehicles. After one catalyst is weighed, the whole piece is crushed, ground to 150-200 mesh powder, and homogeneously mixed. The main composition of the sample is Al 2 o 3 (45.7%), SiO 2 (21.3%), MgO (5.2%), CeO 2 (7.0%), ZrO 2 (10.6%), La 2 o 3 (1.88%) and BaO (3.6%) and Fe 2 o 3 (0.6%) etc.

[0030] Weigh 1.0 g of the dried sample, put it into a polytetrafluoroethylene digestion tank with a volume of 30 mL, and operate according to the dissolution, separation and determination steps in Example 1. According to analysis and calculation, the contents of Pd and Rh in this sample were 1359g / t and 215g / t respectively, and no Pt was detected.

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PUM

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Abstract

The invention discloses a method of separating, gathering and measuring platinum, palladium and rhodium in automotive catalyst. The method comprises the following steps: (1) the dissolution of a sample: weighting 0.5-1.5g of uniform catalyst sample with the grain size of 150 meshes or less to place in a polytetrafluoroethylene digestion tank, adding HCl and H2O2, closing the lid; placing the digestion tank in a constant temperature oven to dissolve the catalyst, withdrawing the digestion tank, transferring all the materials into a beaker by using distilled water, evaporating, filtrating, adding filtrate in a volumetric flask, performing constant volume, mixing evenly; (2) the coprecipitation, separation and enrichment of tellurium: pipetting a certain amount of sample solution into a beaker, adding concentrated hydrochloric acid and tellurium solution, controlling the solution to boil on an electric hot plate, dropwise adding SnCl2 solution to ensure that the yellow color disappears, alarge number of precipitate is prepared and some SnCl2 solution is excessive, heating continuously, replenishing tellurium solution, boiling the solution to boiling gently, taking the beaker down tocool the solution to room temperature, filtrating the solution, washing with water, precipitating; dropwise adding fresh warm aqua regia to dissolve, washing the funnel with water for several times; heating the solution to be nearly dry, transferring the obtained product with HCl to a volumetric flask, performing constant volume, mixing evenly; (3) measuring the content of Pt, Pd and Rh with ICP-AES under optimum instrument conditions.

Description

technical field [0001] The invention relates to an accurate and rapid determination method for platinum, palladium and rhodium in automobile catalysts, in particular to a method for accurately and rapidly determining platinum, palladium and rhodium, which can eliminate measurement interference after tellurium co-precipitation, separation and enrichment. Background technique [0002] With the rapid development of my country's automobile industry, the number of automobiles has increased rapidly, and the environmental pollution caused by carbon monoxide and nitrogen oxides in automobile exhaust has become increasingly serious. It has become an important factor of environmental pollution and has attracted the attention of the whole society. Controlling and treating tail gas pollution has become an important task at present. The installation of automobile exhaust purification catalyst is the main means to reduce exhaust pollution. [0003] Automobile exhaust gas purification cat...

Claims

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Application Information

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IPC IPC(8): G01N21/73G01N1/28G01N1/40
Inventor 方卫赵云昆马媛胡洁
Owner GUIYAN DETECTION TECH YUNNAN CO LTD
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