Method for measuring rhodium content in rhodium-containing compound

The technology of a rhodium compound and a determination method is applied in the field of compound element rhodium content determination, which can solve the problems of error in determination results, cumbersome steps, influence on the accuracy of results and the like, and achieves the effects of convenient operation, good recovery rate and high accuracy

Inactive Publication Date: 2014-01-22
CHINA NAT OFFSHORE OIL CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is complicated and the steps are cumbersome
[0006] At present, commonly used instrumental analysis such as atomic absorption method (FAAS) and inductively coupled plasma mass spectrometry (ICP-MS)] need to repeatedly dilute the rhodium-containing test solution by hundreds to tens of thousands of times to make the rhodium concentration within 100PPM In order to be suitable for measurement, resulting in a large error in the measurement results
Due to the interference of other elements in X-ray fluorescence spectrometry, the accuracy of the results is affected

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 1g of rhodium trichloride, roast at 700°C for 1 hour, and cool to obtain crude rhodium oxide; grind the crude rhodium oxide, soak it in 2mol / L hydrochloric acid for 3 hours at a temperature of 60°C, and filter to obtain a filter residue; the filter residue is placed in Put the quartz boat into the tube furnace, first pass nitrogen gas into the tube furnace for 10 minutes, then pass hydrogen gas for reduction, the temperature is 700 degrees, and reduce for 1 hour to make rhodium oxide into rhodium powder; weigh the rhodium powder, and the weight is 0.3884g , to calculate the rhodium content in the rhodium compound.

[0022] The calculation formula of rhodium content is: Rh%=weight of rhodium powder / weight of rhodium trichloride*100%

Embodiment 2

[0024] Weigh 5g of rhodium trichloride, roast at 1000°C for 1 hour, and cool to obtain crude rhodium oxide; grind the crude rhodium oxide, soak it in 1mol / L hydrochloric acid for 5 hours at a temperature of 70°C, and filter to obtain a filter residue; the filter residue is placed in Put the quartz boat into the tube furnace, first pass nitrogen gas into the tube furnace for 10 minutes, then pass hydrogen gas for reduction, the temperature is 800 degrees, and reduce for 1 hour to make rhodium oxide into rhodium powder; weigh the rhodium powder, and the weight is 1.9510g , to calculate the rhodium content in the rhodium compound.

Embodiment 3

[0026] Weigh 10 g of rhodium trichloride, roast at 650° C. for 3 hours, cool to obtain crude rhodium oxide; grind the crude rhodium oxide, soak in 6 mol / L hydrochloric acid for 1 hour at a temperature of 50° C., filter to obtain a filter residue, and wash with water; The filter residue is placed in a quartz boat and put into a tube furnace. First, nitrogen is passed into the tube furnace for 10 minutes, and then hydrogen is reduced. The temperature is 600 degrees, and the reduction is 3 hours, so that rhodium oxide becomes rhodium powder; the rhodium powder is weighed, and the weight For 3.9122g, calculate the rhodium content in the rhodium compound.

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Abstract

The invention relates to a method for measuring the rhodium content in rhodium-containing compound. The method comprises the steps of: 1) roasting by using high-temperature air to decompose rhodium-containing compound to be rough rhodium oxide; 2) grinding the rough rhodium oxide, immersing with 1-6mol/L hydrochloric acid for 1-5h at 50-70 DEG C and filtering to obtain filter residue; 3) reducing the filter residue with high-temperature nitrogen to change the rhodium oxide into rhodium powder; 4) weighing the rhodium powder and calculating rhodium content in the rhodium-containing compound. By adopting the method, rhodium content in the rhodium-containing compound with regular rhodium content which can be decomposed to be oxide by heating can be accurately measured, addition of other reagents for separation of rhodium is not needed, measuring error caused by repeated dilution with a power-spectral method is avoided, and rigorous requirements of high-temperature and strong-oxidizing-property wet digestion on the equipment are avoided. The method is convenient to operate without introducing solid impurities and has the advantages of high accuracy and recovery rate.

Description

field of invention [0001] The invention relates to the determination of rhodium content of compound elements, in particular to a method for determining rhodium content in rhodium-containing compounds with conventional rhodium content. Background technique [0002] Platinum group metals have electrons that can be gradually lost under certain conditions in the outer and sub-outer orbitals, forming a variety of low-valent oxidation states. When certain ligands exist in the solution, they can form stable complexes. The unique electronic structure of platinum group metals makes them have excellent catalytic properties, and are widely used in environmental protection materials, petrochemicals, fine chemicals, biopharmaceuticals and other fields. Rhodium compounds and their complexes are extremely active for reactions such as hydrogenation, carbonyl addition, and acyl hydrogenation in organic synthesis processes, and are widely used. Rhodium catalysis has become one of the most ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/04
Inventor 李继霞蒋凌云于海斌李俊李晨郝婷婷郑书忠
Owner CHINA NAT OFFSHORE OIL CORP
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