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Method for measuring ruthenium content using ethyne-air flame atomic absorption spectrometry

A flame atomic absorption and spectrometry technique is applied in the field of determination of ruthenium content in ruthenium-containing catalysts. high effect

Active Publication Date: 2009-08-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that (1) hydrogen peroxide heating is prone to explosion, which endangers the personal safety of test personnel; (2) the test time is long, and it takes 24 hours to dissolve the standard substance and the sample

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Spectroscopically pure ruthenium powder was used to prepare a standard solution, and the content of ruthenium in the ruthenium-carbon catalyst was determined.

[0026] Dry the ruthenium-carbon catalyst sample at 105 for 4 hours to remove moisture; weigh 0.4064 g (dry basis) of the sample and place it in a nickel crucible, burn it in a muffle furnace for 6 hours, and control the temperature at 500 ° C to remove the residual ash. Take out the crucible to cool down; weigh 0.1025 g of spectroscopically pure ruthenium powder and place it in a nickel crucible; prepare the sample solution and standard solution at the same time as follows: add 1.0 g of potassium hydroxide to the ruthenium powder and the sample respectively, heat to dissolve, and control the temperature at 380 °C. Cool to room temperature after dissolution. Transfer the sample and standard to a beaker, add 20ml of hydrochloric acid (hydrochloric acid: water = 1:1; hydrochloric acid is commercially available hydr...

Embodiment 2

[0035] A commercially available ruthenium standard solution was used as the mother liquor to prepare a standard solution, and the content of ruthenium in the ruthenium-carbon catalyst was determined.

[0036] Dry the ruthenium-carbon catalyst sample at 110°C for 3 hours to remove moisture, weigh 0.3831 g (dry basis) of the sample, place it in a nickel crucible, and burn it in a muffle furnace at 550°C for 5 hours to remove the residual ash. After cooling, add 1.0 g of potassium hydroxide, heat to dissolve, and control the temperature to 370°C. Add 25ml of hydrochloric acid (hydrochloric acid: water = 1:1), transfer to a 250ml volumetric flask, add desalted water to constant volume, and obtain the sample solution. Use the national standard ruthenium solution (the number is GSB G62037-90, the concentration is 1000 μg / mg, the medium is: 10% hydrochloric acid) as the mother solution, and dilute it into 10mg / l, 30mg / l, 50mg / l, 70mg / l with the sample blank solution And 100mg / l test...

Embodiment 3

[0043] Repeatability test of standard sample

[0044] Take 0.1035 g, 0.09958 g, and 0.1058 g of spectrally pure ruthenium powder, add 1.0 g of potassium hydroxide, heat to 380 ° C to dissolve, add 25 ml of hydrochloric acid (hydrochloric acid: water = 1:1) after cooling, transfer to a 250 ml volumetric flask, add demineralized water to set To make 1#, 2#, 3# samples.

[0045] Using the method in Example 2, use the commercially available national standard ruthenium solution as the mother solution to configure the standard solution for the test, adjust the parameters of the spectrometer, adjust the sample blank solution to zero, measure the standard solution, and draw a standard curve. Input the data of each sample separately, and measure the sample solution. For comparison, a group of pure ruthenium powders were determined by using the sealed tube chlorination-thiourea spectrophotometry at the same time. The results of the two methods are shown in Table 1.

[0046] Table 1 ...

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Abstract

The invention provides a method for determining ruthenium content by acetylene-air flame atom absorption spectrum method, the procedures for which are: a sample is dried under 100-120 centigrade, burned under 400-600 centigrade, residual ash is removed; potassium hydroxide is added in a reference pure ruthenium powder and sample, which is heated under 360-390 centigrade to dissolve; surplus chlorhydric acid is added, so that the solution is acid; some de-saline water is added in the solution to prepare standard mother solution and sample solution; standard solutions of different concentrations are prepared by taking sample blank liquid as thinner; the spectrometer wavelength is adjusted to 344.9 nm, the acetylene flow 65 l / h, lamp current 10 mA; the zero is calibrated by using sample blank liquid, the standard solution is determined, and a standard work curve is established, parameters of the sample are input, the concentration and content of the ruthenium are measured in the sample. The invention has a rapid measuring speed, high accuracy, low harm on the operator, and is applicable for determining the ruthenium content in various solid or liquid multi-component substances, especially the ruthenium content in ruthenium / carbon catalyzer.

Description

technical field [0001] The invention relates to a method for measuring ruthenium content by acetylene-air flame atomic absorption spectrometry, in particular to a method for measuring ruthenium content in ruthenium-containing catalysts. Background technique [0002] Ruthenium is a precious metal widely used in medical, chemical, metallurgy and other fields. In order to effectively prepare and use ruthenium catalysts, fully utilize or recover ruthenium metal, it is necessary to determine the content of ruthenium in multi-component substances. Known methods for determining the content of ruthenium include the method of sealing tubes and chlorination to dissolve standard substances and samples, and the determination of ruthenium content by thiourea spectrophotometry. That is, put the standard or sample in sealed tubes, add hydrochloric acid and hydrogen peroxide, heat and dissolve in a special steel bomb to make a standard solution and sample solution, add thiourea developer, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/31
Inventor 袁宏伟陈淼高立新韩丽红高秀霞
Owner CHINA PETROLEUM & CHEM CORP
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