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Preparation method and application of high-purity rhenium standard sample for GD-MS component analysis

A GD-MS, standard sample technology, used in the preparation of test samples, analysis of materials, and testing of metal components, etc., to achieve the effect of long storage time

Inactive Publication Date: 2022-04-26
国合通用测试评价认证股份公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when there is a lack of standard samples, the computer can automatically calculate the mass fraction of each element according to the "typical relative sensitivity factor" in the instrument software, and only semi-quantitative analysis results can be obtained.

Method used

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  • Preparation method and application of high-purity rhenium standard sample for GD-MS component analysis
  • Preparation method and application of high-purity rhenium standard sample for GD-MS component analysis
  • Preparation method and application of high-purity rhenium standard sample for GD-MS component analysis

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preparation example Construction

[0033] The preparation method of the high-purity rhenium standard sample for GD-MS component analysis of the present invention, the obtained high-purity rhenium sample can be used for trace element analysis, comprising the following steps:

[0034] (1) High-purity rhenium standard sample composition design: design pure rhenium sample composition according to pure rhenium product standards, high-purity rhenium standard samples include Ag, Al, As, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu , Fe, Ga, K, Mg, Mn, Mo, Na, Ni, Pb, Pt, Sb, Se, Si, Sn, Te, Ti, Tl, W, Zn a total of 30 trace impurity elements, each impurity element The content of 0.1mg / kg~500mg / kg;

[0035] Ammonium rhenate with a purity of 99.95% is used as the raw material, and superior pure silver nitrate, aluminum nitrate, sodium arsenate, barium nitrate, beryllium carbonate, bismuth nitrate, calcium carbonate, cadmium nitrate, cobalt nitrate, nitric acid are quantitatively added to it according to the design value Chromium, co...

Embodiment

[0049] 1. Weigh 25kg of ammonium rhenate (purity>99.95%); 0.2g each of beryllium carbonate and thallium nitrate; 0.5g each of silver nitrate, barium nitrate, cadmium nitrate, gallium nitrate, and chloroplatinic acid; Magnesium, sodium arsenate, ammonium molybdate, sodium selenate, sodium telluride each 1g; bismuth nitrate, cobalt nitrate, nickel nitrate, lead nitrate, titanium powder, zinc chloride each 2g; chromium nitrate, copper nitrate, potassium nitrate, Manganese nitrate, antimony trioxide, sodium silicate, tin tetrachloride, ammonium paratungstate each 3g; ferrous sulfate 10g.

[0050] 2. Dissolve and mix the samples in step 1 with high-purity water, MOS-grade hydrochloric acid or nitric acid, place them in a vertical heating mixer for evaporation and crystallization for 24 hours, and then place them in a tubular reduction furnace for hydrogen reduction at 950°C for 6 hours. The hydrogen flow rate is 20L / h, and the rhenium powder standard sample candidate material is ob...

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Abstract

The invention relates to a preparation method and application of a high-purity rhenium standard sample for GD-MS component analysis, and belongs to the field of rare metal analysis. The method comprises the following steps: quantitatively adding corresponding simple substances or compounds of 30 impurity elements of Ag, Al, As, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, K, Mg, Mn, Mo, Na, Ni, Pb, Pt, Sb, Se, Si, Sn, Te, Ti, Tl, W and Zn into an ammonium rhenate solution, mixing, reducing, grinding, homogenizing, tabletting, shaping and sintering to obtain the pure rhenium standard sample. And carrying out uniformity test and stability test on 30 elements in the sample, and carrying out accurate valuation. The high-purity rhenium standard sample obtained through the method is regular in shape, uniform in component, good in stability, accurate in fixed value and convenient to store, and can be used for correction of high-purity rhenium trace element measurement results and monitoring of instrument and equipment states.

Description

technical field [0001] The invention relates to a preparation method and application of a high-purity rhenium standard sample for GD-MS (glow discharge mass spectrometry) component analysis, belonging to the field of rare metal analysis. Background technique [0002] Rhenium is a rare refractory metal with high melting point, high strength, good plasticity and mechanical stability. It is widely used in aerospace, national defense, petrochemical, mechanical and electronic industries. One of the important new materials for products such as high temperature instruments. The purity of rhenium is critical to obtain highly dense, high-performance rhenium products. In recent years, with the continuous improvement of the domestic rhenium purification process, the application range of high-purity rhenium in high-tech fields has become wider and wider, and the demand has also increased. The requirements for the accuracy of high-purity rhenium testing and evaluation methods have also ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/38G01N1/44G01N27/68G01N33/202
CPCG01N1/28G01N1/286G01N1/38G01N1/44G01N27/68G01N33/202G01N2001/2866
Inventor 张晓徐青陈雄飞张芳墨淑敏贾国斌
Owner 国合通用测试评价认证股份公司
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