Method for determining content of impurity elements in highly-pure bismuth

A technology of impurity element and determination method, applied in the field of chemical testing, can solve the problems of cumbersome removal method of bismuth matrix, long analysis process, poor precision, etc., and achieve the effect of shortening analysis period, improving analysis efficiency and convenient operation.

Active Publication Date: 2018-01-26
CNBM CHENGDU OPTOELECTRONICS MATERIAL
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  • Claims
  • Application Information

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Problems solved by technology

In the national standard GB / T 91521995, GFAAS and other methods are used to determine impurities in metal bismuth, but this method must be matched with the matrix, the analysis process is long, and the precision is poor
There are also people who use strong basic anion exchange resin to separate bismuth matrix, and inductively coupled plasma mass spectrometry to measure impurities in metal bismuth, but the removal method of bismuth matrix in this method is cumbersome and error-prone

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  • Method for determining content of impurity elements in highly-pure bismuth
  • Method for determining content of impurity elements in highly-pure bismuth
  • Method for determining content of impurity elements in highly-pure bismuth

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Effect test

Embodiment 1

[0043] After the HCl gas of the present invention is volatilized to remove the bismuth main body, the content of impurity elements in the high-purity bismuth product Bi-05 is detected by the ICP-OES method, specifically:

[0044]Weigh 3.000 grams of sample to the nearest 0.001 grams. Measure the blank amount of impurity elements along with the sample. Put the sample in a quartz crucible, heat it, add 4-6ml of nitric acid dropwise to dissolve, heat to evaporate, add hydrochloric acid dropwise to dissolve to obtain the test solution. Put the crucible containing the test solution in the volatilization chamber, connect the device, start the jet pump, turn on the electricity to heat, turn the dropping funnel piston at about 200°C, add hydrochloric acid dropwise to the sulfuric acid in the flat bottom flask, and generate hydrogen chloride at a continuous and countable speed of bubbles The gas reacts with the test solution, keeps at 280±30°C to volatilize and remove bismuth trichlor...

Embodiment 2

[0049] After adopting the HCl gas of the present invention to volatilize and remove the bismuth main body, the content of impurity elements in the high-purity bismuth product Bi-06 is detected by the ICP-OES method, specifically:

[0050] Weigh 3.000 grams of sample to the nearest 0.001 grams. Measure the blank amount of impurity elements along with the sample. Put the sample in a quartz crucible, heat at low temperature, add 4-6ml of nitric acid dropwise to dissolve, heat to evaporate, add hydrochloric acid dropwise to dissolve to obtain the test solution. Put the crucible containing the test solution in the volatilization chamber, connect the device, start the jet pump, turn on the electricity to heat, turn the dropping funnel piston at about 200°C, add hydrochloric acid dropwise to the sulfuric acid in the flat bottom flask, and generate hydrogen chloride at a continuous and countable speed of bubbles The gas reacts with the test solution, keeps at 280±30°C to volatilize a...

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Abstract

The invention discloses a method for determining the content of impurity elements in highly-pure bismuth. HCl gas volatilization is adopted to remove a bismuth main body in order to solve the problemsof main body interference and difficulty in removal of the main body; bismuth reacts with a hydrogen chloride gas to generate bismuth trichloride, and volatilization removal is carried out, so a bismuth matrix is effectively removed without introducing new impurity elements, and the background interference of the main body element is effectively avoided, thereby the main peaks of elements to be measured are significant, the sensitivity is increased, and the reappearance is high. The analysis method used in the invention has the advantages of realization of simultaneous determination of multiple elements, convenience in operation, fast analysis speed, shortening of the analysis period, improvement of the analysis efficiency, and reduction of the labor intensity of analysis operator. A determination result obtained by using the method for determining the content of the impurity elements in the highly-pure has good stability, good reappearance and good accuracy. Test proves that the method is reliable and practical, and can meet the requirements of the detection of the content of the impurity elements in the highly-pure bismuth used for production and researches.

Description

technical field [0001] The invention belongs to the technical field of chemical testing, in particular to a method for measuring the content of impurity elements in high-purity bismuth. Background technique [0002] Metal bismuth is mainly used to manufacture low-melting point alloys, nuclear reactor coolants, bismuth salts, etc. Pure bismuth containing more than 99.999% bismuth is high-purity metal bismuth, which is widely used in the preparation of compound semiconductors, high-purity alloys, electronic refrigeration components, thermoelectric conversion Components and liquid cooling carriers in nuclear reactors, etc., the research and development of high-purity bismuth has broad prospects. With the wide application and in-depth research of high-purity bismuth in various fields, the detection of impurity element content in high-purity bismuth has been paid more and more attention. In the national standard GB / T 91521995, GFAAS and other methods are used to determine impuri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73
Inventor 彭寿马立云潘锦功殷新建陈有兰
Owner CNBM CHENGDU OPTOELECTRONICS MATERIAL
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