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Method for eliminating bismuth interference in determination of lead content of mineral by EDTA (ethylenediaminetetraacetic acid) volumetric method

A lead content and volumetric method is applied in the field of eliminating bismuth interference, which can solve the problems of bismuth interference, high analysis results, and undiscovered problems, and achieves the effects of eliminating interference, simple method, and meeting the needs of production and analysis.

Inactive Publication Date: 2016-07-20
CHINA NONFERROUS METAL (GUILIN) GEOLOGY & MINING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when using the existing national standard analysis method of lead concentrate to determine the lead content of bismuth-containing lead ores and alloys, the existence of a large amount of bismuth will cause great interference. The applicant believes that this is because the basic formula formed by the partial hydrolysis of bismuth Co-precipitation of bismuth sulfate and lead sulfate occurs, so that bismuth also consumes EDTA while EDTA complexometrically titrates lead, thus making the analysis result higher
In the prior art, no relevant reports have been found to eliminate the interference of bismuth by adding 2,3-dimercaptopropanol (BAL)

Method used

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  • Method for eliminating bismuth interference in determination of lead content of mineral by EDTA (ethylenediaminetetraacetic acid) volumetric method
  • Method for eliminating bismuth interference in determination of lead content of mineral by EDTA (ethylenediaminetetraacetic acid) volumetric method
  • Method for eliminating bismuth interference in determination of lead content of mineral by EDTA (ethylenediaminetetraacetic acid) volumetric method

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Experimental program
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Effect test

Embodiment 1

[0058] Embodiment 1: standard sample analysis

[0059] Select national standard sample GBW07172, add 6mg bismuth standard respectively in each part of sample before precipitation lead, adopt method of the present invention (specifically as follows) and analyze sample by method described in GB / T8152.1-2006 respectively:

[0060] The method of the present invention: Weigh 0.20g (accurate to 0.0001g) sample and 0.006g bismuth standard in a 250mL beaker, moisten with a small amount of water, add 15mL hydrochloric acid, cover with a watch glass, heat and dissolve at 120-150°C for 5min Finally, add 5mL of nitric acid, continue to heat until the sample is completely decomposed, then add 6mL of bismuth standard solution, then add 20mL (1+1) sulfuric acid, heat until thick white smoke of sulfur trioxide is emitted, remove and cool, and rinse the surface with a small amount of water Continue to heat the dish and cup wall until smoking, then remove and cool. Then add 50mL of water to it...

Embodiment 2

[0067] Embodiment 2: standard sample analysis

[0068] Select national standard sample GBW07167, add 10mg bismuth standard respectively in each part of sample before precipitation lead, adopt respectively method described in the present invention (specifically as follows) and analyze sample by method described in GB / T8152.1-2006:

[0069] The method of the present invention: Weigh 0.10g (accurate to 0.0001g) sample and 0.010g bismuth standard in a 250mL beaker, moisten with a small amount of water, add 15mL hydrochloric acid, cover with a watch glass, heat and dissolve at 120-150°C for 5min Finally, add 5mL nitric acid, continue to heat until the sample is completely decomposed, then add 20mL (1+1) sulfuric acid, heat until thick white smoke of sulfur trioxide is emitted, remove and cool, rinse the watch glass and cup wall with a small amount of water, and continue heating until smoking, remove and cool. Then add 50mL of water to it, heat and boil to dissolve the soluble salt...

Embodiment 3

[0074] Select the sample A sent by Guilin Jinzeli Mining Co., Ltd., measure the content of bismuth in this sample through the national standard analysis method GB / T15926-2010 to be 4.68%, adopt the method of the present invention (as follows) and press GB / T8152. The method described in 1-2006 analyzes the content of lead in the sample:

[0075] The method of the present invention: Weigh 0.10g (accurate to 0.0001g) sample and 0.010g bismuth standard in a 250mL beaker, moisten with a small amount of water, add 15mL hydrochloric acid, cover with a watch glass, heat and dissolve at 120-150°C for 5min Finally, add 5mL nitric acid, continue to heat until the sample is completely decomposed, then add 20mL (1+1) sulfuric acid, heat until thick white smoke of sulfur trioxide is emitted, remove and cool, rinse the watch glass and cup wall with a small amount of water, and continue heating until smoking, remove and cool. Then add 50mL of water to it, heat and boil to dissolve the solubl...

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Abstract

The invention discloses a method for eliminating bismuth interference in the determination of lead content of a mineral by EDTA (ethylenediaminetetraacetic acid) volumetric method. The method using the mineral as a specimen includes the steps of specimen digesting, acid driving, lead sulfate precipitate forming, lead sulfate precipitate dissolving, and titrating. The method is differed from the prior art in that before titrating lead acetate solution obtained in the step of lead sulfate precipitate dissolving, 2,3-dimercaprol is added; the 2,3-dimercaprol is used to react with bismuth to generate a substance with a stability constant higher than that of Bi-EDTA, the interference due to the presence of bismuth in the determination of lead content of the mineral by EDTA volumetric method is effectively eliminated accordingly, and the method is simple and quick, has reliable results and can meet the production analytical requirement.

Description

technical field [0001] The invention relates to a non-ferrous metal analysis and testing technology, in particular to a method for eliminating bismuth interference when using EDTA volumetric method to measure lead content in minerals. Background technique [0002] Lead-containing polymetallic ores and alloys are very important raw materials in the lead smelting and processing industry. Accurate determination of lead (Pb) content in polymetallic ores and alloys is particularly important for guiding mine development and processing and production of mineral processing enterprises. There are many methods for determining lead. For lead ore (lead content ≥ 5%), the EDTA volumetric method is usually selected as the lead content analysis and determination method. However, when the existing national standard analysis method of lead concentrate is used to determine the lead content of bismuth-containing lead ores and alloys, the existence of a large amount of bismuth will cause great...

Claims

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Application Information

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IPC IPC(8): G01N31/16
CPCG01N31/16
Inventor 袁永海施意华尹昌慧徐华
Owner CHINA NONFERROUS METAL (GUILIN) GEOLOGY & MINING CO LTD
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