Accurate determination method for lead content in white soot containing bismuth

A technology for accurate determination of white soot, applied in chemical analysis by titration method, preparation of test samples, etc., can solve problems not involving antimony and bismuth masking or elimination, achieve simple operation, improve work efficiency, and short analysis process Effect

Inactive Publication Date: 2019-04-02
CHANGCHUN GOLD RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, none of these methods involve the masking or removal of antimony and bismuth

Method used

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  • Accurate determination method for lead content in white soot containing bismuth
  • Accurate determination method for lead content in white soot containing bismuth
  • Accurate determination method for lead content in white soot containing bismuth

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] It includes the following steps:

[0045] (1) Weigh 0.27g of antimony-containing bismuth ore sample, place it in a 400ml beaker, add 0.5g of ammonium fluoride, wet with a small amount of water, add 10mL of sulfuric acid, 5mL of nitric acid, cover with a watch glass, and heat to dissolve to produce trioxide Sulfur white smoke, take it down and cool;

[0046] (2) Add 3 mL of hydrobromic acid, heat it to produce white smoke of sulfur trioxide, remove it slightly, add 3 mL of hydrobromic acid again, heat again to produce white smoke of sulfur trioxide and keep it for 2 minutes to drive off the hydrobromic acid, take Cool down

[0047] (3) Rinse the watch glass and the wall of the cup with a small amount of water, add 80 mL of water, heat and keep slightly boiling for 10 minutes, cool to room temperature, add 10 mL of absolute ethanol, and leave for more than 1 hour;

[0048] (4) Filter with a slow quantitative filter paper, wash the beaker 2 times with dilute sulfuric acid washing...

Embodiment 2

[0059] It includes the following steps:

[0060] (1) Weigh 0.29g of antimony-containing bismuth ore sample, place it in a 400ml beaker, add 0.5g of ammonium fluoride, moisten with a small amount of water, add 13mL of sulfuric acid, 5mL of nitric acid, cover with a watch glass, and heat to dissolve to produce trioxide Sulfur white smoke, take it down and cool;

[0061] (2) Add 4mL of hydrobromic acid, heat it to produce white smoke of sulfur trioxide, remove it slightly, add 4mL of hydrobromic acid again, heat again to produce white smoke of sulfur trioxide and keep it for 3 minutes to drive off the hydrobromic acid, take Cool down

[0062] (3) Rinse the watch glass and the wall of the cup with a small amount of water, add 80 mL of water, heat and keep slightly boiling for 10 minutes, cool to room temperature, add 10 mL of absolute ethanol, and leave for more than 1 hour;

[0063] (4) Filter with a slow quantitative filter paper, wash the beaker 2 times with dilute sulfuric acid washi...

Embodiment 3

[0074] It includes the following steps:

[0075] (1) Weigh 0.30g of antimony-containing bismuth ore sample, place it in a 400ml beaker, add 0.5g of ammonium fluoride, moisten with a small amount of water, add 15mL of sulfuric acid, 5mL of nitric acid, cover with a watch glass, and heat to dissolve to produce trioxide Sulfur white smoke, take it down and cool;

[0076] (2) Add 5 mL of hydrobromic acid, heat it to produce sulfur trioxide white smoke, remove it slightly, add 5 mL of hydrobromic acid again, heat again to produce sulfur trioxide white smoke and keep it for 3 minutes to drive off the hydrobromic acid, take Cool down

[0077] (3) Rinse the watch glass and the wall of the cup with a small amount of water, add 80 mL of water, heat and keep slightly boiling for 10 minutes, cool to room temperature, add 10 mL of absolute ethanol, and leave for more than 1 hour;

[0078] (4) Filter with slow quantitative filter paper, wash the beaker 2 times with dilute sulfuric acid washing sol...

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Abstract

The invention provides an accurate determination method for lead content in white soot containing bismuth, and belongs to the determination method for the lead content in the white soot. The method comprises the following steps of: dissolving a sample by using ammonium fluoride solid, nitric acid, sulfuric acid and hydrobromic acid, forming lead sulfate precipitate in the sulfuric acid medium, filtering and separating from most coexisting elements; dissolving the lead sulfate precipitate in acetic acid-sodium acetate buffer solution; using xylenol orange solution as an indicator when the pH value is adjusted from 1.40 to 1.60 with nitric acid; performing complexation titration with a Na2EDTA titration solution which does not complex with lead to remove bismuth; and adjusting the pH to 5.40to 5.60 with ammonia water and titrating with a Na2EDTA standard titration solution; and calculating the lead content according to the consumed volume of the Na2EDTA standard titration solution. Theadvantage is that: the addition of hydrobromic acid can effectively remove the interference of arsenic, selenium and antimony in the sample; the pH is adjusted, the interference of the bismuth can beeliminated by the titration with the dilute Na2EDTA standard solution at a pH of 1.40 to 1.60; the analysis process is short, the operation is simple, and the work efficiency is effectively improved.

Description

Technical field [0001] The invention relates to the field of methods for measuring lead content in white soot, in particular to an accurate method for measuring lead in white soot containing antimony and bismuth. Background technique [0002] There are currently multiple standards that can determine the amount of lead in ore. For example, GB / T 7739.5-2007 "Methods for chemical analysis of gold concentrates Part V: Determination of lead content", GB / T 20899.5-2007 "Methods for chemical analysis of gold ore Part V: Determination of lead content", YS / T 445.7 -2001 "Silver Concentrate Chemical Analysis Method for Lead Determination". However, none of these methods involves the masking or elimination of antimony and bismuth. [0003] Therefore, it is necessary to seek a suitable analytical method to completely dissolve the white soot containing antimony and bismuth, and eliminate the interference of antimony and bismuth, so as to accurately determine the lead content in the white soot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16G01N1/34G01N1/44G01N1/28
CPCG01N1/28G01N1/34G01N1/44G01N31/16
Inventor 穆岩赵亚明陈永红洪博葛仲义
Owner CHANGCHUN GOLD RES INST
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