A method for analyzing arsenic in ore samples

An analysis method, ore sample technology, is applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions. It can solve problems such as the difficulty of arsenic determination, and achieve reduced reducing acidity and good accuracy. performance, precision, and improved operating conditions

Inactive Publication Date: 2011-12-28
有研资源环境技术研究院(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have high accuracy and reproducibility, but they are all used for the analysis of trace arsenic in iron ore, and it is difficult to directly apply it to the determination of arsenic in general ore samples

Method used

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  • A method for analyzing arsenic in ore samples
  • A method for analyzing arsenic in ore samples
  • A method for analyzing arsenic in ore samples

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 0.5065g of sample into a beaker, add 20ml of nitric acid and 0.5g of potassium chlorate, heat to dissolve for 10min, cool slightly, add 7.5ml of sulfuric acid, continue to heat to dissolve and evaporate to smoke of sulfur trioxide for 5 minutes, after cooling to room temperature, add 30ml of water and 0.1g of copper sulfate, boil to dissolve the salts, and cool slightly. Add 10ml hydrochloric acid, then add sodium hypophosphite to Fe 3+ The yellow color fades away completely, and an excess of 2g is added, boiled, and kept at a slight boil for 50 minutes, so that the arsenic precipitates and coagulates. Knead a small ball with absorbent cotton and stuff it in the funnel, while filling the funnel neck with water. Filter the arsenic precipitate, wash the beaker and the precipitate 4-5 times each with hydrochloric acid (1+3) solution containing sodium hypophosphite, then wash the beaker 3-4 times with 5% ammonium chloride solution, and check the filtered out with pH ...

Embodiment 2

[0019] Weigh 0.1066g of sample into a beaker, add 20ml of nitric acid and 0.5g of potassium chlorate, heat to dissolve for 10min, cool slightly, add 7.5ml of sulfuric acid, continue to heat to dissolve and evaporate to smoke of sulfur trioxide for 5 minutes, after cooling to room temperature, add 30ml of water and 0.1g of copper sulfate, boil to dissolve the salts, and cool slightly. Add 10ml hydrochloric acid, then add sodium hypophosphite to Fe 3+ The yellow color fades away completely, and an excess of 2g is added, boiled, and kept at a slight boil for 50 minutes, so that the arsenic precipitates and coagulates. Knead a small ball with absorbent cotton and stuff it in the funnel, while filling the funnel neck with water. Filter the arsenic precipitate, wash the beaker and the precipitate 4-5 times each with hydrochloric acid (1+3) solution containing sodium hypophosphite, then wash the beaker 3-4 times with 5% ammonium chloride solution, and check the filtered out with pH ...

Embodiment 3

[0021] Weigh 0.1023g of sample into a beaker, add 20ml of nitric acid and 0.5g of potassium chlorate, heat to dissolve for 10min, cool slightly, add 7.5ml of sulfuric acid, continue to heat to dissolve and evaporate to smoke of sulfur trioxide for 5 minutes, after cooling to room temperature, add 30ml of water and 0.1g of copper sulfate, boil to dissolve the salts, and cool slightly. Add 10ml hydrochloric acid, then add sodium hypophosphite to Fe 3+ The yellow color fades away completely, and an excess of 2g is added, boiled, and kept at a slight boil for 50 minutes, so that the arsenic precipitates and coagulates. Knead a small ball with absorbent cotton and stuff it in the funnel, while filling the funnel neck with water. Filter the arsenic precipitate, wash the beaker and the precipitate 4-5 times each with hydrochloric acid (1+3) solution containing sodium hypophosphite, then wash the beaker 3-4 times with 5% ammonium chloride solution, and check the filtered out with pH ...

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Abstract

The invention relates to a method for analyzing arsenic in ore samples. The steps include: adding nitric acid and potassium chlorate to a certain amount of sample, adding sulfuric acid to continue heating and dissolving and evaporating until thick smoke of sulfur trioxide is emitted for several minutes, cooling, adding water to blow Wash, heat to dissolve, add copper sulfate, add hydrochloric acid, then add sodium hypophosphite until the Fe3+ yellow color completely fades, and then overdose, boil at this reducing acidity, and keep a certain slight boiling time to make the arsenic precipitate and condense; Filter the precipitate, wash the beaker and the precipitate with hydrochloric acid solution containing sodium hypophosphite, and then wash the beaker and the precipitate with ammonium chloride solution until the pH is 5; transfer the absorbent cotton ball to the original beaker, add buffer, starch solution, accurately add iodine standard solution, and drop sodium thiosulfate standard solution until the blue color disappears, which is the end point. The method avoids the use of highly toxic reagent sodium arsenite, reduces reducing acidity, and improves operating conditions. Direct titration of excess iodine solution with sodium thiosulfate does not require repeated titration of standard solution, the result is accurate and reliable, and is more suitable for the analysis and determination of process samples.

Description

technical field [0001] The invention relates to an analysis method for arsenic in ore samples, in particular to an analysis method for measuring arsenic content in ore samples by redox titration. Background technique [0002] For the determination of arsenic in ore samples, the national standard method adopts the base phosphate titration method. This method uses the highly toxic reagent sodium arsenite, which seriously pollutes the environment. It is reduced under the acidity of hydrochloric acid (1+1), filtered, and has poor operating conditions. It is necessary to titrate the standard solution many times, which is necessary for referee analysis, and is not suitable for the determination of process samples. There are many reports on the determination of arsenic in iron ore, such as oscillographic polarography, graphite furnace atomic absorption spectrometry and X-ray fluorescence spectrometry and other instrumental analysis methods. These methods have high accuracy and rep...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/79
Inventor 屈伟宋永胜姚国成刘爽王正模
Owner 有研资源环境技术研究院(北京)有限公司
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