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Method for analyzing arsenic in ore sample

An analysis method and technology of ore samples, which are applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions, can solve problems such as difficulties in arsenic determination, reduce reducing acidity, and improve operations. Conditions, Effects of Good Accuracy and Precision

Inactive Publication Date: 2010-06-09
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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  • Method for analyzing arsenic in ore sample
  • Method for analyzing arsenic in ore sample
  • Method for analyzing arsenic in ore sample

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 an ore sample, comprising the following steps of: adding nitric acid and potassium chlorate in a certain amount of sample; adding sulphuric acid heating, dissolving and evaporating until sulfur trioxide smother smokes for a few minutes, cooling and adding water and blowing and washing; heating and dissolving; adding copper sulfate and hydrochloric acid; then adding sodium hypophosphite until the yellow of Fe3<+> completely fades; excessively adding and boiling under the reducing acidity and keeping for a certain micro boiling time to enable the arsenic to settle and agglomerate; settling and filtering the arsenic; washing a beaker and the sedimentation by using a hydrochloric acid solution containing sodium hypophosphite; washing the beaker and the sedimentation by using an ammonium chloride solution until the pH value is 5; transferring a degreasing cotton wool to an original beaker; adding a buffer solution and a starch solution into the beaker; accurately adding an iodine standard liquid; and dropping a sodium thiosulfate standard liquid to blue until the blue color disappears, i.e. an end point is achieved. The method avoids the use of a rank poison of sodium arsenite, reduces the reducing acidity and improves the operation conditions. The invention can be directly used for titrating an excessive iodine solution with sodium thiosulfate without repeatedly titrating the standard liquid for multiple times, can obtain accurate and reliable result and is more applicable for analysis and measurement of a flow sample.

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 Applications(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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