Method for determining rhenium in smelted waste acid by employing complexing separation of tartaric acid hydrogen peroxide

A hydrogen peroxide and complex separation technology, applied in the field of chemical analysis, can solve the problems of low rhenium content, matrix effect and coexisting ion interference, difficulty in direct and accurate determination of smelting foul acid rhenium, etc., so as to improve the recovery rate and improve the accuracy. and reliability effects

Active Publication Date: 2015-03-04
NORTHWEST RES INST OF MINING & METALLURGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for the determination of rhenium in smelting sewage acid by complexing and separating tartaric acid hydrogen peroxide, so as to solve the problem of low rhenium content in smelting sewage acid and the interference of matrix effect and coexisting ions in smelting sewage acid, which lead to smelting Difficult to directly and accurately measure rhenium in polluted acid

Method used

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  • Method for determining rhenium in smelted waste acid by employing complexing separation of tartaric acid hydrogen peroxide
  • Method for determining rhenium in smelted waste acid by employing complexing separation of tartaric acid hydrogen peroxide
  • Method for determining rhenium in smelted waste acid by employing complexing separation of tartaric acid hydrogen peroxide

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Step 1. Accurately pipette 5mL of a smelting acid solution into a 100mL beaker, add 5mL tartaric acid solution (mass volume concentration: 500g / L), shake well, and adjust the solution with sodium hydroxide solution (mass volume concentration: 600g / L) pH to weakly alkaline (pH=8-9), shake well, slowly add 5mL hydrogen peroxide solution (commercially available, 30% by volume), shake well, heat on an electric heating plate until excess peroxide Hydrogen decomposition is complete (no small bubbles are generated), add 10mL sodium hydroxide solution (mass volume concentration: 600g / L) and shake to dissolve the salts. After cooling, transfer the solution to a 60mL separatory funnel and flush to 30mL.

[0021] Step 2. Add 10 mL of acetone for extraction and shake for 3 minutes. After the solution is separated, keep the organic phase, then extract the water phase with 10 mL of acetone and shake for 3 minutes. After the solution is separated, combine the organic phase and discard ...

Embodiment 2

[0025] Step 1. Accurately pipette 20mL of a copper smelting dirty acid solution into a 100mL beaker, add 10mL tartaric acid solution (500g / L), shake well, and adjust the pH of the solution with sodium hydroxide solution (mass volume concentration: 600g / L) to Weak and weak alkaline (pH=8-9), shake well, slowly add 1mL hydrogen peroxide solution (commercially available), shake well, heat on the electric heating plate until the excess hydrogen peroxide is completely decomposed (no small bubbles are generated), Add 10mL sodium hydroxide solution (mass volume concentration: 600g / L) and shake to dissolve the salts. After cooling, transfer the solution to a 60mL separatory funnel and flush to 30mL.

[0026] Step 2. Add 10mL of acetone for extraction, shake for 2min, keep the organic phase after the solution is separated, then extract the water phase with 10mL of acetone, shake for 2min, after the solution is separated, combine the organic phase, discard the water phase; use 20mL Sodi...

Embodiment 3

[0030] Step 1. Accurately pipette 10mL of a certain smelting acid solution into a 100mL beaker, add 8mL of tartaric acid solution (500g / L), shake well, and adjust the pH of the solution to weak with sodium hydroxide solution (mass volume concentration: 600g / L) Alkaline (PH=8-9), shake well, slowly add 3mL hydrogen peroxide solution (commercially available, 30% by volume), shake well, heat on the electric heating plate until the excess hydrogen peroxide is completely decomposed ( No small bubbles), add 10mL sodium hydroxide solution (mass volume concentration: 600g / L) and shake to dissolve the salts, transfer the solution to a 60mL separatory funnel after cooling, and flush to 30mL.

[0031] Step 2. Add 10 mL of acetone for extraction and shake for 3 minutes. After the solution is separated, keep the organic phase, then extract the water phase with 10 mL of acetone and shake for 3 minutes. After the solution is separated, combine the organic phase and discard the water phase; us...

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Abstract

The invention discloses a method for determining rhenium in a smelted waste acid by employing complexing separation of tartaric acid hydrogen peroxide, which aims at solving the problem that rhenium in the smelted waste acid is difficult to accurately determine due to the matrix effect of the smelted waste acid and the interference of coexisting ions in determination of low-content rhenium in the smelted waste acid. Tartaric acid is adopted as a compelxing agent to complex impurity ions in the smelted waste acid; a smelted waste acid solution is adjusted to be in alkalescence; rhenium in the smelted waste acid is oxidized to be in the highest valance state (only rhenium with the highest valence state can be extracted by acetone under the listed conditions) by hydrogen peroxide as an oxidant; and rhenium is separated from the impurity ions and a sulfuric acid matrix in the smelted waste acid by employing acetone extraction under the condition of a strong base, so that the extraction rate of rhenium is improved; the influences on determination caused by impurity element ions and the sulfuric acid matrix in the determination process are removed; and the accuracy and the reliability of the analysis result are improved.

Description

technical field [0001] The invention belongs to chemical analysis technology, in particular to a method for analyzing and testing rhenium in smelting sewage acid. Background technique [0002] Rhenium belongs to scattered metals, and its content in the earth's crust is about 0.001×10 -4 %, in nature, rhenium is mainly distributed in molybdenite, rare earth ore and niobium tantalum ore, and the content is very low. In molybdenite may be rhenium disulfide ReS 2 Or rhenium heptasulfide Re 2 S 7 The form exists, the content is slightly higher. Pure rhenium is soft and has good mechanical properties. It is a metal with a high melting point. It is used to make electric filaments, shells of artificial satellites and rockets, and protective plates for atomic reactors. It is also used as a catalyst in the chemical industry. [0003] By consulting the literature, there are many relevant literature reports on the determination of rhenium in solid samples, but there are no literatu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/71G01N1/34
Inventor 郑省政王同敏赵海军王红燕方彦霞路军兵齐白羽张彦翠展之旺
Owner NORTHWEST RES INST OF MINING & METALLURGY INST
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