Synchronous analysis method of SO4<2->, SO3<2->, S2O6<2-> and S2O8<2-> in pyrolusite leaching solution

A SO32-, synchronous analysis technology, applied in the analysis of materials, material separation, measuring devices, etc., can solve the problems of difficult quantification of interfering substances, difficult simultaneous analysis, and high detection peaks, etc., to achieve small errors, fast speed, and accuracy high degree of effect

Active Publication Date: 2012-05-09
SICHUAN UNIV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current analysis methods are mostly chemical analysis methods based on distillation-iodometric method, which is not only difficult to simultaneously analyze SO 4 2- , SO 3 2- , S 2 o 6 2- , S 2 o 8 2- , and the error is large, the general error is greater than 3%
U.S. Lloyd M.Petrie, M.Emmelyn.Jakel etc. have reported using ion chromatography to analyze SO in pyrolusite leaching solution 4 2- , SO 3 2- , S 2 o 6 2- three ions, but the method used in this report is for high concentration SO 4 2- Without pretreatment measures, SO is prone to occur 4 2- The phenomenon that the detection peak is too high affects the determination, and the method does not use gradient elution, for Cl - It is difficult to meet the quantitative requirements of major interfering substances such as

Method used

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Examples

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Comparison scheme
Effect test

Embodiment 1

[0021] Use a pipette to pipette 25 mL of pyrolusite leaching solution and 5% BaCl concentration to be tested respectively. 2 Put 10mL of the solution in a collection bottle, plug it with a stopper, shake it with an oscillator at a speed of 150r / min for about 45min, and then filter it with a 0.45μm water filter micromembrane. Calculate the SO in the filter residue 4 2- content. The obtained filtrate was analyzed by IC chromatography. The chromatographic conditions are as follows: the chromatographic analysis column is AS14 anion analysis column, the guard column is AG14, the suppressor is ASRS-ULTRA, the detector is a conductivity detector, the temperature of the column and detection cell is about 28°C; the injection volume is 25 μL, and the injection The time is about 1.5min, the current is 17mA, the eluent is composed of deionized water and NaOH solution with a mass concentration of 25mol / L, the flow rate of the eluent is about 0.4ml / min, and the gradient eluent is used fo...

Embodiment 2

[0023] Use a pipette to pipette 25 mL of pyrolusite leaching solution and a mass concentration of 8% BaCl 2 Put 10mL of the solution in a collection bottle, plug it with a stopper, shake it with an oscillator at a speed of 200r / min for about 30min, and then filter it with a 0.45μm water filter micromembrane. Calculate the SO in the filter residue 4 2- content, the resulting filtrate was analyzed with an IC chromatograph. The chromatographic conditions are as follows: the chromatographic analysis column is AS14 anion analysis column, the guard column is AG14, the suppressor is ASRS-ULTRA, the detector is a conductivity detector, the column temperature and detection cell temperature are 31°C; the injection volume is 20 μL, and the injection time is It is about 1.6min, the current is 25mA, the eluent is composed of deionized water and NaOH solution with a mass concentration of 35mol / L, the flow rate of the eluent is about 0.3ml / min, and the gradient eluent is used for elution. ...

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Abstract

The invention discloses a synchronous analysis method of SO4<2->, SO3<2->, S2O6<2-> and S2O8<2-> in a pyrolusite leaching solution, which mainly comprises the steps of: separating and removing part of SO4<2-> from a sample pyrolusite leaching solution with a BaCl2 solution with the mass concentration of 5 percent to 10 percent through a titration precipitation method and then filtering; calculating the content of SO4<2-> in filtration residue; analyzing filtrate by an IC chromatographic instrument; adopting a AS14 anion analytical column which is subjected to gradient elution by leacheate prepared by ionized water and NaOH solution with the mass concentration of 15 to 50 mol / L; measuring the standard substance retention time and peak area of SO4<2->, SO3<2->, S2O6<2-> and S2O8<2-> by the IC chromatographic instrument; and comparing the retention time and peak area with the measured result of the filtrate so as to obtain the content of each sulphur-containing anion in the filtrate, and then adding with the amount of SO4<2-> obtained by calculation of the filtration residue to obtain the content of each sulphur-containing anion in the sample pyrolusite leaching solution. The adoption of the method for analyzing the content of sulphur-containing anion is characterized by fast speed, high accuracy, small error, good reproducibility and the like.

Description

technical field [0001] The invention relates to a method for analyzing and measuring sulfur-containing anions in pyrolusite leaching solution, more specifically, relates to a method for synchronously analyzing SO in pyrolusite leaching solution by ion chromatography. 4 2- , SO 3 2- , S 2 o 6 2- , S 2 o 8 2- Methods. Background technique [0002] The liquid-phase reaction between sulfur dioxide and pyrolusite is complicated, and the existing form of sulfur in the leachate contains SO 4 2- , SO 3 2- , S 2 o 6 2- , S 2 o 8 2- etc. To express the reaction kinetics of the system and obtain the engineering design parameters, it is necessary to use the SO in the leaching solution 4 2- , SO 3 2- , S 2 o 6 2- , S 2 o 8 2- Based on exact concentration. However, the current analysis methods are mostly chemical analysis methods based on distillation-iodometric method, which is not only difficult to simultaneously analyze SO 4 2- , SO 3 2- , S 2 o 6 2-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N1/34G01N30/06G01N30/28
Inventor 苏仕军丁桑岚
Owner SICHUAN UNIV
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