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Method for online monitoring metal ion concentration in anodic dissolution process in real time

A technology of metal ion concentration and anode dissolution, which is applied in the field of real-time online monitoring of metal ion concentration in the process of anode dissolution, molten salt electrolytic refining, and spent fuel dry reprocessing. It can solve the problems of long test time and reduce radiation and other hazards. , good accuracy and high sensitivity

Inactive Publication Date: 2019-04-05
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, to know the reaction progress of the anode dissolution process, the ion concentration must be monitored at a certain moment, but the traditional analysis method requires sampling and analysis, and the test time is long

Method used

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  • Method for online monitoring metal ion concentration in anodic dissolution process in real time
  • Method for online monitoring metal ion concentration in anodic dissolution process in real time
  • Method for online monitoring metal ion concentration in anodic dissolution process in real time

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Example 1: At 450°C, LiCl-KCl (mass ratio of 45:38wt.%) was used as the electrolyte system, and Bi-RE (9.7wt.%)-Li (2.4wt.%) alloy was used as the working electrode (electrode Area 1.53cm 2), the spectrally pure graphite rod is the auxiliary electrode, Ag / AgCl is the reference electrode, and the anodic dissolution is performed at the potential of -0.5V (Vs Ag / AgCl), and the anode dissolution is temporarily stopped every 10 minutes, and the working electrode is replaced by a tungsten electrode The other electrodes remain unchanged, and the square wave voltammetry is used for online testing to obtain the current intensities of different anode dissolution times. According to the curve, it can be seen that RE was detected in the first 70 minutes 3+ After 80 minutes, the reduction signals of Bi-Li and Bi-RE alloys were detected. Compared with the standard concentration working curve, the dissolved ion concentration range was 0.14-3.55wt%.

Embodiment 2

[0035] Example 2: At 500°C, with LiCl-KCl (mass ratio of 45:38wt.%) as the electrolyte system, with Bi-RE (9.7wt.%)-Li (2.4wt.%) alloy as the working electrode (electrode Area 1.53cm 2 ), the spectrally pure graphite rod is the auxiliary electrode, Ag / AgCl is the reference electrode, and the anodic dissolution is performed at the potential of -1.0V (Vs Ag / AgCl), and the anode dissolution is temporarily stopped every 10min, and the working electrode is replaced with a tungsten electrode. The other electrodes remain unchanged, and the square wave voltammetry is used for online testing to obtain the current intensities of different anode dissolution times. According to the curve, only RE was detected in the first 50 minutes 3+ The reduction signal of the Bi-Li alloy was detected at 60 minutes, and the reduction signal of the Bi-RE alloy was detected after 110 minutes. Compared with the standard concentration working curve, the dissolved ion concentration range was 0.138-3.8wt%. ...

Embodiment 3

[0036] Example 3: At 600°C, with LiCl-KCl (mass ratio of 45:38wt.%) as the electrolyte system, with Bi-RE (9.7wt.%)-Li (2.4wt.%) alloy as the working electrode (electrode Area 1.53cm 2 ), the spectrally pure graphite rod is the auxiliary electrode, Ag / AgCl is the reference electrode, and the anodic dissolution is performed at the potential of -1.3V (Vs Ag / AgCl), and the anode dissolution is temporarily stopped every 10min, and the working electrode is replaced by a W electrode. The other electrodes remain unchanged, and square wave voltammetry is used for online testing to obtain current intensities at different anode dissolution times. According to the curve, only RE was detected in the first 40min 3+ The reduction signal of the Bi-Li alloy was detected at 50 minutes, and the reduction signal of the Bi-RE alloy was not detected. Compared with the standard concentration working curve, the dissolved ion concentration range was 0.135-4.1wt%.

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Abstract

The invention provides a method for online monitoring metal ion concentration in anodic dissolution process in real time. The rare earth alloy is used as a studied electrode, and the real-time monitoring is performed on the anodic dissolution process of the rare earth alloy in the fused salt by using an electrochemical method; the method comprises the following steps: (1) treating tungsten wire; (2) performing pre-electrolysis; (3) performing anodic dissolution; and (4) performing online monitoring; the concentration range of the monitored ion is 0.13-4.4wt%, the experimental temperature is 450-700 DEG C, and the monitoring range of the method disclosed by the invention is wider in comparison with the 0.14-3.5wt% of the Masatoshi Iizuka and like people; the online test is performed by adopting the square wave voltammetry, the sensitivity is high, and the accuracy is good; the progress of online monitoring the alloy dissolution in real time can be realized, the sampling is unnecessary,the harm on the human body by the sample is avoided, and the working efficiency is improved; the method provided by the invention is free from sampling, the operation step is simplified, and the working efficiency of an analysis worker is improved.

Description

technical field [0001] The invention relates to a method for metal ion concentration, in particular to a method for real-time on-line monitoring of metal ion concentration in the anode dissolution process, which belongs to molten salt electrolytic refining and spent fuel dry aftertreatment. Background technique [0002] Anode dissolution is the first step in electrolytic refining technology, which can replace the front-end chemical dissolution process of traditional spent fuel reprocessing. Anodic dissolution refers to the electrochemical dissolution process of metals after passing an external current / voltage. The advantage is that no chemical reagent is used as the oxidizing agent but electrons are used as the oxidizing agent, the process is simple, and both the potential and the current can be controlled during the anode dissolution process. Because the dissolution rate of anodic oxidation is proportional to the magnitude of the passing current, controlling the current me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/48
CPCG01N27/48
Inventor 韩伟王珊珊李梅汪文娟张密林
Owner HARBIN ENG UNIV
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