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Spectrophotometric method for measuring concentration of perrhenate in aqueous solution simply and conveniently

A spectrophotometry, perrhenate technology, applied in the field of analysis and detection, can solve the problems of high concentration of hydrochloric acid medium, strong toxicity of thiocyanate, complicated operation, etc., to save costs, increase experimental safety, and reduce costs. Effect

Inactive Publication Date: 2016-03-02
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The existing spectrophotometric color reagents for measuring rhenium are mainly sulfur-containing reagents and organic reagents containing oxime groups. The sulfur-containing reagents are mainly thiocyanate. Reagents (such as: lipids and ketones) are used as extraction agents, and the operation is cumbersome, and thiocyanate is highly toxic; in the process of photometric measurement of rhenium with existing oxime organic reagents, the aqueous solution needs to be neutralized to neutral, hydrochloric acid High medium concentration and large dosage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] First prepare 2.5mol / L hydrochloric acid solution, 0.01mol / L dimethylglyoxime solution, and 0.5mol / L stannous chloride solution. Take 1mL of the aqueous solution containing perrhenate in a volumetric flask, and the pH of the solution is 1; sequentially add 0.4mL of 2.5mol / L hydrochloric acid solution, 1mL of 0.01mol / L dimethylglyoxime solution and 1mL of 0.5mol / L stannous chloride solution , after standing for 15 minutes to react, then dilute to volume with deionized water, shake well, and measure the concentration of perrhenate in the aqueous solution at 450nm with a UV-visible spectrophotometer to be 20.16mg / L.

Embodiment 2

[0022] First prepare 2.5mol / L hydrochloric acid solution, 0.01mol / L dimethylglyoxime solution, and 0.5mol / L stannous chloride solution. Take 1mL of the aqueous solution containing perrhenate in a volumetric flask, the pH of the solution is 3; sequentially add 0.4mL of 2.5mol / L hydrochloric acid solution, 1mL of 0.01mol / L dimethylglyoxime solution and 1mL of 0.5mol / L stannous chloride solution , after standing for 15 minutes to react, then dilute to volume with deionized water, shake well, and measure the concentration of perrhenate in the aqueous solution at 450nm with a UV-Vis spectrophotometer to be 20.19mg / L.

Embodiment 3

[0024] First prepare 2.5mol / L hydrochloric acid solution, 0.01mol / L dimethylglyoxime solution, and 0.5mol / L stannous chloride solution. Take 1mL of the aqueous solution containing perrhenate in a volumetric flask, and the pH of the solution is 5; sequentially add 0.4mL of 2.5mol / L hydrochloric acid solution, 1mL of 0.01mol / L dimethylglyoxime solution and 1mL of 0.5mol / L stannous chloride solution , after standing for 15 minutes to react, then dilute to volume with deionized water, shake well, and measure the concentration of perrhenate in the aqueous solution at 450 nm with a UV-Vis spectrophotometer to be 20.06 mg / L.

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Abstract

The invention provides a spectrophotometric method for measuring concentration of perrhenate in an aqueous solution simply and conveniently. The spectrophotometric method is characterized in that with stannous chloride taken as a reduction agent, rhenium and dimethylglyoxime form a stable orange-yellow complex in an acid solution, the solution is diluted to reach a certain volume, and then an ultraviolet-visible spectrophotometer is used for measurement. Compared with the prior art, the detection method has the advantages that pretreatment of a sample solution is not required, operation is simple and convenient, the concentration of a hydrochloric acid medium is low, few hydrochloric acid media are consumed and the like.

Description

technical field [0001] The invention belongs to the field of analysis and detection, and in particular relates to a spectrophotometric method for simply measuring the concentration of perrhenic acid in aqueous solution. Background technique [0002] Rhenium is a strategic rare metal element. During the smelting process, most rhenium is converted to perrhenate (ReO 4 - ) form into the acidic aqueous solution, a simple analytical test method for the determination of perrhenate in aqueous solution, which is of great significance to the monitoring and control of rhenium in the production process. [0003] At present, the analysis methods of rhenium mainly include inductively coupled mass spectrometry, X-ray fluorescence spectrometry, neutron activation method and spectrophotometry. Inductively coupled bulk-mass spectrometry, X-ray fluorescence spectrometry, and neutron activation are expensive instruments, require a large investment in equipment, require high continuous operat...

Claims

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Application Information

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IPC IPC(8): G01N21/33
CPCG01N21/33
Inventor 胡晖张举斌田亚运耿桂秀姜邦强
Owner FUZHOU UNIV
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