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Method for efficiently detecting content of trace germanium ions and application of method in germanium ore metallurgy

A technology of ion content and ion, applied in the metallurgy of germanium ore, in the field of high-efficiency detection of germanium ion content in trace amounts, can solve problems such as unsatisfactory repeatability, low sensitivity, and high cost, and achieve improved detection sensitivity, high sensitivity, and easy operation easy effect

Pending Publication Date: 2022-02-01
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above defects or improvement needs of the prior art, the purpose of the present invention is to provide a method for highly efficient detection of germanium ion content in trace amounts and its application in germanium ore metallurgy. Based on the glassy carbon electrode modified by bismuth film, the electrochemical method is used to The detection of germanium ion content is realized, especially the sensitive detection of trace germanium ions, and the detection linear range is 1.0×10 -4 ~1.0×10 -2 μmol / L, the detection limit can reach 1.0×10 -5 μmol / L; The method for detecting germanium ion content in a trace amount in the present invention is especially applicable to germanium ore metallurgy, and can effectively solve the problem of high cost and sensitivity of the detection method for germanium content in some specific samples (especially microorganisms) in the prior art. Low, large interference, unsatisfactory repeatability and other issues

Method used

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  • Method for efficiently detecting content of trace germanium ions and application of method in germanium ore metallurgy
  • Method for efficiently detecting content of trace germanium ions and application of method in germanium ore metallurgy
  • Method for efficiently detecting content of trace germanium ions and application of method in germanium ore metallurgy

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Experimental program
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Embodiment 1

[0043] Electrode pretreatment: 1.0, 0.3 and 0.05 μm Al for bare glassy carbon electrodes, respectively 2 o 3 Powder polishing, followed by ultrasonic cleaning in ultrapure water, ethanol, and ultrapure water for 3 min, and then air-dried. Take an appropriate amount of germanium ion standard solution and bismuth ion standard solution, and use 0.1mol / L acetic acid-sodium acetate buffer solution (pH 4.5) to settle to 10mL to make the solution to be tested, so that Bi in the solution to be tested 3+ The ion concentration is 30 μg / L, insert the three-electrode system into the solution to be tested, scan and record the dissolution curve of germanium ions by square wave stripping voltammetry, conduct qualitative analysis according to the stripping potential, and perform quantitative analysis according to the current of the stripping peak.

[0044] The relationship between the concentration of different germanium ion standard solutions and the current was investigated, and the concen...

Embodiment 2

[0046] In order to further investigate the influence of the concentration of bismuth ions on the detection of germanium ions in step (1), after the bare glassy carbon electrode is processed, take a certain amount of bismuth ion standard solution and germanium ion standard solution, and use 0.1mol / L acetic acid-sodium acetate buffer solution (pH4.5) to 10mL, so that the germanium ion concentration in the solution to be tested is fixed at 0.1μmol / L, the bismuth ion concentration is 10, 20, 30, 40, 50μg / L respectively, the fixed deposition time is 540s, and the deposition potential It is -1.3V, according to the method described in Example 1, stripping voltammetry is measured.

[0047] The result is as figure 2 shown. The germanium ion peak current measured by square wave voltammetry showed a trend of first increasing and then decreasing with the increase of bismuth ion concentration in the range of 10-50μg / L. When the concentration of bismuth ions is 30 μg / L, the maximum peak ...

Embodiment 3

[0049] In order to investigate the influence of deposition time on the detection of germanium ions in step (2), after the glassy carbon electrode is processed, the concentration of germanium ions in the solution to be tested is fixed at 0.1 μmol / L, the concentration of bismuth ions is 10 μg / L, and the concentration of 0.1 mol / L acetic acid - Sodium acetate has a pH of 4.0. The deposition potential was fixed at -1.3V, and the deposition time was selected to be 120, 180, 240, 300, 360, 420, 480, 540 and 600s to detect germanium ions.

[0050] The result is as image 3 As shown, when the deposition time increased from 120s to 540s, the peak current of germanium ions increased significantly, and reached the peak value at 540s. When the deposition time was longer than 540s, the peak current began to decrease. When the deposition time is too short, a dense and uniform bismuth film cannot be formed on the surface of the bare glassy carbon electrode, and the germanium ions cannot be ...

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Abstract

The invention belongs to the technical field of electrochemical detection methods, and discloses a trace high-efficiency germanium ion content detection method and application thereof in germanium ore metallurgy, wherein the method comprises the following steps: (1) preparing a standard solution; (2) adopting a three-electrode system, firstly carrying out electro-deposition, and then dissolving out metal by using a square wave voltammetry to obtain a standard working curve of a peak current and a germanium ion concentration value; and (3) detecting a sample to be detected to obtain a peak current aiming at germanium ions in the sample to be detected, and obtaining a germanium ion concentration value corresponding to the peak current by contrasting with the standard working curve. On the basis of the bismuth film modified glassy carbon electrode, the germanium ion content is detected by an electrochemical method, particularly the sensitive detection of trace germanium ions can be realized, the detection linear range is 1.0 * 10<-4> to 1.0 * 10<-2> mu mol / L, the detection limit can reach 1.0 * 10<-5> mu mol / L; the method can be particularly applied to germanium ore metallurgy.

Description

technical field [0001] The invention belongs to the technical field of electrochemical detection methods, and more specifically relates to a method for highly efficient detection of germanium ion content in trace amounts and its application in germanium ore metallurgy. Background technique [0002] Germanium is located in the fourth main group of the fourth cycle of the periodic table of elements. In 1886, German chemist C.A. Winkler discovered and named it germanium, which is a "silicon-like element". Germanium is a typical dispersed element in the earth's crust, and it has long been considered as an associated component of other minerals. However, with the discovery of large-scale germanium deposits in various places, such as the paragenetic germanium deposit in the Shengli coalfield in Inner Mongolia and the super-large germanium deposit in Lincang, Yunnan, it has been shown that germanium is in a certain Under certain conditions, independent ore deposits or industrial or...

Claims

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Application Information

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IPC IPC(8): G01N27/26G01N27/48
CPCG01N27/26G01N27/48
Inventor 余龙江朱圆敏陈雪敏王雨奇
Owner HUAZHONG UNIV OF SCI & TECH