Method for measuring content of copper, cadmium, nickel and cobalt in zinc electrolyte simultaneously

A zinc electrolyte and content technology, applied in the field of analysis and testing, can solve the problems of simultaneous determination of difficult metal ions, real-time monitoring of unfavorable impurity ions, low sensitivity of spectrophotometry, etc., to achieve accurate and reliable measurement results, fast detection speed, and selective sex high effect

Active Publication Date: 2017-09-19
CENT SOUTH UNIV
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  • Abstract
  • Description
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Problems solved by technology

Among them, spectrophotometry has low sensitivity and complex operation, and generally requires pretreatment of zinc electrolyte, and it is difficult to realize the simultaneous determination of copper, cadmium, nickel and cobalt; atomic absorption method and atomic emission spectrometry, the instruments are expensive, and will be interfered by the matrix In addition, when using the existing polarographic method to measure the content of copper, cadmium, nickel and cobalt in the zinc electrolyte, because the zinc ion content in the zinc electrolyte is too high, it is easy to cause wave peaks to overlap (especially cobalt waves), and different metal ions are detected at the same time. The sensitivity of the system is different, and it is difficult to realize the simultaneous determination of various metal ions including copper, cadmium, nickel and cobalt. In practical applications, the polarographic method, which is limited to single ion detection, undoubtedly increases the detection time and workload, which is not conducive to the detection of impurities. Real-time monitoring of ions

Method used

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  • Method for measuring content of copper, cadmium, nickel and cobalt in zinc electrolyte simultaneously
  • Method for measuring content of copper, cadmium, nickel and cobalt in zinc electrolyte simultaneously
  • Method for measuring content of copper, cadmium, nickel and cobalt in zinc electrolyte simultaneously

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1Cu 2+ 、Cd 2+ 、Ni 2+ and Co 2+ Determination of the standard curve of the assay system

[0044] (1) Take Cu 2+ The standard solution was diluted with double distilled water to the appropriate concentration of Cu 2+ Standard solution; measure 1×10 -6 mol / L, 2×10 -6 mol / L, 4×10 -6 mol / L, 6×10 -6 mol / L, 8×10 -6 mol / L, 2×10 -5 mol / L, 4×10 -5 mol / L, 8×10 -5 mol / L, 1×10 -4 mol / L, 2×10 -4 mol / L, 3×10 -4 mol / L, 6×10 -4 mol / L, 8×10 -4 mol / L Cu 2+ Put 0.5mL of each standard solution in 13 10mL volumetric flasks, add 1.0mL Zn to the volumetric flasks respectively 2+ solution (2.6mol / L) and 0.15mL dimethylglyoxime ethanol solution (11g / L), shake for 3min, then add 3mL sodium citrate solution (1mol / L), 4mL sodium borate (0.15mol / L) and 1mL Sodium hydroxide solution (2mol / L), constant volume, let stand for 5min, respectively pour the solution into the electrolytic cup to measure the produced Cu 2+ The complex absorbs the polarographic wave and obtains the ...

Embodiment 2

[0048] Cu in the new solution of embodiment 2 zinc electrolysis 2+ 、Cd 2+ 、Ni 2+ and Co 2+ Determination of content

[0049] (1) Measure 1mL of the new zinc electrolyte solution and place it in a 10mL volumetric flask, add 0.15mL of ethanol solution of dimethylglyoxime, shake for 3min until uniform, then add 3mL of sodium citrate solution (1mol / L) and 4mL of boric acid in sequence Sodium (0.15mol / L), adjust its pH value to 9.4 by adding 2mol / L sodium hydroxide solution dropwise, constant volume, let stand for 5min, pour the solution into the electrolytic cup to measure the Cu produced 2+ 、Ni 2+ 、Co 2+ The adsorption polarographic wave of the complex obtained its corresponding second-order derivative peak currents were 125.2nA, 667.1nA, and 214.7nA, and the detection results were as follows Figure 5 shown, and on this basis, 6mol / L sulfuric acid was added dropwise to adjust its pH value to 4.2, and the Cd produced was measured 2+ The adsorption polarographic wave of th...

Embodiment 3

[0052] Cu in the neutral supernatant of embodiment 3 2+ 、Cd 2+ 、Ni 2+ and Co 2+ Determination of content

[0053] (1) Measure 1 mL of neutral supernatant in a 100 mL volumetric flask, and distill it to volume with double distilled water, and use this as the solution to be tested;

[0054] (2) Measure 1mL of the solution to be tested in a 10mL volumetric flask, add 0.15mL of ethanol solution of dimethylglyoxime, shake for 3min until uniform, then add 3mL of sodium citrate solution (1mol / L) and 4mL of sodium borate (0.15mol / L), adjust its pH value to 9.3 by dropping 2mol / L sodium hydroxide solution, constant volume, let stand for 5min, pour the solution into the electrolytic cup to measure the Cu produced 2+ 、Ni2+ 、Co 2+ The adsorption polarographic wave of the complex obtained its corresponding second-order derivative peak currents of 22.5nA, 53nA, and 233.1nA, respectively, and the detection results are as follows Figure 9 shown, and on this basis, 6mol / L sulfuric acid ...

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Abstract

The invention discloses a method for measuring the content of copper, cadmium, nickel and cobalt in zinc electrolyte simultaneously. The method comprises the steps as follows: a to-be-measured zinc electrolyte is reacted with a detection system composed of sodium borate, sodium citrate and dimethylglyoxime, adsorption polarographic waves of copper, cadmium, nickel and cobalt complexes are determined, and the content of copper, cadmium, nickel and cobalt is calculated based on an obtained second derivative wave crest current. According to the method, sodium borate, sodium citrate and dimethylglyoxime are adopted as the detection system, and the content of copper, cadmium, nickel and cobalt is measured simultaneously by adjustment of the pH value; the detection system can completely shelter interference of zinc ions, and pretreatment of the measured zinc electrolyte is not needed; through a standard addition method, an influence of other coexisting ions in the to-be-measured zinc electrolyte is weakened, the selectivity is high, and measurement results are accurate; adopted instruments are cheap and easy to operate; few types of reagents are used, the stability is good, price is low, no sediment is produced in a detection process, analysis speed is high, automation is easy to realize, and the method is applicable to online detection.

Description

technical field [0001] The invention relates to the technical field of analysis and testing, in particular to a method for measuring the content of copper, cadmium, cobalt and nickel in a zinc electrolyte. Background technique [0002] Zinc is the basic raw material and strategic material supporting the development of the national economy and national defense industry. At present, about 80% of zinc is produced through hydrometallurgy. For zinc hydrometallurgy, excess impurity ions not only affect the current efficiency during electrolysis, but also affect the surface morphology and cathodic polarization of deposited zinc. The impurities that have a greater impact in the process of electrodepositing zinc are mainly copper, cadmium, nickel and cobalt, so the content of these impurities in the zinc electrolyte flowing into the electrolytic cell must be strictly monitored. [0003] Zn in zinc electrolyte 2+ The content of zinc is as high as 130-170g / L, and the mass ratio of zi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/26
Inventor 阳春华杜娟张泰铭朱红求李勇刚陈俊名桂卫华
Owner CENT SOUTH UNIV
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