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Method for determining germanium content of cobalt-nickel slag by atomic fluorescence spectrometry

A technology of atomic fluorescence spectroscopy and atomic fluorescence, which is applied in the field of metallurgical industry analysis, can solve the problems of large interference of analysis results and low accuracy of detection results, and achieve the effects of low environmental requirements, fast measurement and high precision

Inactive Publication Date: 2014-05-07
BAIYIN NONFERROUS GROUP
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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for measuring germanium content in cobalt-nickel slag by atomic fluorescence spectrometry, which can quickly and accurately detect the germanium content in cobalt-nickel slag, an intermediate product of hydrometallurgy operation, to solve the existing detection method The matrix zinc in the sample greatly interferes with the analysis results, resulting in low accuracy of the test results

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  • Method for determining germanium content of cobalt-nickel slag by atomic fluorescence spectrometry

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Embodiment 1

[0035] A method for measuring germanium content in cobalt-nickel slag by atomic fluorescence spectrometry, comprising the following steps:

[0036] (1) Preparation of germanium stock solution: Accurately weigh 1.0000g of metal germanium and place it in a beaker with a volume of 100 mL, add 1 mL of 30% H 2 o 2 , 1 mL of ammonia water with a density of 0.9g / mL, 20 mL of high-purity water, heated and dissolved in a boiling water bath, cooled to room temperature, and transferred to a volumetric flask with a volume of 1000 mL, diluted to the mark with high-purity water, and shaken well, the germanium in the obtained germanium stock solution The content is 1mg / mL;

[0037] (2) Pipette the germanium stock solution to prepare a germanium standard solution: pipette the germanium stock solution and dilute step by step according to the volume relationship of 10 times, dilute to the scale of the container with a phosphoric acid solution with a volume ratio of 5%, shake well, and obtain ...

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Abstract

The invention belongs to the technical field of metallurgical industry analysis and discloses a method for determining germanium content of a cobalt-nickel slag by atomic fluorescence spectrometry. The method comprises the following steps: preparing a germanium standard solution, a zinc standard solution and a thiourea-ascorbic acid mixed solution, and drawing a germanium standard solution curve; weighing a cobalt-nickel slag sample to prepare a sample solution; determining the fluorescence intensity of germanium in the sample by using an atomic fluorescence spectrometer; and comparing with the germanium standard solution curve and analyzing the content of the germanium in the sample solution. According to the method, after the approximate equal amount of zinc is added into the germanium standard solution, the germanium standard curve is drawn to eliminate the inferences to a detection result by the base body zinc. The method disclosed by the invention has the characteristics of low detection limit, wide linear range, low maintenance cost, rapidness in measurement, simplicity in operation, good accuracy, high precision, capability of simultaneously and rapidly determining elements to be detected and the like; furthermore, the method has the characteristics of few needed reagents, low cost and high automation degree, is suitable for analyzing a large batch of samples and has a very good industrial utilization value.

Description

technical field [0001] The invention belongs to the technical field of metallurgical industry analysis, and specifically relates to a method for determining germanium content in cobalt-nickel slag by atomic fluorescence spectrometry in a zinc hydrometallurgy process. Background technique [0002] Germanium is a rare element, there is no ore for industrial mining, and it accounts for 7.0×10 mass in the earth's crust -4 , Contains a small amount in coal, silver, tin, zinc, copper and other ores. Modern industrial production is mainly recovered from zinc sulfide ore, coal and metallurgical waste or flue dust. The highest concentration in the earth's crust is only 7ppm, and it often coexists with zinc and silver. Cobalt-nickel slag, the intermediate product of zinc hydrometallurgy, is the purified slag of zinc sulfide ore hydrometallurgy, and is one of the intermediate products with the highest germanium content according to the general survey. Accurately analyzing the conten...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64G01N1/28G01N1/38
Inventor 吕彦玲陈化玲马得莉张金霞孙海霞孙雁南叶小琴
Owner BAIYIN NONFERROUS GROUP
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