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Method for rapidly detecting trace germanium in copper-cobalt-iron alloy

A detection method and ferroalloy technology, applied in the preparation of test samples, thermal excitation analysis, material excitation analysis, etc., can solve the problems of poor detection precision and accuracy, cumbersome steps, and harsh operations, and achieve environmental accuracy. , less operation steps, the effect of eliminating hazards

Inactive Publication Date: 2018-01-30
TIANJIN MAOLIAN SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First, the use of organic reagents in the process is cumbersome and time-consuming, and the organic reagents are more harmful to the human body
Second, spectrophotometry has relatively poor precision and accuracy for the detection of trace elements, and requires more stringent operations

Method used

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  • Method for rapidly detecting trace germanium in copper-cobalt-iron alloy
  • Method for rapidly detecting trace germanium in copper-cobalt-iron alloy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The present invention is a rapid detection method for trace amounts of germanium in a copper-cobalt-iron alloy, and its specific operation steps are:

[0015] Put the substance to be detected into a beaker, then take nitric acid, phosphoric acid and ammonium bifluoride and mix them according to the proportion to form a digestion system, add the mixed digestion system into the beaker, heat the digestion system after adding, at low temperature Decompose the alloy by heating; prepare a set of standard curves containing germanium, add a certain amount of copper, cobalt, and iron to the standard to match the matrix, remove the influence of interfering elements, and improve the detection accuracy; use ICP to make the standard curve, use the standard curve containing germanium The content is the abscissa, and the strength of the germanium obtained by the test is the ordinate, and the proportional relationship between the germanium content and the strength is obtained, that is, ...

Embodiment 2

[0017] see figure 1 , a copper-cobalt-iron alloy containing 10% copper, 17% cobalt, and 65-68% iron. Firstly, take 0.5g of the sample into a 500ml beaker, add a little ammonium bifluoride, phosphoric acid and nitric acid, heat and decompose it on a low-temperature electric heating plate until the solution is clear. Take it out and transfer it to a 100ml volumetric flask when it is slightly cooled, dilute to volume, and mix well.

[0018] Then configure a group of germanium standard solutions containing matrix copper 10%, cobalt 17%, and iron 65-68%, and use a plasma emission spectrometer to test the light intensity to obtain a light intensity-concentration working curve. Finally, the light intensity of the sample was tested under the same instrument settings, and the concentration of germanium in the sample checked according to the working curve was 3.4378ug / ml.

[0019] Germanium content:

[0020] W%=3.3911ug / ml*100 / 0.5*10 -4 =0.068%

[0021] Data comparison between this...

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Abstract

The present invention provides a method for rapidly detecting trace germanium in a copper-cobalt-iron alloy. The concrete operation steps comprise: placing a substance to be detected in a beaker; taking nitric acid, phosphoric acid and ammonium hydrogen fluoride, and mixing according to a certain ratio to form a digestion system; adding the obtained digestion system into the beaker; heating at a low temperature, and decomposing the alloy; preparing a matrix-matched standard curve; and detecting with inductively coupled plasma emission spectrometry (ICP-AES) to obtain the germanium content. According to the present invention, the method has advantages of low detection limit, high accuracy, wide linear range, low interference by the matrix, and the like; and with the method, the matrix matching is performed during the detection, such that the interference by the matrix is eliminated, the detection limit is low, and the accuracy is good.

Description

technical field [0001] The invention relates to the field of chemical detection of nonferrous metals, in particular to a detection method for trace amounts of germanium in copper-cobalt-iron alloys. Background technique [0002] Germanium is a contemporary high-tech new material, which plays an extremely important role in semiconductors, computers, digital communications, aerospace, agriculture, medicine and health. Germanium is very scattered, and there are almost no relatively concentrated germanium ores. Germanium is often mixed in many lead ores, copper ores, iron ores, and silver ores. Therefore, it is mostly associated with other metal minerals, and copper, lead, zinc, iron and other elements Mixed together, it is called "scattered metals". [0003] Nowadays, the detection of trace germanium mostly adopts the mixed acid system of phosphoric acid-nitric acid-ammonium bifluoride to digest, extract with carbon tetrachloride, and adopt the phenylfluorone photometric metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N1/38G01N1/44
Inventor 田桂舫刘淑媛严楼杨
Owner TIANJIN MAOLIAN SCI & TECH