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Method for measuring ICP atomic emission spectroscopy of silver in aluminum alloy

A technique of atomic emission spectrometry and determination method, which is applied in the field of ICP atomic emission spectrometry determination of silver in aluminum alloys, can solve problems such as instability of silver ammonia complex ions, analysis errors, different storage time, etc., and achieve stable and reliable results

Inactive Publication Date: 2017-05-10
SOUTHWEST ALUMINUM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The dissolved solution has more salts, which can easily cause the instrument to turn off
And the silver ammonium ion is unstable, the storage time is different, the results are different, resulting in analysis errors

Method used

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  • Method for measuring ICP atomic emission spectroscopy of silver in aluminum alloy

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preparation example Construction

[0031] The preparation method of copper solution of the present invention is preferably specifically:

[0032] Weigh copper and mix it with nitric acid solution. After the reaction stops, heat slowly until completely dissolved, cool, and transfer to a volumetric flask.

[0033] The concentration of copper ions in the copper solution of the present invention is preferably 1-10 mg / mL; more preferably 1-8 mg / mL; most preferably 1-6 mg / mL.

[0034] The inventors creatively added copper ion solution to the dissolved aluminum alloy solution. It is precisely because copper ions and aluminum ions constitute a primary battery that the reaction rate is increased and the solubility is improved, thereby helping the determination.

[0035] In the present invention, the mass ratio of the copper ion in the copper solution to the aluminum alloy is 1:(20-30); preferably 1:(20-26); more preferably 1:(20-24); Most preferably, it is 1:(20-23).

[0036] The present invention does not limit the m...

Embodiment 1

[0053] Instrument: ACTIVA Plasma Atomic Emission Spectrometer of JY Company in France, the measurement performance requirements meet Class A. The operating software is ACTIVAnalyst5.4.

[0054] Instrument parameters: Power: 1050w Working frequency: 40.68MHZ (crystal control). The pump speed is selected as 20 rpm, the Flow carrier gas flowmeter is adjusted to 0.89ml / min, the Plasma Gas cooling gas flow rate is adjusted to 12L / min; the Sheath Gas auxiliary gas flow rate is adjusted to 2L / min.

[0055] Analysis of spectral lines: the error should be less than 0.003nm when Ag298.068nm is selected for peak-finding.

[0056] Reagent:

[0057] Aluminum (>99.9%) In this method, the purity of aluminum is not required to be high. Since the higher the purity of aluminum, the more difficult it is to dissolve, so it is required that the aluminum does not contain silver.

[0058] Nitric acid 50%, superior grade.

[0059] Copper (>99.99%).

[0060] Copper solution (10mg / mL): Weigh 10.0...

Embodiment 2

[0065] Prepare instruments and reagents according to Example 1 of the present invention, and process the sample into chips. Accurately weigh 0.2000g of the aluminum alloy sample into a 250mL beaker. Add 15mL of 50% nitric acid, dissolve on the electric heating plate at 100°C, add 10mL, 1mg / mL copper solution, and transfer the sample to a 100mL volumetric flask to volume after dissolution. Then Ag328.068 was measured on an ACTIVA ICP atomic emission spectrometer. Repeat three times and take the average value.

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Abstract

The invention provides a method for measuring ICP atomic emission spectroscopy of silver in an aluminum alloy. The method comprises the following steps of A) dissolving the aluminum alloy with nitric acid, adding a copper solution to help solubilization, and obtaining a sample, wherein the dissolution temperature is 100-120 DEG C, and the mass ratio of the copper ion in the copper solution to the aluminum alloy is 1:(20-30); and B) measuring the sample by using an ICP atomic emission spectrometer. The aluminum alloy sample is dissolved with the nitric acid, and moreover, the copper ion is added to help solubilization, and the copper ion and the aluminum ion form a primary element effect, so that dissolving the aluminum alloy with the nitric acid is promoted, and the effect of helping solubilization is exerted. Besides, dissolving at the specific temperature also plays a role in helping solubilization. No hydrochloric acid needs to be added, no silver chloride precipitate is produced, and dissolving the precipitate with a large quantity of ammonia chloride is not needed either, so that the problem of shutdown of an instrument caused by excessive salts is not caused, the copper ion does not interfere with the measurement either, and the result is stable and reliable.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to an ICP atomic emission spectrometry method for silver in aluminum alloys. Background technique [0002] Aluminum alloy is a non-ferrous metal material with a wide range of uses. As a new type of alloying element in aluminum alloy materials, silver can refine the grain and improve the performance of the material after aging strengthening. With the extension of aging time, it can suddenly Increases hardening rate. In order to ensure the specificity of aluminum alloy materials, it is necessary to control and accurately determine silver in aluminum alloys. [0003] The methods for determining silver in aluminum alloys in the prior art include methods such as flame atomic absorption spectrometry, catalytic manganese-persulfuric acid reaction system method, and the like. The catalytic manganese-persulfuric acid reaction system method has a narrow determination range, com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N1/28
CPCG01N1/28G01N21/73
Inventor 谭家英
Owner SOUTHWEST ALUMINUM GRP
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