Analysis and detection method for impurity elements in tin and tin alloy

A technology of impurity elements and detection methods, which is applied in the field of analysis and detection of impurity elements in tin and tin alloys, can solve the problems of affecting the service life of the torch and the lower limit of determination, so as to eliminate matrix interference and other chemical interference, improve sensitivity, environmental friendly effect

Inactive Publication Date: 2019-04-12
云南锡业矿冶检测中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the impurity elements have not been enriched, and the lower limit of the method is relatively high
At the same time, when the inductively coupled plasma atomic emission spectrometry is used for measurement, a large amount of tin matrix is ​​easily adsorbed on the torch in the form of tin dioxide, which affects the service life of the torch

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Analysis and detection method of impurity elements in tin and tin alloys, weigh 5.0g (accurate to 0.0001g) high-purity tin sample into a 200mL quartz beaker, add 15mL hydrochloric acid (1+1), 5mL nitric acid, and decompose completely on a temperature-controlled electric furnace at 100°C , to completely oxidize tin to tetravalent tin (IV), and evaporate to dryness, then add 2mL of hydrochloric acid (1+1), heat and evaporate to dryness on a temperature-controlled electric furnace at 100°C; add hydrochloric acid repeatedly and heat to evaporate to dryness Step 5-6 times, until the tin is basically volatilized completely, and the residual rate of the tin matrix is ​​as low as less than 2%. Then add 2mL of hydrochloric acid (1+1) and 5mL of water, heat to dissolve the sample, take it off to cool, transfer it to a 10mL volumetric flask with water, and mix well. Determination of impurity elements in tin and tin alloys, including but not limited to Ag, Al , As, Au, Bi, Ca, Cd,...

Embodiment 2

[0024] Weigh 2.0g (accurate to 0.0001g) refined tin sample into a 200mL quartz beaker, add 10mL hydrochloric acid (1+1) and 3mL nitric acid, and decompose completely on a temperature-controlled electric furnace at 120°C to completely oxidize tin to tetravalent tin, and evaporate to dryness; add 2mL of hydrochloric acid (1+1), heat and evaporate to dryness in a temperature-controlled electric furnace at 120°C, repeat this step (the step of adding hydrochloric acid and heating and evaporating to dryness) 4 to 5 times, until the tin is basically volatilized completely . Then add 5mL hydrochloric acid (1+1) and 5mL water, heat and dissolve the sample on a temperature-controlled electric furnace, remove and cool, transfer to a 25mL volumetric flask with water, mix well, and use a spectrophotometer, atomic absorption spectrometer, atomic fluorescence spectrometer Determination of impurity elements in tin and tin alloys, including but not limited to Ag, Al, As, Au, Bi, Ca, Cd, Ce , ...

Embodiment 3

[0026] Weigh 1.0g (accurate to 0.0001g) SnAg0.3Cu0.5 alloy in a 200mL quartz beaker, add 10mL hydrochloric acid (1+1) and 3mL nitric acid, and decompose completely on a temperature-controlled electric furnace at 150°C to completely oxidize tin to four tin, and evaporate to dryness; add 2mL hydrochloric acid (1+1), heat and evaporate to dryness in a temperature-controlled electric furnace at 80°C; repeat this step 4 to 5 times, until the tin is basically volatilized; add 5mL hydrochloric acid (1+1 ), 5mL water, heat and dissolve the sample on a temperature-controlled electric furnace, remove and cool, transfer to a 25mL volumetric flask with water, mix well, and use a spectrophotometer, atomic absorption spectrometer, atomic fluorescence spectrometer, inductively coupled plasma atomic emission spectrometer Determination of impurity elements in tin and tin alloys by any one of the inductively coupled plasma mass spectrometers, including but not limited to Ag, Al, As, Au, Bi, Ca, ...

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PUM

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Abstract

The invention discloses an analysis and detection method for impurity elements in tin and tin alloy. The method comprises adding a tin or tin alloy sample into a mixed solution of hydrochloric acid and nitric acid or a mixed solution of hydrochloric acid and hydrogen peroxide, performing decomposition on the tin or tin alloy sample by heating to ensure complete oxidation of tin to tetravalent tin,then adding the hydrochloric acid, heating evaporate to dryness, and repeating the steps of adding the hydrochloric acid and heating to evaporate to dryness at least 3 times until the tin is substantially completely evaporated; adding the hydrochloric acid, continuously heating to completely dissolve, moving into a volumetric flask with water after cooling, uniformly mixing, and performing constant volume; and determining the impurity elements in the solution by any one of a spectrophotometer, an atomic absorption spectrophotometer, an atomic fluorescence spectrometer, an inductively coupledplasma atomic emission spectrometry, and an inductively coupled plasma mass spectrometry to analyze and detect the impurity elements in the tin and tin alloy. The analysis and detection method for theimpurity elements in the tin and the tin alloy is simple to operate, environmentally friendly, high in sensitivity, and good in accuracy.

Description

technical field [0001] The invention belongs to the technical field of metal detection and analysis methods, and in particular relates to an analysis and detection method of impurity elements in tin and tin alloys. Background technique [0002] The determination of impurity elements in tin and tin alloys currently mainly uses spectrophotometry, flame atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry, and inductively coupled plasma mass spectrometry. In order to achieve the purpose of impurity enrichment and accurate measurement, the following methods are usually used to eliminate tin interference: [0003] 1) Hydrochloric acid - hydrobromic acid volatile tin removal method. "GB / T 3260-2013 Tin Chemical Analysis Method" mostly adopts this method. This method is the most classic tin discharge method, and its advantages are good tin discharge effect, simple and fast operation. The disadvantage is that hydrobromic acid has certain toxicit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28
CPCG01N1/28
Inventor 王骏峰解瑞松苏爱萍黄劲松赖妍洁张丽梅石如祥张振华张有才
Owner 云南锡业矿冶检测中心有限公司
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