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Method for determining content of Al, Ca and Fe in highly pure nanometer ITO powder

A technology for the content of aluminum and iron in powder, applied in the field of determination of impurity element content, can solve the problems of long process, high detection limit, inappropriate impurity elements, etc., and achieve the effect of low detection limit, easy to grasp and high sensitivity

Inactive Publication Date: 2015-05-06
GUOBIAO BEIJING TESTING & CERTIFICATION CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Generally, DC arc atomic emission spectrometry is used to directly inject powder into samples for impurity content analysis, or inductively coupled plasma emission spectrometry is used for analysis, but these methods generally have a long process and high detection limits, and are not suitable for impurity elements in high-purity materials Analysis

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  • Method for determining content of Al, Ca and Fe in highly pure nanometer ITO powder
  • Method for determining content of Al, Ca and Fe in highly pure nanometer ITO powder
  • Method for determining content of Al, Ca and Fe in highly pure nanometer ITO powder

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Embodiment Construction

[0035] The present invention will be further described below in conjunction with specific embodiments.

[0036] The present invention uses microwave digestion to process the sample, and uses an inductively coupled plasma mass spectrometer to measure the content of Al, Ca, and Fe in high-purity nano-ITO. The test experiment of the present invention is carried out in a high-purity laboratory, and the specific steps are as follows:

[0037] 1. Sample pretreatment

[0038] Weigh 0.1g of high-purity nano-ITO sample, accurate to 0.0001g, into a polytetrafluoroethylene digestion tank, add 2mL of concentrated hydrochloric acid and 1mL of concentrated nitric acid, use microwave digestion for sample pretreatment, and do a blank test with the sample.

[0039] The temperature control procedure for microwave digestion is as follows:

[0040] In the first step, it takes 10 minutes to raise the temperature to 120°C and keep it for 10 minutes;

[0041] In step 2, heat up to 180°C in 10 minu...

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Abstract

The invention relates to a method for determining the content of Al, Ca and Fe in highly pure nanometer ITO powder. The method comprises the following steps: carrying out microwave digestion treatment on an ITO sample, and carrying out dry filtration to obtain a solution to be detected; preparing a series of standard solutions of Al, Ca and Fe, wherein the Al, Ca and Fe concentrations of the standard solutions are 0, 20ng / mL, 40ng / mL, 60ng / mL, 80ng / mL and 100ng / mL respectively; selecting working conditions of an inductively coupled plasma mass spectrometer, and selecting <27>Al, <40>Ca and <56>Fe to determine; determining to obtain the work curves of Al, Ca and Fe; and determining to obtain a signal intensity ratio Y<Al>, Y<Ca> and Y<Fe> of <27>Al, <40>Ca and <56>Fe in a blank solution and the ITO solution to be detected to an internal standard Sc element, and calculating to obtain the mass percentages of Al, Ca and Fe in the ITO sample. The method allows the detection result to be highly reliable, and can well meet the analysis of the ITO material with the content of Al, Ca and Fe of 0.0001-0.010%.

Description

technical field [0001] The invention relates to a method for determining the content of aluminum, calcium and iron in high-purity nano-ITO (nano-indium tin oxide) powder, in particular to the determination of aluminum, calcium and iron in high-purity nano-ITO by using microwave digestion to treat samples and inductively coupled plasma mass spectrometry. The invention discloses a method for the percentage content of calcium and iron impurities, belonging to the technical field of measuring the content of impurity elements. Background technique [0002] At present, there are few studies on the analysis of impurity content in high-purity nano-ITO powder. Generally, DC arc atomic emission spectrometry is used to directly inject powder into samples for impurity content analysis, or inductively coupled plasma emission spectrometry is used for analysis, but these methods generally have a long process and high detection limits, and are not suitable for impurity elements in high-puri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62G01N1/28G01N1/38G01N1/44G01N27/626
Inventor 墨淑敏
Owner GUOBIAO BEIJING TESTING & CERTIFICATION CO LTD
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