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Method for detecting metallic silicon impurity content by using X-ray fluorescent spectrometry

A technology of fluorescence spectroscopy and impurity content, which is applied in the field of X-ray fluorescence spectroscopy to detect the impurity content of metal silicon, can solve the problem that metal silicon is not easy to directly melt and sample, and solve the problem of low-grade metal silicon detection with high accuracy , the effect of strong applicability

Inactive Publication Date: 2010-05-12
CHEM MINERALS & METALLIC MATERIALS INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention proposes a sample preparation method of first dissolving, evaporating to dryness, and then melting the residue with a flux, which solves the problem that metal silicon is not easy to directly melt and prepare samples

Method used

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  • Method for detecting metallic silicon impurity content by using X-ray fluorescent spectrometry
  • Method for detecting metallic silicon impurity content by using X-ray fluorescent spectrometry

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Experimental program
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Effect test

preparation example Construction

[0032] (1) Preparation of test samples

[0033] (1), sample dissolution, flying silicon

[0034] ① Weigh a certain amount of sample dried at 105°C in a platinum dish, and use a dropper to moisten it with pure water; to avoid direct addition of reagents and excessive reaction with the sample, which may cause sample splashing and affect the measurement accuracy.

[0035] ② According to the sample size, add hydrofluoric acid in a ratio of 1:20 to 1:40, and add 1:1 nitric acid in a ratio of 1:2 to 1:4 according to the sample size (mix 1 part of pure water with 1 part of nitric acid); The sample is completely decomposed.

[0036] ③Add a few drops of 1:1 sulfuric acid (mix 1 part of purified water with 1 part of sulfuric acid) into the solution, heat it on an electric stove, and steam until 5±2ml remains.

[0037] ④Transfer the solution in the platinum dish into a platinum yellow crucible, place it on an electric furnace, heat it and evaporate it to dryness, then put it in a muffl...

Embodiment

[0064] (1), the preparation of the test sample:

[0065] Weigh 1.0000g metal silicon sample which has been dried at 105°C in a platinum dish, add 6 drops of pure water to wet it with a dropper, so as to avoid direct addition of reagents and sample reaction too violently and cause sample splashing to affect measurement accuracy, add 20mL For hydrofluoric acid, add 2 mL of 1:1 nitric acid (1 part of pure water mixed with 1 part of nitric acid) drop by drop with a pipette to completely decompose the sample. Add two drops of 1:1 sulfuric acid (mixed with 1 part of pure water and 1 part of sulfuric acid) into the solution, heat and steam on an electric furnace until 5±2ml remains, transfer the solution in the platinum dish into a platinum yellow crucible, heat and steam on the electric furnace Dry it, then put it into a 500°C muffle furnace to emit white smoke, take it out and cool it.

[0066] Weigh 6.0000g of lithium tetraborate and 0.3000g of ammonium iodide in a platinum yello...

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Abstract

The invention relates to a method for detecting the metallic silicon impurity content by using an X-ray fluorescent spectrometry, which comprises the following steps: 1, preparation of a test sample wafer, which comprises the steps of (1), dissolving a sample and flying silicon and (2) performing melting to prepare the sample; 2, preparation of a standard sample wafer, which is performed according to the preparation steps of the test sample wafer after a standard solution of impurity elements to be tested is added; 3, establishment of a working curve for the X-ray fluorescent spectrometry, namely establishing the working curve for the X-ray fluorescent spectrometry by using the prepared standard sample wafer; and 4, measurement, namely putting the prepared sample wafer into an X-ray fluorescence spectrometer, performing the measurement by using the established working curve, and automatically calculating the content of each impurity element in the sample after the detection by the X-ray fluorescence spectrometer. The method solves the problems that metallic silicon is difficult to be melted directly to prepare the sample. Through experimental textual researches, the method has high accuracy and achieves the measurement of a plurality of elements. The method has a wide measurement range, not only meets the requirements of detecting over 97.5 percent metallic silicon but also solves the problems of detecting low-grade metallic silicon, and has strong applicability.

Description

technical field [0001] The invention relates to a method for detecting the content of metal impurities, in particular to a method for detecting the content of metal silicon impurities by using X-ray fluorescence spectrometry. Background technique [0002] X-ray fluorescence spectrometry is a modern general analysis method for elemental analysis of various materials. It is widely used in environmental protection, geology, metallurgy, cement, inspection and quarantine and other departments. Good sex and other characteristics. The application of X-ray fluorescence spectrometer is mainly for quantitative analysis, and the content of each element in the sample can be obtained by measuring the prepared sample. The preparation of samples is mainly two kinds of sample preparation by molten glass method and pressing. The quality of sample preparation directly affects the accuracy of measurement results. [0003] Inspection and quarantine departments, customs, scientific research un...

Claims

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Application Information

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IPC IPC(8): G01N23/223G01N1/28G01N1/44
Inventor 谷松海宋义魏红兵陈焱郭芬潘宏伟魏伟
Owner CHEM MINERALS & METALLIC MATERIALS INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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