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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Problems solved by technology

The invention proposes a sample preparation method of first dissolving, evaporating to dryness, and then melting th

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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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Example Embodiment

[0032] (1) Preparation of test samples

[0033] (1) Sample dissolution, flying silicon

[0034] ①Weigh a certain amount of the dried sample at 105°C and place it in a platinum dish, and use a dropper to add pure water to moisten it; to avoid the direct reaction of the reagent with the sample being too violent, the sample splashing and affecting the measurement accuracy.

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

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

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

Example Embodiment

[0063] Examples:

[0064] (1) Preparation of test samples:

[0065] Weigh 1.0000g of the metal silicon sample dried at 105℃ in a platinum dish, and use a dropper to add 6 drops of pure water to wetting, to avoid the direct reaction of the reagent and the sample, causing the sample to splash and affect the measurement accuracy, add 20mL Hydrofluoric acid, 2mL 1:1 nitric acid (mixed with 1 part of pure water and 1 part of nitric acid) was added dropwise 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) to the solution, heat it on an electric furnace and steam until the remaining 5±2ml, transfer the solution in the platinum dish into a platinum yellow crucible and place it on the electric furnace for heating and steaming Dry, then put it in a 500℃ muffle furnace to emit white smoke, take it out and cool.

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

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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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