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Preparation method of standardized sample for X-ray fluorescence analysis

A fluorescence analysis and production method technology, which is applied in the preparation of test samples, material analysis by using wave/particle radiation, material analysis, etc., can solve problems affecting the accuracy of element content determination by X-ray fluorescence method, and achieve flexible formula , Strong pertinence, guaranteed accuracy and stability

Inactive Publication Date: 2015-06-03
SHANGHAI BAOSTEEL IND TECHNOLOGICAL SERVICE
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Problems solved by technology

In actual use of the calibration sample, it is difficult to distinguish whether the abnormal analysis value of the standard sample is due to the deterioration of the standardized sample or the offset of the calibration curve, or other uncertain factors, which affect the accuracy of the determination of the element content of the X-ray fluorescence method.

Method used

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Embodiment Construction

[0013] The preparation method of the standardized sample that the present invention is used for X-ray fluorescence analysis comprises the steps:

[0014] Step 1. Use a crucible to mix the elemental material and / or alloy material with a mixed flux and use high-frequency melting to centrifugally cast it in a mold to make an alloy block. The total mass of the elemental material and / or alloy material and the mixed flux is 40-60g. The mass ratio is 1:1 to 1:5, in which the elemental materials include metal titanium, metal magnesium, metal zinc, metal tin or carbon powder, and alloy materials include ferrosilicon, ferromanganese, ferrochrome, ferronickel, phosphorus Iron, ferrosulfur, ferrovanadium or ferromolybdenum;

[0015] Step 2. Grinding and polishing the surface of the alloy block, using 60-mesh corundum, silicon carbide, zirconia and any mixture thereof to grind the surface of the alloy block, the grinding depth is greater than 0.2mm; then sequentially use 180-mesh , 500-me...

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Abstract

The invention discloses a preparation method of a standardized sample for X-ray fluorescence analysis. The method comprises the following steps: carrying out high frequency melting centrifuge casting on a single substance material and / or an alloy material and a mixed flux in a mold by using a crucible to obtain an alloy piece, wherein the total mass of the simple substance material and / or the alloy material and a pure iron flux is 40-60g, a mass ratio of the simple substance material and / or the alloy material to the pure iron flux is 1:1-1:5, and metallic chromium and / or metallic nickel introduced to the mixed flux account(s) for 8-14% of the total mass of the alloy pieces; and grinding and polishing the surface of the alloy piece to obtain the mirror standardized sample. The method has the advantages of short preparation period of the standardized sample, flexible formula and low cost, and the sample prepared in the invention has strong pertinence, stable physical and chemical properties, accords with analysis precision requirements, meets daily analysis demands, and guarantees the determination accuracy and stability of the content of all elements in the X-ray fluorescence analysis.

Description

technical field [0001] The invention relates to a preparation method of a standardized sample for X-ray fluorescence analysis. Background technique [0002] Due to the influence of factors such as indoor temperature and humidity, input voltage fluctuations, or the aging of the X-ray generator and counter in the instrument, the measured value of the general X-ray fluorescence spectrometer is not a constant value, and it is gradually no longer consistent with the calibration curve. Raw X-ray intensity values ​​match, thereby affecting the accuracy of the analysis results. In order to correct the drift of the calibration curve caused by such environmental factors and equipment aging, before using the X-ray fluorescence spectrometer to determine the element content, a standardized calibration must be carried out, and the sample used for the standardized calibration is called a standardized sample. [0003] Choosing an appropriate standardized sample can avoid the error caused b...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N23/223
Inventor 董凌鸣顾卿贇刘文华郁剑
Owner SHANGHAI BAOSTEEL IND TECHNOLOGICAL SERVICE
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