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Method for measuring content of alloy elements in ferrosilicon and silicon-aluminum-barium-calcium by X-ray fluorescent spectrometry

A technology of ray fluorescence spectroscopy and silicon aluminum barium calcium, which is applied in the field of physical and chemical detection, can solve problems such as corrosion, achieve good accuracy, good promotion and application prospects, and eliminate the effect of corroding platinum crucibles

Inactive Publication Date: 2015-04-29
HBIS COMPANY LIMITED HANDAN BRANCH COMPANY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The invention provides a method for measuring alloy element content in ferrosilicon and silicon-aluminum-barium-calcium by X-ray fluorescence spectrometry. By changing the pre-oxidation container and selecting a reasonable ratio of mixed flux and other measures, it can completely solve the problem of ferrosilicon, silicon-aluminum-barium-calcium The problem of corroding the crucible during the melting sample preparation process, and at the same time solved the problem of accurate analysis and determination of alloy element content by X-ray fluorescence spectroscopy for ferrosilicon and silicon aluminum barium calcium

Method used

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  • Method for measuring content of alloy elements in ferrosilicon and silicon-aluminum-barium-calcium by X-ray fluorescent spectrometry
  • Method for measuring content of alloy elements in ferrosilicon and silicon-aluminum-barium-calcium by X-ray fluorescent spectrometry
  • Method for measuring content of alloy elements in ferrosilicon and silicon-aluminum-barium-calcium by X-ray fluorescent spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1: adopt the inventive method to measure the content of silicon, manganese, phosphorus, aluminum, chromium in ferrosilicon:

[0015] Take by weight unit the ferrosilicon standard sample and sample 0.15g whose particle size is less than 0.125 mm, potassium nitrate, boric acid, anhydrous sodium carbonate mixed according to the weight ratio of 1:2:3 mixed flux 4.0g; test procedure is : (1) Oxidative melting of the sample: mix the ferrosilicon standard sample and the sample with the mixed flux, wrap it with quantitative filter paper, put it into a 50ml porcelain crucible nest filled with graphite carbon powder with a purity of 99.85%, and heat it at 800°C Burn in a muffler furnace for 25 minutes, take it out and cool it; (2) Melt the sample: weigh 6.0 g of anhydrous lithium tetraborate in a clean platinum crucible, add 0.2 g of ammonium iodide solid, mix with Tweezers put the iron alloy oxidized pellets in the graphite carbon powder into the platinum crucible, me...

Embodiment 2～3

[0029] Embodiment 2~3: adopt the inventive method to measure the content of silicon, manganese, phosphorus, aluminum, chromium in ferrosilicon:

[0030] The test steps (1) to (2) are the same as in Example 1. The weights of samples and standard samples and the selection of parameters during the test are shown in Table 5 below, and other parameters are the same as in Example 1;

[0031] Table 5 Sample melting conditions

[0032]

[0033] (3) Draw the working curve: select 15 ferrosilicon standard samples same as those in Example 1 to make glass frits, and the numbers and contents of the standard samples are shown in Table 1. The working curve was drawn according to the instrument measurement conditions in Table 2, and a curve with better linearity was obtained. The correlation coefficient of the working curve is shown in Table 6.

[0034] Table 6 Correlation coefficients of working curves under different conditions

[0035]

[0036] (4) Determine the content of silicon...

Embodiment 4

[0047] Embodiment 4, adopt the inventive method to measure the content of silicon, aluminum, barium, calcium in silicon aluminum barium calcium:

[0048]Weigh silicon aluminum barium calcium standard sample and sample 0.15g with particle size less than 0.125 mm by weight unit, potassium nitrate, boric acid, anhydrous sodium carbonate mixed according to the weight ratio of 1:2:3 mixed flux 4.0g; test The steps are: (1) Oxidation and melting of the sample: mix the silicon aluminum barium calcium standard sample and the sample with the mixed flux, wrap it with quantitative filter paper, and put it into a 50ml porcelain crucible nest filled with graphite carbon powder with a purity of 99.85% , burn in a muffler furnace at 800°C for 25 minutes, take it out and cool it; (2) Sample melting production: Weigh 6.0 g of anhydrous lithium tetraborate in a clean platinum crucible according to the weight unit, add 0.2 g of ammonium iodide solid Mix well, use tweezers to put iron alloy oxidi...

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Abstract

The invention discloses a method for measuring the content of alloy elements in ferrosilicon and silicon-aluminum-barium-calcium by X-ray fluorescent spectrometry, belongs to the technical field of physicochemical detection, and aims to solve the technical problem of corrosion of a platinum crucible during a sample melting manufacturing process. According to the technical scheme, the method comprises four steps: (1) oxidizing and melting a sample; (2) melting and manufacturing a sample piece; (3) drawing a working curve; (4) measuring the content of the alloy elements in the sample, wherein a sample oxidizing and melting container is a ceramic crucible which is filled with graphite carbon powder being higher than or equal to 99.85 percent in purity; a mixed flux is formed by mixing potassium nitrate, boracic acid and anhydrous sodium carbonate in the weight ratio of 1:2:3. According to the method, the possibility of the corrosion of the platinum crucible during the sample melting process is eliminated thoroughly by selecting the oxidizing container and the mixed flux; the problem about accurately analyzing and measuring the content of the alloy elements in the ferrosilicon and the silicon-aluminum-barium-calcium by the X-ray fluorescent spectrometry is solved by controlling an oxidizing agent, the melting temperature and the time and optimizing the weight the weighed sample and various reagents; therefore, the method has a good popularization prospect.

Description

technical field [0001] The invention relates to an analysis method for determining the content of primary and secondary elements silicon, manganese, phosphorus, aluminum, chromium and silicon, aluminum, barium, and calcium in silicon, aluminum, barium, and calcium by using X-ray fluorescence spectroscopy, which belongs to physical and chemical detection technology field. Background technique [0002] X-ray fluorescence spectroscopy has been widely used in the field of metallurgical chemical analysis and determination. The particle size effect and mineral effect of the sample can be eliminated by melting samples, and the analysis results are stable and accurate. Compared with traditional wet chemical analysis, X-ray fluorescence spectroscopy The advantages are very obvious, fast, accurate, easy to operate, and less environmental pollution. Because there are a lot of metal elements in iron alloy, they will form eutectic with platinum at high temperature and corrode the platin...

Claims

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Application Information

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IPC IPC(8): G01N23/223
Inventor 鲍希波冯超杜彩霞闫文喜殷雪霞左丽峰李才红石毓霞卢女平
Owner HBIS COMPANY LIMITED HANDAN BRANCH COMPANY
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