Method for preparing ferrovanadium alloy fusing sample for X-ray spectrofluorimetry

A vanadium-iron alloy and fluorescence spectroscopy technology, applied in the field of analysis and detection, can solve the problems of large amount of ammonium iodide used, affecting the quality of the melting sheet, corrosion of platinum crucibles, etc., and achieves the effects of strong application value, easy operation and short sample preparation time.

Inactive Publication Date: 2012-11-14
JIANGSU SUPERVISION & INSPECTION INST FOR PROD QUALITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses a large amount of ammonium iodide, which can easily cause incomplete demolding and affect the q...

Method used

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  • Method for preparing ferrovanadium alloy fusing sample for X-ray spectrofluorimetry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 0.2000g of the ferrovanadium sample and put it into a platinum crucible, add about 1ml of deionized water to soak the sample; add 3ml of 1+1 nitric acid dropwise into the platinum crucible (be careful to avoid sample loss caused by violent reaction), and then add 1ml 1+1 sulfuric acid, heat at 60°C until the sample is completely dissolved, evaporate to dryness; weigh 1.0000g of lithium carbonate and put it in a platinum crucible, then weigh 7.0000g of lithium tetraborate to cover the surface of lithium carbonate, add dropwise 1ml of 300g / L ammonium bromide solution. Put the platinum crucible into the melting furnace, the melting temperature is 1100 ° C, the standing time before the melting process is 3 minutes, the furnace body swing time is 20 minutes, and the resting time is 2 minutes; take out the melted ferrovanadium sample, cool to room temperature, and obtain Uniform vanadium-iron alloy glass frit ( figure 1 ), meeting the determination requirements of X-ra...

Embodiment 2

[0029] Weigh 0.3000g of ferrovanadium sample into a platinum crucible, add about 1ml of deionized water to soak the sample; add 4ml of 1+1 nitric acid dropwise to the platinum crucible (be careful to avoid sample loss caused by violent reaction), and then add 1ml 1+1 sulfuric acid, heat at 80°C until the sample is completely dissolved, evaporate to dryness; weigh 1.0000g of lithium carbonate and put it in a platinum crucible, then weigh 7.0000g of lithium tetraborate to cover the surface of lithium carbonate, add dropwise 1ml of 300g / L ammonium bromide solution. Put the platinum crucible into the melting furnace, the melting temperature is 1050°C, the standing time before the melting process is 3 minutes, the furnace swing time is 20 minutes, and the resting time is 2 minutes; take out the melted ferrovanadium sample, cool to room temperature, and obtain Uniform vanadium-iron alloy glass frit meets the determination requirements of X-ray fluorescence spectrometry.

Embodiment 3

[0031] Weigh 0.2500g of ferrovanadium sample and put it into a platinum crucible, add about 1ml of deionized water to soak the sample; add 3.5ml of 1+1 nitric acid dropwise to the platinum crucible (be careful to avoid sample loss caused by violent reaction), and then add 1ml of 1+1 sulfuric acid, heat at 70°C until the sample is completely dissolved, and evaporate to dryness; weigh 1.0000g of lithium carbonate and put it in a platinum crucible, then weigh 8.0000g of lithium tetraborate to cover the surface of lithium carbonate, add dropwise 0.8ml of 300g / L ammonium bromide solution. Put the platinum crucible into the melting furnace, the melting temperature is 1050°C, the standing time before the melting process is 3 minutes, the furnace swing time is 20 minutes, and the resting time is 2 minutes; take out the melted ferrovanadium sample, cool to room temperature, and obtain Uniform vanadium-iron alloy glass frit meets the determination requirements of X-ray fluorescence spe...

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Abstract

The invention belongs to the field of an analysis and detection technology, and relates to a method for preparing a ferrovanadium alloy fusing sample for X-ray spectrofluorimetry. The method for preparing ferrovanadium alloy fusing sample provided by the invention is as follows: placing the ferrovanadium into a platinum crucible, adding a certain amount of nitric acid and sulphoric acid to dissolve the ferrovanadium in turn, and evaporating the ferrovanadium to dryness after the ferrovanadium is fully dissolved; adding an antioxidant and a fluxing agent into the platinum crucible; and placing the platinum crucible into a sample fusing furnace to fuse so as to prepare a ferrovanadium glass fuse piece for the X-ray spectrofluorimetry in the sample fusing furnace. According to the method, the platinum crucible can not be corroded, the sampling time is short, and the prepared glass fuse piece is uniform, so that the grain-size effect and the mineral effect are eliminated completely. According to the method, the operation is simple and convenient, the safety and reliability are realized, and the repeatability is good.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and relates to a vanadium-iron alloy melting sample preparation method for X-ray fluorescence spectrum analysis. Background technique [0002] Ferro-vanadium alloy is an important alloy raw material required for steelmaking production in iron and steel enterprises. At present, the traditional wet chemical analysis method is mainly used to analyze the main elements in the vanadium-iron alloy. This method is cumbersome to operate and has a long detection cycle, which cannot meet the actual needs of steelmaking production. [0003] X-ray fluorescence spectrometry has the advantages of fast analysis speed, wide determination range of element content, high precision and accuracy, and has been widely used in metallurgy and building materials and other fields. At present, there are two common sample preparation methods for X-ray fluorescence spectrometry, the tablet method and the meltin...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N23/223
Inventor 姚强朱宇宏王燕
Owner JIANGSU SUPERVISION & INSPECTION INST FOR PROD QUALITY
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