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Melted sampling method for aluminum magnesium calcium iron alloy for X-ray fluorescence spectrum analysis

A fluorescence spectrum, aluminum-magnesium-calcium-iron technology, which is applied in the field of analysis and detection, can solve the problems of high melting temperature, strong corrosion of sample preparation vessels, infeasibility, etc., and achieves the effects of simple operation, short sample preparation time and good reproducibility.

Inactive Publication Date: 2012-01-25
HBIS COMPANY LIMITED HANDAN BRANCH COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, when the fusion method is used to analyze ferroalloys, due to the high melting temperature, the sample will cause strong corrosion to the sample preparation vessel—platinum crucible, so it is generally considered unfeasible and has become a difficult problem in the analysis field
The physical and chemical testing laboratory of Handan Iron and Steel Co., Ltd. has accumulated rich experience in the analysis of ferroalloys by melting method, as described in patents CN200910074796.4 and CN201010111253.8. For conventional ferroalloys such as ferrosilicon and ferromanganese, the melting method has been realized, but As a new type of iron alloy, Al-Mg-Ca-Fe alloy has not been involved

Method used

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  • Melted sampling method for aluminum magnesium calcium iron alloy for X-ray fluorescence spectrum analysis
  • Melted sampling method for aluminum magnesium calcium iron alloy for X-ray fluorescence spectrum analysis
  • Melted sampling method for aluminum magnesium calcium iron alloy for X-ray fluorescence spectrum analysis

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Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1: This fusion sample preparation method is completed through the following steps:

[0021] 1. Weigh 7.0000g of lithium tetraborate in a platinum crucible, melt it at 1000°C, slowly rotate the crucible after taking it out, and hang a layer of protective wall with a certain height and uniformity in the platinum crucible;

[0022] 2. Weigh 0.2000g aluminum magnesium calcium iron sample, 0.5000g potassium iodide and 1.5000g lithium carbonate, put them into a platinum crucible, and mix well;

[0023] 3. Uniformly cover 2.0000g of lithium tetraborate on the surface of the mixed sample mixture;

[0024] 4. Put the platinum crucible into the muffle furnace that has been heated to 800°C for pre-oxidation. During this process, the platinum crucible should be preheated at the furnace door for 1.5 minutes, and then slowly enter the furnace step by step for about 18 minutes. After the oxidation is complete The sample should be a flowable liquid, and there are no black p...

Embodiment 2

[0027] Embodiment 2: This fusion sample preparation method is completed through the following steps:

[0028] 1. Weigh 5.0000g of lithium tetraborate in a platinum crucible, melt it at 1050°C, slowly rotate the crucible after taking it out, and hang a layer of protective wall with a certain height and uniformity in the platinum crucible;

[0029] 2. Weigh 0.5000g aluminum magnesium calcium iron sample, 0.5000g potassium iodide and 2.5000g lithium carbonate, put them into a platinum crucible, and mix well;

[0030] 3. Evenly cover the surface of the mixed sample mixture with 1.0000g of lithium tetraborate;

[0031] 4. Put the platinum crucible into the muffle furnace that has been heated to 800°C for pre-oxidation. During this process, the platinum crucible should be preheated at the furnace door for 1.0min, and then slowly enter the furnace step by step for about 15min. After the oxidation is complete The sample should be a flowable liquid, and there are no black particles in...

Embodiment 3

[0034] Embodiment 3: This fusion sample preparation method is completed through the following steps:

[0035] 1. Weigh 8.0000g of lithium tetraborate in a platinum crucible, melt it at 1050°C, slowly rotate the crucible after taking it out, and hang a protective wall with a certain height and uniformity in the platinum crucible;

[0036] 2. Weigh 0.2500g aluminum magnesium calcium iron sample, 0.5000g potassium iodide and 2.5000g lithium carbonate, put them into a platinum crucible, and mix well;

[0037] 3. Uniformly cover 3.0000g of lithium tetraborate on the surface of the above sample mixture that has been mixed;

[0038] 4. Put the platinum crucible into the muffle furnace that has been heated to 800°C for pre-oxidation. During this process, the platinum crucible should be preheated at the furnace door for 2.0 minutes, and then slowly enter the furnace step by step for about 20 minutes. After the oxidation is complete The sample should be a flowable liquid, and there are...

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Abstract

The invention discloses a melted sampling method for aluminum magnesium calcium iron alloy for X-ray fluorescence spectrum analysis. The melted sampling method is characterized by comprising the following steps of: hanging a layer of uniform lithium tetraborate protective wall in a platinum crucible; putting an aluminum magnesium calcium iron sample, lithium carbonate and potassium iodide into the platinum crucible in which the protective wall is hung, mixing uniformly, and covering a layer of lithium tetraborate; pre-oxidizing the aluminum magnesium calcium iron sample; and melting the oxidized aluminum magnesium calcium iron sample, and cooling to obtain a glass fuse piece of the aluminum magnesium calcium iron alloy. By the method, the sampling time is short, the manufactured glass fuse piece is uniform and perfect, and the specification of a mineral effect and a granularity effect can be eliminated completely. The glass fuse piece can be used for the X-ray fluorescence spectrum analysis, the obtained analytic result is accurate and reliable, and the requirements of modern enterprises on quick and accurate detection of analytic data are met. The method is safe, reliable, easy to operate and high in repeatability, and the application range of an X-ray fluorescence spectrum method is broadened.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, in particular to a melting sample preparation method of an aluminum-magnesium-calcium-iron alloy used for X-ray fluorescence spectrum analysis. Background technique [0002] Al-Mg-Ca-Fe alloy is a new type of deoxidizer for steelmaking. It has the characteristics of low silicon, low carbon, and low sulfur. It has incomparable advantages over high-silicon ferro-silicon, silicon-calcium and other high-silicon ferroalloys for smelting low-silicon steel. The element content in the Al-Mg-Ca-Fe alloy is not only an important basis for the adjustment of the steelmaking process parameters, but also the basis for the price calculation of most companies that sell and purchase this type of ferroalloy, so it is very important to accurately determine the element content in the Al-Mg-Ca-Fe alloy . However, there are currently no product standards and testing standards for Al-Mg-Ca-Fe alloys, an...

Claims

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Application Information

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IPC IPC(8): G01N1/44G01N23/223
Inventor 王彬果李兰群徐静赵靖商英滕海雨韩斌李志明张军米东海
Owner HBIS COMPANY LIMITED HANDAN BRANCH COMPANY
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