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X-ray fluorescence spectroscopy analysis fusion sample preparation method of aluminum, manganese, calcium and iron alloy

A technology of fluorescence spectroscopy and fusion sample preparation, which is applied in the field of analysis and detection, can solve the problems of difficult, time-consuming, laborious and cumbersome fusion sample preparation methods, and achieve the effects of accurate and reliable analysis results, expanded application range, and simple operation

Inactive Publication Date: 2012-07-25
HBIS COMPANY LIMITED HANDAN BRANCH COMPANY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Therefore, as a new type of ferroalloy, aluminum-manganese-calcium-ferroalloy is being used more and more widely. Among them, aluminum, manganese, calcium and iron are the four main constituent elements, and they are also the elements that must be checked for incoming material settlement. Although it can be used Traditional wet analysis is used for element determination, but the process is cumbersome, time-consuming and labor-intensive
Instrumental analysis methods such as X-ray fluorescence spectrometry are simple and fast, but the fusion sample preparation method is a difficult problem, because the reducing iron alloy sample will cause strong corrosion to the sample preparation vessel—platinum crucible, and it is generally considered unfeasible. Therefore, X-ray fluorescence spectrometry analysis method is limited

Method used

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  • X-ray fluorescence spectroscopy analysis fusion sample preparation method of aluminum, manganese, calcium and iron alloy

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Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1: This fusion sample preparation method is completed through the following steps:

[0020] 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;

[0021] 2. Weigh 0.2000g aluminum manganese calcium iron test sample, 0.5000g potassium iodide, 2.0000g lithium tetraborate and 1.5000g lithium nitrate, put them into a platinum crucible, and mix well;

[0022] 3. Uniformly cover 2.0000g of lithium tetraborate on the surface of the mixed sample mixture;

[0023] 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 ...

Embodiment 2

[0026] Embodiment 2: This fusion sample preparation method is completed through the following steps:

[0027] 1. Weigh 5.0000g of lithium tetraborate in a platinum crucible, melt it at 1020°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;

[0028] 2. Weigh 0.5000g aluminum manganese calcium iron test sample, 0.5000g sodium iodide, 1.0000g mixed flux of 50wt% lithium tetraborate + 50wt% lithium metaborate and 2.5000g lithium carbonate, put them into a platinum crucible, and mix well;

[0029] 3. Put the platinum crucible into the muffle furnace for pre-oxidation by temperature programming. The process is 550°C for 3 minutes, 600°C for 3 minutes, 650°C for 3 minutes, 700°C for 3 minutes, 750°C for 5 minutes, and 800°C. After 5 minutes, the sample should be a flowable liquid after the oxidation is completed, and there are no black particles in the sample;

[0030] 4. Put the oxid...

Embodiment 3

[0032] Embodiment 3: This fusion sample preparation method is completed through the following steps:

[0033] 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;

[0034] 2. Weigh 0.2500g aluminum manganese calcium iron test sample, 0.5000g potassium iodide, 2.5000g potassium nitrate and 3.0000g lithium metaborate, put them into a platinum crucible, and mix well;

[0035] 3. 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 no black particles in the sample;

[0036] 4. Put the oxidized sample into the melting fu...

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Abstract

The invention discloses an X-ray fluorescence spectroscopy analysis fusion sample preparation method of an aluminum, manganese, calcium and iron alloy, which comprises the steps of: firstly, coating a uniform protection wall layer in a platinum crucible by using lithium tetraborate, then placing an aluminum, manganese, calcium and iron sample, an oxidizing agent, a lithium borate solvent and a releasing agent into the platinum crucible in which the protection wall is coated, uniformly mixing, and then pre-oxidizing the aluminum, manganese, calcium and iron sample; and finally, melting the pre-oxidized aluminum, manganese, calcium and iron sample, and cooling to obtain an aluminum, manganese, calcium and iron sample glass fuse piece, wherein the aluminum, manganese, calcium and iron sample is a detection sample or calibration sample of the aluminum, manganese, calcium and iron alloy, and the sample glass fuse piece is a detection sample glass fuse piece or calibration sample glass fuse piece of the aluminum, manganese, calcium and iron alloy. On the premise of no corrosion to the valuable platinum crucible, the glass fuse piece can be prepared, and the prepared sample is excellent and uniform, thus the mineral effect and the grain size effect are completely eliminated.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, in particular to a melting sample preparation method for X-ray fluorescence spectrum analysis of Al-Mn-Ca-Fe alloy. Background technique [0002] Al-manganese alloys have been widely used as deoxidizers for steelmaking in recent years. Although they have the advantages of high specific gravity, easy sinking in molten steel, and the ability to achieve manganese alloying at the same time, the deoxidizers are formed during the deoxidation process. Al 2 o 3 In the form of strips, the toughness and ductility of steel are reduced. At the same time, since Al 2 o 3 With a high melting point, it is easy to block the nozzle during continuous casting and cause continuous casting accidents. It was later found that adding calcium to the aluminum-manganese alloy can not only improve the Al 2 o 3 The shape of the inclusions makes it spheroidized, thereby improving the toughness and ductili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44G01N23/223
Inventor 王彬果李兰群左丽峰吴章海刘洁张建忠白书霞闫文喜
Owner HBIS COMPANY LIMITED HANDAN BRANCH COMPANY
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