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Iron alloy fusing sample preparation method for X-ray fluorescence spectrum analysis

A technology of fluorescence spectroscopy and fusion sample preparation, which is applied in the field of analysis and detection, can solve the problems of not being able to effectively oxidize samples into glass flakes, increase the complexity and difficulty of high-temperature melting samples, and have higher requirements for the sample preparation process, so as to achieve accurate analysis results Reliable, eliminate mineral effects, method safe and reliable results

Inactive Publication Date: 2011-10-05
HBIS COMPANY LIMITED HANDAN BRANCH COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since ferrosilicon, silicon-calcium, silicon-aluminum-barium and other types of iron alloys contain a large amount of lighter elements, any unoxidized particles such as elemental silicon, sulfur and carbon may form eutectic mixtures with platinum at high temperatures The "poisoning" of platinum utensils reduces its corrosion resistance, and at the same time leads to the failure of sample preparation, which requires higher requirements for the sample preparation process and increases the complexity and difficulty of high-temperature melting samples. The above-mentioned wall-hanging fusion sample preparation technology cannot Effectively oxidize the sample and make a uniform glass sheet, not to mention it is not suitable for sample preparation of ferro-molybdenum, ferro-titanium, ferro-chromium, ferro-niobium, ferro-vanadium, etc.

Method used

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  • Iron alloy fusing sample preparation method for X-ray fluorescence spectrum analysis
  • Iron alloy fusing sample preparation method for X-ray fluorescence spectrum analysis
  • Iron alloy fusing sample preparation method for X-ray fluorescence spectrum analysis

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Effect test

Embodiment 1

[0018] Embodiment one, take ferrosilicon as example to illustrate the method involved in the present invention:

[0019] Silicon in ferrosilicon alloy is the No. 14 element of the fourth main group. It is an amphoteric substance, weakly reducing, and difficult to oxidize. Taking ferrosilicon as an example, it can illustrate the versatility of this method, that is, the applicability of the present invention to general ferroalloy samples. Strong features.

[0020] One. The preparation of ferrosilicon glass frit is completed by the following steps

[0021] 1. Weigh 8.0000g of lithium tetraborate in a platinum crucible, melt it at 1000°C, slowly rotate the crucible after taking it out, and hang a uniform protective wall on the inner wall of the platinum crucible; (currently, the specification of the platinum crucible for general fusion sample preparation is The diameter of the bottom is 34mm, and the height is about 25mm, which can meet the requirements with 8.0000g.)

[0022] 2...

Embodiment 2

[0037] Embodiment two, take ferromanganese as example to illustrate the method involved in the present invention:

[0038] One. The preparation of ferromanganese glass frit is completed through the following steps

[0039] 1. Weigh 8.0000g of lithium tetraborate into a platinum crucible, melt it at 1030°C, slowly rotate the crucible after taking it out, and hang a uniform protective wall on the inner wall of the platinum crucible;

[0040] 2. Weigh 0.2000g ferromanganese sample, weigh Li 2 CO 3 、Na 2 CO 3 and KNO 3 Each 0.5000g, weigh 1.0000g67%Li 2 B 4 o 7 and 33% LiBO 3 Put the mixed flux into a platinum crucible and mix well;

[0041] 3. Add 5g (20 drops) of ammonium iodide release agent with a concentration of 300g / L;

[0042] 4. Put the crucible into a muffle furnace at 810°C for pre-oxidation. In this process, first preheat the crucible at the furnace door for 1 min, and then gradually move the crucible into the furnace for pre-oxidation for 20 min. The sample ...

Embodiment 3

[0054] Embodiment three, take silicon-manganese alloy as an example to illustrate the method involved in the present invention:

[0055] One. The preparation of silicon-manganese alloy glass frit is completed through the following steps

[0056] 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 uniform protective wall on the inner wall of the platinum crucible;

[0057] 2. Weigh 0.2000g silicon manganese alloy sample, weigh Li 2 CO 3 、Na 2 CO 3 and KNO 3 Each 0.5000g, weigh 1.0000g 67% Li 2 B 4 o 7 and 33% LiBO 3 Put the mixed flux into a platinum crucible and mix well;

[0058] 3. Add 4.5g (18 drops) of 300g / L ammonium iodide release agent;

[0059] 4. Put the crucible into a muffle furnace at 790°C for pre-oxidation. In this process, first preheat the crucible at the furnace door for 1.5 minutes, and then gradually move the crucible into the furnace for pre-oxidation for 18 ...

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Abstract

The invention relates to an iron alloy fusing sample preparation method for X-ray fluorescence spectrum analysis, belonging to the technical field of materialization detection and aiming to solve the problem that fusing a film production alloy sample can erode a platinum crucible. The method comprises the steps of building up wall of the platinum crucible, preparing an oxidizing agent, pre-oxidizing an iron alloy sample and fusing and preparing sample from the iron alloy sample. The invention provides the fusing sample preparation method suitable for various iron alloys such as ferromanganese, silicomanganese, calcium silicon, ferrosilicon, ferromolybdenum, ferrotitanium, cymrite, ferrochrome, ferrocolumbium, ferrovanadium, silicon silicomanganese and the like. By adopting the method, a glass fusing piece can be manufactured without eroding the valuable platinum crucible, the sample can be completely oxidized in the sample preparation process, the sample preparation time is short, theprepared glass fusing piece is uniform and perfect, and the mineral effect and the granularity effect can be completely eliminated. The invention has safe and reliable method, simple and convenient operation and good repeatability, is suitable for various iron alloy samples and widens the application range of the fluorescence analysis.

Description

technical field [0001] The invention relates to a ferroalloy sample preparation method, in particular ferroalloy samples suitable for X-ray fluorescence spectroscopic analysis include ferromanganese, silicomanganese, silicon calcium, ferrosilicon, ferromolybdenum, ferrotitanium, silicon aluminum barium, ferrochromium, niobium The invention discloses a melting sample preparation method for iron, vanadium iron, carbon silicon manganese, etc., belonging to the technical field of analysis and detection. Background technique [0002] Ferro-manganese, silicon-manganese, composite carbon-silicon-manganese, ferrosilicon, silicon-calcium, silicon-aluminum-barium and other ferroalloys are important purchased alloy raw materials for steelmaking production in iron and steel enterprises. The content analysis of the main alloy elements silicon, manganese, and phosphorus in this type of ferroalloy is not only the basis for the calculation of the price of raw materials and fuels purchased b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/44G01N23/223
Inventor 王彬果李兰群赵靖徐静刘洁商英
Owner HBIS COMPANY LIMITED HANDAN BRANCH COMPANY
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