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

A technique of fluorescence spectroscopy and fusion sample preparation, which is applied in the field of analysis and detection, can solve the problems of increasing the complexity and difficulty of high-temperature melting samples, the inability to effectively oxidize samples into glass sheets, and the higher requirements of the sample preparation process, so as to achieve accurate analysis results Reliable, eliminate mineral effects, method safe and reliable results

Inactive Publication Date: 2010-09-15
HBIS COMPANY LIMITED HANDAN BRANCH COMPANY
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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Embodiment 1

[0018] Embodiment 1, taking ferrosilicon as an example to illustrate the method involved in the present invention:

[0019] Silicon in the ferrosilicon alloy is the 14th element of the fourth main group, which is an amphoteric substance, weakly reducing, and relatively difficult to oxidize. Taking ferrosilicon as an example can illustrate the versatility of this method, that is, the applicability of the present invention to general ferroalloy samples Strong characteristics.

[0020] 1. 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℃, slowly rotate the crucible after taking it out, and hang a layer of uniform protective wall in the platinum crucible; (the current specifications of the platinum crucible for general melting sample preparation are The bottom diameter is 34 mm, and the height is about 25 mm. It can meet the requirements with 8.0000g.)

[0022] 2. Weigh ...

Embodiment 2

[0037] The second embodiment takes ferromanganese as an example to illustrate the method involved in the present invention:

[0038] 1. The preparation of ferromanganese glass frit is completed by the following steps

[0039] 1. Weigh 8.0000g lithium tetraborate in a platinum crucible, melt it at 1030℃, slowly rotate the crucible after taking it out, and hang a uniform protective wall in the platinum crucible;

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

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

[0042] 4. Put the crucible in the muffle furnace at 810℃ for pre-oxidation. In this process, preheat the crucible at the door of the furnace for 1 min, and then slowly move the crucible into the furnace for pre-oxidation for 20 min. The sample after oxidation should be Flowable liquid without black particl...

Embodiment 3

[0054] In the third embodiment, silico-manganese alloy is taken as an example to illustrate the method involved in the present invention:

[0055] 1. The preparation of silico-manganese alloy glass frit is completed by the following steps

[0056] 1. Weigh 8.0000g of lithium tetraborate in a platinum crucible, melt it at 1050℃, slowly rotate the crucible after taking it out, and hang a uniform protective wall in the platinum crucible;

[0057] 2. Weigh 0.2000g silico-manganese alloy sample and weigh Li 2 CO 3 , Na 2 CO 3 And KNO 3 0.5000g each, weigh out 1.0000g 67% Li 2 B 4 O 7 And 33% LiBO 3 Put the mixed flux in the platinum crucible and mix well;

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

[0059] 4. Put the crucible into the muffle furnace at 790℃ for pre-oxidation. In this process, preheat the crucible at the door of the furnace for 1.5 minutes, and then slowly move the crucible into the furnace for pre-oxidation for 18 minutes. The sample after oxida...

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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, the prepared 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 method for preparing ferroalloy samples, in particular to ferroalloy samples suitable for X-ray fluorescence spectroscopy including ferromanganese, silicomanganese, silicon-calcium, ferrosilicon, ferromolybdenum, ferro-titanium, silicon-aluminum-barium, ferrochrome, and niobium The melting sample preparation method of iron, vanadium, carbon, silicon, manganese, etc. belongs to the technical field of analysis and detection. Background technique [0002] Ferromanganese, silico-manganese, composite carbon-silico-manganese, ferrosilicon, silicon-calcium, silicon-aluminum-barium and other ferroalloys are important purchased alloy raw materials required for steelmaking production by iron and steel enterprises. The analysis of the content of the main elements of silicon, manganese, and phosphorus in this type of ferroalloy is not only the basis for calculating the price of raw materials and fuels purchased by enterprises, but also an imp...

Claims

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Application Information

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