CN101008593B - Sample preparation method of material containing silicon carbide used for x-ray spectrometric analysis - Google Patents
Sample preparation method of material containing silicon carbide used for x-ray spectrometric analysis Download PDFInfo
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- CN101008593B CN101008593B CN2006100237099A CN200610023709A CN101008593B CN 101008593 B CN101008593 B CN 101008593B CN 2006100237099 A CN2006100237099 A CN 2006100237099A CN 200610023709 A CN200610023709 A CN 200610023709A CN 101008593 B CN101008593 B CN 101008593B
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Abstract
This invention relates to one sampling method for X ray spectrum analysis of carbon silicon materials, which comprises the following steps: processing mixture of oxygen agent; processing fuse hanging bottom foil pot; pulling the mixture carbon silicon anti-fire materials sample ad mixture oxygen agent into the pot; putting the pot onto high temperature chamber for heating of oxidation in low temperature to process the glass rollers for the spectrum analysis for X ray.
Description
Technical field
The present invention relates to a kind of X-ray spectral analysis spectrum analysis of carbon silicon materials that is used for.
Background technology
How quick, easy, accurate, precision advantages of higher that the X-ray fluorescence spectra analysis has along with the development of instrument and software engineering, brings into play the advantage that X-ray fluorescence spectra is analyzed, and the preparation effect of its sample becomes key point.Requirement to the sample analyzed is: surfacing, pollution-free, element are evenly distributed, and no grain effect and mineral effect are stablized and required the physical form of standard model and specimen to be consistent, and could guarantee precision of analysis.At present, the method for making sample of X-ray fluorescence spectra analysis mainly contains following 4 kinds:
1, bulk sample method: as metal sample is cut, polishing.
2, powder pressing method:, comprise that ore, slag, rock, anti-material etc. carry out fragmentation, levigate compressing tablet as with analysis of material.
The shortcoming of the method is to be difficult to eliminate fully grain effect and mineral effect, is difficult to find the standard articles for use that are complementary, the poor accuracy of analysis.
3, fusion method: with powdered sample and flux, the potpourri of sodium tetraborate, lithium tetraborate or lithium tetraborate and lithium metaborate etc. for example, fusion forms beaded glass in platinum crucible.
The advantage of the method is effectively to overcome grain effect and mineral effect, but its shortcoming is analysis of material to be contained the material that corrodes platinum crucible then can't prepare, as contains metal, silit etc.
4, solwution method: be that sample preparation is become solution.
The advantage of the method is effectively to overcome grain effect and mineral effect, and element is evenly distributed, but its shortcoming is the instrument that needs configuration special, and safe reliability is low, needs to use a large amount of soda acids.
The silicon carbide-containing fire resistive material is one of important fire resistive material, in common refractory, add the performance that a certain amount of silit can improve fire resistive material, as strengthen heat conductance and wearing quality, reduce thermal expansivity etc., and can be many local uses, as various sprue gates, torpedo car, slag runner, spray gun etc.
Described silit is emery again, and as abrasive material, it has similar adamantine structure industrial, destroy the crystal of silit, must destroy a large amount of strong covalence keys, so decomposition temperature is very high, about about 2200 ℃, conventional laboratory can't reach this condition it is decomposed greatly.
Traditional conventional wet chemical analysis method is adopted in the analysis of silicon carbide-containing fire resistive material, because it can corrode the consumption platinum crucible, cost is quite high, and complex operation, analytical cycle are long, a large amount of bronsted lowry acids and bases bronsted lowry of use when analyzing simultaneously, contaminated environment.
As adopting conventional beaded glass fusion technology, then platinum crucible can be subjected to serious corrosion to the silicon carbide-containing fire resistive material.
Patent CN1249425A discloses the preparation method who is used to adopt specimen such as x ray fluorescence spectrometry assaying, be characterized in, element conversion to be measured in the sample is changed into the meltability salt, the mixed solution that adds citric acid (sodium) and EDTA, citric acid in the solution (sodium) concentration is 15g/l～25g/l, and EDTA concentration is 6g/l～10g/l, and the pH value of solution is 4～9, add agarose again, make gel solid shape print.The described method of this patent, its element is evenly distributed, no granularity effect, but do not produce leakage, print long preservation, have the advantage of solwution method and solid process concurrently.
But above-mentioned patent CN1249425A at first needs to adopt conventional method that element conversion to be measured in the sample is changed into the meltability salt, use a large amount of acid; be unfavorable for environmental protection; operation steps is many, and the time is long, and the silit conversion can't be changed into the meltability salt.
Summary of the invention
The object of the present invention is to provide a kind of X-ray spectral analysis spectrum analysis of carbon silicon materials that is used for, the beaded glass of making that is used for the X-ray fluorescence spectra analysis, element is evenly distributed, no grain effect and mineral effect, but long preservation; In sample making course, the silicon carbide decomposition in the silicon carbide-containing fire resistive material sample can be oxidized to the material that can not corrode platinum crucible simultaneously, method of operating is simple, safety, and preparation time is short, but the print long preservation.
For achieving the above object, the invention provides a kind of X-ray spectral analysis spectrum analysis of carbon silicon materials that is used for, it comprises following steps:
Step 1, preparation hybrid oxidant;
Step 2, in platinum crucible, add flux, and described platinum crucible is put into the high temperature smelting furnace fusion, make the platinum crucible of flux wall built-up bottoming;
Step 3, with behind silicon carbide-containing fire resistive material sample and the hybrid oxidant preparation mixing, pour in the platinum crucible by the bottoming of flux wall built-up;
Step 4, the platinum crucible that silicon carbide-containing fire resistive material sample and hybrid oxidant will be housed are put into high temperature smelting furnace, and heated oxide is at low temperatures made and is used for the beaded glass that X-ray fluorescence spectra is analyzed.
In the step 1, described hybrid oxidant can be that 60%～70% barium dioxide and massfraction are that 30%～40% sodium nitrate is made by massfraction.
In the step 1, described hybrid oxidant can be that 60%～70% barium dioxide and massfraction are that 30%～40% potassium nitrate is made by massfraction.
In the step 1, described hybrid oxidant can be that 60%～70% barium dioxide and massfraction are that 30%～40% lithium nitrate is made by massfraction.
In the step 1, described hybrid oxidant can be that 60%～70% sodium peroxide and massfraction are that 30%～40% sodium nitrate is made by massfraction.
In the step 1, described hybrid oxidant can be that 60%～70% sodium peroxide and massfraction are that 30%～40% potassium nitrate is made by massfraction.
In the step 1, described hybrid oxidant can be that 60%～70% sodium peroxide and massfraction are that 30%～40% lithium nitrate is made by massfraction.
In the step 2, described flux is lithium tetraborate.
In the step 2, the temperature of described high-temperature fusion is 1000～1200 ℃.
In the step 2, the melting time of described platinum crucible is 3～10 minutes.
In the step 3, described silicon carbide-containing fire resistive material sample and hybrid oxidant are prepared mixing with 1: 3～7 ratio.
In the step 4, specifically comprise following steps:
Step 4.1, the platinum crucible that silicon carbide-containing fire resistive material sample and hybrid oxidant will be housed are put into high temperature smelting furnace and are heated, and from 650 ℃, whenever temperature raises 50～70 ℃, just are incubated 5～10 minutes, reach 850 ℃ until temperature;
Step 4.2, continuation heat up, and reach 1100～1200 ℃ until temperature, fusion 15～25 minutes;
Step 4.3, taking-up platinum crucible are cooled to room temperature, make beaded glass.
The X-ray spectral analysis spectrum analysis of carbon silicon materials that is used for provided by the invention, the beaded glass of making that is used for the X-ray fluorescence spectra analysis, element is evenly distributed, no grain effect and mineral effect, but long preservation.
Provided by the invention to be used for the X-ray spectral analysis spectrum analysis of carbon silicon materials very reliable, and the sample preparation success ratio reaches 100%, guarantees to adopt X-ray fluorescence spectra to analyze the accuracy of the fire resistive material of silicon carbide-containing.
The X-ray spectral analysis spectrum analysis of carbon silicon materials that is used for provided by the invention, contain silit in the Tercod sample and be decomposing oxidation at low temperatures, it produces the material that can not corrode platinum crucible in the process of 650～850 ℃ of oxygenolysis; Simultaneously owing in advance platinum crucible is carried out the bottoming of flux wall built-up, with fusing point be 920 ℃ flux as separation layer, sample can directly not contact with platinum crucible in 650～850 ℃ oxidation decomposition course; Thus, can not corrode platinum crucible, improve the serviceable life of platinum crucible, reduce cost.
The X-ray spectral analysis spectrum analysis of carbon silicon materials that is used for provided by the invention, simple to operate, and do not use acid in the operating process, and reduce cost greatly, reduce environmental pollution; Can shorten the sense cycle of sample greatly.
Embodiment
Below, further specify method of the present invention by 2 specific embodiments:
Embodiment 1, employing the present invention are to the K in the fire resistive material of silicon carbide-containing aluminium matter
2O, Fe
2O
3, MnO, MgO, CaO, Al
2O
3, TiO
2, P
2O
5, TSi the X-ray fluorescence spectra analysis:
At first, preparation standard beaded glass:
1, takes by weighing silicon carbide-containing aluminium matter standard model and hybrid oxidant, put into porcelain crucible and mix.
2, take by weighing lithium tetraborate, put into platinum crucible, add 0.03～0.06g ammonium iodide simultaneously,, take out the platinum crucible of lithium tetraborate wall built-up bottoming, cool off standby 1100 ℃ of fusions 5 minutes.
3, the potpourri in the porcelain crucible is poured in the platinum crucible of lithium tetraborate wall built-up bottoming.
4, the platinum crucible that contains potpourri is put into high temperature smelting furnace,, just be incubated 5～10 minutes from 50～70 ℃ of 650 ℃ of every risings, reach 850 ℃ up to temperature, be warming up to 1100～1200 ℃ then, fusion 15～25 minutes, taking-up is cooled to room temperature, makes beaded glass.
Second step, preparation specimen beaded glass, operation steps is consistent with the preparation standard beaded glass.
The 3rd step, test: use Xray fluorescence spectrometer, measure the intensity of each element in the sample, calculate each components contents in the sample.
What table 1 was listed is the contrast of adopting resulting X-ray spectral analysis result of method for making sample of the present invention and chemical score:
The assay value that table l, employing the present invention obtain and the comparison (%) of chemical score
From table 1, obviously as can be seen, adopt analysis result of the present invention and chemical analysis value quite identical, the accuracy height.
Embodiment 2, employing the present invention are to the K in the siliceous fire resistive material of silicon carbide-containing
2O, Fe
2O
3, MnO, MgO, CaO, Al
2O
3, TiO
2, P
2O
5, TSi the X-ray fluorescence spectra analysis:
At first, preparation standard beaded glass:
1, takes by weighing siliceous standard model of silicon carbide-containing and hybrid oxidant, put into porcelain crucible and mix.
2, take by weighing lithium tetraborate, put into platinum crucible, add 0.03～0.06g ammonium iodide simultaneously,, take out the platinum crucible of lithium tetraborate wall built-up bottoming, cool off standby 1100 ℃ of fusions 5 minutes.
3, the potpourri in the porcelain crucible is poured in the platinum crucible of lithium tetraborate wall built-up bottoming.
4, the platinum crucible that contains potpourri is put into high temperature smelting furnace,, just be incubated 5～10 minutes from 50～70 ℃ of 650 ℃ of every risings, reach 850 ℃ up to temperature, be warming up to 1100～1200 ℃ then, fusion 15～25 minutes, taking-up is cooled to room temperature, makes beaded glass.
Second step, preparation specimen beaded glass, operation steps is consistent with the preparation standard beaded glass.
The 3rd step, test: use Xray fluorescence spectrometer, measure the intensity of each element in the sample, calculate each components contents in the sample.
What table 2 was listed is the contrast of adopting resulting X-ray spectral analysis result of method for making sample of the present invention and chemical score:
The assay value that table 2, employing the present invention obtain and the comparison (%) of chemical score
From table 2, obviously as can be seen, adopt analysis result of the present invention and chemical analysis value quite identical, the accuracy height.
In sum, provided by the invention to be used for the X-ray spectral analysis spectrum analysis of carbon silicon materials very reliable, guarantees to adopt X-ray fluorescence spectra to analyze the accuracy of the fire resistive material of silicon carbide-containing.
Simultaneously, the X-ray spectral analysis spectrum analysis of carbon silicon materials that is used for provided by the invention, simple to operate, preparation time is short; Applied widely, can bring huge social benefit and economic benefit.
Claims (4)
1. one kind is used for the X-ray spectral analysis spectrum analysis of carbon silicon materials, is characterised in that it comprises following steps:
Step 1, preparation hybrid oxidant; Described hybrid oxidant is that 60%～70% barium dioxide and massfraction are 30%～40% sodium nitrate by massfraction, perhaps potassium nitrate, and perhaps lithium nitrate is made; Perhaps described hybrid oxidant is that 60%～70% sodium peroxide and massfraction are 30%～40% sodium nitrate by massfraction, perhaps potassium nitrate, and perhaps lithium nitrate is made;
Step 2, in platinum crucible, add flux, and described platinum crucible is put into the high temperature smelting furnace fusion, make the platinum crucible of flux wall built-up bottoming; Described flux is lithium tetraborate;
Step 3, with behind silicon carbide-containing fire resistive material sample and the hybrid oxidant preparation mixing, pour in the platinum crucible by the bottoming of flux wall built-up;
Step 4, the platinum crucible that silicon carbide-containing fire resistive material sample and hybrid oxidant will be housed are put into high temperature smelting furnace, heated oxide at low temperatures, and described low temperature is 650～850 ℃, makes to be used for the beaded glass that X-ray fluorescence spectra is analyzed;
In the step 4, specifically comprise following steps:
Step 4.1, the platinum crucible that silicon carbide-containing fire resistive material sample and hybrid oxidant will be housed are put into high temperature smelting furnace and are heated, and from 650 ℃, whenever temperature raises 50～70 ℃, just are incubated 5～10 minutes, reach 850 ℃ until temperature;
Step 4.2, continuation heat up, and reach 1100～1200 ℃ until temperature, fusion 15～25 minutes;
Step 4.3, taking-up platinum crucible are cooled to room temperature, make beaded glass.
2. the X-ray spectral analysis spectrum analysis of carbon silicon materials that is used for as claimed in claim 1 is characterized in that, in the step 2, described high-temperature fusion temperature is 1000～1200 ℃.
3. the X-ray spectral analysis spectrum analysis of carbon silicon materials that is used for as claimed in claim 1 is characterized in that, in the step 2, the melting time of described platinum crucible is 3～10 minutes.
4. the X-ray spectral analysis spectrum analysis of carbon silicon materials that is used for as claimed in claim 1 is characterized in that, described silicon carbide-containing fire resistive material sample and hybrid oxidant are prepared mixing with 1: 3～7 ratio.
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| CN101592571B (en) * | 2009-06-19 | 2011-06-08 | 河北钢铁股份有限公司 | Method for detecting contents of alloying elements in ferrotitanium and ferrovanadium by X-fluorescence fusion method |
| CN101718720B (en) * | 2009-11-10 | 2011-06-08 | 天津出入境检验检疫局化矿金属材料检测中心 | Method for detecting content of carborundum impurities by applying X-ray fluorescent spectrometry |
| CN101832891B (en) * | 2010-02-22 | 2011-10-05 | 河北钢铁股份有限公司邯郸分公司 | Iron alloy fusing sample preparation method for X-ray fluorescence spectrum analysis |
| CN102401756B (en) * | 2010-09-07 | 2013-12-11 | 鞍钢股份有限公司 | Preparation method for ferromolybdenum sample melting glass body |
| CN102156142A (en) * | 2011-05-19 | 2011-08-17 | 马鞍山钢铁股份有限公司 | Method for analyzing ferrosilicon alloy components for X-ray fluorescence spectrum analysis |
| CN103529067B (en) * | 2013-10-29 | 2015-08-19 | 吉林建龙钢铁有限责任公司 | X fluorescence spectrum method measures detection reagent and the method for iron ore |
| CN105651745A (en) * | 2015-12-29 | 2016-06-08 | 郑州旭飞光电科技有限公司 | Fluorescence detection method of zirconia content in TFT glass |
| CN105784746A (en) * | 2016-03-09 | 2016-07-20 | 重庆钢铁(集团)有限责任公司 | Method for detecting ferrosilicon element by combing graphite crucible sample melting with X-ray fluorescence |
| CN106840839B (en) * | 2017-01-16 | 2019-05-10 | 武汉科技大学 | A kind of preparation method of XRF glass sheet sample |
| JP7076835B2 (en) * | 2020-09-11 | 2022-05-30 | 株式会社リガク | How to make a glass bead for a fluorescent X-ray analyzer |
| CN112903663A (en) * | 2021-01-20 | 2021-06-04 | 山东钢铁股份有限公司 | Dissolving method for silicon carbide sample |
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| CN2694266Y (en) * | 2003-08-08 | 2005-04-20 | 国家地质实验测试中心 | Automatic forming high temperature electrothermal sample smelting furnace used for sample preparation of X-ray fluorescence analysis |
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| CN2694266Y (en) * | 2003-08-08 | 2005-04-20 | 国家地质实验测试中心 | Automatic forming high temperature electrothermal sample smelting furnace used for sample preparation of X-ray fluorescence analysis |
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