CN102156142A - Method for analyzing ferrosilicon alloy components for X-ray fluorescence spectrum analysis - Google Patents
Method for analyzing ferrosilicon alloy components for X-ray fluorescence spectrum analysis Download PDFInfo
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- CN102156142A CN102156142A CN 201110131226 CN201110131226A CN102156142A CN 102156142 A CN102156142 A CN 102156142A CN 201110131226 CN201110131226 CN 201110131226 CN 201110131226 A CN201110131226 A CN 201110131226A CN 102156142 A CN102156142 A CN 102156142A
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Abstract
The invention discloses a method for analyzing ferrosilicon alloy components for X-ray fluorescence spectrum analysis. A method for preparing a sample comprises the following steps of: selecting a proper oxidant; adding a flux into a platinum crucible, putting the platinum crucible in a high temperature furnace, and melting the flux at high temperature to manufacture a wall built-up flux crucible with the basement of flux; mixing a ferrosilicon alloy test sample, the flux and the oxidant, pouring the mixture into the flux crucible, and covering a certain amount of mixed flux; and putting the flux crucible filled with the ferrosilicon alloy test sample, the flux, the oxidant and the mixed flux into the high temperature furnace, preliminarily oxidizing at low temperature, shifting into a high temperature zone, and melting at high temperature to prepare the ferrosilicon alloy test sample glass sample for the X-ray fluorescence spectrum analysis. In the technical scheme, elements are uniformly distributed in the prepared glass sample, and the glass sample has no particle effect and can be preserved for a long time; moreover, the operation method is simple and safe, the preparation time of the sample is short, and primary and secondary quantity elements in the ferrosilicon alloy are rapidly and accurately measured.
Description
Technical field
The invention belongs to the technical field that steel and iron industry is produced, relate to the analytical approach of Antaciron composition, more particularly, the present invention relates to a kind of analytical approach that X-ray fluorescence spectra is analyzed the Antaciron composition that is used for.
Background technology
Antaciron is the alloy of silicon and iron, is a kind of good deoxidizer, is mainly used in the addition agent that deoxidizer or alloying element are made in steel-making and casting.Silica, steel cuttings, coke are the primary raw materials of producing ferrosilicon.
At present, Antaciron changes into branch and analyzes and to adopt chemical analysis usually because its silicon content is very high, during experiment molten sample formality numerous and diverse, analytical cycle is long, analyst's labour intensity height, reagent consumption is big, and agents useful for same easily works the mischief to environment.
Also useful ray fluorescence spectrometry is analyzed Antaciron, but its pattern method adopts pressed disc method usually, owing to be subjected to factor affecting such as matrix of samples effect, the analysis result accuracy of this method is not ideal enough, and data reliability is relatively poor.
X-ray fluorescence spectra (XRF) analytic approach is that a kind of important chemical constitution is analysed means, have quick, easy, accurate, analytical element is many, wide, the precision advantages of higher of content range measured, can directly analyze the constituent content in solid, powder and the liquor sample simultaneously.
When carrying out X-ray spectral analysis, require analytic sample smooth smooth, element is evenly distributed, do not have grain effect and mineral effect, print is stable, can long preservation, and require the physical form of standard model and specimen to be consistent.Therefore, the preparation effect of its sample becomes key link.
At present, carrying out the sample preparation methods that X-ray spectral analysis mainly adopts both at home and abroad has following several:
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, carbon etc.
4, liquid and 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 leak of liquid takes place its shortcoming easily, instrument is produced harmful effect, and standard specimen and sample all are difficult to long preservation, and because use a large amount of soda acids, easily environment are polluted.
Summary of the invention
Problem to be solved by this invention provides a kind of analytical approach that X-ray fluorescence spectra is analyzed the Antaciron composition that is used for, and its objective is that element is evenly distributed no grain effect, but long preservation in the feasible glass print of making; And the mensuration fast and accurately of primary and secondary quantitative elements in the Antaciron is carried out in realization simultaneously with x-ray fluorescence method.
To achieve these goals, the technical scheme taked of the present invention is:
The analytical approach that is used for X-ray fluorescence spectra analysis Antaciron composition provided by the present invention, described analytical approach comprises the method for making sample of Antaciron specimen, described method for making sample may further comprise the steps:
1, select barium dioxide as oxygenant;
2, add lithium tetraborate in platinum crucible and make flux, platinum crucible is put into high temperature furnace, the flux high-temperature fusion is made the flux crucible of flux bottoming wall built-up;
3, with after Antaciron specimen, flux and the oxygenant mixing, pour in the flux crucible of the wall built-up that feels secure, cover a certain amount of mixed flux above, the content in the described mixed flux is 33% lithium tetraborate and 67% lithium metaborate by mass percentage;
4, the flux crucible that described Antaciron specimen, flux, oxygenant and mixed flux will be housed is put into high temperature furnace, pre-oxidation at low temperatures earlier, move into the high-temperature region then, high-temperature fusion is made and is used for the Antaciron specimen glass print that X-ray fluorescence spectra is analyzed.
Above-described analytical approach is analyzed the X-ray fluorescence spectra of the Si in the Antaciron, Fe, Mn, P, Al, Ca, may further comprise the steps:
The first step, preparation standard glass print:
A, take by weighing the ferrosilicon standard model of 0.1500g, add the barium dioxide of 2.0000g, put into weighing disk, fully behind the mixing, be moved on the filter paper, cover the described mixed flux of 2.0000g above, standby after wrapping with filter paper packet;
B, take by weighing the lithium tetraborate of 7.000g, place platinum crucible, it is that 1050 ℃ muffle furnace fusion was taken out after 5 minutes that platinum crucible is placed temperature, shakes platinum crucible, make solution evenly be attached to platinum crucible wall and bottom, make the flux crucible of bottoming wall built-up;
C, the potpourri that makes among the step a, wrap with filter paper packet put into the flux crucible of the wall built-up that feels secure;
D, the flux crucible that will put into potpourri are put into 800 ℃ of muffle furnace pre-oxidation 30min. and are taken out, and cooling drips 10 200g/L ammonium bromide solution, fusion is 15 minutes in 1050 ℃ of muffle furnaces, shake up fused mass in the flux crucible during this period, take out the back cooling and peel off, preparation melten glass print.
In second step, preparation specimen glass print: operation steps is consistent with preparation standard glass print.
The 3rd step, test: be with the intensity of each element in the Xray fluorescence spectrometer test silicon ferroalloy specimen, calculate each components contents in the sample.
The present invention adopts technique scheme, overcomes the deficiencies in the prior art, carries out the x-ray fluorescence analysis Antaciron with the fusion sample preparation, and element is evenly distributed no grain effect, but long preservation in the feasible glass print of making; Simultaneously, simple, the safety of method of operating, print preparation time are short; Can carry out the mensuration of primary and secondary quantitative elements in the Antaciron simultaneously, therefore, can save a large amount of test materials, shorten sense cycle greatly, the liberation labour increases work efficiency.Analytical cycle shortened in 1 hour from 8～16 hours, and operating personnel reduce to 1 people by 3～4 people.And, except that the platinum yellow crucible being had small corrosion and a spot of reagent material consumption, almost there is not other to consume, a large amount of heavy metal waste liquid pollution on the environment when having avoided chemical analysis.Enforcement of the present invention is for the research of the iron alloy fusing sample x-ray fluorescence analysis of other types provides useful reference.
Embodiment
Below the specific embodiment of the present invention is described in further detail, inventive concept of the present invention, technical scheme is had more complete, accurate and deep understanding to help those skilled in the art.
The present invention is a kind of analytical approach that X-ray fluorescence spectra is analyzed the Antaciron composition that is used for, and described analytical approach comprises the method for making sample of Antaciron specimen.
In order to solve the problem that exists at the described present known technology of this instructions background technology part and to overcome its defective, realize that element is evenly distributed in the feasible glass print of making, no grain effect, goal of the invention with long preservation period, the technical scheme that the present invention takes is:
The analytical approach that is used for X-ray fluorescence spectra analysis Antaciron composition provided by the present invention, described method for making sample may further comprise the steps:
1, select barium dioxide as oxygenant;
2, add lithium tetraborate in platinum crucible and make flux, platinum crucible is put into high temperature furnace, the flux high-temperature fusion is made the flux crucible of flux bottoming wall built-up;
3, with after Antaciron specimen, flux and the oxygenant mixing, pour in the flux crucible of the wall built-up that feels secure, cover a certain amount of mixed flux above, the content in the described mixed flux is 33% lithium tetraborate and 67% lithium metaborate by mass percentage;
4, the flux crucible that described Antaciron specimen, flux, oxygenant and mixed flux will be housed is put into high temperature furnace, pre-oxidation at low temperatures earlier, move into the high-temperature region then, high-temperature fusion is made and is used for the Antaciron specimen glass print that X-ray fluorescence spectra is analyzed.
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method for making sample that is used for X-ray spectral analysis Antaciron chemical constitution is provided, element is evenly distributed no grain effect, but long preservation in the feasible glass print of making; Simultaneously, method of operating is simple, safety, and the print preparation time is short, but and long preservation.
Analytical approach of the present invention may further comprise the steps the X-ray fluorescence spectra analysis of the Si in the Antaciron, Fe, Mn, P, Al, Ca:
The first step, preparation standard glass print:
A, take by weighing the ferrosilicon standard model of 0.1500g, add the barium dioxide of 2.0000g, put into weighing disk, fully behind the mixing, be moved on the filter paper, cover the described mixed flux of 2.0000g above, standby after wrapping with filter paper packet;
B, take by weighing the lithium tetraborate of 7.000g, place platinum crucible, it is that 1050 ℃ muffle furnace fusion was taken out after 5 minutes that platinum crucible is placed temperature, shakes platinum crucible, make solution evenly be attached to platinum crucible wall and bottom, make the flux crucible of bottoming wall built-up;
C, the potpourri that makes among the step a, wrap with filter paper packet put into the flux crucible of the wall built-up that feels secure;
D, the flux crucible that will put into potpourri are put into 800 ℃ of muffle furnace pre-oxidation 30min. and are taken out, and cooling drips 10 200g/L ammonium bromide solution, fusion is 15 minutes in 1050 ℃ of muffle furnaces, shake up fused mass in the flux crucible during this period, take out the back cooling and peel off, preparation melten glass print.
In second step, preparation specimen glass print: operation steps is consistent with preparation standard glass print.
The 3rd step, test: be with the intensity of each element in the Xray fluorescence spectrometer test silicon ferroalloy specimen, calculate each components contents in the sample.
Table 1 is learned the assay value contrast for adopting gained x-ray fluorescence analysis result of the present invention to assimilate.
The comparison (%) of table 1:X fluorescent value and chemical score
As shown in Table 1, adopt analysis result assimilation of the present invention to learn assay value and coincide, accuracy is higher.
Carry out the x-ray fluorescence analysis Antaciron with the fusion sample preparation, can carry out the mensuration of primary and secondary quantitative elements in the Antaciron simultaneously, therefore, can save a large amount of test materials, shorten sense cycle greatly, the liberation labour increases work efficiency.Analytical cycle shortened in 1 hour from 8～16 hours, and operating personnel can have 3-4 to reduce to 1 people.And except that the platinum yellow crucible being had small corrosion and a spot of reagent material consumption, almost there is not other to consume, a large amount of heavy metal waste liquid pollution on the environment when having avoided chemical analysis.Enforcement of the present invention simultaneously is for the research of the iron alloy fusing sample x-ray fluorescence analysis of other types provides useful reference.
Above the present invention has been carried out exemplary description; obviously specific implementation of the present invention is not subjected to the restriction of aforesaid way; as long as adopted the improvement of the various unsubstantialities that method of the present invention design and technical scheme carry out; or design of the present invention and technical scheme are directly applied to other occasion without improving, all within protection scope of the present invention.
Claims (2)
1. one kind is used for the analytical approach that X-ray fluorescence spectra is analyzed the Antaciron composition, and described analytical approach comprises the method for making sample of Antaciron specimen, it is characterized in that: described method for making sample may further comprise the steps:
1), select barium dioxide as oxygenant;
2), in platinum crucible, add lithium tetraborate and make flux, platinum crucible is put into high temperature furnace, the flux high-temperature fusion is made the flux crucible of flux bottoming wall built-up;
3), Antaciron specimen, flux and oxygenant mixed after, pour in the flux crucible of the wall built-up that feels secure, cover a certain amount of mixed flux above, the content in the described mixed flux is 33% lithium tetraborate and 67% lithium metaborate by mass percentage;
4), the flux crucible that described Antaciron specimen, flux, oxygenant and mixed flux will be housed is put into high temperature furnace, pre-oxidation at low temperatures earlier, move into the high-temperature region then, high-temperature fusion is made and is used for the Antaciron specimen glass print that X-ray fluorescence spectra is analyzed.
2. according to the described analytical approach that is used for X-ray fluorescence spectra analysis Antaciron composition of claim 1, it is characterized in that: described analytical approach may further comprise the steps the X-ray fluorescence spectra analysis of the Si in the Antaciron, Fe, Mn, P, Al, Ca:
The first step, preparation standard glass print:
A, take by weighing the ferrosilicon standard model of 0.1500g, add the barium dioxide of 2.0000g, put into weighing disk, fully behind the mixing, be moved on the filter paper, cover the described mixed flux of 2.0000g above, standby after wrapping with filter paper packet;
B, take by weighing the lithium tetraborate of 7.000g, place platinum crucible, it is that 1050 ℃ muffle furnace fusion was taken out after 5 minutes that platinum crucible is placed temperature, shakes platinum crucible, make solution evenly be attached to platinum crucible wall and bottom, make the flux crucible of bottoming wall built-up;
C, the potpourri that makes among the step a, wrap with filter paper packet put into the flux crucible of the wall built-up that feels secure;
D, the flux crucible that will put into potpourri are put into 800 ℃ of muffle furnace pre-oxidation 30min. and are taken out, and cooling drips 10 200g/L ammonium bromide solution, fusion is 15 minutes in 1050 ℃ of muffle furnaces, shake up fused mass in the flux crucible during this period, take out the back cooling and peel off, preparation melten glass print.
In second step, preparation specimen glass print: operation steps is consistent with preparation standard glass print.
The 3rd step, test: be with the intensity of each element in the Xray fluorescence spectrometer test silicon ferroalloy specimen, calculate each components contents in the sample.
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| CN102607934A (en) * | 2012-03-07 | 2012-07-25 | 河北钢铁股份有限公司邯郸分公司 | X-ray fluorescence spectroscopy analysis fusion sample preparation method of aluminum, manganese, calcium and iron alloy |
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Application publication date: 20110817 |