CN106442073A - Fusion sample preparation method for X-ray fluorescence analysis of element contents of silicon and phosphorus in silicon-manganese ball alloy - Google Patents
Fusion sample preparation method for X-ray fluorescence analysis of element contents of silicon and phosphorus in silicon-manganese ball alloy Download PDFInfo
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- CN106442073A CN106442073A CN201611199111.5A CN201611199111A CN106442073A CN 106442073 A CN106442073 A CN 106442073A CN 201611199111 A CN201611199111 A CN 201611199111A CN 106442073 A CN106442073 A CN 106442073A
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- sample
- silicon
- flux
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- ball
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
Abstract
The invention discloses a fusion sample preparation method for X-ray fluorescence analysis of element contents of silicon and phosphorus in silicon-manganese ball alloy. The method includes steps: (1) weighing a mixed flux, and spreading out in a platinum yellow crucible; (2) weighing an oxidant fluxing agent, and centralizing in the middle of the surface of the mixed flux in the platinum yellow crucible at the step (1); (3) weighing a silicon-manganese ball sample, and putting above the oxidant fluxing agent, obtained at the step (2), in the platinum yellow crucible; (4) stirring the sample, obtained at the step (3) in the platinum yellow crucible, and well mixing; (5) dropwise adding a release agent into the sample obtained at the step (4), fusing the platinum yellow crucible and the sample into a sample melting furnace, taking out, and completely cooling fuse pieces to obtain glass fuse pieces of the silicon-manganese ball alloy. The method has advantages of operation simplification, analysis cost reduction, labor intensity relief and test efficiency improvement, and the problem of test result instability caused by a grain size effect and a mineral effect of a pelleting-fluorescence analysis method is solved.
Description
Technical field
The present invention relates to technical field of analysis and detection, more particularly, to a kind of x-ray fluorescence analysis silicomanganese ball Silicon In Alloys unit
Element and the MTG YBCO bulk method of phosphorus element content.
Background technology
Silicomangan is the important alloy in steelmaking process, and the current method of inspection is mainly national standard method, i.e. humid analysis,
This analysis result is stable, but its operating procedure complexity is loaded down with trivial details, and each element is independent analysis, and analytical cycle is up to 8 hours.In order to
Shorten round of visits, existing enterprise development goes out tabletting-fluorescence analysiss, but the method is subject to granularity effect and mineral effects,
Cause assay unstable.
With the development of metallurgy industry, novel alloy occurs：Compound silicomanganese ball.Due to each alloy production producer proportioning raw materials
Difference, compound silicomanganese ball cannot realize tabletting-fluorescence analysiss.
Liu Wei, Cao Jixiang et al. report《Silicomanganese phosphorus in MTG YBCO bulk-x-ray fluorescence spectrometry silicomangan》,
To alloy, advanced row pre-oxidation flow process, prepares bead, then carries out X-ray fluorescence spectroscopy measurement, but the party
Method early stage preoxidation process is complicated, for up to 1.5 hours, and requires higher for firing equipment.
Content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of x-ray fluorescence analysis silicomanganese
Ball Silicon In Alloys element and the MTG YBCO bulk method of phosphorus element content, overcome the operation of the method for inspection present in prior art multiple
The problems such as miscellaneous, cycle is long.
To achieve these goals or other purposes, the present invention is achieved by the following technical solutions：
A kind of x-ray fluorescence analysis silicomanganese ball Silicon In Alloys element and the MTG YBCO bulk method of phosphorus element content, including such as
Lower step：
(1) weigh mixed flux, be placed in platinum yellow crucible, pave；
(2) weigh oxidant flux, concentrate the surface interposition of mixed flux in the platinum yellow crucible being placed in step (1)
Put；
(3) weigh silicomanganese ball sample, be placed in above step (2) gained platinum yellow crucible inner oxidizing agent flux；
(4) by the silicomanganese ball sample in centre position in platinum yellow crucible in step (3) and oxidant flux and mixed flux
Stirring and evenly mixing, should avoid silicomanganese ball sample to contact with the side wall of platinum yellow crucible and bottom with oxidant flux in whipping process；
(5) instill releasing agent along platinum yellow crucible wall in step (4) gained sample, then platinum yellow crucible and sample are put
Take out after entering melting in sample-melting stove, after fuse piece is sufficiently cool, that is, obtain the bead of silicomanganese ball alloy.
Further, in step (1), mixed flux consumption is 6.0000g～8.000g；Oxidant flux in step (2)
Consumption be 0.5000g～2.0000g；In step (3), the consumption of silicomanganese ball sample is 0.1000g～0.5000g；Step (5)
Middle releasing agent consumption is 0.3ml～0.5ml.
Preferably, in step (1), mixed flux consumption is 8.000g；In step (2), the consumption of oxidant flux is
1.0000g；In step (3), the consumption of silicomanganese ball sample is 0.2000g；In step (5), releasing agent consumption is 0.5ml.
Further, the described mixed flux of step (1) can be sodium tetraborate, lithium tetraborate, lithium carbonate and lithium metaborate
It is used in mixed way Deng to be used alone or by different proportion.Preferably, mixed flux of the present invention is Li2B4O7And LiBO2's
Mixture, Li2B4O7And LiBO2Mass percent be respectively 67% and 33%.Because silicomanganese ball alloy is with complex compound
Presented in, therefore, can be single borated stable for the chemical conversion of tested elemental oxygen after adding mixed flux and oxidant
Compound, is easy to detect.
Further, oxidant flux described in step (2) is potassium nitrate.
Further, due in silicomanganese ball simple substance class such as silicon, aluminum, carbon and ferrum etc. in high temperature can with platinum formed co-melting
Thing, heavy corrosion platinum crucible, therefore, should avoid in whipping process in step (4) silicomanganese ball sample and platinum yellow crucible bottom and
Sidewall contact.
Further, because the vitreous body of melting has the tendency of to adhere to or invade profit platinum crucible, fuse piece is made to be bonded at platinum earthenware
On crucible, lead to fuse piece to rupture, therefore add releasing agent can adjust molten mass surface tension, make molten mass smooth with platinum crucible
Depart from, make glass sheet surface brighter and cleaner, the amount that releasing agent adds should be within the scope of of the present invention, and going beyond the scope, it is de- to occur
Imitate poor, the sliver phenomenon of fruit.Preferably, in step (5), releasing agent is ammonium bromide saturated solution.
Further, in step (5) sample-melting stove melt temperature be 950 DEG C～1100 DEG C, the melting time be 10min～
20min.
Preferably, the front time of repose of described melting time is 2min, body of heater duration of oscillation 12min, rear time of repose
1min.
Step (5) melting is taken out after terminating, and fuse piece is placed on cooling in the environment of 20 DEG C～28 DEG C of room temperature.
Further, in platinum yellow crucible, the mass ratio of platinum and gold is 95:5, inner bottom surface diameter 30mm, for ensureing molten mass
Analysis surface smoothness, its bottom thickness should be greater than 1mm.
Heretofore described silicomanganese ball sample is processed by GB/T 4010 regulation using front, silicomanganese after treatment
Ball sample should make described silicomanganese ball sample particle diameter be less than 0.075mm by the sieve aperture of 200 mesh (aperture is 0.075mm).
The present invention can carry out detection silicon and P elements using x-ray fluorescence spectrometry method through the fuse piece that said method is obtained
Content.
Method provided by the present invention, silicomanganese ball sample particle size reduction, and without pre-oxidation treatment, after fuse piece is made in melting
The Check-Out Time carrying out element silicon during fluorescence analysiss was foreshortened to 2 hours by original 8 hours, and can detect element silicon simultaneously
And P elements, decrease the independent operation detecting P elements, simplify operational approach, reduce analysis cost, reduce labor intensity,
Improve checkability；And the assay shakiness solving tabletting-fluorescence analysis method granularity effect and mineral effect and leading to
Fixed.
Brief description
Fig. 1 is the canonical plotting of element silicon；
Fig. 2 is the standard curve of P elements；
Fig. 3 is the schematic diagram of sample preparation step (1) operational approach；
Fig. 4 is the schematic diagram of sample preparation step (2) operational approach；
Fig. 5 is the schematic diagram of sample preparation step (3) operational approach；
Fig. 6 is the schematic diagram of sample preparation step (4) operational approach.
Component label instructions
1 platinum yellow crucible
2 mixed fluxs
3 oxidant fluxs
4 silicomanganese ball alloy samples
Specific embodiment
Below by way of particular specific embodiment, embodiments of the present invention are described, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.The present invention can also be by addition different concrete
Embodiment is carried out or applies, and the every details in this specification can also be based on different viewpoints and application, is not carrying on the back
Carry out various modifications and changes under the spirit of the present invention.It should be noted that, in the case of not conflicting, following examples and reality
Apply the feature in example can be mutually combined.
Refer to Fig. 1 to Fig. 6.It should be noted that the diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of invention, only shows the assembly relevant with the present invention rather than then according to package count during actual enforcement in schema
Mesh, shape and size are drawn, and during its actual enforcement, the kenel of each assembly, quantity and ratio can be a kind of random change, and its
Assembly layout kenel is likely to increasingly complex.
In step (1) of the present invention, mixed flux consumption is 6.0000g～8.000g；Oxidant in step (2)
The consumption of flux is 0.5000g～2.0000g；In step (3), the consumption of silicomanganese ball sample is 0.1000g～0.5000g；Step
Suddenly in (5), releasing agent consumption is 0.3ml～0.5ml.Carry out the sample preparation fuse piece that any combinations obtain within this range and belong to this
The protection domain of invention.
The automatic sample-melting stove being adopted is the automatic sample-melting stove of RYL-05 type of Luoyang Dynastat experimental facilitiess company limited.
It is pure that the flux being adopted is analysis.
The preparation of silicomanganese ball alloy fuse piece
In embodiments of the present invention, in step (1), mixed flux consumption is 8.000g；Oxidant flux in step (2)
Consumption be 1.0000g；In step (3), the consumption of silicomanganese ball sample is 0.2000g；In step (5), releasing agent consumption is
0.5ml.
Specifically sample preparation step is：
(1) weigh 8.0000g Li2B4O7And LiBO2Mixed flux, be placed in platinum yellow crucible, pave, wherein Li2B4O7
And LiBO2Mass percent be respectively 67% and 33%；
(2) weigh 1.0000g KNO3Concentration is placed in the surface centre position of flux in the platinum yellow crucible in step (1)；
(3) weigh 0.2000g silicomanganese ball sample, be placed in above step (2) gained platinum yellow crucible inner oxidizing agent flux；
(4) by the silicomanganese ball sample in centre position in step (3) and oxidant flux and mixed flux stirring and evenly mixing, stir
Avoid sample and platinum yellow crucible bottom and sidewall contact during mixing, mix；
(5) instill 0.5ml NH along platinum yellow crucible wall in step (4) gained sample4Br saturated solution, puts into molten sample
In stove, melting 15min takes out, and wherein, melt temperature is 1000 DEG C, and the front time of repose of melting is 2min, body of heater duration of oscillation
12min, rear time of repose 1min, fuse piece are placed on cooling in the environment of 20 DEG C of room temperature, that is, obtain the glass of silicomanganese ball alloy
Fuse piece.
The analysis of x-ray fluorescence spectrometry instrument
Carry out element silicon, phosphorus element content detection using x-ray fluorescence spectrometry instrument.
Wherein, the x-ray fluorescence spectrometry instrument being adopted is the Simultix 14 type X-ray of Rigaku Co., Ltd.
Fluorescence spectrophotometer, analysis process Instrumental imposes a condition and is shown in Table 1.
Table 1X- ray fluorescence spectrometer imposes a condition
| Element | Light tube voltage | Tube current | Crystal | 2 θ angles | PHA scope |
| Si | 50 | 60 | RX4 | 144.78 | 100-300 |
| P | 50 | 60 | GE | 141.19 | 100-300 |
1st, being plotted as of standard curve：Standard sample used in the present invention all requires according to the sample preparation with sample in addition
Process, that is, silicomanganese standard sample after treatment should make described silicomanganese mark by the sieve aperture of 200 mesh (aperture is 0.075mm)
Quasi- sample particle diameter is less than 0.075mm.Silicomanganese ball examination with the silicomanganese standard sample of different content with through humid analysis definite value respectively
Sample several, with sample identical fluorescence analysiss under the conditions of tested, then respectively with measurement intensity as vertical coordinate, phosphorus unit
Element, the percentage composition of element silicon are abscissa, draw standard curve, and wherein, Fig. 1 is the standard curve of element silicon, its phase relation
Number is shown in Table 2；Fig. 2 is the standard curve of P elements, and correlation coefficient is shown in Table 3.
The calibration curve coefficient correlation of table 2 element silicon
The calibration curve coefficient correlation of table 3 P elements
2nd, in sample silicon, phosphorus content mensure：Weigh 10 silicomanganese ball alloy samples respectively, according to silicomanganese ball alloy fuse piece
Preparation method carry out sample preparation, after prepared fuse piece, tested under above-mentioned x-ray fluorescence spectrometry instrument imposes a condition, measured strong
From standard curve, after degree, obtain the percentage composition of silicon and phosphorus, the results are shown in Table 4.
3rd, comparative test：Take above-mentioned 10 samples respectively, carry out the mensure of silicon, phosphorus content using conventional humid analysis,
Measurement result is shown in Table 4.
Table 4 adopts the silicon of sample 1-10, phosphorus element content and the humid analysis result pair of present invention method test
According to
The assay method that data above can be seen that embodiment of the present invention employing measures silicomanganese ball Silicon In Alloys, phosphorus content
Less with humid analysis phase ratio error, illustrate the inventive method accurately and reliably.And, the inventive method good stability.
And the fuse piece that method for making sample of the present invention is made, when carrying out fluorescence analysiss, during the detection of element silicon
Between be 2 hours, compared with the 8 of humid analysis hours, effectively shorten the time, improve work efficiency；The present invention is permissible simultaneously
Detection silicon, P elements, simplify operational approach than the operation of detection P elements independent in conventional method, reduction is parsed into simultaneously
This, reduce labor intensity.
Above-described embodiment only principle of the illustrative present invention and its effect, not for the restriction present invention.Any ripe
The personage knowing this technology all can carry out modifications and changes without prejudice under the spirit and the scope of the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
All equivalent modifications becoming or change, must be covered by the claim of the present invention.
Claims (7)
1. a kind of MTG YBCO bulk method of x-ray fluorescence analysis silicomanganese ball Silicon In Alloys element and phosphorus element content, its feature exists
In comprising the steps：
(1) weigh mixed flux, be placed in platinum yellow crucible, pave；
(2) weigh oxidant flux, concentrate the surface centre position being placed in mixed flux in the platinum yellow crucible of step (1)；
(3) weigh silicomanganese ball sample, be placed in above step (2) gained platinum yellow crucible inner oxidizing agent flux；
(4) by the silicomanganese ball sample in centre position in platinum yellow crucible in step (3) and oxidant flux and mixed flux stirring
Mix, silicomanganese ball sample in whipping process, should be avoided to contact with the side wall of platinum yellow crucible and bottom with oxidant flux；
(5) instill releasing agent along platinum yellow crucible wall in step (4) gained sample, then platinum yellow crucible and sample are put into molten
Take out after melting in sample stove, after fuse piece is sufficiently cool, that is, obtain the bead of silicomanganese ball alloy.
2. MTG YBCO bulk method according to claim 1 it is characterised in that in step (1) mixed flux consumption be
6.0000g～8.000g；In step (2), the consumption of oxidant flux is 0.5000g～2.0000g；Silicomanganese ball in step (3)
The consumption of sample is 0.1000g～0.5000g；In step (5), releasing agent consumption is 0.3ml～0.5ml.
3. MTG YBCO bulk method according to claim 1 is it is characterised in that the described mixed flux of step (1) is Li2B4O7
And LiBO2Mixture, Li2B4O7And LiBO2Mass percent be respectively 67% and 33%.
4. MTG YBCO bulk method according to claim 1 is it is characterised in that oxidant flux described in step (2) is
Potassium nitrate.
5. MTG YBCO bulk method according to claim 1 it is characterised in that in step (5) releasing agent be ammonium bromide saturation
Solution.
6. MTG YBCO bulk method according to claim 5 it is characterised in that in step (5) melt temperature of sample-melting stove be
950 DEG C～1100 DEG C, the melting time is 10min～20min.
7. MTG YBCO bulk method according to claim 6 is it is characterised in that the front time of repose of described melting time is
2min, body of heater duration of oscillation 12min, rear time of repose 1min.
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|---|---|---|---|---|
| CN108982563A (en) * | 2018-08-03 | 2018-12-11 | 武汉科技大学 | The preparation method of the XRF analysis sheet glass of demolding aids effect |
| CN109358083A (en) * | 2018-12-14 | 2019-02-19 | 南京钢铁股份有限公司 | A kind of rapid analysis method for silicon, manganese, P elements in silicomangan |
| CN109358082A (en) * | 2018-12-14 | 2019-02-19 | 南京钢铁股份有限公司 | A kind of method that MTG YBCO bulk-x-ray fluorescence measures alloying element in ferrotianium |
| CN109358080A (en) * | 2018-12-14 | 2019-02-19 | 南京钢铁股份有限公司 | A kind of MTG YBCO bulk-X fluorescence spectrum method measuring ferro-molybdenum major and minor component |
| CN110596168A (en) * | 2019-10-28 | 2019-12-20 | 五矿营口中板有限责任公司 | Sample preparation method of silicon-manganese alloy molten sample for spectral analysis |
| CN111239172A (en) * | 2020-02-24 | 2020-06-05 | 河北龙凤山铸业有限公司 | Method for determining phosphorus content in coal |
| CN112649455A (en) * | 2020-12-18 | 2021-04-13 | 山东莱钢永锋钢铁有限公司 | Fluorescence detection method for steel plant |
| CN113466274A (en) * | 2021-06-07 | 2021-10-01 | 宁夏建龙龙祥钢铁有限公司 | Preparation method for determining manganese-silicon-phosphorus sample in manganese-silicon alloy by X-ray fluorescence method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108982563A (en) * | 2018-08-03 | 2018-12-11 | 武汉科技大学 | The preparation method of the XRF analysis sheet glass of demolding aids effect |
| CN108982563B (en) * | 2018-08-03 | 2021-02-19 | 武汉科技大学 | Method for preparing glass sheet for XRF analysis of release aid effect |
| CN109358083A (en) * | 2018-12-14 | 2019-02-19 | 南京钢铁股份有限公司 | A kind of rapid analysis method for silicon, manganese, P elements in silicomangan |
| CN109358082A (en) * | 2018-12-14 | 2019-02-19 | 南京钢铁股份有限公司 | A kind of method that MTG YBCO bulk-x-ray fluorescence measures alloying element in ferrotianium |
| CN109358080A (en) * | 2018-12-14 | 2019-02-19 | 南京钢铁股份有限公司 | A kind of MTG YBCO bulk-X fluorescence spectrum method measuring ferro-molybdenum major and minor component |
| CN110596168A (en) * | 2019-10-28 | 2019-12-20 | 五矿营口中板有限责任公司 | Sample preparation method of silicon-manganese alloy molten sample for spectral analysis |
| CN111239172A (en) * | 2020-02-24 | 2020-06-05 | 河北龙凤山铸业有限公司 | Method for determining phosphorus content in coal |
| CN112649455A (en) * | 2020-12-18 | 2021-04-13 | 山东莱钢永锋钢铁有限公司 | Fluorescence detection method for steel plant |
| CN113466274A (en) * | 2021-06-07 | 2021-10-01 | 宁夏建龙龙祥钢铁有限公司 | Preparation method for determining manganese-silicon-phosphorus sample in manganese-silicon alloy by X-ray fluorescence method |
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