CN107271253A - The method that ferroalloy class sample founds X-ray fluorescence spectra analysis sheet glass - Google Patents
The method that ferroalloy class sample founds X-ray fluorescence spectra analysis sheet glass Download PDFInfo
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- CN107271253A CN107271253A CN201710729273.3A CN201710729273A CN107271253A CN 107271253 A CN107271253 A CN 107271253A CN 201710729273 A CN201710729273 A CN 201710729273A CN 107271253 A CN107271253 A CN 107271253A
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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
- G01N1/38—Diluting, dispersing or mixing samples
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
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Abstract
The present invention relates to a kind of method that ferroalloy class sample founds X-ray fluorescence spectra analysis sheet glass, belong to metallurgy industry ferroalloy class sample chemical analysis technical field.Technical scheme is：Include following processing step：（1）Graphite powder is covered in the inner surface of evaporating dish；（2）Poured into after the alloy sample of 0.3 ± 0.0002g potassium nitrate, 7.7 ± 0.0002g lithium tetraborate and lithium metaborate mixed flux and 0.2 ± 0.0002g is fully mixed in evaporating dish；（3）It is put into Muffle furnace, natural cooling formation pie sample after glassy state is melted at 920 DEG C；（4）Pie sample is put into platinum crucible, heating melting：Melt to melt to wave melting 9min at 5min, 1100 DEG C and add at 2min, 1100 DEG C at 800 DEG C and analyze pure lithium bromide；（5）Cooling and shaping in mould are poured into, sheet glass is made.The beneficial effects of the invention are as follows：Ferroalloy class mother glass piece can be quickly founded, with the higher degree of accuracy, repeatability, repeatability.
Description
Technical field
The present invention relates to a kind of method that ferroalloy class sample founds X-ray fluorescence spectra analysis sheet glass, belong to smelting
Golden industry ferroalloy class sample chemical analysis technical field.
Background technology
At present, due to the characteristic of ferroalloy class sample, easy alloying platinum crucible, fusion cast glass piece is difficult, limits always
Make the application on Xray fluorescence spectrometer.Magazine publication wall built-up crucible oxygenation pretreatment method, the method complex operation, repeatability
Difference, corrosion of crucible probability is big.Also useful graphite substrate, filter paper, which is wrapped up, uses the mixed flux method for pretreating such as boric acid, natrium carbonicum calcinatum,
This method has four deficiencies：（1）Need the carbonization filter paper that first opens the door, the bad control of furnace temperature；（2）Because reaction is violent, easily occur
Sample, which collapses, to be splashed, and causes sample loss, and repeatability is bad；（3）There is sample transfer dilution again, easily cause sample transfer not
Completely, measurement result is inaccurate；（4）The bad control of time length, the time is too short, and pre-oxidation is incomplete, and the time is oversize, and sample block holds
It is easy to foaming.Tested for this it is a kind of it is new it is simple, quick, stably, the method for the fusion cast glass piece of safety it is very necessary, expand X and penetrate
Line spectrofluorimetry technology reduces the environmental pollution that chemical method is brought in the application in alloy production field, and reduction is artificial
Labor intensity.
The content of the invention
It is an object of the present invention to provide a kind of method that ferroalloy class sample founds X-ray fluorescence spectra analysis sheet glass,
Ferroalloy class mother glass piece quickly, stably can be founded, and be analyzed by X-ray fluorescence spectra, measure ferroalloy class sample
Product chemical composition, solves problem present in background technology.
This practicality invention technical scheme be：
A kind of method that ferroalloy class sample founds X-ray fluorescence spectra analysis sheet glass, includes following processing step：
（1）By graphite powder uniform fold evaporating dish inner surface；
（2）By 0.3 ± 0.0002g potassium nitrate, 7.7 ± 0.0002g lithium tetraborate and lithium metaborate mixed flux and 0.2
After ± 0.0002g alloy sample is mixed, pour into above-mentioned evaporating dish, lithium tetraborate and the lithium metaborate mixed flux
It is 67% to match percent by volume:33%；
（3）The evaporating dish for filling flux and alloy sample is put into Muffle furnace, melted at 920 DEG C, to being melt into glass
Taken out after state, naturally cool to room temperature, form pie sample；
（4）After the graphite powder adhered on pie sample is cleaned up, it is put into platinum crucible, and by following procedure melting：
First：2min is melted at 800 DEG C；
Second：5min is melted at 1100 DEG C；
3rd：Wave melting 9min at 1100 DEG C, described to wave melting be exactly to wave platinum crucible while melting, and is added
Enter and analyze pure lithium bromide, melting terminates；
（5）Cooling and shaping in mould are poured into melting after terminating, sheet glass is made.
The step（2）The cumulative weight of middle potassium nitrate and lithium tetraborate and lithium metaborate mixed flux is 8g, ferroalloy
The granularity of sample is less than 150 mesh.
The step（3）In fill the evaporating dish of flux and alloy sample the melting time be at 920 DEG C in Muffle furnace
20min。
The step（1）The thickness of graphite powder is not less than 0.5mm, and requires that surface is smooth.
The sheet glass being made of the above method, its lower surface is used as analysis face, upper surface labeling.And by drawing fluorescence
Curve, measures ferroalloy class sample chemical composition.
The beneficial effects of the invention are as follows：Ferroalloy class mother glass piece can be quickly founded, and passes through X-ray fluorescence spectra
Analysis, measures ferroalloy class sample chemical composition, with the higher degree of accuracy, repeatability, repeatability.Expand XRF
Spectral analysis technique reduces the environmental pollution that chemical method is brought in the application in alloy production field.
Brief description of the drawings
Fig. 1 is schematic diagram after flux of the present invention and alloy sample are melted in Muffle furnace；
Fig. 2 is pie sample schematic diagram of the present invention；
Fig. 3 is that pie sample of the present invention is put into schematic diagram after platinum crucible；
Fig. 4 sheet glass schematic diagrames of the present invention.
Embodiment
Below in conjunction with accompanying drawing, by example, the invention will be further described.
A kind of method that ferroalloy class sample founds X-ray fluorescence spectra analysis sheet glass, includes following processing step：
（1）By graphite powder uniform fold evaporating dish inner surface；
（2）By 0.3 ± 0.0002g potassium nitrate, 7.7 ± 0.0002g lithium tetraborate and lithium metaborate mixed flux and 0.2
After ± 0.0002g alloy sample is well mixed, pour into above-mentioned evaporating dish, lithium tetraborate and the lithium metaborate mixing is molten
The proportioning of agent is 67%:33%；
（3）The evaporating dish for filling flux and alloy sample is put into Muffle furnace, melted at 920 DEG C, to being melt into glass
Taken out after state, naturally cool to room temperature, form pie sample；
（4）After the graphite powder adhered on pie sample is cleaned up, it is put into platinum crucible, and by following procedure melting：
First：2min is melted at 800 DEG C；
Second：5min is melted at 1100 DEG C；
3rd：Wave melting 9min at 1100 DEG C, described to wave melting be exactly to wave platinum crucible while melting, and is added
Enter and analyze pure lithium bromide, melting terminates；
（5）Cooling and shaping in mould are poured into melting after terminating, sheet glass is made.
In the present embodiment, the method that ferroalloy class sample founds X-ray fluorescence spectra analysis sheet glass, specifically according to
Following steps are carried out：
（1）Prepare 100ml porcelain evaporating dish, with graphite powder uniform fold inner surface, it is desirable to which graphite thickness is not less than
0.5mm, and be compacted with another evaporating dish, it is ensured that surface is smooth；
（2）0.3g is accurately weighed with measuring cup and analyzes pure KNO3, 7.7g lithium tetraborate and metaboric acid fully finely ground with agate mortar
Lithium mixed flux, lithium tetraborate and lithium metaborate mixed flux proportioning 67%+33%, it is desirable to which particle is uniform, fine size, weighs 0.2g
Alloy sample, it is desirable to which granularity is less than 150 mesh, and alleged flux is fully mixed with alloy sample, concentration, which is poured into, to be ready for
Evaporating dish center；
（3）The evaporating dish for filling flux and alloy sample is put into Muffle furnace, 20min is melted at 920 DEG C, to being melt into
After glassy state, accompanying drawing 1 is seen, taking-up is cooled to room temperature, and formation surface is smooth, neat in edge pie sample, sees accompanying drawing 2, uses tweezer
Son is taken out, and the graphite powder of attachment is cleaned with hairbrush；
（4）The pie sample cleaned out is put into platinum crucible, accompanying drawing 3 is seen, heats up and melts by following procedure：
First：2min is melted at 800 DEG C；Second：5min is melted at 1100 DEG C；3rd：Melting is waved at 1100 DEG C
9min, it is exactly to wave platinum crucible while melting to wave melting, melting 16min is amounted in platinum crucible, in 11min
When, the pure LiBr of analysis of a small spoon is added, melting terminates；
（5）Cooling and shaping in mould are poured into melting after terminating, sheet glass is made, accompanying drawing 4 is seen.Lower surface is used as analysis face, upper table
Face labeling.
Ferrosilicon, ferromanganese, silicomangan are melting into sheet glass by above method for making sample, and draw fluorescence curve, to numbering
Distinguish sample preparation 4 times, its measurement result such as table 1 for YSBC19601-90 ferrosilicon sample.
The ferrosilicon measurement result of table 1
Shown by above experimental data, the repeatability that the method for making sample has had, confirm that this method is linear good by curve,
, can be with practical application with the higher degree of accuracy, repeatability, repeatability.
Claims (4)
1. a kind of method that ferroalloy class sample founds X-ray fluorescence spectra analysis sheet glass, it is characterised in that comprising as follows
Processing step：
（1）By graphite powder uniform fold evaporating dish inner surface；
（2）By 0.3 ± 0.0002g potassium nitrate, 7.7 ± 0.0002g lithium tetraborate and lithium metaborate mixed flux and 0.2
After ± 0.0002g alloy sample is well mixed, pour into above-mentioned evaporating dish, lithium tetraborate and the lithium metaborate mixing is molten
The proportioning of agent is 67%:33%；
（3）The evaporating dish for filling flux and alloy sample is put into Muffle furnace, melted at 920 DEG C, to being melt into glass
Taken out after state, naturally cool to room temperature, form pie sample；
（4）After the graphite powder adhered on pie sample is cleaned up, it is put into platinum crucible, and by following procedure melting：
First：2min is melted at 800 DEG C；
Second：5min is melted at 1100 DEG C；
3rd：Wave melting 9min at 1100 DEG C, described to wave melting be exactly to wave platinum crucible while melting, and is added
Enter and analyze pure lithium bromide, melting terminates；
（5）Cooling and shaping in mould are poured into melting after terminating, sheet glass is made.
2. the method that ferroalloy class sample according to claim 1 founds X-ray fluorescence spectra analysis sheet glass, it is special
Levy and be：The step（2）The cumulative weight of middle potassium nitrate, lithium tetraborate and lithium metaborate mixed flux is 8g, ferroalloy examination
The granularity of sample is less than 150 mesh.
3. the method that ferroalloy class sample according to claim 1 founds X-ray fluorescence spectra analysis sheet glass, it is special
Levy and be：The step（3）In fill the evaporating dish of flux and alloy sample the melting time be at 920 DEG C in Muffle furnace
20min。
4. the method that ferroalloy class sample according to claim 1 founds X-ray fluorescence spectra analysis sheet glass, it is special
Levy and be：The step（1）The thickness of graphite powder is not less than 0.5mm, and requires that surface is smooth.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110646452A (en) * | 2019-08-29 | 2020-01-03 | 邯郸钢铁集团有限责任公司 | Method for measuring major elements in ferrochrome alloy by X fluorescence fuse link method |
| CN111141774A (en) * | 2020-01-21 | 2020-05-12 | 鞍钢股份有限公司 | Preparation method of sample sheet for iron alloy by X-ray fluorescence spectrum analysis |
| CN111521467A (en) * | 2020-06-04 | 2020-08-11 | 河北省地质实验测试中心 | Graphite detection method |
| CN113030140A (en) * | 2021-02-04 | 2021-06-25 | 江阴兴澄特种钢铁有限公司 | Preparation method of sample molten glass sheet for analysis by X-ray fluorescence spectrometry |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110646452A (en) * | 2019-08-29 | 2020-01-03 | 邯郸钢铁集团有限责任公司 | Method for measuring major elements in ferrochrome alloy by X fluorescence fuse link method |
| CN111141774A (en) * | 2020-01-21 | 2020-05-12 | 鞍钢股份有限公司 | Preparation method of sample sheet for iron alloy by X-ray fluorescence spectrum analysis |
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| CN113030140A (en) * | 2021-02-04 | 2021-06-25 | 江阴兴澄特种钢铁有限公司 | Preparation method of sample molten glass sheet for analysis by X-ray fluorescence spectrometry |
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