CN103149073A - Molten sample preparation method of silicon-iron, silicon-calcium-barium, silicon-manganese, aluminum-iron or titanium-iron alloy sample for X-ray fluorescence spectroscopy - Google Patents
Molten sample preparation method of silicon-iron, silicon-calcium-barium, silicon-manganese, aluminum-iron or titanium-iron alloy sample for X-ray fluorescence spectroscopy Download PDFInfo
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Abstract
The invention discloses a simple, quick and more reliable molten sample preparation method capable of avoiding corroding a platinum-gold crucible. The method comprises the following steps: a. weighing right amounts of lithium tetraborate, lithium carbonate, oxidizer and sample material, and evenly mixing to obtain balls; b. putting the balls obtained in the step a into a crucible with graphite powder on the bottom, and carrying out melting preoxidation in a high-temperature furnace; taking out the crucible, and cooling to obtain the preoxidated molten balls; c. weighing a certain amount of fluxing agent, adding the fluxing agent into the platinum gold crucible, and adding releasing agent and molten balls; melting at 1100-1200 DEG C for 12-20 minutes, taking out, shaking up, and removing bubbles; and melting, taking out, shaking up, and cooling by standing to obtain the molten sheet. The invention does not need to carry out wall built-up treatment on the platinum gold crucible, simplifies the operation, and basically avoids corroding the platinum gold crucible in the preoxidation process; and the prepared molten sheet is uniform and flawless, and satisfies the requirements of X-ray fluorescence spectroscopy.
Description
Technical field
The invention belongs to technical field of analysis and detection, be specifically related to the melting method for making sample that a kind of X-ray fluorescence spectra is analyzed ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium sample.
Background technology
The alloys such as ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum, ferrotianium are mainly used to deoxidizer and the adjuvant as steel-making, with technique and the performance of improving steel, there is strict standard in country to its content, its each element acceptability limit is relative narrower but, and each constituent content is to affect direct, the main factor of its performance.Therefore, the alloy chemical composition is carried out fast, accurate analysis is very important.At present, primary and secondary trace element analysis in alloy, domestic metallurgy industry generally adopts the traditional chemical analysis to carry out single element and measures, these method complex operations, analytical cycle is long, and efficient is low, and need more and more to be not suitable with the modern production control requirement with hazardous chemicalses such as perchloric acid, hydrofluorite.
X ray fluorescence spectrometry has that analyst coverage is wide, precision is high, the easy characteristics such as fast, is widely used in technical analysis.X-ray fluorescence spectra is analyzed the technology of preparing that the alloy difficult point is sample, generally adopts two kinds of pressed disc method and fusion methods.Pressed disc method is easy and simple to handle, but due to granularity effect and matrix effect, the analysis result accuracy is not ideal enough, adopt the melting sample preparation method that sample is made the uniform glass fuse piece, can imitate the elimination granularity effect, reduce simultaneously the absorption enhancement effect of matrix, improve the accuracy of xrf analysis.But for belonging to the iron alloy fusing sample because a large amount of metals in sample exist, make platinum yellow gold crucible alloying when high-temperature fusion, the crucible Eroded has limited the x ray fluorescence spectrometry application.
CN101832891A discloses a kind of iron alloy fusing sample preparation method for the X-ray fluorescence spectra analysis, and described method is carried out according to following step: platinum yellow gold crucible wall built-up; The configuration oxygenant; Iron alloy samples is carried out pre-oxidation; Iron alloy samples melting sample preparation.The method has 2 deficiencies: the one, need platinum yellow gold crucible (being called for short the platinum yellow crucible) wall built-up and sample preoxidation process, and strict and loaded down with trivial details to the wall built-up operation, slightly make mistakes, will cause valuable platinum yellow crucible to produce corrosion; The 2nd, the pre-oxidation agent is not selected according to the characteristic of analytic sample, and general is lithium carbonate, sodium carbonate and lithium nitrate, affects the adequacy of oxidation.
CN101592571B discloses a kind of X-fluorescence fusion method and has measured alloying element content method in ferrotianium, vanadium iron, adopt in strict accordance with proportioning in the sample preparation of normal glass sheet and tested sample glass sheet preparation process and add order, layering is inserted flux, highly basic, detected sample, release agent etc. in the platinum yellow crucible, coordinate melt temperature, the control of melting time, successfully prepare ferrotianium or vanadium iron glass sheet under the condition that the platinum yellow crucible is not caused corrosion and damage.This invention melting film-making pre-oxidation is carried out in the platinum yellow crucible equally, and operating conditions is harsh, slightly makes mistakes, and will cause valuable platinum yellow crucible to produce corrosion.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of fast easy and avoid more reliably corroding the melting method for making sample of platinum yellow crucible.
The technical solution adopted for the present invention to solve the technical problems is: X-ray fluorescence spectra is analyzed the melting method for making sample of ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium sample, comprises the steps:
The lithium carbonate of a, the lithium tetraborate that accurately takes 2 weight portions, 1 weight portion and the test portion of 0.2 weight portion mix, and are rolled into spherical; Described test portion is ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium test portion;
B, the glomerate material of step a parcel is put into the rebasing crucible of dag, then be placed in high temperature furnace and carry out the molten prepolymer oxidation; Take out crucible, cooling, obtain the molten ball after pre-oxidation;
C, take a certain amount of flux in the platinum yellow crucible, the molten ball that adds release agent and step b to obtain; Then be placed in the temperature environment melting 12～20min of 1100～1200 ℃, take out, shake up, catch up with the pure qi (oxygen) bubble; And then be placed in the temperature environment melting 12～20min of 1100～1200 ℃, and take out, shake up, standing cooling, obtain fuse piece;
D, fuse piece is taken out, is cooled to room temperature, be put in exsiccator after sign.
Wherein, in step a, be test portion to be rolled into spherical with filter paper.
Wherein, in said method step b, described molten prepolymer oxidation refers to that in the high temperature furnace of 400 ℃, fire door stays the 15mm gap, is warming up to gradually 850～900 ℃, with material melting 14～16min.
Wherein, flux described in said method step c is the lithium tetraborate of 4 weight portions.
Wherein, in said method, when the test portion described in step a was ferrosilicon, Si-Ca-Ba, ferro-aluminum or ferro-titanium test portion, the release agent described in step c was the 0.4mL300g/L liquor kalii iodide; When the test portion described in step a was the silicomangan test portion, the release agent described in step c was the 0.4mL200g/L lithium-bromide solution.
The invention has the beneficial effects as follows: for solving in the prior art of melting film-making metal alloy sample to the corrosion difficult problem of platinum yellow crucible, the vacuum remelting casing process need be used Special Equipment, is difficult to apply; Platinum yellow crucible wall built-up, method for pre-oxidizing, wall built-up complex operation and strict, careless slightly or preoxidation process can not be completely oxidized all can corrode the platinum yellow crucible; The molten rear melting flaking method complex operation of acid is unwell to and produces check in enormous quantities.The invention provides a kind of new melting method for making sample of avoiding the platinum yellow crucible to be corroded, the method does not need to carry out platinum yellow crucible wall built-up to be processed, easy operation.The present invention with the lithium tetraborate-lithium carbonate of specific proportioning as the agent of pre-oxidation melt oxidation, with crucible pre-oxidation fusing sample at the bottom of graphite pads, utilize the high temperature replacement reaction of mixed melting oxygenant, guaranteed that all simple substance element oxidations are fully complete, solved the difficult problem of the difficult oxidation of ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium, infusibility solution, the risk that when fundamentally having avoided pre-oxidation, the platinum yellow crucible is etched, be spherical after the sample pre-fusion simultaneously, conveniently be transferred to platinum yellow crucible melting film-making; Use suitable flux, melting time and temperature in step c melting film-making process of the present invention, match with step a and b, make the fuse piece homogeneous transparent zero defect of preparation, can eliminate mineral effect and granularity effect fully, satisfy X-ray fluorescence spectra and analyze requirement.Further, the present invention according to the metal alloy sample characteristics of for example, selects different release agents in step c, and the bead of preparation is easier to the demoulding.
Embodiment
The below utilizes embodiment and embodiment, and the present invention is further described.
X-ray fluorescence spectra of the present invention is analyzed the melting method for making sample of ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium sample, comprises the steps:
The lithium carbonate of a, the lithium tetraborate that accurately takes 2 weight portions, 1 weight portion and the test portion of 0.2 weight portion mix, and are rolled into spherical; Described test portion is ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium test portion;
B, the glomerate material of step a parcel is put into the rebasing crucible of dag, then be placed in high temperature furnace and carry out the molten prepolymer oxidation; Take out crucible, cooling, obtain the molten ball after pre-oxidation;
C, take a certain amount of flux in the platinum yellow crucible, the molten ball that adds release agent and step b to obtain; Then be placed in the temperature environment melting 12～20min of 1100～1200 ℃, take out, shake up, catch up with the pure qi (oxygen) bubble; And then be placed in the temperature environment melting 12～20min of 1100～1200 ℃, and take out, shake up, standing cooling, obtain fuse piece;
D, fuse piece is taken out, is cooled to room temperature, be put in exsiccator after sign.
In bead X-fluorescence method to the containing metal sample, usually after lithium tetraborate fusing, cooling wall built-up then adds sample and Ba0 in crucible in the platinum yellow crucible
2, Na
2O
2Carry out low-temperature oxidation in oxygenant.But the oxidant content that this method needs is larger, causes dilution ratio excessive, and the determination of trace element fluctuation is large, and the pre-oxidation treatment time is longer, and the lithium tetraborate of wall built-up easily breaks, and is difficult to avoid crucible by the risk of etch.Lithium tetraborate and lithium carbonate are at high temperature weak oxidants, has function preferably at the oxidation fusion connection metal, lithium carbonate can prevent the sample assembly, the gas that produces and boiling are few, sample does not lose, lithium tetraborate-lithium carbonate mixed flux melts in the crucible at the bottom of graphite pads and is spherical after cooling, molten ball convenient transfer.Therefore the alloys such as ferrosilicon, ferro-aluminum, ferrotianium, Si-Ca-Ba we directly select the lithium tetraborate of specific proportioning and lithium carbonate mixed flux as pre-oxidation melting agent, obtained good effect.
In step c, if melt temperature lower than 1100 ℃, smelt flow is bad, principal element X-fluorescence intensity is unstable and higher, so for final measurement result is stable, melt temperature of the present invention between 1100～1200 ℃, melting time 12～20min.
Preferably, in order to make the pre-oxidation effect best, in said method step b, described molten prepolymer oxidation refers to that in the high temperature furnace of 400 ℃, fire door stays the 15mm gap, is warming up to gradually 850～900 ℃, with material melting 14～16min.
Sample size of the present invention, oxidant content, flux amount, all to take into account pre-oxidation and fuse piece, should guarantee that sample pre-oxidation is complete, look after again the print found evenly, without bubble, do not break, also to guarantee the preci-sion and accuracy of the mensuration of main amount, micro constitutent.The present invention is when adding solvent, and preferred described flux is the lithium tetraborate of 4 weight portions.
Preferably, in said method, when the test portion described in step a was ferrosilicon, Si-Ca-Ba, ferro-aluminum or ferro-titanium test portion, the release agent described in step c was the 0.4mL300g/L liquor kalii iodide; When the test portion described in step a was the silicomangan test portion, the release agent described in step c was the 0.4mL200g/L lithium-bromide solution.
Below by embodiment, the specific embodiment of the present invention is further described, but therefore protection scope of the present invention is not limited in the middle of embodiment.
The preparation of embodiment one Antaciron bead
1, molten prepolymer oxidation in crucible at the bottom of graphite pads
Take 0.2g ± 0.1mg ferrosilicon test portion, be placed in the taper filter paper that fills 2.0000g lithium tetraborate, 1.0000g lithium carbonate, sample is stirred evenly, be bundled into spherically, put into the crucible at the bottom of graphite pads, be placed in 400 ℃ of high temperature furnaces, fire door stays the 15mm gap, is warming up to gradually 850 ℃～900 ℃, melting 15min, take out, cooling.
2, in the platinum yellow crucible, melting prepares bead
To melt the ball taking-up and sweep clean dag, be placed in the platinum yellow crucible that fills the 4.0000g lithium tetraborate, add the 0.4mL300g/L liquor kalii iodide.At 1120 ± 20 ℃ of melting 15min, take out, expose crucible at the bottom of rotation catch up with the pure qi (oxygen) bubble, fully shake up, again at 1120 ± 20 ℃ of melting 15min, take out, expose crucible at the bottom of rotation catch up with the pure qi (oxygen) bubble, shake up fast, level standing cooling after, fuse piece is poured on clean filter paper, after sign, namely obtain uniform bead, be used for the content that the X-ray fluorescence spectra analytic approach is measured the elements such as Antaciron silicon, manganese, phosphorus, aluminium, chromium, calcium simultaneously.
The preparation of embodiment two silicomangan beads
1, molten prepolymer oxidation in crucible at the bottom of graphite pads
Take 0.2g ± 0.1mg silicomanganese test portion, be placed in the taper filter paper that fills 2.0000g lithium tetraborate, 1.0000g lithium carbonate, sample is stirred evenly, be bundled into spherically, put into the crucible at the bottom of graphite pads, be placed in 400 ℃ of high temperature furnaces, fire door stays the 15mm gap, is warming up to gradually 850 ℃～900 ℃, melting 15min, take out, cooling.
2, in the platinum yellow crucible, melting prepares bead
To melt the ball taking-up and sweep clean dag, be placed in the platinum yellow crucible that fills the 4.0000g lithium tetraborate, add the 0.4mL200g/L lithium-bromide solution.At 1120 ± 20 ℃ of melting 15min, take out, expose crucible at the bottom of rotation catch up with the pure qi (oxygen) bubble, fully shake up, again at 1120 ± 20 ℃ of melting 15min, take out, expose crucible at the bottom of rotation catch up with the pure qi (oxygen) bubble, shake up fast, level standing cooling after, fuse piece is poured on clean filter paper, after sign, namely obtain uniform bead, be used for the content that the X-ray fluorescence spectra analytic approach is measured the elements such as silicomangan silicon, manganese, phosphorus simultaneously.
The preparation of embodiment three calsibar alloy beads
1, molten prepolymer oxidation in crucible at the bottom of graphite pads
Take 0.2g ± 0.1mg calsibar alloy test portion, be placed in the taper filter paper that fills 2.0000g lithium tetraborate, 1.0000g lithium carbonate, sample is stirred evenly, be bundled into spherically, put into the crucible at the bottom of graphite pads, be placed in 400 ℃ of high temperature furnaces, fire door stays the 15mm gap, is warming up to gradually 850 ℃～900 ℃, melting 15min, take out, cooling.
2, in the platinum yellow crucible, melting prepares bead
To melt the ball taking-up and sweep clean dag, be placed in the platinum yellow crucible that fills the 4.0000g lithium tetraborate, add the 0.4mL300g/L liquor kalii iodide.At 1120 ± 20 ℃ of melting 15min, take out, expose crucible at the bottom of rotation catch up with the pure qi (oxygen) bubble, fully shake up, again at 1120 ± 20 ℃ of melting 15min, take out, expose crucible at the bottom of rotation catch up with the pure qi (oxygen) bubble, shake up fast, level standing cooling after, fuse piece is poured on clean filter paper, after sign, namely obtain uniform bead, be used for the content that the X-ray fluorescence spectra analytic approach is measured the elements such as calsibar alloy silicon, calcium, barium aluminium, phosphorus simultaneously.
The preparation of embodiment four alfer beads
1, molten prepolymer oxidation in crucible at the bottom of graphite pads
Take 0.2g ± 0.1mg alfer test portion, be placed in the taper filter paper that fills 2.0000g lithium tetraborate, 1.0000g lithium carbonate, sample is stirred evenly, be bundled into spherically, put into the crucible at the bottom of graphite pads, be placed in 400 ℃ of high temperature furnaces, fire door stays the 15mm gap, is warming up to gradually 850 ℃～900 ℃, melting 15min, take out, cooling.
2, in the platinum yellow crucible, melting prepares bead
To melt the ball taking-up and sweep clean dag, be placed in the platinum yellow crucible that fills the 4.0000g lithium tetraborate, add the 0.4mL300g/L liquor kalii iodide.At 1120 ± 20 ℃ of melting 15min, take out, expose crucible at the bottom of rotation catch up with the pure qi (oxygen) bubble, fully shake up, again at 1120 ± 20 ℃ of melting 15min, take out, expose crucible at the bottom of rotation catch up with the pure qi (oxygen) bubble, shake up fast, level standing cooling after, fuse piece is poured on clean filter paper, after sign, namely obtain uniform bead, be used for the content that the X-ray fluorescence spectra analytic approach is measured the elements such as alfer aluminium, silicon, phosphorus simultaneously.
The preparation of embodiment five ferrotianium beads
1, molten prepolymer oxidation in crucible at the bottom of graphite pads
Take 0.2g ± 0.1mg ferro-titanium test portion, be placed in the taper filter paper that fills 2.0000g lithium tetraborate, 1.0000g lithium carbonate, sample is stirred evenly, be bundled into spherically, put into the crucible at the bottom of graphite pads, be placed in 400 ℃ of high temperature furnaces, fire door stays the 15mm gap, is warming up to gradually 850 ℃～900 ℃, melting 15min, take out, cooling.
2, in the platinum yellow crucible, melting prepares bead
To melt the ball taking-up and sweep clean dag, be placed in the platinum yellow crucible that fills the 4.0000g lithium tetraborate, add the 0.4mL300g/L liquor kalii iodide.At 1120 ± 20 ℃ of melting 15min, take out, expose crucible at the bottom of rotation catch up with the pure qi (oxygen) bubble, fully shake up, again at 1120 ± 20 ℃ of melting 15min, take out, expose crucible at the bottom of rotation catch up with the pure qi (oxygen) bubble, shake up fast, level standing cooling after, fuse piece is poured on clean filter paper, after sign, namely obtain uniform bead, be used for the content that the X-ray fluorescence spectra analytic approach is measured the elements such as ferro-titanium titanium, silicon, phosphorus, manganese, aluminium, manganese simultaneously.
Embodiment six accuracy tests
The fuse piece that makes with the inventive method is used for the X-ray fluorescence spectra analysis, and its result and chemical method analysis result contrast, with paired data t check.Show each composition t as table 1 to table 5 statistics
StatisticsAll less than t
Critical, illustrate that there are not system's difference in the fuse piece measurement result and the chemical method that make with the inventive method, illustrate that the inventive method accurately and reliably.
Table 1 ferrosilicon and chemical method results of comparison
Table 2 manganese silicon and chemical method results of comparison
Table 3 Si-Ca-Ba and chemical method results of comparison
Table 4 ferro-aluminum and chemical method results of comparison
Table 5 ferrotianium and chemical method results of comparison
Claims (4)
1.X the melting method for making sample of fluorescent x ray spectroscopy x ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium sample is characterized in that comprising the steps:
The lithium carbonate of a, the lithium tetraborate that accurately takes 2 weight portions, 1 weight portion and the test portion of 0.2 weight portion mix, and are rolled into spherical; Described test portion is ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium test portion;
B, the glomerate material of step a parcel is put into the rebasing crucible of dag, then be placed in high temperature furnace and carry out the molten prepolymer oxidation; Take out crucible, cooling, obtain the molten ball after pre-oxidation;
C, take a certain amount of flux in the platinum yellow crucible, the molten ball that adds release agent and step b to obtain; Then be placed in the temperature environment melting 12～20min of 1100～1200 ℃, take out, shake up, catch up with the pure qi (oxygen) bubble; And then be placed in the temperature environment melting 12～20min of 1100～1200 ℃, and take out, shake up, standing cooling, obtain fuse piece;
D, fuse piece is taken out, is cooled to room temperature, be put in exsiccator after sign.
2. X-ray fluorescence spectra according to claim 1 is analyzed the melting method for making sample of ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium sample, it is characterized in that: in step b, described molten prepolymer oxidation refers in the high temperature furnace of 400 ℃, fire door stays the 15mm gap, be warming up to gradually 850～900 ℃, with material melting 14～16min.
3. X-ray fluorescence spectra according to claim 1 is analyzed the melting method for making sample of ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium sample, and it is characterized in that: flux described in step c is the lithium tetraborate of 4 weight portions.
4. X-ray fluorescence spectra according to claim 1 is analyzed the melting method for making sample of ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium sample, it is characterized in that: when the test portion described in step a was ferrosilicon, Si-Ca-Ba, ferro-aluminum or ferro-titanium test portion, the release agent described in step c was the 0.4mL300g/L liquor kalii iodide; When the test portion described in step a was the silicomangan test portion, the release agent described in step c was the 0.4mL200g/L lithium-bromide solution.
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| CN114034536A (en) * | 2021-11-15 | 2022-02-11 | 新疆八一钢铁股份有限公司 | Automatic demoulding sample preparation method for chemical analysis of silicon-manganese alloy |
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