CN102607934A - X-ray fluorescence spectroscopy analysis fusion sample preparation method of aluminum, manganese, calcium and iron alloy - Google Patents
X-ray fluorescence spectroscopy analysis fusion sample preparation method of aluminum, manganese, calcium and iron alloy Download PDFInfo
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- CN102607934A CN102607934A CN201210057564XA CN201210057564A CN102607934A CN 102607934 A CN102607934 A CN 102607934A CN 201210057564X A CN201210057564X A CN 201210057564XA CN 201210057564 A CN201210057564 A CN 201210057564A CN 102607934 A CN102607934 A CN 102607934A
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Abstract
The invention discloses an X-ray fluorescence spectroscopy analysis fusion sample preparation method of an aluminum, manganese, calcium and iron alloy, which comprises the steps of: firstly, coating a uniform protection wall layer in a platinum crucible by using lithium tetraborate, then placing an aluminum, manganese, calcium and iron sample, an oxidizing agent, a lithium borate solvent and a releasing agent into the platinum crucible in which the protection wall is coated, uniformly mixing, and then pre-oxidizing the aluminum, manganese, calcium and iron sample; and finally, melting the pre-oxidized aluminum, manganese, calcium and iron sample, and cooling to obtain an aluminum, manganese, calcium and iron sample glass fuse piece, wherein the aluminum, manganese, calcium and iron sample is a detection sample or calibration sample of the aluminum, manganese, calcium and iron alloy, and the sample glass fuse piece is a detection sample glass fuse piece or calibration sample glass fuse piece of the aluminum, manganese, calcium and iron alloy. On the premise of no corrosion to the valuable platinum crucible, the glass fuse piece can be prepared, and the prepared sample is excellent and uniform, thus the mineral effect and the grain size effect are completely eliminated.
Description
Technical field
The invention belongs to technical field of analysis and detection, the fusion method for making sample is used in especially a kind of X-ray fluorescence spectra analysis of aluminium manganese Ca-Fe alloy.
Background technology
Alumal had obtained using widely as deoxidizer in steel production in recent years, though it has than great, in molten steel, was easy to, and can realize the advantage of alloying of manganese simultaneously, the Al that this deoxidizer generates in deoxidation process
2O
3Be strip, the toughness of steel and ductility are reduced.Simultaneously, because Al
2O
3Have high fusing point, when continuous casting, be easy to stop up the mouth of a river, be prone to cause the continuous casting accident.Find in alumal, to add calcium afterwards, and not only can improve Al
2O
3Inclusion morphology makes its nodularization, and then improves the toughness and the ductility of steel, and the adding of calcium can also make deoxidation products generate calcium-aluminate; Has low fusing point; Be easy to come-up, reduce the obstruction probability at the mouth of a river in the casting process, also make inclusion content of steel reduce.
Therefore, aluminium manganese Ca-Fe alloy is as a kind of novel ferroalloy kind, by use more and more widely; Wherein aluminium, manganese, calcium and iron are four main components, also be supplied materials clearing must examine element, though can adopt the conventional wet analysis to carry out element determination; But process is loaded down with trivial details, wastes time and energy.That instrument analytical method such as x ray fluorescence spectrometry have is easy, characteristics fast; But the fusion method for making sample is a difficult problem; Because the iron alloy samples of reductibility can cause strong corrosion to sample preparation vessel-platinum crucible; It is generally acknowledged it also is infeasible, so the x ray fluorescence spectrometry analytic approach is restricted.
Summary of the invention
The technical matters that the present invention will solve provides a kind ofly can not use the fusion method for making sample to the X-ray fluorescence spectra analysis that valuable platinum crucible produces the aluminium manganese Ca-Fe alloy of corrosion, to be used for the X-ray fluorescence spectra analysis.
For solving the problems of the technologies described above, the technical scheme that the present invention taked is: it hangs the layer of even protective bulkhead with lithium tetraborate earlier in platinum crucible; Again aluminium manganese calcium iron sample, oxygenant, lithium borate flux and release agent are put into the platinum crucible that hangs with protective bulkhead, mixing carries out pre-oxidation to aluminium manganese calcium iron sample then; Carry out fusion to the good aluminium manganese calcium iron sample of pre-oxidation at last, cooling promptly gets the mother glass fuse piece of aluminium manganese Ca-Fe alloy; Described aluminium manganese calcium iron sample is the test sample or the calibration sample of aluminium manganese Ca-Fe alloy, and described mother glass fuse piece is the test sample glass fuse piece or the calibration sample glass fuse piece of aluminium manganese Ca-Fe alloy.
The further processing step of the present invention is: lithium tetraborate is got in platinum crucible in (1), 1000～1050 ℃ of following fusions; The fusing back is taken out platinum crucible and is slowly rotated, and makes lithium tetraborate in platinum crucible, hang the layer of even protective bulkhead;
(2) get aluminium manganese calcium iron sample, oxygenant, lithium borate flux and release agent and put into platinum crucible, mixing;
(3) put into platinum crucible 800 ℃ muffle furnace, aluminium manganese calcium iron sample is carried out pre-oxidation 15～20min;
(4) put into sample-melting stove to the good aluminium manganese calcium iron sample of pre-oxidation, carry out fusion;
(5) take out the aluminium manganese calcium iron sample that melts, be cooled to room temperature, promptly get the mother glass fuse piece of aluminium manganese Ca-Fe alloy.
Further, the consumption of lithium tetraborate is 5.0000g～8.0000g in the said step (1).
Further; In the said step (2); Oxygenant is a kind of in lithium carbonate, sodium carbonate, lithium nitrate, potassium nitrate or the sodium nitrate, and release agent is potassium iodide or sodium iodide, and lithium borate flux is the potpourri of lithium tetraborate or lithium tetraborate and lithium metaborate arbitrary proportion; The weight ratio of aluminium manganese calcium iron sample and oxygenant is 1:5～10, and the consumption of aluminium manganese calcium iron sample is 0.2000～0.5000g; The consumption of release agent is 0.5000g; The consumption of lithium borate flux is 1.0000～3.0000g.
Further again, in the said step (3), platinum crucible is earlier at muffle furnace doorway preheating 1～2min, and then slowly progressively moves into and carry out pre-oxidation in the burner hearth; Or adopt the mode of temperature programme, temperature program(me) is progressively risen to 800 ℃ accomplish to pre-oxidation.
Further again, in the said step (4), melt temperature is 1000 ℃; Time of repose 3min before the melting process, body of heater duration of oscillation 15min, back time of repose 2min.
In the fusion sample preparation of X-ray fluorescence spectra analysis usefulness; The glass fuse piece of preparing has formed a kind of solid solution in essence; Sample is through decompose in lithium borate behind the high temperature fully, and different minerals is eliminated mutually fully, and final sample and flux have reached the mixing of atomic level level; So this has just fundamentally eliminated source of error, has improved accuracy of analysis.
Adopt the beneficial effect that technique scheme produced to be: the present invention adopts oxygenant, lithium borate flux and release agent that aluminium manganese calcium iron is carried out the fusion sample preparation, has solved fusion sample preparation etching problem; Adopt this method under the prerequisite that valuable platinum crucible is not produced corrosion, to process the glass fuse piece, the print of processing is evenly perfect, has eliminated mineral effect and granularity effect fully.The glass fuse piece that obtains is used for the X-ray fluorescence spectra analysis, the analysis result that obtains accurately and reliably, analysis data is rapid, the needs of accuracy to detecting to meet modern enterprise.That the inventive method has is safe and reliable, simple to operate, the characteristics of favorable reproducibility, has expanded the range of application of X-ray fluorescence spectra analytic approach.
Embodiment
Below in conjunction with specific embodiment the present invention is done further detailed explanation.
The XRF light analysis of this aluminium manganese Ca-Fe alloy comprises steps such as wall built-up, pre-oxidation, fusion with spectrum fusion method for making sample, comes the simple substance class material in the aluminium oxide manganese Ca-Fe alloy through pre-oxidation, thereby eliminates the corrosion of melting process to platinum crucible.The technological difficulties of pre-oxidation are choosing of oxygenant, and used oxygenant will guarantee that oxidation completely under the prerequisite, do not corrode platinum crucible.Among the present invention oxygenant to choose mechanism following: be commonly referred to be for the mechanism of carbonate or nitrate high oxidation activity and realize by its carbon dioxide or oxynitrides that at high temperature decomposes release.Between 500～800 ℃, decomposition temperature is variant slightly under the different atmosphere usually for the decomposition temperature of such oxygenant.Oxygenant begins to decompose release of carbon dioxide or oxynitrides when sample temperature is heated to 500 ℃, and oxidation reaction takes place, and lasts till that always oxygenant decomposes fully.Because this state is the process that a type discharge goes out gas; So the effect of stirring has been played in the effusion of gas to a certain extent; Abundant mixing to sample and oxygenant contacts very favourable; The lithium borate flux that mixes in the sample can absorb certain heat again, alleviates reaction velocity, thereby has prevented the splash of sample.Simultaneously, because the fusing point of lithium tetraborate is 921 ℃, and pre-oxidation is to carry out in the muffle furnace under 800 ℃; So the protective bulkhead that lithium tetraborate forms at the crucible inwall is during 800 ℃ of oxidations; Still can keep solid-state, play the effect that isolated reagent contacts with the crucible inwall, like this in whole oxidizing process; Elemental metals has no chance to contact with platinum dish, makes whole preoxidation process under safe and reliable condition, to carry out.
Embodiment 1: this fusion method for making sample is accomplished through following steps:
1, take by weighing the 7.0000g lithium tetraborate in platinum crucible, 1000 ℃ of following fusions, the taking-up back is the rotation crucible slowly, and in platinum crucible, hanging one deck has certain altitude and uniform protective bulkhead;
2, take by weighing 0.2000g aluminium manganese calcium iron test sample, 0.5000g potassium iodide, 2.0000g lithium tetraborate and 1.5000g lithium nitrate, put into platinum crucible, mixing;
3, evenly cover the lithium tetraborate of 2.0000g on the surface of the above-mentioned sample mixture of mixing;
4, put into the muffle furnace that is warming up to 800 ℃ to platinum crucible and carry out pre-oxidation; This process should let platinum crucible at stove gate preheating 1.5min; The slow about 18min of burner hearth that gets into of substep gets final product then, and the sample after the oxidation fully should be flowable liquid, and does not have the black particle thing in the sample;
5, put into sample-melting stove to well-oxygenated test sample, 1000 ℃ of melt temperatures, time of repose 3min before the melting process, body of heater duration of oscillation 15min, back time of repose 2min;
6, take out, obtain evenly the perfectly test sample glass fuse piece of aluminium manganese Ca-Fe alloy after the cooling.
Embodiment 2: this fusion method for making sample is accomplished through following steps:
1, take by weighing the 5.0000g lithium tetraborate in platinum crucible, 1020 ℃ of following fusions, the taking-up back is the rotation crucible slowly, and in platinum crucible, hanging one deck has certain altitude and uniform protective bulkhead;
2, take by weighing the mixed flux and the 2.5000g lithium carbonate of 0.5000g aluminium manganese calcium iron test sample, 0.5000g sodium iodide, 1.0000g 50wt% lithium tetraborate+50wt% lithium metaborate, put into platinum crucible, mixing;
3, put into muffle furnace to platinum crucible and take the mode of temperature programme to carry out pre-oxidation, process is 550 ℃ of insulation 3min, 600 ℃ of insulation 3min; 650 ℃ of insulation 3min; 700 ℃ of insulation 3min, 750 ℃ of insulation 5min, 800 ℃ of insulation 5min; Sample should be flowable liquid after oxidation was accomplished, and did not have the black particle thing in the sample;
4, put into sample-melting stove to well-oxygenated sample, 1000 ℃ of melt temperatures, time of repose 3min before the melting process, body of heater duration of oscillation 15min, back time of repose 2min;
5, take out, obtain evenly the perfectly test sample glass fuse piece of aluminium manganese Ca-Fe alloy after the cooling.
Embodiment 3: this fusion method for making sample is accomplished through following steps:
1, take by weighing the 8.0000g lithium tetraborate in platinum crucible, 1050 ℃ of following fusions, the taking-up back is the rotation crucible slowly, and in platinum crucible, hanging one deck has certain altitude and uniform protective bulkhead;
2, take by weighing 0.2500g aluminium manganese calcium iron test sample, 0.5000g potassium iodide, 2.5000g potassium nitrate and 3.0000g lithium metaborate, put into platinum crucible, mixing;
3, put into the muffle furnace that is warming up to 800 ℃ to platinum crucible and carry out pre-oxidation; This process should let platinum crucible at stove gate preheating 2.0min; The slow about 20min of burner hearth that gets into of substep gets final product then, and the sample after the oxidation fully should be flowable liquid, and does not have the black particle thing in the sample;
4, put into sample-melting stove to well-oxygenated sample, 1000 ℃ of melt temperatures, time of repose 3min before the melting process, body of heater duration of oscillation 15min, back time of repose 2min;
5, take out, obtain evenly the perfectly test sample glass fuse piece of aluminium manganese Ca-Fe alloy after the cooling.
The X-ray fluorescence spectra analysis of this aluminium manganese Ca-Fe alloy is with the checking of the stability of fusion method for making sample: in order to verify the stability this method is from weighing, pre-oxidation to melting process; Same sample has been carried out continuous 6 times identical weighing; Melting operation; Investigate the stability of this method from the reappearance of experimental data, experimental data is as shown in table 1.The relative standard deviation of each element all in small range, explains that this method is reliable to the whole process stabilization of fusion from weighing, pre-oxidation.
Table 1: method reappearance experimental data
| Number of times | Al(wt%) | Mn(wt%) | Ca(wt%) | Fe(wt%) |
| 1 | 55.42 | 17.19 | 1.36 | 25.92 |
| 2 | 55.58 | 17.26 | 1.38 | 25.93 |
| 3 | 55.54 | 17.24 | 1.34 | 25.88 |
| 4 | 55.64 | 17.40 | 1.36 | 26.11 |
| 5 | 55.68 | 17.44 | 1.35 | 26.22 |
| 6 | 55.46 | 17.41 | 1.35 | 26.25 |
| Average | 55.54 | 17.32 | 1.36 | 26.05 |
| Standard deviation | 0.11 | 0.105 | 0.011 | 0.162 |
| Relative standard deviation % | 0.20 | 0.60 | 0.83 | 0.62 |
Test Example: composite manual calibration sample, making working curve and the present invention measure the accuracy testing of aluminium manganese Ca-Fe alloy.
The first, the foundation of typical curve:
With benchmark fine aluminium, pure manganese, pure iron and benchmark lime carbonate is standard model, is re-dubbed the calibration sample of aluminium manganese calcium iron, after the glass fuse piece is prepared in fusion, measures the fluorescence intensity of each element and draws calibration curve.
The second, measure the accuracy testing of aluminium manganese Ca-Fe alloy:
Because aluminium manganese Ca-Fe alloy do not have standard model, have neither part nor lot in the composite magnalium calcium of the standard model iron sample of calibration curve through use, verify the accuracy of this method.The result is as shown in table 2, and it is very approaching to measure result and standard value, explains that this method is accurately and reliably.
In sum, the fusion method for making sample that is used for the aluminium manganese Ca-Fe alloy class sample that X-ray fluorescence spectra analyzes provided by the invention is very reliable, can greatly improve precision of analysis and stability, quotes when having realized multielement.
Claims (7)
1. the fusion method for making sample is used in the X-ray fluorescence spectra analysis of an aluminium manganese Ca-Fe alloy, it is characterized in that: it hangs the layer of even protective bulkhead with lithium tetraborate earlier in platinum crucible; Again aluminium manganese calcium iron sample, oxygenant, lithium borate flux and release agent are put into the platinum crucible that hangs with protective bulkhead, mixing; Then aluminium manganese calcium iron sample is carried out pre-oxidation; Carry out fusion to the good aluminium manganese calcium iron sample of pre-oxidation at last, cooling promptly gets the mother glass fuse piece of aluminium manganese Ca-Fe alloy; Described aluminium manganese calcium iron sample is the test sample or the calibration sample of aluminium manganese Ca-Fe alloy, and described mother glass fuse piece is the test sample glass fuse piece or the calibration sample glass fuse piece of aluminium manganese Ca-Fe alloy.
2. the fusion method for making sample is used in the X-ray fluorescence spectra analysis of aluminium manganese Ca-Fe alloy according to claim 1, it is characterized in that, its processing step is:
(1) gets lithium tetraborate in platinum crucible, 1000～1050 ℃ of following fusions; The fusing back is taken out platinum crucible and is slowly rotated, and makes lithium tetraborate in platinum crucible, hang the layer of even protective bulkhead;
(2) get aluminium manganese calcium iron sample, oxygenant, lithium borate flux and release agent and put into platinum crucible, mixing;
(3) put into platinum crucible 800 ℃ muffle furnace, aluminium manganese calcium iron sample is carried out pre-oxidation 15～20min;
(4) put into sample-melting stove to the good aluminium manganese calcium iron sample of pre-oxidation, carry out fusion;
(5) take out the aluminium manganese calcium iron sample that melts, be cooled to room temperature, promptly get the mother glass fuse piece of aluminium manganese Ca-Fe alloy.
3. the fusion method for making sample is used in the X-ray fluorescence spectra analysis of aluminium manganese Ca-Fe alloy according to claim 1 and 2, it is characterized in that: the consumption of said lithium tetraborate is 5.0000g～8.0000g.
4. the fusion method for making sample is used in the X-ray fluorescence spectra analysis of aluminium manganese Ca-Fe alloy according to claim 1 and 2, it is characterized in that: described oxygenant is lithium carbonate, sodium carbonate, lithium nitrate, potassium nitrate or sodium nitrate; Described release agent is potassium iodide or sodium iodide; Described lithium borate flux is lithium tetraborate, or the potpourri of lithium tetraborate and lithium metaborate arbitrary proportion.
5. the fusion method for making sample is used in the X-ray fluorescence spectra analysis of aluminium manganese Ca-Fe alloy according to claim 1 and 2, it is characterized in that: the weight ratio of said aluminium manganese calcium iron sample and oxygenant is 1:5～10; The consumption of said aluminium manganese calcium iron sample is 0.2000～0.5000g; The consumption of said release agent is 0.5000g; The consumption of said lithium borate flux is 1.0000～3.0000g.
6. the fusion method for making sample is used in the X-ray fluorescence spectra analysis of aluminium manganese Ca-Fe alloy according to claim 2; It is characterized in that: in the said step (3); Platinum crucible is earlier at muffle furnace doorway preheating 1～2min, and then slowly progressively moves into and carry out pre-oxidation in the burner hearth; Or temperature is progressively risen to 800 ℃ accomplish to pre-oxidation.
7. the fusion method for making sample is used in the X-ray fluorescence spectra analysis of aluminium manganese Ca-Fe alloy according to claim 2, it is characterized in that: in the said step (4), melt temperature is 1000 ℃; Time of repose 3min before the melting process, body of heater duration of oscillation 15min, back time of repose 2min.
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