AU2016378266A1 - Method and system for analyzing a sample material - Google Patents
Method and system for analyzing a sample material Download PDFInfo
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- AU2016378266A1 AU2016378266A1 AU2016378266A AU2016378266A AU2016378266A1 AU 2016378266 A1 AU2016378266 A1 AU 2016378266A1 AU 2016378266 A AU2016378266 A AU 2016378266A AU 2016378266 A AU2016378266 A AU 2016378266A AU 2016378266 A1 AU2016378266 A1 AU 2016378266A1
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- Australia
- Prior art keywords
- sample material
- fluxing agent
- agent mixture
- tablet
- melting
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- 238000001533 laser emission spectroscopy Methods 0.000 claims abstract description 22
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- 206010037660 Pyrexia Diseases 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
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- GDTSJMKGXGJFGQ-UHFFFAOYSA-N 3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound O1B([O-])OB2OB([O-])OB1O2 GDTSJMKGXGJFGQ-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910017356 Fe2C Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
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- 229910052729 chemical element Inorganic materials 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
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- 238000007689 inspection Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
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- 239000000289 melt material Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- KAQHZJVQFBJKCK-UHFFFAOYSA-L potassium pyrosulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OS([O-])(=O)=O KAQHZJVQFBJKCK-UHFFFAOYSA-L 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- 150000004763 sulfides Chemical class 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
- G01J3/443—Emission spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/02—Details
- G01J3/0205—Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows
- G01J3/0218—Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows using optical fibers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/202—Constituents thereof
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/205—Metals in liquid state, e.g. molten metals
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
- G01N21/95—Investigating the presence of flaws or contamination characterised by the material or shape of the object to be examined
- G01N21/9508—Capsules; Tablets
Abstract
The invention relates to a method for analyzing a sample material, wherein the sample material is ground, formed into a tablet, optionally processed, and then analyzed. Said method is characterized in that the analysis is performed by means of laser emission spectroscopy. A system suitable for performing such a method comprises at least a mill for grinding the sample material, a device for forming a tablet from the ground sample material, preferably a tablet press, and a device for analyzing the sample material by means of laser emission spectroscopy.
Description
The invention relates to a method for analyzing a sample material, wherein the sample material is ground, formed into a tablet, optionally processed, and then analyzed. Said method is characterized in that the analysis is performed by means of laser emission spectroscopy. A system suitable for performing such a method comprises at least a mill for grinding the sample material, a device for forming a tablet from the ground sample material, preferably a tablet press, and a device for analyzing the sample material by means of laser emission spectroscopy.
(57) Zusammenfassung: Ein Verfahren zur Analyse eines Probenmaterials, wobei das Probenmaterial gemahlen, zu einer Tablette geformt, ggf. bearbeitet und anschlieBend analysiert wird, ist dadurch gekennzeichnet, dass die Analyse mittels Laseremissionsspektroskopie durchgefuhrt wird. Eine zur Durchfhhrung eines solchen Verfahrens geeignete Anlage umfasst zumindest eine Miihle zum Mahlen des Probenmaterials, eine Vorrichtung zum Formen einer Tablette aus dem gemahlenen Probenmaterial, vorzugsweise eine Tablettenpresse, sowie eine Vorrichtung zur Analyse des Probenmaterials mittels Laseremissionsspektroskopie.
wo 2017/108810 Al lllllllllllllllllllllllllllllllllllll^
Veroffentlicht:
— mit internationalem Recherchenbericht (Artikel 21 Absatz 3)
Method and System for Analyzing a Sample Material
The invention relates to a method for analyzing a sample material, in which the sample material is ground, converted into a tablet shape, optionally processed further and subsequently analyzed. The invention furthermore relates to a system suitable for carrying out such a method.
It is known to produce such tablets as pressed tablets, by the sample material being ground and processed further while applying pressure and/or binder to form the tablet.
It is furthermore known to produce tablets ready for analysis from a melt. In this case, the sample material is mixed with a fluxing agent, this sample material/fluxing agent mixture is melted, and the melt is cast into a tablet mold and cooled therein. However, such cooling with simultaneous shaping is expensive in terms of process technology and in terms of equipment. For instance, the cooling of a melt tablet needs to be carried out under very controlled conditions, since excessively rapid cooling can lead to fracture of the tablet, while the melt may crystallize in the event of excessively slow cooling, so that the tablet inter alia would lose its strength.
WO 2015/000571 A1 and US 5,257,302 respectively disclose methods for producing a tablet comprising a sample material, in which a material mixture comprising the sample material is melted and recooled. The vitreous material formed in this way is subsequently ground and then pressed to form the tablet.
The object of the invention was to provide an improved method for analyzing a sample material.
This object is achieved by means of a method as claimed in patent claim 1. A system suitable for carrying out a method according to the invention is the subject of patent claim 21. Advantageous embodiments of the method according to the invention and advantageous configurations of the system according to the invention are the subjects of the further patent claims, and may be found in the following description of the invention.
In a method for analyzing a sample material, in which the sample material is ground, shaped into a tablet and subsequently analyzed, according to the invention the analysis is carried out by means of laser emission spectroscopy.
A system suitable for carrying out a method according to the invention comprises at least a mill for grinding the sample material and a device for shaping a tablet from the ground sample material (preferably a tablet press). A system according to the invention is furthermore characterized by a device for analyzing the sample material by means of laser emission spectroscopy.
Laser emission spectroscopy, which is also referred to as laser-induced plasma spectroscopy or by the abbreviation LIBS, which stands for “laser-induced breakdown spectroscopy”, is a method for determining the chemical composition of a sample material, in which relatively short laser pulses are applied to the sample material, so that relatively small amounts of the sample material are vaporized and ionized. During the subsequent decay of the plasma, light is emitted which is characteristic of the chemical elements contained in the sample material. The spectrum of the light may then be evaluated by means of a spectrometer.
One advantage of laser emission spectroscopy is the relatively simple way it can be carried out, as well as the fact that no particularly great demands are placed on preparation of the sample material therefor. By use in the case of sample material which is in a tablet form with a homogeneous, representative surface, a high analysis accuracy can be achieved in a straightforward way for the laser emission spectroscopy.
According to the invention, a “tablet” is intended to mean a solid body in a defined three-dimensional shape, which consists at least partially of the sample material or of a material mixture comprising the sample material.
Furthermore preferably, in the scope of carrying out the laser emission spectroscopy, the laser used therefor may be applied to at least one surface of the tablet at a plurality of positions, and in particular also only pointwise (i.e. only in an area which corresponds to the active area of the laser). This makes it possible to carry out an analysis on various portions of the sample material, and to combine, in particular to average, the individual analysis results obtained in this way to form an overall analysis result, so that a higher accuracy can be obtained for the overall analysis result used as final result.
In one preferred embodiment of the method according to the invention, the sample material may be at least partially mixed with a fluxing agent (in particular a fluxing salt and/or an acid) before or after the grinding (and preferably before the shaping of the tablet). To this end, the system according to the invention may have a mixing device for mixing the sample material with a further material, in particular a fluxing agent. By diluting the sample with a fluxing agent, the sample matrix can be unified, and the socalled matrix effect in the scope of the analysis can thereby be reduced.
In an advantageous embodiment of the method according to the invention, the sample material or the sample material/fluxing agent mixture may additionally be at least partially melted before the analysis. An analysis by means of laser emission spectroscopy can then be carried out directly on the melted sample material or the melted sample material/fluxing agent mixture, in the case of preferably provided locally limited and in particular pointwise melting, for example at the melt pools then occurring.
To this end, a system according to the invention may have a corresponding device for melting the sample material (or a material mixture comprising the sample material).
An effect achievable by the melting of the sample material or of the sample material/fluxing agent mixture is that it is converted into a homogeneous, or chemically homogeneous, melt, which helps to improve analysis of the sample material with the aid of the melt. In this way, it is possible to reduce or even eliminate influences which arise, for example, from the particle size distribution and the density, as well as from mineralogical properties, for example crystal structure and crystallinity, of the original sample. As a function of the sample material used (or the material mixture comprising the sample material), iron can also be bound to boron by the melting, so that advantages can be obtained during calibration.
In one alternative embodiment of a method according to the invention, the tablet may be analyzed by means of laser emission spectroscopy without prior melting of the sample material (or of a material mixture comprising the sample material).
In one preferred refinement of a method according to the invention, in which the sample material or the sample material/fluxing agent mixture is at least partially melted before the analysis, solidification of the melt may be carried out before the analysis, the solidified melt already having the tablet shape or only subsequently being converted into the tablet shape. In this way, tablets can be prepared for subsequent analysis by means of laser emission spectroscopy.
In a further preferred refinement of a method according to the invention, in which the sample material or the sample material/fluxing agent mixture is at least partially melted before the analysis, the sample material or the sample material/fluxing agent mixture can be cooled (actively) during the melting. This may, for example, be done by means of an air flow and in particular by means of compressed air. To this end, the system according to the invention may have a corresponding cooling device. Without such cooling, recrystallization of the sample material or of the sample material/fluxing agent mixture may take place (more greatly).
As an alternative or in addition, in a method according to the invention in which the sample material or the sample material/fluxing agent mixture is at least partially melted before the analysis, at least a fraction, intended for melting, of the sample material or of the sample material/fluxing agent mixture may also be preheated before the melting and/or supplementarily heated during the melting. To this end, the system according to the invention may have a corresponding heating device. Preheating and/or supplementary heating of the sample material or of the sample material/fluxing agent mixture can prevent or reduce stresses in the tablet, so that dislocations or cracks in the tablet during the melting may possibly be prevented. The preheating and/or the supplementary heating of the tablet may, for example, be carried out by means of a heating plate (“resistive heating device”), a (hightemperature) IR radiator or else by means of a laser. The sample material or the sample material/fluxing agent mixture may in this case be heated from the upper side (provided for the melting) or the lower side. For example, temperatures of between 400°C and 600°C may be set up in the material to be preheated, or to be supplementarily heated. A temperature to be set up, or a temperature range to be set up, may in this case be regulated.
In a preferred refinement of a method according to the invention, in which the sample material or the sample material/fluxing agent mixture is at least partially melted before the analysis, the sample material or the sample material/fluxing agent mixture may be melted by means of laser radiation, plasma radiation, high-temperature infrared radiation, microwave radiation and/or electron radiation. Use of laser radiation, plasma radiation, high-temperature infrared radiation, microwave radiation and/or electron radiation allows a very exactly definable, locally limitable and/or locally very high energy introduction into the sample material to be melted, or the sample material/fluxing agent mixture to be melted, which can have a positive effect on the melting, and in particular can also allow simple and at the same time very exact regulation of the melting process. By locally exactly defined energy introduction, heat dissipation incurred when carrying out a method according to the invention can additionally be minimized. Also, by the use according to the invention of laser radiation, plasma radiation, high-temperature infrared radiation, microwave radiation and/or electron radiation, relatively rapid melting of the sample material intended therefor, or of the sample material/fluxing agent mixture intended therefor, can be achieved, which can correspondingly have an advantageous effect on the time required for production of the tablet.
In a method according to the invention in which the sample material or the sample material/fluxing agent mixture is at least partially melted before the analysis, and preheating of at least a fraction, intended for the melting, of the sample material or of the sample material/fluxing agent mixture is also provided, at least the fraction, intended for the melting, of the sample material or of the sample material/fluxing agent mixture may furthermore be preheated by means of laser radiation, and the sample material or the sample material/fluxing agent mixture may be melted by means of laser radiation of the same laser. In this way, double use of a laser may advantageously be achieved, by which the design outlay for a system according to the invention can be kept low.
In the case of melting of the sample material or of the sample material/fluxing agent mixture by means of laser radiation, this may be carried out by the same laser as is also used in the scope of the analysis by means of laser emission spectroscopy. This laser may then also be used for preheating of the sample material or of the sample material/fluxing agent mixture. As an alternative, however, a different laser may also be used for the melting.
When carrying out an embodiment of a method according to the invention which comprises melting of the sample material or of the sample material/fluxing agent mixture, the sample material or the sample material/fluxing agent mixture may additionally be melted selectively by means of the laser radiation, plasma radiation and/or electron radiation. In this case, “selectively” is intended to mean gradually carried out melting of the sample material/fluxing agent mixture, or of the fraction thereof intended therefor, by moving the laser beam, the plasma beam and/or the electron beam, the coverage of which is smaller than the area covered by the sample material/fluxing agent mixture to be melted, along this area, so that the sample material/fluxing agent mixture is gradually melted over this area. In this case, during the melting of one partial area, another partial area already melted beforehand may already resolidify.
The melting process can be influenced by the number of exposure steps (single or multiple exposure). In the case of single exposure, for example, a laser beam (or pulsed laser beam) travels over each “point” exactly once (for example only in forward movement). In the case of multiple exposure, for example, the laser beam travels over each “point” several times. A backward and/or sideways movement is in this case superimposed on the forward movement. The type of exposure may be adjusted material-dependently (inter alia as a function ofthe sample material).
For an analysis by means of laser emission spectroscopy, a YAG laser may preferably be used. This may then furthermore preferably be operated in pulsed fashion (for example nanosecond pulses). A YAG laser may likewise advantageously be used for preferably provided preheating and/or melting of the sample material or of the sample material/fluxing agent mixture, although as an alternative a CO2 laser may also for example be used. The laser used therefor may in this case preferably be operated continuously, i.e. not in a pulsed fashion.
In the scope of a method according to the invention, the sample material may furthermore preferably be ground until a particle size of at most 100 pm, particularly preferably of at most 63 pm, is reached. This has an advantageous effect on the homogenization of the sample material or of the sample material/fluxing agent mixture in the scope of the melting.
In one refinement of a method according to the invention, in which the sample material is mixed with a fluxing agent, the sample material may be preground in a first grinding step, and ground further in a further grinding step after mixing with the fluxing agent. In this case, the grinding of the sample material/fluxing agent mixture can primarily be used for the purpose of mixing the already ground sample material with the fluxing agent. This is made possible, in particular, by the fact that fluxing agent is often already in a finely divided form. One advantage which may arise therefrom is that both the grinding of the sample material and the mixing of the sample material with the fluxing agent can be carried out in the same device, namely
- 8 a suitable (fine) mill. It is thereby possible to avoid provision of an additional mixing device.
Correspondingly, according to the invention “grinding” is not necessarily intended to mean a method step in which processing of a material or material mixture is linked with achieving a reduction of the particle size of the material or material mixture. Rather, such “grinding” may be used exclusively or primarily for blending a material mixture, if grinding of the material or material mixture by the same method procedure, or by the use of the same device (mill) used for this, were in principle possible, i.e. with method parameters differing therefrom. The rotational speed of the (fine) mill may be adapted to the mixing effect to be achieved (possibly a low speed), and may differ from a grinding rotational speed.
Good blending of the fluxing agent with the sample material can have the advantage for the subsequent melting, in particular for melting by means of laser radiation, that each so-called “pool” (zone that is remelted) then has the most uniform possible composition (particle size distribution from sample to fluxing agent always as far as possible the same).
Optionally, the fluxing agent may also be mixed with the sample material in a dosed fashion in the form of a solid body, so that dosing of sample material and fluxing agent in a predefined ratio can be simplified. In this case, it may be expedient also to grind the fluxing agent solid body in at least one of the grinding steps, i.e. to reduce it to particles of defined (maximum) particle size.
In a furthermore preferred embodiment of the method according to the invention, the solidification of the melt may be carried out in such a way that a vitreous component (the resolidified melt) of the tablet is formed. In particular embodiments of the method according to the invention, however, a semicrystalline configuration of the solidified melt may also be sufficient or even advantageous.
- 9 In this case, “vitreous” or “vitreous component” is intended to mean an amorphous material structure, which does not have any ordered crystalline structure after cooling from the melt. Conversion of the melt into a vitreous component may, in particular, be achieved by cooling the melt sufficiently rapidly, so that crystallization of the melt material is prevented.
The vitreous component is particularly advantageously suitable for the analysis of the sample material, because the homogeneous mixture, which results from the melting of the sample material together with the fluxing agent, is preserved in it and it is geometrically stable.
The formation of a vitreous component of the solidified melt may also be reinforced by active cooling, for example by means of a gas flow (for example air or a protective gas). The system according to the invention may have a cooling device for this purpose. In this case, regulation of the active cooling, or of the cooling device, may also be provided to the extent that crystallization is avoided as far as possible.
As a fluxing agent which may advantageously be used when carrying out the method according to the invention, for example lithium tetra- or metaborate, sodium tetra- or metaborate, sodium carbonate, potassium disulfate and/or an acid, for example boric acid, or a mixture thereof - also with addition of additives (for example flow agents such as LiBr) - may be used.
Furthermore preferably, the fluxing agent may be mixed with the sample material in a ratio of between 40:1 and 2:1, preferably of between 10:1 and 2:1.
In one advantageous embodiment of the method according to the invention, the sample material or the sample material/fluxing agent mixture may be melted and solidified layerwise (i.e. successively in a plurality of layers). This may allow relatively rapid production of the melt because of an exactly dosed and very high local energy introduction into the sample material or the sample material/fluxing agent mixture (or the fraction thereof intended for the melting).
In this case, the layerwise melting and solidification of the fluxing agent/sample material mixture may particularly preferably be used as a generative production method for producing the tablet (or the corresponding component thereof). The system according to the invention may to this end comprise a device for generative production of a tablet from the ground sample material. A generative production method is characterized in that a three-dimensional body is produced layerwise from a material, particularly a material in powder form, by applying, melting and solidifying material layerwise, starting from a base layer, onto this base layer. One relevant advantage of such a generative production method is that, because material is melted only in a relatively thin layer and in a locally limited way, it is possible to obviate receiving the melt during the solidification in a negative mold corresponding to the intended shape of the resolidified melt (i.e. in the shape of the tablet or of the corresponding component thereof).
Suitable specific embodiments for the production of the tablet or of a component thereof by a generative production method are the widely known selective laser sintering, selective laser melting and (selective) electron beam melting.
Layerwise melting and solidification may also be carried out by initially melting and solidifying a surface layer, and subsequently melting and solidifying a layer lying underneath (i.e. spatially separated by the surface layer relative to a radiation source carrying out the melting). This may be continued stepwise until the intended thickness of the tablet to be produced, or of the tablet component to be produced, has been reached. In this case, a different absorption for the laser radiation, plasma radiation and/or electron radiation by the sample material/fluxing agent mixture on the one hand, and the resolidified melt on the other hand, may optionally be used.
In one refinement of a method according to the invention, in which the sample material or the sample material/fluxing agent mixture is melted, the solidified melt may furthermore be ground and subsequently converted, and in particular pressed, into the tablet shape. A pressed tablet may therefore be formed from the solidified and then ground melt. By such an embodiment of the method according to the invention, simple producibility of a tablet comprising a sample material, in the form of a pressed tablet, is combined with the homogenization of the sample material by melting, which is advantageous for the subsequent analysis. In this procedure, use is made of the fact that the homogenization of the sample material, advantageously achieved by the melting, is not negatively influenced (to a relevant extent) by the grinding.
In a further preferred embodiment of the method according to the invention, the ground sample material or the sample material/fluxing agent mixture (optionally after admixture of a binder) may be pressed before melting. This may, in particular, be advantageous when it is not intended to form the entire tablet in the form of a resolidified melt, and therefore the entire amount of the sample material or of the sample material/fluxing agent mixture is not intended to be melted. In particular, the tablet may therefore in principle be formed in the form of a pressed tablet, while only a surface layer intended primarily for the subsequent analysis is melted and resolidified, in order to correspondingly improve the analysis by the preferably obtainable vitreous and therefore amorphous structure and by homogenization of the sample material in this surface layer. In this case, the surface layer may advantageously have a thickness of between 30 pm and 300 pm.
An effect advantageously achievable by preferably provided melting of the sample material or of the sample material/fluxing agent mixture by means of laser radiation, plasma radiation, high-temperature infrared radiation, microwave radiation and/or electron radiation, is that the melting and/or the carrying out of the solidification of the melt (and active cooling optionally used in this case) can be monitored, and optionally regulated, in real time. The system according to the invention may to this end comprise a corresponding device for real-time monitoring of melting of the sample material and/or of cooling of the sample material and/or of the melt. In this case, use may also be made of the fact that power regulation of the device generating the laser radiation, plasma radiation, high-temperature infrared radiation, microwave radiation and/or electron radiation leads very rapidly, or substantially immediately, to a corresponding regulation of the heat energy introduced into the sample material/fluxing agent mixture. Very rapid and exact regulation of the melting process can therefore be carried out. Such real-time monitoring may in particular comprise real-time temperature regulation, for example on the basis of a temperature measurement by means of one or more pyrometers. In this way, for example, the melting temperature can be kept constant during melting, in which case for example a melting temperature of between 1000°C and 1200°C may be set up, and in particular regulated.
Such monitoring may advantageously be carried out by using imaging sensors, for example a CMOS, thermal imaging and/or infrared camera, and/or a pyrometer.
In a furthermore preferred embodiment of the method according to the invention, a decontaminant may be ground in a mill, and the sample material, the sample material/fluxing agent mixture or the solidified melt may subsequently be ground in the same mill. This may be used to decontaminate the mill, which may possibly have already been used beforehand for grinding another type of sample material, or to deliberately contaminate it with the sample material subsequently to be ground. In this way, contamination of the sample material, which could lead to vitiation of the result of a subsequent analysis of this sample material, can be ruled out as far as possible.
The decontaminant may preferably be, or at least comprise, a first portion of the sample material or of the sample material/fluxing agent mixture. A portion of the solidified melt may likewise be used as a decontaminant. This may, in particular, be expedient when another portion of the solidified melt is subsequently ground in the mill, in order to form a pressed tablet therefrom. Therefore, a mill may also be decontaminated by means of a first decontaminant, which preferably comprises a first portion of the sample material, for subsequent grinding of a further portion of the sample material, this further portion of the sample material subsequently being mixed with the fluxing agent and melted according to the invention. Subsequently, in the same mill or a different mill, a first portion of the solidified melt may be ground in order to decontaminate the mill, and a further portion of the solidified melt may subsequently be ground in order to form a pressed tablet therefrom.
As an alternative or in addition, the decontaminant may also be or comprise a material different to the sample material, for example quartz sand, corundum and/or any desired refractory material (or material containing fireclay).
In one embodiment of the method according to the invention, the ground decontaminant may be discarded, so that it is at least not used further in the scope of the method according to the invention. In this case, in particular, the decontaminant may be disposed of.
It is also possible for the ground decontaminant/s to be pressed and used as a carrier layer for sample material to be pressed or sample material/fluxing agent mixture to be pressed and/or an amount (portion) of solidified and subsequently ground melt to be pressed. In this case, a selection of the decontaminant (or at least of a component thereof) may also be carried out on the basis of suitability as a carrier layer. Pressing of the decontaminant/s may preferably (respectively) be carried out in a molding ring. The height of the latter may in this case advantageously be greater than, preferably at least two times as great as, the layer thickness of the carrier layer. The unit consisting of the carrier layer and the molding ring may then be used as a vessel-like negative (of the intended tablet shape) mold for the amount, subsequently to be introduced therein, of the sample material or of the sample material/fluxing agent mixture or of an amount of ground solidified melt formed therefrom, which may also be processed further, in particular pressed and/or melted, therein.
Advantageously, the molding ring may consist at least partially of stainless steel or a refractory metal (or alternatively cermet) with a low thermal expansion coefficient.
In order to ensure secure holding of the pressed tablet inside the molding ring, the latter may preferably form at least one internal recess into which the sample material or the sample material/fluxing agent mixture (respectively in powder or vitreous form) and/or decontaminant can penetrate during the respective pressing, so that a form-fit connection can be formed between the pressed tablet to be produced and the molding ring. As an alternative, the molding ring may internally on a top side have a groove, or alternatively converge conically on the inside overall.
The sample material may in particular be one or more natural rocks or ores, for example silicates, carbonates, sulfates, sulfides, salts and/or oxides. Furthermore, the sample material may in particular comprise industrial process products, for example slag, fly ash and/or cement clinker.
The indefinite articles (“a”, “an”), particularly in the patent claims and in the description generally explaining the patent claims, are to be understood as such and not as numerals. Correspondingly, it is to be understood therefore that components thereby specified occur at least once and may occur several times.
The invention will be explained in more detail below with the aid of exemplary embodiments represented in the drawings. In the drawings
Fig. 1 schematically shows a tablet produced in the scope of a first embodiment of a method according to the invention;
Fig. 2 schematically shows a tablet produced in the scope of a second embodiment of a method according to the invention;
Fig. 3 schematically shows one variant for the production of a pressed tablet in the scope of a method according to the invention, and a device used in this case;
Fig. 4 schematically shows another variant for the production of a pressed tablet in the scope of a method according to the invention, and a device used in this case;
Fig. 5 schematically shows a first step during the analysis of a tablet comprising a sample material in the scope of a method according to the invention; and
Fig. 6 schematically shows a second step during the analysis of the tablet according to Fig. 5.
Fig. 1 shows a tablet 26, which comprises a sample material and has been produced in the scope of a first embodiment of a method according to the invention.
In this embodiment of a method according to the invention, a first portion (for example 5 to 6 g) of the sample material to be prepared and analyzed is initially dosed into a fine mill (not represented) and ground therein as a flushing or preliminary sample. In this way, the fine mill is deliberately contaminated with the sample material to be prepared. This first portion of the sample material is therefore used as a decontaminant.
The sample material portion used as a decontaminant is pressed after the grinding in the fine mill by means of a tablet press (not represented) into a molding ring 1, for example made of stainless steel (cf. Fig. 1), in order to form a carrier layer 2 for a further layer 3 of a mixture of a second portion of the sample material and a fluxing agent (for example a fluxing salt). This further layer 3, or a component thereof, is used for subsequent analysis of the sample material. The carrier layer 2 is unsuitable therefor because of possible contamination by impurities contained in the fine mill. For example, a layer thickness of from three to four millimeters may be provided for the carrier layer 2. This layer thickness may correspond to about 50% of the height of the molding ring 1. After cleaning of the molding ring 1 and of the carrier layer 2, the unit formed by these two components is rotated through 180° (with respect to a radial axis), so that this unit forms an upwardly open vessel into which the further portion of the sample material can be introduced.
Subsequently, a further portion of the sample material is dosed into the fine mill and ground therein in a first grinding step. The rotational speed with which the fine mill is operated, and the milling time, may in this case be adjusted as a function of the sample material to be processed. After completion of the first grinding step, a fluxing agent (for example lithium tetraborate) is mixed according to a predetermined mixing ratio into this ground portion of the sample material (for example with a mixing ratio of 1:5, i.e., in the case of an amount of the further portion of the sample material of 2 g, an amount of the fluxing agent of 10 g). Subsequently, this sample material/fluxing agent mixture is ground in a second grinding step in the fine mill, and thereby blended as optimally as possible. The sample material/fluxing agent mixture is then introduced into the vessel formed by the molding ring 1 and the carrier layer 2, and pressed in the tablet press. The pressed tablet 26 formed in this way initially consists of two layers, namely the carrier layer 2 which consists of the possibly contaminated first portion of the sample material, and the further layer 3 to be taken into account during the subsequent analysis, which consists of the pressed sample material/fluxing agent mixture.
The free surface of this further layer 3 is subsequently irradiated by means of a laser (not represented in Fig. 1) and thereby melted. The corresponding surface is in this case remelted, or broken down, fully or in small sections by means of continuous or pulsed laser radiation (for example by means of a fiber laser). After solidification of this melt by cooling, the tablet 26 to be produced comprises a vitreous layer 4, which is characterized by a particularly homogeneous material structure. This vitreous layer 4 is advantageously suitable for a subsequent analysis of the sample material, which is carried out according to the invention in the scope of laser emission spectroscopy (cf. Figs 5 and 6).
In one possible variant, for melting the sample material/fluxing agent mixture in the free surface of the layer 3 with a laser beam, the surface of the further layer 3 is scanned point by point (area by area). In this case, very small “melt pools” are produced, which solidify again vitreously a short time later. By the continuous process due to the laser method, the entire surface is broken down homogeneously and converted into a vitreous layer 4.
The purpose of the melt breakdown is to convert the sample material together with a fluxing agent into a homogeneous melt, which solidifies vitreously during cooling. By the breakdown, influences on the measurement results of the laser emission spectroscopy, which may for example be based on the particle size distribution and the mineralogical original state of the sample material, are eliminated or at least reduced. The breakdown leads to a uniform bonding form of the elements and by dilution reduces the mutual influence of the elements by secondary excitation and absorption (matrix effects).
The remelting is a chemical process. The fluxing agent in this case breaks down the compounds of the sample material and chemically converts them. For example, borates are from silicates, aluminates, carbonates and sulfates of the sample material (if these are present). By remelting or fusion of for example Fe2C>3, Fe3C>4, FeO, FeCb, FeS2, FeCC>3 with tetraborate, Fe borates are formed. The influences of the chemical bonding are minimized by conversion into Fe borates.
In an alternative embodiment (according to Fig. 2) of the method described above, a carrier layer 2 is not produced. Rather, a pressed tablet 26 is formed exclusively from the sample material/fluxing agent mixture. To this end, a first portion of the sample material is again initially ground as a flushing sample or decontaminant, but subsequently discarded. After decontamination of the mill has been carried out, a second portion of the sample material (for example 2 g) is again prepared in two grinding steps. In the first grinding process, only this second portion of the sample material is ground. For the second grinding step, a fluxing agent is then added in a ratio, which is as exact as possible, of for example 1:5 (sample material to fluxing agent), and ground together with the sample material in order to achieve the best possible blending of these components. The mixture of the sample material and the fluxing agent is then transferred into a tablet press (not represented). There, the mixture is pressed to form a layer 3 substantially corresponding to the shape of the tablet 26 to be produced. Subsequently, the melting and solidifying of a surface layer of the pressed tablet 26 may be carried out according to the above-described embodiment of a method according to the invention, in order to form a vitreous layer
4.
The molding ring 1 used in the scope of carrying out the method described above has two circumferential V-shaped recesses 5 on its inner side. One of the recesses 5 is in this case located in the upper axial half, and the other recess 5 in the lower axial half of the molding ring 1. The molding ring 1 has, for example, an (axial) height of 8.5 mm. One of the recesses 5 is located for example at an axial height of 2.5 mm starting from one of the axial ends of the molding ring 1, and the other recess at an axial height of 6 mm (starting from the same axial end of the molding ring 1).
Fig. 3 schematically shows the production of a tablet 26 comprising a sample material in the scope of a method according to the invention in a third embodiment, and a device used in this case.
This method is based on the method of selective laser melting (SLM). The powder processed in this case consists of a mixture of a sample material and a fluxing agent. This powder is prepared according to the procedure in the two above-described embodiments of methods according to the invention, that is to say after possible decontamination of a fine mill (not represented), a portion of the sample material is ground in a first grinding step in the fine mill, and subsequently mixed with the fluxing agent, and the sample material/fluxing agent mixture is subsequently blended in a second grinding step in the fine mill.
Subsequently, a sufficient amount of the sample material/fluxing agent mixture is fed through an inlet 6 to a doser 7 of the device used to carry out this embodiment of a method according to the invention, and is stored there. In the region of an outlet 8, the doser 7 comprises two dosing sliders 9, 10 spaced apart parallel to one another, which in the known way allow separation of a defined volume of the sample material/fluxing agent mixture from the total amount of the sample material/fluxing agent mixture stored in the doser 7, by opening the upper dosing slider 10 when the lower dosing slider 9 is closed, so that sample material/fluxing agent mixture can fall into the dosing space 11 formed between the dosing sliders 9, 10. By closing the upper dosing slider 10, a portion of the sample material/fluxing agent mixture corresponding to the volume of the dosing space 11 is then separated from the remaining amount of the sample material/fluxing agent mixture stored in the doser 7. This separated portion can then be released from the doser 7 by opening the lower dosing slider 9.
A portion of the sample material/fluxing agent mixture released in this way falls onto a plate 12 of a reception device 13 arranged below the doser 7. The plate 12 can be moved in a vertical direction inside a guide 14 of this reception device 13. The reception device 13 furthermore comprises a vibrator 15, by means of which the reception device 13 can be set in vibration. This is used for loosening of the portion of the sample material/fluxing agent mixture resting on the plate 12, as well as for initial surface distribution of this portion on the plate 12.
Subsequently, by means of a distributor slider 16, the sample material/fluxing agent mixture is distributed in a layer with maximal uniform thickness on the plate 12, while excess sample material/fluxing agent mixture is delivered into a sample cup 18 through a sample run-off 17. This excess sample material/fluxing agent mixture may be fed back from the sample cup 18 into the doser 7 for reuse. To this end, the sample cup 18 may be removed by means of an automatic handling device, for example a robot (not represented), and moved to the inlet 6 of the doser 7. As an alternative, the excess sample material/fluxing agent mixture may also be removed from the sample cup 18, for example suctioned by means of a suction device 19, and then optionally disposed of.
The smoothed layer of the sample material/fluxing agent mixture, resting on the plate 12 of the reception device 13, is subsequently irradiated by means of a laser 20 and thereby selectively melted. To this end, a mirror 21 that can be tilted in an automated fashion is provided, the tilting movement of which makes it possible to irradiate, and thereby melt, a defined region of the layer of the sample material/fluxing agent mixture gradually by means of a laser beam generated by the laser 20 (as an alternative, direct energy input without a mirror is also possible). After solidification of the melt produced in this way, a vitreous layer is formed. This vitreous layer may already be the tablet 26 to be produced. It is, however, also possible to form a multiplicity of such vitreous layers (connected to one another with a material fit) layerwise above one another, by respectively carrying out in succession application of a dosed portion of the sample material/fluxing agent mixture onto the plate 12 of the reception device 13, distribution or smoothing of this portion, and melting and solidification of this portion, for each cycle the plate 12 being moved downward by a distance which corresponds essentially to the intended layer thickness of the vitreous layer to be formed.
The vitreous layer(s) produced in this way may then optionally be applied onto a carrier layer (not represented) in order to increase the geometrical stability of the tablet 26 to be produced.
By means of a transport device 22, for example a suction gripper element, the tablet 26, or the vitreous layer(s), may then be removed from the reception device 13 and transferred into an analyzer (not represented), for example an X-ray fluorescence analyzer. Optionally, the vitreous layer(s) formed in this way may also (optionally in conjunction with the carrier layer) be placed beforehand into a sample carrier 23 in order to improve the handleability in the scope of the analysis of the tablet 26 produced.
Fig. 4 schematically shows the production of a tablet 26 comprising a sample material in the scope of a method according to the invention in a fourth embodiment, and a device used in this case.
This embodiment of a method according to the invention is also based on the method of selective laser melting (SLM). The powder processed in this case again consists of a mixture of the sample material with a fluxing agent. This powder is prepared according to the procedure in the above-described embodiments of methods according to the invention, i.e. after possible decontamination of a fine mill (not represented), a portion of the sample material is ground in a first grinding step in the fine mill, and subsequently mixed with the fluxing agent, and the sample material/fluxing agent mixture is subsequently blended in a second grinding step in the fine mill.
Subsequently, a sufficient amount of the sample material/fluxing agent mixture is fed through an inlet 6 to a doser 7 of the device used to carry out this embodiment of a method according to the invention, and is stored there. In the region of an outlet 8, the doser 7 comprises two dosing sliders 9, 10 spaced apart parallel to one another, which in the known way allow separation of a defined volume of the sample material/fluxing agent mixture from the total amount of the sample material/fluxing agent mixture stored in the doser 7, by opening the upper dosing slider 10 when the lower dosing slider 9 is closed, so that sample material/fluxing agent mixture can fall into the dosing space 11 formed between the dosing sliders 9, 10. By closing the upper dosing slider 10, a portion of the sample material/fluxing agent mixture corresponding to the volume of the dosing space 11 is then separated from the remaining amount of the sample material/fluxing agent mixture stored in the doser 7. This separated portion can then be released from the doser 7 by opening the lower dosing slider 9.
A portion of the sample material/fluxing agent mixture released in this way falls onto a plate 12 of a reception device 13 arranged below the doser 7. The plate 12 can be moved in a vertical and horizontal direction inside a tubular guide 14 of this reception device 13. The reception device 13 furthermore comprises a vibrator 15, by means of which the reception device 13 can be set in vibration. This is used for loosening of the portion of the sample material/fluxing agent mixture resting on the plate 12, as well as for initial surface distribution of this portion on the plate 12.
Subsequently, by means of a distributor slider 16, the sample material/fluxing agent mixture is distributed in a layer with maximal uniform thickness on the plate 12, while excess sample material/fluxing agent mixture is delivered into a sample cup 18 through a sample run-off 17. This excess sample material/fluxing agent mixture may be fed back from the sample cup 18 into the doser 7 for reuse. To this end, the sample cup 18 may be removed by means of an automatic handling device, for example a robot (not represented), and moved to the inlet 6 of the doser 7. As an alternative, the excess sample material/fluxing agent mixture may also be removed from the sample cup 18, for example suctioned by means of a suction device 19, and then optionally disposed of.
The smoothed layer of the sample material/fluxing agent mixture, resting on the plate 12 of the reception device 13, is subsequently irradiated by means of a laser 20 and thereby selectively melted. To this end, a mirror 21 that can be tilted in an automated fashion is provided, the tilting movement of which makes it possible to irradiate, and thereby melt, a defined region of the layer of the sample material/fluxing agent mixture gradually by means of a laser beam generated by the laser 20 (as an alternative, direct energy input without a mirror is also possible). After solidification, a melted and cooled layer is formed. A multiplicity of such layers (connected to one another with a material fit) can optionally be formed layerwise above one another, by respectively carrying out in succession application of a dosed portion of the sample material/fluxing agent mixture onto the plate 12 of the reception device 13, distribution or smoothing of this portion, and melting and solidification of this portion, for each cycle the plate 12 being moved vertically (downward) by a distance which corresponds essentially to the intended layer thickness of the melted layer being formed.
After the formation of one or more melted and cooled layers, the plate 12 is moved horizontally, so that the melted and cooled layer or layers fall into a reception container 24. As soon as there is a sufficient amount of melted and cooled material (i.e. the melted layer(s) 4, optionally broken into fragments) in the reception container 24, the reception container 24 is removed by means of an automatic handling device, for example a robot, and delivered to a precomminuting device 25. The melted and cooled material may to this end, for example, be precomminuted in the reception container 24 by means of a mortar or a suitable impact device. Subsequently, the precomminuted particles are delivered to a fine mill and ground therein. After the grinding, a pressed tablet 26 ready for analysis is formed from the previously melted and cooled material in a tablet press. To this end, the melted, cooled and then ground material may be pressed in a molding ring, as was described with the aid of Figs 1 and 2.
In all described embodiments, instead of melting of the sample material/fluxing agent mixture by means of laser radiation, melting by means of plasma radiation, hightemperature infrared radiation, microwave radiation or electron radiation may also be carried out, without the other described method steps having to be modified for this purpose. Under certain circumstances, individual method steps may also take place under protective gas (for example argon).
In principle, in all methods according to the invention, and therefore also in the above-described embodiments of methods according to the invention, additional method steps may advantageously be carried out, which in particular are used to ensure a sufficient quality of the tablet 26 to be produced. In this case, in particular, the melting of the sample material/fluxing agent mixture and the resolidification of the melt may be monitored regularly or continuously, in particular by means of a measurement of the temperature of the melt, for example by means of a pyrometer (not represented) and/or by means of monitoring of the heat distribution of the melt, for example by means of a thermal imaging camera (not represented) and corresponding image processing software. Likewise, an observation of the melting process by means of a camera (in particular CMOS; not represented) may be carried out. Likewise, monitoring of the formation of the melted layer, or a quality inspection of the glass thereby formed, may also be carried out by means of a camera (not represented). Some or all of these steps may advantageously also be provided in a configuration as a real-time monitoring system (online system).
Figs 5 and 6 show two steps during the analysis of a tablet 26 comprising a sample material in the scope of a method according to the invention.
For the analysis, which is carried out according to the invention by means of laser emission spectroscopy, a very short pulse of high-energy laser radiation 27 is focused pointwise onto the surface to be inspected of the tablet 26. The high power density in the focused section of the surface of the tablet 26 leads to heating of a portion 32 of the material there, in general to values of a few tens of thousands of degrees Celsius. These high temperatures lead to the formation of a light-emitting plasma 28, this light emission 31 being characteristic of the material to be examined of the tablet 26. For the analysis, the light emission 31 of the plasma is delivered, for example, through an optical fiber 29 to a spectrometer, so that the atomic composition of the material can be determined qualitatively and quantitatively from the spectrum of the light emission 31 of the plasma 28 generated.
of References:
molding ring carrier layer layer of a sample material/fluxing agent mixture vitreous, or melted and cooled, layer recess inlet of the doser doser outlet of the doser lower dosing slider upper dosing slider dosing space plate of the reception device reception device guide of the reception device vibrator distributor slider sample run-off sample cup suction device laser mirror transport device sample carrier reception container precomminuting device (pressed) tablet laser radiation plasma optical fiber spectrometer light emission portion of the material of the tablet
Claims (22)
- Patent Claims1. A method for analyzing a sample material, wherein the sample material is ground, shaped into a tablet and subsequently analyzed, characterized in that the analysis is carried out by means of laser emission spectroscopy.
- 2. The method as claimed in claim 1, characterized in that a laser is applied to a surface of the tablet at a plurality of positions in the scope of the laser emission spectroscopy.
- 3. The method as claimed in claim 1 or 2, characterized in that the sample material is at least partially mixed with a fluxing agent before or after the grinding.
- 4. The method as claimed in one of the preceding claims, characterized in that the sample material or the sample material/fluxing agent mixture is at least partially melted before the analysis.
- 5. The method as claimed in claim 4, characterized in that solidification of the melt is carried out, the solidified melt already having the tablet shape or being converted into the tablet shape.
- 6. The method as claimed in claim 4 or 5, characterized in that the sample material or the sample material/fluxing agent mixture is cooled during the melting.
- 7. The method as claimed in one of claims 4 to 6, characterized in that at least a fraction, intended for the melting, of the sample material or of the sample material/fluxing agent mixture is preheated before the melting and/or supplementarily heated during the melting.
- 8. The method as claimed in one of claims 4 to 7, characterized in that the sample material or the sample material/fluxing agent mixture is melted by means of laser radiation, plasma radiation, high-temperature infrared radiation, microwave radiation and/or electron radiation.
- 9. The method as claimed in claims 7 and 8, characterized in that at least the fraction, intended for the melting, of the sample material or of the sample material/fluxing agent mixture is preheated by means of laser radiation, and the sample material or the sample material/fluxing agent mixture is melted by means of laser radiation of the same laser.
- 10. The method as claimed in claim 8 or 9, characterized in that the sample material or the sample material/fluxing agent mixture is at least partially melted by means of laser radiation, to which end the same laser is used as for carrying out the subsequent laser emission spectroscopy.
- 11. The method as claimed in one of claims 4 to 10, characterized in that the sample material or the sample material/fluxing agent mixture is melted selectively.
- 12. The method as claimed in claim 3 or one of the claims dependent on claim 3, characterized in that the sample material is preground in a first grinding step, and is ground further in a further grinding step after mixing with the fluxing agent.
- 13. The method as claimed in claim 5 or one of the claims dependent on claim 5, characterized in that the solidification is carried out in such a way that a vitreous component of the tablet is formed.
- 14. The method as claimed in claim 5 or one of the claims dependent on claim 5, characterized in that the sample material or the sample material/fluxing agent mixture is melted and solidified layerwise.
- 15. The method as claimed in claim 5 or one of the claims dependent on claim 5, characterized in that the solidified melt is ground and subsequently converted into the tablet shape.
- 16. The method as claimed in claim 5 or one of the claims dependent on claim 5, characterized in that the melting and/or the carrying out of the solidification of the melt is monitored in real time.
- 17. The method as claimed in claim 16, characterized in that the monitoring is carried out by using imaging sensors or a pyrometer.
- 18. The method as claimed in one of the preceding claims, characterized in that a decontaminant is ground in a mill, and the sample material, the sample material/fluxing agent mixture or the solidified melt is subsequently ground in the same mill.
- 19. The method as claimed in claim 18, characterized in that the decontaminant comprises a first portion of the sample material, of the sample material/fluxing agent mixture or of the solidified melt.
- 20. The method as claimed in claim 18 or 19, characterized in that the decontaminant comprises a material different to the sample material.
- 21. A system for analyzing a sample material, comprising a mill for grinding the sample material and a device for shaping a tablet from the ground sample material, characterized by a device for analyzing the sample material by means of laser emission spectroscopy.
- 22. The system as claimed in claim 16, characterized by • a mixing device for mixing the sample material with a further material, and/or • a device for melting at least a part of the sample material, and/or • a heating device, and/or • a cooling device, and/or • a device for generative production of a tablet from the ground sample material, and/or • a device for real-time monitoring of melting of the sample material, and/or • a molding ring for receiving the ground sample material.1/4 twFig. 22/4Fig. 3ΟCM3/4LOCMOCMA/ALD .00IDCM
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102015122408.9A DE102015122408A1 (en) | 2015-12-21 | 2015-12-21 | Method and installation for analyzing a sample material |
| DE102015122408.9 | 2015-12-21 | ||
| PCT/EP2016/081951 WO2017108810A1 (en) | 2015-12-21 | 2016-12-20 | Method and system for analyzing a sample material |
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| US3890089A (en) * | 1973-10-17 | 1975-06-17 | Aluminum Co Of America | Homogeneous fusion system and method |
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| DE4428920A1 (en) * | 1994-08-16 | 1996-02-22 | Krupp Polysius Ag | Material prepn. and application of X=ray fluorescence analysis |
| DE102008010176B3 (en) * | 2008-02-20 | 2009-11-12 | Thyssenkrupp Steel Ag | Producing standard sample to calibrate analysis devices to determine non-metallic inclusions in metals, comprises mixing powdered metal- and powdered non-metallic solid particles and then hot isostatically pressing in inert gas atmosphere |
| WO2011006156A2 (en) * | 2009-07-10 | 2011-01-13 | University Of Florida Research Foundation, Inc. | Method and apparatus to laser ablation-laser induced breakdown spectroscopy |
| EP2677301B1 (en) * | 2011-02-18 | 2020-05-06 | Tsinghua University | Method and system for improving precision of element measurement based on laser-induced breakdown spectroscopy |
| US8664589B2 (en) * | 2011-12-29 | 2014-03-04 | Electro Scientific Industries, Inc | Spectroscopy data display systems and methods |
| EP2976620B1 (en) * | 2013-03-22 | 2017-08-09 | FOSS Analytical A/S | System for and method of combined libs and ir absorption spectroscopy investigations |
| DE102013106998A1 (en) | 2013-07-03 | 2015-01-08 | Thyssenkrupp Industrial Solutions Ag | Method and device for producing a tablet |
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