AU2016227675B2 - Method for producing a tablet which comprises a sample material - Google Patents

Method for producing a tablet which comprises a sample material Download PDF

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Publication number
AU2016227675B2
AU2016227675B2 AU2016227675A AU2016227675A AU2016227675B2 AU 2016227675 B2 AU2016227675 B2 AU 2016227675B2 AU 2016227675 A AU2016227675 A AU 2016227675A AU 2016227675 A AU2016227675 A AU 2016227675A AU 2016227675 B2 AU2016227675 B2 AU 2016227675B2
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Australia
Prior art keywords
sample material
fluxing agent
tablet
layer
ground
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AU2016227675A1 (en
Inventor
Marc BORNEFELD
Oliver Maier
Jürgen Schneberger
Reinhard Teutenberg
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Thyssenkrupp Polysius GmbH
ThyssenKrupp AG
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Thyssenkrupp Polysius GmbH
ThyssenKrupp AG
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2202—Preparing specimens therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2866—Grinding or homogeneising

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention relates to a method for producing a tablet which comprises a sample material, the sample material being ground. Said method is characterized by mixing the ground sample material at least to some extent with a melting agent, at least partially melting the mixture of sample material and melting agent and then causing the melt to solidify in tablet form.

Description

The invention relates to a method for producing a tablet which comprises a sample material, the sample material being ground. Said method is characterized by mixing the ground sample material at least to some extent with a melting agent, at least partially melting the mixture of sample material and melting agent and then causing the melt to solidify in tablet form.
(57) Zusammenfassung: Ein Verfahren zur Herstellung einer ein Probenmaterial umfassenden Tablette, bei dem das Probenmaterial gemahlen wird, ist dadurch gekennzeichnet, dass das gemahlene Probenmaterial zumindest teilweise mit einem Schmelzmittel vermischt, die ProbenmaterialSchmelzmittel-Mischung zumindest teilweise aufgeschmolzen und anschlieBend eine Erstarrung der Schmelze in der Tablettenform herbeigefuhrt wird.
WO 2016/139240 Al llllllllllllllllllllllllllllllllllllllllllllllllll^ (84) Bestimmungsstaaten (soweit nicht anders angegeben, fur jede verfugbare regionale Sckutzrechtsartf. ARIPO (BW, GH, GM, KE, LR, LS, MW, MZ, NA, RW, SD, SL, ST, SZ, TZ, UG, ZM, ZW), eurasisches (AM, AZ, BY, KG, KZ, RU, TJ, TM), europaisches (AL, AT, BE, BG, CH, CY, CZ, DE, DK, EE, ES, FI, FR, GB, GR, HR, HU, IE, IS, IT, LT, LU, LV, MC, MK, MT, NL, NO, PL, PT, RO, RS, SE, SI, SK, SM, TR), OAPI (BF, BJ, CF, CG, CI,
CM, GA, GN, GQ, GW, KM, ML, MR, NE, SN, TD, TG).
Veroffentlicht:
— mit internationalem Recherchenbericht (Artikel 21 Absatz 3) ι
2016227675 30 Apr 2018
Method for producing a tablet which comprises a sample material
The invention relates to a method of producing a tablet comprising a sample material intended for use in an analysis of the sample material.
It is known that tablets of this kind can be produced as compressed tablets by grinding the sample material and processing it further to give the tablet with employment of pressure and/or binders. A method of this kind requires the sample material already to be in a physical consistency suitable for the finished tablet prior to the grinding.
It is also known that tablets of this kind can be produced from a melt. This involves mixing the sample material with a fluxing agent, melting this sample material/fluxing agent mixture and pouring the melt into a tablet mold and cooling it therein.
However, such a cooling operation with simultaneous shaping is complex both from an engineering and from an apparatus point of view. Thus, a melt tablet has to be cooled under very controlled conditions, since excessively rapid cooling can lead to fracture of the tablet, whereas the melt would crystallize in the event of excessively slow cooling, as a result of which the tablet would likewise lose its strength.
WO 2015/000571 Al and US 5,257,302 each disclose methods of producing a tablet comprising a sample material, in which a material mixture comprising the sample material is melted and cooled again. The resultant vitreous material is then ground and subsequently compressed to the tablet.
It was an object of the invention to specify an improved method of producing a tablet comprising a sample material.
A first aspect provides a method of producing a tablet comprising a sample material, in which the sample material is ground (preferably down to a maximum grain size of
100 pm, more preferably of 63 pm), the ground sample material is at least partly mixed with a fluxing agent, the sample material/fluxing agent mixture is at least
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2016227675 30 Apr 2018 partly melted and then solidification of the melt in tablet form is induced, wherein the sample material/fluxing agent mixture is melted and solidified layer by layer.
The melting of the sample material/fluxing agent mixture can achieve conversion thereof to a homogeneous melt, which may help to improve examination of the sample material using the resolidified melt. This is because it may be possible in this way to eliminate or reduce effects that would otherwise arise from the grain size distribution and the original mineral state of the sample material. Because the melt is induced to solidify in tablet form, the tablet can be used for sample analysis directly after this method step. As a result, it may be possible to avoid further method steps that would be necessary in order to convert a melt that solidifies in an uncontrolled manner to tablet form, as is known from WO 2015/000571 Al or US 5,257,302.
“Tablet” is understood in accordance with the invention to mean a solid body in a defined spatial form that includes a material mixture comprising the sample material.
In a preferred embodiment of the method of the invention, it may be the case that the sample material is subjected to preliminary grinding in a first grinding step and, after being mixed with the fluxing agent, to further grinding in a further grinding step. In this case, the grinding of the sample material/fluxing agent mixture can serve the primary purpose of mixing the already ground sample material with the fluxing agent in an optimal manner. This may especially be enabled by the fluxing agent in many cases already being in the form of fine grains. One advantage that can arise from this is that both the grinding of the sample material and the mixing of the sample material with the fluxing agent can be conducted in the same apparatus, namely a suitable (fine) mill. Provision of an additional mixing apparatus can thus be avoided. A further advantage which can result from the further grinding step is that a possibly heterogeneous grain size distribution of sample material and fluxing agent can be corrected.
Accordingly, “grinding” in accordance with the invention is not necessarily understood to mean a method step in which processing of a material or material mixture is associated with achievement of a reduction in the grain size of the material
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2016227675 30 Apr 2018 or material mixture. Instead, such a “grinding” operation can serve exclusively or primarily for mixing of a material mixture, if grinding of the material or material mixture would be possible in principle, i.e. with different method parameters, through the use of the same apparatus (mill) utilized here.
If appropriate, fluxing agent may also be mixed with the sample material in dosed form as a solid body, for example as a tablet with a specific weight, by means of which dosage of sample material and fluxing agent in a predefined ratio can be simplified. In this case, it may be advisable also to grind the solid fluxing agent body in at least one of the grinding steps, i.e. to reduce it to particles of a defined (maximum) grain size.
In a further-preferred embodiment of the method of the invention, it may be the case that the solidification of the melt is induced by forming a vitreous constituent (the resolidified melt) of the tablet.
“Vitreous” or “vitreous constituent” is understood to mean an amorphous material configuration which, after cooling from the melt, does not have a crystal structure. Conversion of the melt to a vitreous constituent can especially be achieved by cooling the melt with sufficient speed, which prevents crystallization of the molten material.
The vitreous constituent may be particularly advantageously suitable for the analysis 20 of the sample material because the homogeneous mixture that results from the melting of the sample material together with the fluxing agent is conserved therein, and the fluxing agent is dimensionally stable.
A fluxing agent usable advantageously in the performance of an embodiment of the method of the invention may, for example, be lithium tetra- or metaborate, sodium tetra- or metaborate, potassium disulfate and/or an acid, for example boric acid, or a mixture thereof - with addition of additives as well (e.g. fluxes such as LiBr).
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2016227675 30 Apr 2018
It may further be preferable that the fluxing agent is mixed with the sample material in a ratio of between 40:1 to 2:1, preferably between 10:1 and 2:1.
The sample material/fluxing agent mixture is melted and solidified layer by layer (i.e. successively in multiple layers). This may enable relatively rapid generation of the melt as a result of exactly dosed and very high local introduction of energy into the sample material/fluxing agent mixture (or the fraction thereof envisaged for the melting).
It may more preferably be the case that the layer-by-layer melting and solidification of the fluxing agent/sample material mixture is utilized as an additive manufacturing method for production of the tablet (or the corresponding constituent thereof). An additive manufacturing method is characterized in that a three-dimensional body composed of a pulverulent material in particular is generated layer by layer, by starting from a base layer and, in a layer-by-layer manner, applying material to this base layer, melting it and solidifying it. A relevant advantage of such an additive manufacturing method is that, by virtue of material being melted in an only relatively thin layer and in a locally limited manner, it may be possible to dispense with accommodation of the melt during the solidification in a negative mold corresponding to the envisaged shape of the resolidified melt (i.e. in the form of the tablet or the corresponding constituent thereof).
Suitable specific embodiments for production of the tablet or a constituent thereof by an additive manufacturing method are selective laser sintering, which is common knowledge, selective laser melting and (selective) electron beam melting.
Layer-by-layer melting and solidification can also be affected by first melting and solidifying a surface layer, and then melting and solidifying a layer beneath (i.e. a layer which is spatially separated by the surface layer with respect to a radiation source that brings about the melting). This can be continued step-by-step until the intended thickness of the tablet to be produced or of the component of the tablet to be produced has been attained. As the case may be, it may be possible here to exploit
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2016227675 30 Apr 2018 different absorption for energy radiation by the sample material/fluxing agent mixture on the one hand and the resolidified melt on the other hand.
Melting of the sample material/fluxing agent mixture or the proportion thereof envisaged for melting can preferably be effected by means of a laser beam, an electron beam and/or a plasma jet. Alternative methods to this, which may in principle be based on conduction, convection and/or thermal radiation, may likewise be employed.
In a preferred embodiment of the method of the invention, it may be the case that the sample material/fluxing agent mixture (optionally after mixing-in of a binder) is compressed prior to melting. This may especially be advantageous if there is no intention to form the entire tablet in the form of a resolidified melt and hence no intention to melt the entire sample material/fluxing agent mixture. It may thus be especially possible in principle to form the tablet in the form of a compressed tablet, while only a surface layer envisaged primarily for the later analysis is melted and resolidified, in order to correspondingly improve the analysis by virtue of the vitreous and hence amorphous structure which is preferably to be obtained, and homogenization of the sample material in this surface layer. The surface layer here may advantageously have a thickness of between 30 pm and 300 pm.
The sample material/fluxing agent mixture can preferably be compressed in a mold 20 ring. This mold ring may constitute the negative mold with respect to the envisaged tablet form at least over the circumference. Advantageously, the mold ring may consist at least partly of stainless steel or a refractory metal having a low coefficient of thermal expansion.
In a further-preferred embodiment of the method of the invention, it may be the case 25 that a decontaminating agent is ground in a mill and then the sample material to be mixed with the fluxing agent is ground in the same mill. This can serve to decontaminate the mill that may already have been utilized for grinding of a different kind of sample material beforehand, or to deliberately contaminate it with the sample material to be ground subsequently. In this way, it may be possible to as far as
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2016227675 30 Apr 2018 possible rule out contamination of the sample material that could lead to distortion of the result of any subsequent analysis of this sample material.
The decontaminating agent may preferably be or at least comprise a first portion of the sample material. Alternatively or additionally thereto, however, the decontaminating agent may also be or comprise a material other than the sample material, such as, more particularly, sand, corundum and/or any refractory material (including fireclay-containing material).
In one embodiment of the method of the invention, it may be the case that the ground decontaminating agent is discarded, such that it is at least not utilized any further within the context of the method of the first aspect of the invention. It may especially be the case here that the decontaminating agent is disposed of.
It may also be possible that the ground decontaminating agent is compressed and utilized as base layer for the sample material/fluxing agent mixture. In this case, a selection of the decontaminating agent (or at least of a constituent thereof) can also be made with regard to suitability as base layer. Compression of the decontaminating agent can preferably be effected in a mold ring, the height of which is greater and preferably at least twice as great as the layer thickness of the base layer. The unit composed of base layer and mold ring can then serve as vessel-like negative mold (with respect to the tablet form envisaged) for the sample material/fluxing agent mixture to be introduced subsequently therein, which can also be processed further, especially compressed and/or melted, therein.
In order to assure a reliable hold of the compressed tablet within the mold ring, it may preferably be the case that it forms at least one depression on the inside, into which the sample material and/or decontaminating agent can penetrate in the respective compression operation, which can result in formation of a form-fitting bond between the compressed tablet and the mold ring.
Another aspect of the invention further relates to a method of analyzing a material sample of a sample material, wherein a tablet comprising the sample material is
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2016227675 30 Apr 2018 produced by means of a method of the first aspect of the invention and then an analysis of the sample material is conducted using the tablet. In the analysis of the sample material, it may especially be possible to conduct an x-ray fluorescence analysis.
The sample material may especially comprise one or more natural rocks, for example silicates, carbonates, sulfates, sulfides, salts, phosphates and/or oxides. In addition, the sample material may especially comprise industrial process products, for example slag, fly ash, alloys and/or other metal compounds.
The indefinite article (“a”), especially in the claims and in the description that elucidates the claims in general, should be understood as such and not to mean “one”. Components correspondingly specified therewith should thus be understood such that these are present at least once and may be present more than once.
Embodiments of the invention is elucidated in detail hereinafter by way of example only with reference to working examples shown in the drawings. The drawings show:
Fig. 1: a schematic of a tablet produced by means of a first embodiment of a method of the invention;
Fig. 2: a schematic of a tablet produced by means of a second embodiment of a method of the invention; and
Fig. 3: a schematic of the procedure of a method of the invention in a third embodiment and an apparatus utilized therein.
Fig. 1 shows a tablet which comprises a sample material and has been produced by means of a first embodiment of a method of the invention. In this embodiment of a method of the invention, first of all, a first portion (e.g. 5 to 6 g) of the sample material to be processed and analyzed is metered into a fine mill (not shown) and ground therein as purge sample or preliminary sample. This deliberately
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2016227675 30 Apr 2018 contaminates the fine mill with the sample material to be processed. This first portion of the sample material therefore serves as decontaminating agent.
The portion of the sample material utilized as decontaminating agent, after grinding in the fine mill, is pressed by means of a tableting press (not shown) into a mold ring 1 made, for example, of stainless steel (cf. fig. 1), in order to form a base layer 2 for a further layer 3 of a mixture of a second portion of the sample material and a fluxing agent. This further layer 3 or a constituent thereof serves for subsequent analysis of the sample material. The base layer 2 is unsuitable for this purpose as a result of possible contamination by the impurities present in the fine mill. For the base layer 2, for example, a layer thickness of three to four millimeters may be envisaged. This layer thickness may correspond to about 50% of the height of the mold ring 1. After cleaning of the mold ring 1 and the base layer 2, the unit formed from these two components is turned by 180° (about a radial axis), such that this unit forms a vessel open at the top into which the further portion of the sample material can be introduced.
Subsequently, the further portion of the sample material is metered into the fine mill and ground in a first grinding step therein. The speed with which the fine mill is operated and the grinding time can be adjusted according to the sample material to be processed. After the conclusion of the first grinding step, a fluxing agent (e.g. lithium tetraborate) is mixed into this ground portion of the sample material in accordance with a defined mixing ratio (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 the fine mill in a second grinding step and mixed as thoroughly as possible. The sample material/fluxing agent mixture is then introduced into the vessel formed by the mold ring 1 and the base layer 2 and compressed in the tableting press. The compressed tablet thus formed consists of two layers at first, namely the base layer 2 of the optionally contaminated first portion of the sample material, and of the further layer 3 which is to be the subject in the subsequent analysis, consisting of the compressed sample material/fluxing agent mixture.
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The free surface of this further layer 3 is then irradiated and melted by means of a laser (not shown in fig. 1). The corresponding surface is remelted/fused in full 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 as a result of cooling, the tablet to be produced comprises a vitreous layer 4 characterized by a very homogeneous material configuration. This vitreous layer 4 is advantageously suitable for a subsequent analysis of the sample material in, for example, an x-ray fluorescence analyzer (not shown).
In one possible variant, the laser beam is used to scan the surface of the further layer 3 point by point (area by area). This produces very small “melt puddles” which solidify again in vitreous form a short time later. As a result of the flowing process resulting from the movement of the laser, the entire surface is homogeneously fused and converted to a vitreous layer 4.
The point of the melt fusion is to convert the sample material together with a fluxing agent to a homogeneous melt which solidifies in vitreous form on cooling. The fusion eliminates or at least reduces effects on the intensity of the fluorescence radiation within the x-ray fluorescence analysis that are caused by the grain size distribution and the mineralogical original state of the sample material. The fusion leads to a homogeneous binding form of the elements and, through dilution, reduces the effect of the elements on one another through secondary excitation and absorption.
Remelting is a chemical operation. The fluxing agent breaks down the compounds of the sample material and chemically converts them. Silicates, aluminates, carbonates and sulfates of the sample material (if present) thus become borates, for example.
Remelting or fusion of, for example, Fe2O3, Fe3C>4, FeO, FeCh, FeS2, FeCO3 with tetraborate gives rise to iron borates. Through conversion to iron borates, the influences of the chemical bonding are minimized.
In an alternative embodiment of the above-described method of producing a tablet comprising a sample material (according to fig. 2), no base layer 2 is generated.
10121589_1 (GHMatters) P106825.AU
2016227675 30 Apr 2018 ίο
Instead, a compressed tablet is formed exclusively from the sample material/fluxing agent mixture. For this purpose, a first portion of the sample material is again first ground as purge sample or decontaminating agent, but then discarded. On completion of decontamination of the mill, a second portion of the sample material (e.g. 2 g) is again processed in two grinding steps. In the first grinding operation, only this second portion of the sample material is ground. For the second grinding step, in a very exact ratio of, for example, 1:5 (sample material to fluxing agent), a fluxing agent is then added and ground together with the sample material in order to achieve very thorough mixing of these components. The mixture of the sample material and the fluxing agent is then transferred to a tableting press (not shown). The mixture is compressed therein to a layer 3 corresponding essentially to the form of the tablet to be produced. Subsequently, the melting and solidification of a surface layer of the compressed tablet can be conducted in accordance with the above-described embodiment of a method of the invention in order to form a vitreous layer 4.
The mold ring 1 utilized in the course of performance of the above-described methods has, on its inside, two circumferential V-shaped (or else oval) depressions 5. One of the depressions 5 is in the upper axial half and the other depression 5 in the lower axial half of the mold ring 1. The mold ring 1 has, for example, an (axial) height of 8.5 mm. One of the depressions 5, proceeding from one of the axial ends of zu the mold ring 1, is, for example, at an axial height of 2.5 mm, and the other depression (proceeding from the same axial end of the mold ring 1) at an axial height of 6 mm.
Fig. 3 shows, in schematic form, the procedure for a method of the invention in a third embodiment, and an apparatus utilized in the performance of this method.
This embodiment of a method of the invention is based on the method of selective laser melting (SLM). The powder processed consists of a mixture of a sample material and a fluxing agent. This powder is processed in accordance with the procedure in the two above-described embodiments of method of the invention, i.e., after possible decontamination of a fine mill (not shown), a portion of the sample
10121589_1 (GHMatters) P106825.AU
2016227675 30 Apr 2018 material is ground in the fine mill in a first grinding step and subsequently mixed with the fluxing agent, and then the sample material/fluxing agent mixture is mixed in the fine mill in a second grinding step.
Subsequently, a sufficient amount of the sample material/fluxing agent mixture is supplied via an inlet 6 to a metering device 7 of the apparatus utilized for the performance of this embodiment of a method of the invention and stored here. In the region of an outlet 8, the metering device 7 has two metering valves 9, 10 spaced apart in a parallel manner, which, in a known manner, enable separation of a defined volume of sample material/fluxing agent mixture from the total amount of the sample material/fluxing agent mixture held in the metering device 7, in that, with the lower metering valve 9 closed, the upper metering valve 10 is opened, such that sample material/fluxing agent mixture can fall into the metering space 11 formed between the metering valves 9, 10. By closing the upper metering valve 10, a portion of the sample material/fluxing agent mixture corresponding to the volume of the metering space 11 is then separated from the remaining amount of the sample material/fluxing agent mixture retained in the metering device 7. This separated portion can then be discharged from the metering device 7 by opening the lower metering valve 9.
A portion of the sample material/fluxing agent mixture discharged in this way drops onto a plate 12 of a receiving apparatus 13 arranged beneath the metering device 7.
The plate 12 is movable in vertical direction within a guide system 14 of this receiving apparatus 13. The receiving apparatus 13 further comprises a vibrator 15, by means of which the receiving apparatus 13 can be set in oscillation. This serves to loosen up the portion of the sample material/fluxing agent mixture lying on the plate 12, and for a first areal distribution of this portion on the plate 12.
Subsequently, by means of a distributor valve 16, the sample material/fluxing agent mixture is distributed on the plate 12 in a layer of very substantially homogeneous thickness, and excess sample material/fluxing agent mixture is guided into a sample container 18 via a sample ejector 17. This excess sample material/fluxing agent mixture can be conveyed from the sample container 18 back into the metering device
10121589_1 (GHMatters) P106825.AU
2016227675 30 Apr 2018 for reuse. For this purpose, the sample container 18 can be removed by means of an automatic handling device, for example a robot (not shown), and moved to the inlet 6 of the metering device 7. Alternatively, it may also be the case that the excess sample material/fluxing agent mixture is removed from the sample container 18, for example sucked out by means of a suction apparatus 19, and then optionally disposed of.
The layer of the sample material/fluxing agent mixture lying in smoothed form on the plate 12 of the receiving apparatus 13 is subsequently irradiated and selectively melted by means of a laser 20. For this purpose, a mirror 21 pivotable in an automated manner is provided, the pivoting motion of which enables irradiation and resultant melting of a defined region of the layer of the sample material/fluxing agent mixture by means of a laser beam generated by the laser 20. Solidification of the melt thus generated gives rise to a vitreous layer. This vitreous layer may already be the tablet to be produced. Alternatively, it is possible to form a multitude of such vitreous layers one on top of another layer by layer, in that application of a metered portion of the sample material/fluxing agent mixture to the plate 12 of the receiving apparatus 13, distribution/smoothing of this portion and melting and solidifying of this portion are each conducted in succession, with downward movement of the plate 12 for each cycle by a distance corresponding substantially to the envisaged layer thickness of the vitreous layer to be formed.
The vitreous layer(s) thus generated can then optionally be applied to a base layer (not shown), in order to increase the dimensional stability of the tablet to be produced.
By means of a transport apparatus 22, for example a suction gripping element, the tablet or the vitreous layer(s) can then be removed from the receiving apparatus 13 and transferred into an analyzer (not shown), for example an x-ray fluorescence analyzer. As the case may be, the vitreous layer(s) thus generated (if appropriate in conjunction with the base layer) may also have been inserted into a sample carrier 23 beforehand, in order to improve the ease of handling of the tablet produced in the context of the analysis.
10121589_1 (GHMatters) P106825.AU
2016227675 30 Apr 2018
In principle, in all methods of the invention and hence also in the above-described embodiments of methods of the invention, it may be advantageously possible to conduct additional method steps that especially serve to assure adequate quality of the tablet to be produced. It may especially be the case here that the melting of the sample material/fluxing agent mixture and the re-solidification of the melt are monitored regularly or continuously, especially by means of measurement of the temperature of the melt, for example by means of a pyrometer (not shown), monitoring of the heat distribution of the melt, for example by means of a thermal imaging camera (not shown) and corresponding image processing software. It is likewise possible to observe the melting operation by means of a camera (especially CMOS; not shown). It is likewise also possible by means of a camera (not shown) to conduct monitoring of the formation of the vitreous layer or examination of the quality of the glass formed. Some or all of these steps can advantageously also be designed, in one configuration, in the form of remote monitoring (online system). Such remote monitoring may simultaneously also comprise corresponding remote control of the temperature regulation or of the thermal energy introduced into the sample material/fluxing agent mixture by the heat source used.
It is to be understood that, if any prior art publication is referred to herein, such reference does not constitute an admission that the publication forms a part of the common general knowledge in the art, in Australia or any other country.
In the claims which follow and in the preceding description of the invention, except where the context requires otherwise due to express language or necessary implication, the word “comprise” or variations such as “comprises” or “comprising” is used in an inclusive sense, i.e. to specify the presence of the stated features but not to preclude the presence or addition of further features in various embodiments of the invention.
10121589_1 (GHMatters) P106825.AU
2016227675 30 Apr 2018
2.U
Reference numerals:
mold ring base layer layer of a sample material/fluxing agent mixture vitreous layer depression inlet of the metering device metering device outlet of the metering device lower metering valve upper metering valve metering space plate of the receiving apparatus receiving apparatus guide system of the receiving apparatus vibrator distributor valve sample ejector sample container suction apparatus laser mirror transport apparatus sample carrier
10121589_1 (GHMatters) P106825.AU
2016227675 30 Apr 2018

Claims (15)

  1. Claims:
    1. A method of producing a tablet comprising a sample material, where the sample material is ground, wherein the ground sample material is at least partly mixed with a fluxing agent, the sample material/fluxing agent mixture is at least partly melted and then solidification of the melt in tablet form is induced, wherein the sample material/fluxing agent mixture is melted and solidified layer by layer.
  2. 2. The method as claimed in claim 1, wherein the sample material is subjected to preliminary grinding in a first grinding step and, after being mixed with the fluxing agent, to further grinding in a further grinding step.
  3. 3. The method as claimed in claim 1 or 2, wherein the solidification is brought about by forming a vitreous constituent of the tablet.
  4. 4. The method as claimed in any one of the preceding claims, wherein the fluxing agent used is lithium tetraborate, sodium tetraborate and/or an acid.
  5. 5. The method as claimed in claim 4, wherein the acid is boric acid.
  6. 6. The method as claimed in any one of the preceding claims, wherein the sample material/fluxing agent mixture is compressed before being melted.
  7. 7. The method as claimed in claim 5, wherein the compressed sample material/fluxing agent mixture is melted only in a surface layer.
  8. 8. The method as claimed in one of claims 5 or 6, wherein a decontaminating agent
    20 is ground in a mill and then the sample material to be mixed with the fluxing agent is ground in the same mill.
  9. 9. The method as claimed in claim 7, wherein the decontaminating agent comprises a first portion of the sample material.
  10. 10. The method as claimed in claim 7 or 8, wherein the decontaminating agent
    25 comprises a material other than the sample material.
    10121589_1 (GHMatters) P106825.AU
    2016227675 30 Apr 2018
  11. 11. The method as claimed in any one of claims 7 to 9, wherein the ground decontaminating agent is compressed and utilized as base layer for the sample material/fluxing agent mixture.
  12. 12. The method as claimed in any one of preceding claims 7 to 10, wherein the sample material/fluxing agent mixture and/or the decontaminating agent is compressed in a mold ring that forms at least one depression on the inside to accommodate compressed sample material and/or compressed decontaminating agent.
  13. 13. The method as claimed in any one of the preceding claims, wherein the melting is especially effected selectively by means of a laser beam, an electron beam and/or by means of a plasma jet.
  14. 14. A method of analyzing a sample material, comprising the production of a tablet comprising the sample material according to any one of the preceding claims and the subsequent analysis of the sample material using the tablet.
  15. 15. The method as claimed in claim 14, comprising an x-ray fluorescence analysis.
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DE102015103192.2A DE102015103192A1 (en) 2015-03-05 2015-03-05 Method for producing a tablet comprising a sample material
DE102015103192.2 2015-03-05
PCT/EP2016/054411 WO2016139240A1 (en) 2015-03-05 2016-03-02 Method for producing a tablet which comprises a sample material

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DE102015122408A1 (en) * 2015-12-21 2017-06-22 Thyssenkrupp Ag Method and installation for analyzing a sample material
CN107807107B (en) * 2016-09-08 2022-06-07 中国石油化工股份有限公司 In-situ infrared spectrum sample tabletting device and application
GB201620066D0 (en) * 2016-11-28 2017-01-11 Ucl Business Plc Solid Pharmaceutical dosage formulations and processes
CN113125224A (en) * 2021-04-14 2021-07-16 海检检测有限公司 Test piece of cable target layer, test piece manufacturing method and thickness measuring method

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DE2021667A1 (en) * 1970-05-02 1971-11-25 Siemens Ag Process for the crucible-free digestion of powdered dry material
DE2216035A1 (en) * 1972-04-01 1973-10-18 Schunk & Ebe Gmbh Fused pellets - for direct use in x-ray fluorescent analyses without further treatment
DE4428920A1 (en) * 1994-08-16 1996-02-22 Krupp Polysius Ag Material prepn. and application of X=ray fluorescence analysis

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DE2240809A1 (en) * 1972-08-18 1974-02-28 Siemens Ag PROCESS FOR DEGRADING SILICATES, IN PARTICULAR CEMENT FLOUR
US5257302A (en) 1987-08-31 1993-10-26 Ngk Insulators, Ltd. Fluorescent X-ray analyzing system
DE19714504C2 (en) * 1997-04-08 1999-09-30 Krupp Polysius Ag Method and device for preparing fines samples
DE102013106998A1 (en) 2013-07-03 2015-01-08 Thyssenkrupp Industrial Solutions Ag Method and device for producing a tablet

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DE2021667A1 (en) * 1970-05-02 1971-11-25 Siemens Ag Process for the crucible-free digestion of powdered dry material
DE2216035A1 (en) * 1972-04-01 1973-10-18 Schunk & Ebe Gmbh Fused pellets - for direct use in x-ray fluorescent analyses without further treatment
DE4428920A1 (en) * 1994-08-16 1996-02-22 Krupp Polysius Ag Material prepn. and application of X=ray fluorescence analysis

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ZA201706221B (en) 2019-08-28
EP3265775A1 (en) 2018-01-10
EP3265775B1 (en) 2019-05-08
DK3265775T3 (en) 2019-07-22
DE102015103192A1 (en) 2016-09-08
AU2016227675A1 (en) 2017-10-12

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