EP0042327B1 - Mehrteiliger Schmelztiegel - Google Patents

Mehrteiliger Schmelztiegel Download PDF

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Publication number
EP0042327B1
EP0042327B1 EP81400913A EP81400913A EP0042327B1 EP 0042327 B1 EP0042327 B1 EP 0042327B1 EP 81400913 A EP81400913 A EP 81400913A EP 81400913 A EP81400913 A EP 81400913A EP 0042327 B1 EP0042327 B1 EP 0042327B1
Authority
EP
European Patent Office
Prior art keywords
crucible
platinum
container
receptacle
graphite
Prior art date
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.)
Expired
Application number
EP81400913A
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English (en)
French (fr)
Other versions
EP0042327A1 (de
Inventor
Gérard Willay
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institut de Recherches de la Siderurgie Francaise IRSID
Original Assignee
Institut de Recherches de la Siderurgie Francaise IRSID
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Filing date
Publication date
Application filed by Institut de Recherches de la Siderurgie Francaise IRSID filed Critical Institut de Recherches de la Siderurgie Francaise IRSID
Priority to AT81400913T priority Critical patent/ATE9964T1/de
Publication of EP0042327A1 publication Critical patent/EP0042327A1/de
Application granted granted Critical
Publication of EP0042327B1 publication Critical patent/EP0042327B1/de
Expired legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/04—Crucibles

Definitions

  • the present invention relates to a composite crucible for the inductive fusion of analytical samples.
  • Apparatuses are known, more or less automated, for the preparation, according to a melting-dilution process in a flux, of samples to be analyzed, for example non-metallic samples in the form of beads, intended for fluorescence analysis. of X-rays (FR X).
  • Some of these devices use electrical energy and for this purpose include a melting device constituted by a vertical induction coil, excited by a high frequency current and within which is placed the crucible containing the sample.
  • the melting crucible like the casting nacelle, are made of a material which must have the following essential properties: sufficient mechanical strength when hot, compatible with the weight of the sample, good conductivity of both electricity and heat, finally be as much as possible stainless and chemically inert, even at the high temperatures required by the fusion of the sample.
  • crucibles and nacelles made of noble metal, such as platinum or a platinum alloy, are generally used. These accessories are very expensive and, if the nacelle has a very long lifespan, the crucibles, in fact, are not perfectly unalterable, but must be replaced after a number of fusions varying according to the conditions of use. In this case, we know that certain samples containing metallic phases, such as zinc, can lead to fairly rapid degradation of the crucibles.
  • the subject of the invention is a composite crucible for the fusion of non-metallic analysis samples by inductive means and intended to be placed in an induction heating coil supplied with high frequency electric current, crucible consisting of two separate receptacles, nested one inside the other and separable, characterized in that the outer receptacle is made of noble metal, such as platinum or platinum alloy, in that the removable inner receptacle intended to receive the sample to be melted is carbonaceous material, such as graphite or glassy carbon, and in that means are provided for confining the space between the two containers.
  • platinum container or “grpahite container” will be used to denote the outer container and the inner container respectively, without being able to prejudge nature. exact chemical of the concerned containers.
  • Figures 1 and 3 show, in section, two embodiments of the crucible according to the invention, and Figure 2 a perspective view of the crucible considered.
  • the crucible is shown in place on its support within an induction coil 1 with the interposition of an insulating silica jacket 2 which rests on the base 3.
  • the heating coil 1 when excited by a high frequency current (of the order several Mega hertz), the induced current is attached to the outer platinum container 4, which quickly balances its temperature with that of the inner graphite container 5 by heat exchange which takes place essentially by radiation.
  • This indirect electric heating of the internal container ensures satisfactory fusion of the sample contained therein, substantially as fast as in usual practice (of the order of a minute), but without risk of degradation of the platinum since the latter does not 'is no longer in contact with a molten material capable of damaging it) metallic or reduced phases).
  • the internal graphite container 5 is less justified when the sample to be prepared is not of a chemical nature which can react with platinum and must therefore be able to be removed at will. In addition, it inevitably wears out faster than the outer platinum container and must therefore be able to be replaced more frequently.
  • outer platinum container 4 is provided with a flange 8 which allows it to bear on the upper end of the jacket 2, thus providing an insulation space between the base 3 and the bottom of the container. thermal.
  • the internal container is made of glassy carbon.
  • the vitreous carbon is practically not friable, which avoids entraining, at the time of the casting of the sample, carbon particles torn from the wall and which would risk disturbing the further analysis. It should also be noted that the vitreous carbon wears out during successive fusions but this wear is much slower than that of conventional graphite, and it originates, not from mechanical erosion of the wall, but from chemical reactivity with oxygen (release of CO or CO2) which, in any event, does not pollute the sample. Finally, the vitreous carbon, having by definition the consistency of glass, has non-wetting properties for the sample, which makes it possible to recover all the material at the time of casting, without the need for subsequent cleaning of the container. .
  • the invention can have numerous variant embodiments, both in the form, the nature or the structure of the composite crucible.
  • the crucible can have any geometrical shape insofar as it goes without saying that the two containers which compose it can be nested one inside the other so as to be easily separated, then assembled again. It is understood that in this respect, the most advantageous shape is that of the cylinder, of revolution of pre ference.
  • the inner container 5 may slightly exceed the upper limit of the outer container 4 (a few mm), so as to constitute a possible grip and thus facilitate its introduction into the outer container or its withdrawal. It is understood that such an arrangement also makes it possible, as in the case of the flange 7 previously mentioned with reference to FIG. 3, to avoid smearing of molten material on the platinum crucible during the casting of the sample.
  • this arrangement can be made in different ways, for example as is the case in the figures by using an inner container of height slightly greater than that of the outer container, or by placing a wedge on the bottom thereof.
  • refractory material for example a carbon felt cushion, or equivalent, on which the inner container rests, which makes it possible to obtain the desired height increase.

Landscapes

  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Crucibles And Fluidized-Bed Furnaces (AREA)
  • General Induction Heating (AREA)
  • Glass Compositions (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Claims (5)

1. Zusammengesetzter Schmelztiegel zum Schmelzen nichtmetallischer Analysenproben mittels Induktion, der in einer Induktions-Heizspule (1), welche mit elektrischem Strom hoher Frequenz gespeist ist, angeordnet ist, welcher Schmelztiegel aus zwei verschiedenen, ineinandersetzbaren und trennbaren Behältern besteht, dadurch gekennzeichnet, dass der äussere Behälter (5) aus Edelmetall besteht, dass der auswechselbare innere Behälter (6), welcher dazu bestimmt ist, die zu schmelzende Probe aufzunehmen, aus kohlenstoffhaltigem Material besteht und dass Mittel vorgesehen sind, um den Zwischenraum zwischen den zwei Behältern abzugrenzen.
2. Schmelztiegel nach Anspruch 1, dadurch gekennzeichnet, dass die genannten Begrenzungsmittel für ein Mindestspiel zwischen den zwei Behältern ausgebildet sind, das dem einfachen funktionellen Spielraum entspricht, um ihre Vereinigung oder Trennung zu ermöglichen.
3. Schmelztiegel nach Anspruch 1, dadurch gekennzeichnet, dass die genannten Begrenzungsmittel aus einem Kragen (8) bestehen, der sich am oberen Rand des inneren Behälters (6) befindet und es dem genannten Behälter ermöglicht, sich auf den Rand der Öffnung des äusseren Behälters (5) zu stützen.
4. Schmelztiegel nach Anspruch 1, dadurch gekennzeichnet, dass der innere Behälter aus glasigem Kohlenstoff besteht.
5. Schmelztiegel nach Anspruch 1 oder 4, dadurch gekennzeichnet, dass der äussere Behälter aus Platin besteht.
EP81400913A 1980-06-12 1981-06-09 Mehrteiliger Schmelztiegel Expired EP0042327B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT81400913T ATE9964T1 (de) 1980-06-12 1981-06-09 Mehrteiliger schmelztiegel.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8013111A FR2484284A1 (fr) 1980-06-12 1980-06-12 Creuset composite pour la fusion d'echantillons d'analyse par voie inductive
FR8013111 1980-06-12

Publications (2)

Publication Number Publication Date
EP0042327A1 EP0042327A1 (de) 1981-12-23
EP0042327B1 true EP0042327B1 (de) 1984-10-24

Family

ID=9243028

Family Applications (1)

Application Number Title Priority Date Filing Date
EP81400913A Expired EP0042327B1 (de) 1980-06-12 1981-06-09 Mehrteiliger Schmelztiegel

Country Status (7)

Country Link
US (1) US4446563A (de)
EP (1) EP0042327B1 (de)
JP (1) JPS5715396A (de)
AT (1) ATE9964T1 (de)
CA (1) CA1171141A (de)
DE (1) DE3166801D1 (de)
FR (1) FR2484284A1 (de)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5550353A (en) * 1990-01-31 1996-08-27 Inductotherm Corp. Induction heating coil assembly for prevent of circulating current in induction heating lines for continuous-cast products
US5272720A (en) * 1990-01-31 1993-12-21 Inductotherm Corp. Induction heating apparatus and method
US5257281A (en) * 1990-01-31 1993-10-26 Inductotherm Corp. Induction heating apparatus and method
JPH0685575U (ja) * 1993-05-14 1994-12-06 桂司 久保田 テレビ画面構造
US6211424B1 (en) * 1998-07-30 2001-04-03 Radioactive Isolation Consortium, Llc Advanced vitrification system
US6558308B2 (en) * 2001-05-07 2003-05-06 Radioactive Isolation Consortium, Llc AVS melting process
US6485404B1 (en) * 2002-04-04 2002-11-26 Radioactive Isolation Consortium, Llc Advanced vitrification system improvements
DE10361525B4 (de) * 2003-12-23 2005-11-17 Umicore Ag & Co. Kg Verfahren zur Herstellung von Schmelztabletten zur Bestimmung des Gehaltes von keramischen Pulvern an Platingruppenmetallen mittels RFA
CN101507354A (zh) * 2006-05-30 2009-08-12 豪梅公司 使用石墨熔化容器的熔化方法
DE102021205084B4 (de) 2021-05-19 2023-01-12 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung eingetragener Verein System zur Temperierung von Proben

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR83530E (fr) * 1963-04-18 1964-08-28 Centre Nat Rech Scient Dispositif pour la microanalyse thermique différentielle

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR533426A (fr) * 1921-03-29 1922-03-02 Perfectionnements apportés aux creusets
FR85530E (fr) * 1961-01-30 1965-08-27 Hooker Chemical Corp Compositions bitumineuses retardatrices d'inflammation
US3401227A (en) * 1966-02-09 1968-09-10 Trw Inc Liner for crucibles
GB1108640A (en) * 1966-03-30 1968-04-03 Chyo Balance Corp Temperature measuring device for thermal analysis
US3484840A (en) * 1968-01-26 1969-12-16 Trw Inc Method and apparatus for melting and pouring titanium
US3649734A (en) * 1971-01-29 1972-03-14 Motorola Inc Crucible electron beam evaporation of aluminum
GB1442129A (en) * 1973-01-17 1976-07-07 British Aluminium Co Ltd Containers for molten metal
FR2253565A1 (en) * 1973-12-07 1975-07-04 Ringsdorff Werke Gmbh Carbon or graphite crucible - for laboratory use in the atmosphere at above 500 deg. C
DE2510684C3 (de) * 1975-03-12 1979-11-08 Schweizerische Aluminium Ag, Chippis (Schweiz) Mehrschichtiger Metalltiegel zum Ziehen von Kristallen
US4202400A (en) * 1978-09-22 1980-05-13 General Electric Company Directional solidification furnace

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR83530E (fr) * 1963-04-18 1964-08-28 Centre Nat Rech Scient Dispositif pour la microanalyse thermique différentielle

Also Published As

Publication number Publication date
US4446563A (en) 1984-05-01
CA1171141A (fr) 1984-07-17
JPS5715396A (en) 1982-01-26
JPS6349878B2 (de) 1988-10-06
FR2484284B1 (de) 1983-11-10
EP0042327A1 (de) 1981-12-23
ATE9964T1 (de) 1984-11-15
DE3166801D1 (en) 1984-11-29
FR2484284A1 (fr) 1981-12-18

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