[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

EP0770205A1 - Flask sealing system and microwave treatment apparatus with such a sealing system - Google Patents

Flask sealing system and microwave treatment apparatus with such a sealing system

Info

Publication number
EP0770205A1
EP0770205A1 EP96919884A EP96919884A EP0770205A1 EP 0770205 A1 EP0770205 A1 EP 0770205A1 EP 96919884 A EP96919884 A EP 96919884A EP 96919884 A EP96919884 A EP 96919884A EP 0770205 A1 EP0770205 A1 EP 0770205A1
Authority
EP
European Patent Office
Prior art keywords
flask
plug
axis
abutment surface
sample
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.)
Withdrawn
Application number
EP96919884A
Other languages
German (de)
French (fr)
Inventor
Eric Quentin
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.)
Prolabo SA
Original Assignee
Prolabo SA
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Prolabo SA filed Critical Prolabo SA
Publication of EP0770205A1 publication Critical patent/EP0770205A1/en
Withdrawn legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122Incoherent waves
    • B01J19/126Microwaves
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/12Processes employing electromagnetic waves
    • B01J2219/1203Incoherent waves
    • B01J2219/1206Microwaves
    • B01J2219/1209Features relating to the reactor or vessel
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/12Processes employing electromagnetic waves
    • B01J2219/1203Incoherent waves
    • B01J2219/1206Microwaves
    • B01J2219/1209Features relating to the reactor or vessel
    • B01J2219/1212Arrangements of the reactor or the reactors
    • B01J2219/1218Multiple reactors

Definitions

  • the present invention relates to a closure system for at least one flask of longitudinal axis XX ′, which is open at a first end for the introduction of a sample and which is positioned inside a microwave application cavity for heating the sample.
  • the invention also relates to an apparatus for carrying out a treatment in a humid environment simultaneously on a plurality of samples, the apparatus implementing microwave heating of the samples, and comprising such a sealing system.
  • Such an apparatus finds a particularly advantageous application for the implementation of chemical reactions such as for example mineralization, saponification, hydrolysis, speciation, organic synthesis.
  • the apparatus is the extraction under microwaves in a solvent of organic or inorganic compounds dispersed in soils, sediments, waters, plants, biological products or even polymers.
  • the invention relates to an improvement of the device described in French patent applications Nos. 93 157 35 and FR 2 681 431 belonging to the applicant, this device comprising means for emitting microwaves in a cavity d application of microwaves of cylindrical shape and operating in the open state.
  • Apparatuses of this type already known which operate in the closed state under pressure, generally comprise a microwave application cavity in which are arranged bombs closed by screwed caps.
  • bombs cannot contain large volumes of sample, because the larger the volume of the sample, the greater the gas released under pressure when the sample is heated, which does not allow the bomb to function. .
  • such an apparatus operating with bombs comprising screwing closure devices, can only operate in one state, that is to say in the state closed under pressure. It is not possible to perform a degassing first by operating the device in the open state and then close said device for operation under pressure.
  • the invention proposes a new shutter system which is put in place in a simple way on a flask, allowing an operation of the flask in the open or closed state, which makes it possible to process large volumes of samples, by performing all first degassing before closing the flask.
  • the closure system comprises: a plug intended to be partially inserted into said flask along the axis XX ′ so as to close off its open end,
  • - retaining means capable of holding said plug in a closed position of said associated flask, the part of the plug engaged in said flask comprising a peripheral skirt capable of applying tightly against the internal wall of the flask under the effect an overpressure prevailing therein as a result of microwave heating of the sample.
  • the means for retaining the closure system comprise a stop surface capable of being positioned perpendicular to the axis XX 'above each plug, the relative position of the stop surface and of the plug authorizing the latter to slide inside the flask along the axis XX 'in the direction of the abutment surface, to abut against the latter under the thrust force induced by the overpressure prevailing inside flask when heating the sample.
  • the skirt of each plug is provided with a lip capable of being applied sealingly against the internal wall of the associated flask heated by microwave. under the effect of internal overpressure.
  • it comprises a pressure sensor connected to the abutment surface and capable of recording the overpressure prevailing inside said flask through the abutment surface resting on said plug.
  • the abutment surface of the closure system according to the invention carries at least one detector capable of coming into contact with each plug abutting against said abutment surface and emitting a plug presence signal against said abutment surface.
  • the abutment surface is mounted for rotation about an axis YY 'parallel to the axis X-X', on a support integral with the cavity application between on the one hand an open position in which it is positioned offset with respect to each flask, leaving free access to the open end of said flask for the establishment or removal of the associated plug or allow the heating said flask in the open state, and on the other hand a closed position in which it is positioned above each flask provided with the associated plug closing its opening.
  • the closure system comprises a plurality of plugs, each of said plugs being intended to be inserted into a flask of axis XX ′, said plugs being able to come in abutment against said abutment surface positioned perpendicular to the axis XX 'above said plugs, under the thrust force induced by the overpressure prevailing inside said flasks during the heating by microwave of the samples.
  • FIG. 1 represents a schematic view in longitudinal section of a microwave treatment apparatus comprising a shutter system according to the invention
  • FIG. 2 is a top view of the apparatus of FIG. 1, the shutter system being in the closed position above the flasks,
  • FIG. 3 is a diagrammatic top view of the apparatus of FIG. 1, the shutter system being in the open position,
  • FIG. 4 is a schematic view of details of the plug of the closure system according to the invention, positioned inside a flask.
  • Figure 1 there is shown an apparatus for carrying out a treatment in a humid environment on a plurality of samples contained in a plurality of flasks, here four flasks, the apparatus employing microwave heating of the samples.
  • the application cavity 100 shown here is of cylindrical shape of revolution with a central axis of symmetry YY 'and comprises an upper wall 101, a side wall 102 and a lower wall 103.
  • the side wall 102 of the application cavity 100 comprises a window, not shown here, transparent to the microwave, through which a waveguide (also not shown) opens out inside said cavity.
  • This waveguide is connected to a microwave generator (not shown) and transports the microwaves to the application cavity.
  • the upper wall 101 of the application cavity 100 here has four circular openings 104, only two of which are shown, arranged in pairs symmetrically opposite with respect to the axis Y-Y '.
  • the application cavity 100 carries outside on its upper wall 101 four identical cylindrical wells 105, two of which are shown here.
  • Each cylindrical well 105 extends towards the outside of the cavity, perpendicular to the upper wall 101, from each circular opening 104 provided in said upper wall 101.
  • the section of each well 105 corresponds to the section of each opening 104 and the height of each well is such that it forms an absorption barrier to microwaves in order to prevent their propagation towards the outside of the application cavity.
  • the vertical axes X-X 'of the cylindrical wells 105 are parallel to the axis Y-Y' and pass through the centers of the openings 104.
  • the samples to be processed here are placed in four flasks 10, only two of which are shown in FIG. 1.
  • Each flask 10 is introduced vertically into each well 105 towards the application cavity 100, via the openings 104 so that part of the flask containing the sample bathes in said cavity.
  • the axes X-X 'of the wells correspond to the axes X-X' of the said flasks.
  • the matras are produced for example from quartz or polytetrafluoraethylene.
  • Each flask 10 has an open upper end 1 1 positioned outside each well 105 and allowing the introduction of the sample inside the flask 10.
  • the outer surface 13 of each flask 10, close of its opening 11 has a conical shape flared upwards which rests on the edge of the opening of each well 105.
  • the edge of the opening of each well 105 forms a support for each flask positioned inside of the application cavity 100.
  • the apparatus shown in FIG. 1 comprises a closure system which comprises, for each flask 10, a plug 20 intended to be partially pressed into said flask along the axis XX 'so as to close its open end 11, and retaining means capable of retaining each plug 20 in a position for closing the associated flask.
  • retaining means consist of a closure cover comprising an abutment surface 30 capable of being positioned perpendicular to the axis XX ′ above each plug 20.
  • each plug 20 has a head 21, of cylindrical shape of revolution around the axis XX ′, projecting outside of each flask 10 when said plug is partially inserted in the flask, and a body 22 extending substantially perpendicular to said head 21 along the axis XX ′, engaged in sliding along said axis XX ′ in the flask 10.
  • the body 22 here has at its free end 25 positioned at inside the flask, a peripheral skirt 23 capable of being applied sealingly against the internal wall 12 of the flask associated under the effect of an overpressure prevailing in the latter as a result of the microwave heating of the sample .
  • this skirt 23 has an annular lip 23a which is preferably applied against the internal wall 12 of the flask 10, under the effect of the internal overpressure.
  • the skirt 23 provided with its lip 23a has a cylindrical shape of revolution around the axis XX ′, able to cooperate with a portion of the internal wall 12 of the flask which has a conical shape flared upwards at near its opening 11.
  • This conical shape of the internal wall 12 of the flask advantageously allows the plug 20 of the flask to be easily removed when the heating of the sample is finished.
  • each plug 20 has an axial duct 24 provided in the body 22 of each plug which extends over the entire length of said body 22 as far as the head 21.
  • This symmetrical axial conduit 24 of revolution about the axis XX ' is open at the free end 25 of the body 22 and is extended along the axis XX' by the skirt 23 at this free end 25.
  • the axial conduit 24 is connected near its other closed end, located in the head 21 of the plug 20, to a safety device 50 (shown diagrammatically in FIG. 1).
  • the connection of the safety device 50 and the axial duct 24 is carried out by a duct 27 of axis X i perpendicular to the axis XX 'so that the safety device 50 is subjected to the overpressure prevailing inside said flask via said axial duct 24 via duct 27 of axis X ⁇
  • This safety device is capable of emitting a cut-off signal from the microwave heating above a determined overpressure.
  • the safety device 50 comprises a rupture disc, not shown here, positioned so as to close off said conduit 27 of axis Xj. This rupture disc has, for example, a resistance to a pressure of approximately 40 bars above which it ruptures and triggers the emission of the cut-off signal.
  • the plug 20 is made in two parts.
  • a first part of the plug 20 comprises the head 21 and the body 22 provided with the axial duct 24, and a second part is formed by the peripheral skirt 23 which is extended above by a sleeve 26 intended to be engaged in the axial duct 24 along the 'axis XX' for the assembly of the two parts.
  • the axis 28 of the sleeve 26 of the second part of the plug has been assembled, it coincides with the axis XX ′ of the axial duct 24.
  • the plug 20 is made in one piece.
  • the closure system according to the invention shown in FIGS. 1 to 3 comprises, as has already been explained, a cover comprising a stop surface 30.
  • This cover is mounted for rotation between a closed position and an open position (see Figures 2 and 3) through a shaft 35, around the axis YY 'of the application cavity, this axis YY' being parallel to the axis XX 'of the flasks 10, on a support 110 integral of the application cavity 100 and which extends transversely between the wells.
  • the shaft 35 extends along the axis YY 'between the abutment surface 30 positioned perpendicularly above the plugs 20 and a pressure sensor 40 positioned below the support 110 along the axis Y-Y '.
  • the abutment surface 30 is mechanically connected to the pressure sensor 40.
  • the surface of the stopper 30 is positioned, in the closed position of the cover (see FIG. 2), at a certain distance from the plugs 20
  • the relative position of the abutment surface 30 and of the plugs 20 allows the latter to slide inside the flasks along the axis XX 'in the direction of the abutment surface 30 to come into abutment against the latter (see FIG. 1 ) under the thrust force induced by the overpressure prevailing inside the flasks 10 during heating of the samples.
  • the peripheral skirt 23 provided with its lip 23a is applied sealingly against the internal wall 12 of the associated flask.
  • the cover and the abutment surface 30 have a particular shape comprising cells 31, 32, 33, 34 of essentially circular shape.
  • the abutment surface 30 is provided with four cells.
  • Each of the circular-shaped cells has a diameter slightly greater than the diameter of a flask 10.
  • the cells 31, 32, 33, 34 are positioned two by two symmetrically with respect to the axis Y-Y '.
  • each flask 10 is positioned in each cell 31, 32, 33, 34 of the abutment surface 30 so that said abutment surface 30 is positioned offset with respect to each of the flasks 10.
  • the upper opening 11 of each flask 10 is free to access for the establishment or removal of a plug 20 or also for allow open operation of the microwave and associated equipment. The latter case can be envisaged for prior degassing of the flask at the start of heating.
  • the abutment surface 30 When the cover is in the closed position (see FIG. 2), the abutment surface 30 is positioned in a position offset by an angle ⁇ relative to the open position of the cover. In this closed position, the abutment surface 30 is placed above each plug 20 pressed into each flask 10. Thus when the pressure inside the flasks increases, each plug 20 abuts against said surface stop 30 and provides a seal at the opening 11 of each flask 10.
  • the stop surface 30 is connected below the support 110 to a pressure sensor 40. This pressure sensor 40 is able to record the overpressure prevailing in all four flasks via the abutment surface bearing on the plugs 20. This pressure sensor operates by traction.
  • the plugs 20 bearing on the abutment surface 30 exert on the abutment surface 30 a tensile force directed upwards which causes the compression of a liquid or of calibrated grains contained in the pressure sensor which makes it possible to measure the sum of the pressures prevailing in the matras. It is thus possible to evaluate an average value of the pressure prevailing in the said flask.
  • a sensor is set to approximately 10 to 15 bars. This sensor advantageously makes it possible to control and control the pressure inside the flasks 10 and can allow the device to be controlled according to the pressure measured.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Toxicology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electromagnetism (AREA)
  • Devices For Use In Laboratory Experiments (AREA)
  • Constitution Of High-Frequency Heating (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

A sealing system for sealing one or more flasks (10) with a longitudinal X-X' axis, open at a first end thereof (11) for introducing a sample and positioned inside a microwave application cavity (100) for heating the sample is described. The system of the invention comprises a cap (20) to be partially inserted in the flask along the X-X' axis so as to close the open end thereof and retaining means (30) for holding the cap in a flask sealing position, wherein the portion (22) of said cap which is inserted in the flask has a peripheral skirt (23) capable of sealingly engaging the inner wall (12) of the flask under an excess pressure created therein by heating the sample with microwaves.

Description

"SYSTEME D'OBTURATION D'UN MATRAS ET APPAREIL DE TRAITEMENT PAR "MATTRESS SHUTTERING SYSTEM AND TREATMENT APPARATUS
MICRO-ONDES COMPORTANT UN TEL SYSTEME D'OBTURATION"MICROWAVE HAVING SUCH A SHUTTERING SYSTEM "
La présente invention concerne un système d'obturation d'au moins un matras d'axe longitudinal X-X', qui est ouvert à une première extrémité pour l'introduction d'un ëchantillon et qui est positionné à l'intérieur d'une cavité d'application de micro-ondes en vue du chauffage de l'échantillon.The present invention relates to a closure system for at least one flask of longitudinal axis XX ′, which is open at a first end for the introduction of a sample and which is positioned inside a microwave application cavity for heating the sample.
L'invention concerne également un appareil pour réaliser un traitement en milieu humide simultanément sur une pluralité d'échantillons, l'appareil mettant en oeuvre un chauffage par micro- ondes des échantillons, et comportant un tel système d'obturation.The invention also relates to an apparatus for carrying out a treatment in a humid environment simultaneously on a plurality of samples, the apparatus implementing microwave heating of the samples, and comprising such a sealing system.
Un tel appareil trouve une application particulièrement avantageuse pour la mise en oeuvre de réactions chimiques telles que par exemple la minéralisation, la saponification, l'hydrolyse, la spéciation, la synthèse organique.Such an apparatus finds a particularly advantageous application for the implementation of chemical reactions such as for example mineralization, saponification, hydrolysis, speciation, organic synthesis.
Une autre application particulièrement avantageuse de l'appareil selon l'invention est l'extraction sous micro-ondes dans un solvant de composés organiques ou inorganiques dispersés dans des sols, sédiments, eaux, plantes, produits biologiques ou encore polymères. En particulier, l'invention concerne un perfectionnement de l'appareil décrit dans les demandes de brevets français n° 93 157 35 et FR 2 681 431 appartenant à la demanderesse, cet appareil comportant des moyens pour émettre des micro-ondes dans une cavité d'application des micro-ondes de forme cylindrique et fonctionnant à l'état ouvert. Des appareils de ce type déjà connus qui fonctionnent à l'état fermé sous pression, comprennent généralement une cavité d'application de micro-ondes dans laquelle sont disposées des bombes fermées par des capuchons vissés.Another particularly advantageous application of the apparatus according to the invention is the extraction under microwaves in a solvent of organic or inorganic compounds dispersed in soils, sediments, waters, plants, biological products or even polymers. In particular, the invention relates to an improvement of the device described in French patent applications Nos. 93 157 35 and FR 2 681 431 belonging to the applicant, this device comprising means for emitting microwaves in a cavity d application of microwaves of cylindrical shape and operating in the open state. Apparatuses of this type already known which operate in the closed state under pressure, generally comprise a microwave application cavity in which are arranged bombs closed by screwed caps.
Ce type d'appareil présente cependant plusieurs inconvénients. En effet, les bombes ne peuvent pas contenir de gros volumes d'échantillon, car plus le volume de l'échantillon augmente plus le gaz dégagé sous pression lors du chauffage de l'échantillon est important ce qui ne permet pas à la bombe de fonctionner.However, this type of device has several drawbacks. In fact, bombs cannot contain large volumes of sample, because the larger the volume of the sample, the greater the gas released under pressure when the sample is heated, which does not allow the bomb to function. .
En outre, un tel appareil fonctionnant avec des bombes comprenant des dispositifs de fermeture par vissage, ne peut fonctionner que dans un seul état c'est-à-dire à l'état fermé sous pression. Il n'est pas possible d'effectuer dans un premier temps un dégazage en faisant fonctionner l'appareil à l'état ouvert puis de fermer ledit appareil pour un fonctionnement sous pression.In addition, such an apparatus operating with bombs comprising screwing closure devices, can only operate in one state, that is to say in the state closed under pressure. It is not possible to perform a degassing first by operating the device in the open state and then close said device for operation under pressure.
L'invention propose un nouveau système d'obturation qui est mis en place de façon simple sur un matras, autorisant un fonctionnement du matras à l'état ouvert ou fermé, ce qui permet de traiter des volumes d'échantillons importants, en effectuant tout d'abord un dégazage préalable avant de fermer le matras.The invention proposes a new shutter system which is put in place in a simple way on a flask, allowing an operation of the flask in the open or closed state, which makes it possible to process large volumes of samples, by performing all first degassing before closing the flask.
Plus particulièrement selon l'invention, le système d'obturation comporte : - un bouchon destiné à être enfoncé partiellement dans ledit matras selon l'axe X-X' de façon à obturer son extrémité ouverte,More particularly according to the invention, the closure system comprises: a plug intended to be partially inserted into said flask along the axis XX ′ so as to close off its open end,
- des moyens de retenue aptent à maintenir ledit bouchon dans une position d'obturation dudit matras associé, la partie du bouchon engagée dans ledit matras comportant une jupe périphérique apte à s'appliquer de façon étanche contre la paroi interne du matras sous l'effet d'une surpression régnant dans ce dernier par suite du chauffage par micro-ondes de l'échantillon.- retaining means capable of holding said plug in a closed position of said associated flask, the part of the plug engaged in said flask comprising a peripheral skirt capable of applying tightly against the internal wall of the flask under the effect an overpressure prevailing therein as a result of microwave heating of the sample.
Selon un mode réalisation préféré de l'invention, les moyens de retenue du système d'obturation comprennent une surface de butée apte à être positionnée perpendiculairement à l'axe X-X' au-dessus de chaque bouchon, la position relative de la surface de butée et du bouchon autorisant ce dernier à coulisser à l'intérieur du matras selon l'axe X-X' en direction de la surface de butée, pour venir en butée contre cette dernière sous l'effort de poussée induit par la surpression régnant à l'intérieur du matras lors du chauffage de l'échantillon.According to a preferred embodiment of the invention, the means for retaining the closure system comprise a stop surface capable of being positioned perpendicular to the axis XX 'above each plug, the relative position of the stop surface and of the plug authorizing the latter to slide inside the flask along the axis XX 'in the direction of the abutment surface, to abut against the latter under the thrust force induced by the overpressure prevailing inside flask when heating the sample.
En outre, de manière avantageuse, dans le système d'obturation conforme à l'invention, la jupe de chaque bouchon est munie d'une lèvre apte à s'appliquer de manière étanche contre la paroi interne du matras associé chauffé par micro-ondes sous l'effet de la surpression interne. Conformément au mode de réalisation préféré du système d'obturation selon l'invention, il comporte un capteur de pression relié à la surface de butée et apte à enregistrer la surpression régnant à l'intérieur dudit matras par l'intermédiaire de la surface de butée en appui sur ledit bouchon. En outre, selon ce mode de réalisation préféré , la surface de butée du système d'obturation conforme à l'invention, porte au moins un détecteur apte à rentrer en contact avec chaque bouchon en butée contre ladite surface de butée et à émettre un signal de présence de bouchon contre ladite surface de butée.In addition, advantageously, in the closure system according to the invention, the skirt of each plug is provided with a lip capable of being applied sealingly against the internal wall of the associated flask heated by microwave. under the effect of internal overpressure. In accordance with the preferred embodiment of the closure system according to the invention, it comprises a pressure sensor connected to the abutment surface and capable of recording the overpressure prevailing inside said flask through the abutment surface resting on said plug. In addition, according to this preferred embodiment, the abutment surface of the closure system according to the invention carries at least one detector capable of coming into contact with each plug abutting against said abutment surface and emitting a plug presence signal against said abutment surface.
Selon une caractéristique particulièrement avantageuse du système d'obturation conforme à l'invention, la surface de butée est montée à rotation autour d'un axe Y-Y' parallèle à l'axe X-X', sur un support solidaire de la cavité d'application entre d'une part une position ouverte dans laquelle elle est positionnée de manière décalée par rapport à chaque matras, laissant libre d'accès l'extrémité ouverte dudit matras pour la mise en place ou l'enlèvement du bouchon associé ou bien permettre le chauffage dudit matras à l'état ouvert, et d'autre part une position fermée dans laquelle elle est positionnée au-dessus de chaque matras muni du bouchon associé obturant son ouverture.According to a particularly advantageous characteristic of the closure system according to the invention, the abutment surface is mounted for rotation about an axis YY 'parallel to the axis X-X', on a support integral with the cavity application between on the one hand an open position in which it is positioned offset with respect to each flask, leaving free access to the open end of said flask for the establishment or removal of the associated plug or allow the heating said flask in the open state, and on the other hand a closed position in which it is positioned above each flask provided with the associated plug closing its opening.
Selon un autre mode de réalisation du système d'obturation conforme à l'invention, il comporte une pluralité de bouchons, chacun desdits bouchons étant destinés à être enfoncés dans un matras d'axe X-X', lesdits bouchons étant aptes à venir en butée contre ladite surface de butée positionnée perpendiculairement à l'axe X-X' au-dessus desdits bouchons, sous l'effort de poussée induit par la surpression régnant à l'intérieur desdits matras lors du chauffage par micro-ondes des échantillons. La description qui va suivre en regard du dessin annexé, donnée à titre d'exemples non limitatifs, fera bien comprendre en quoi consiste l'invention et comment elle peut être réalisée. Sur les dessins annexés :According to another embodiment of the closure system according to the invention, it comprises a plurality of plugs, each of said plugs being intended to be inserted into a flask of axis XX ′, said plugs being able to come in abutment against said abutment surface positioned perpendicular to the axis XX 'above said plugs, under the thrust force induced by the overpressure prevailing inside said flasks during the heating by microwave of the samples. The description which follows with reference to the appended drawing, given by way of nonlimiting examples, will make it clear what the invention consists of and how it can be implemented. In the accompanying drawings:
- la figure 1 représente une vue schématique en coupe longitudinale d'un appareil de traitement sous micro-ondes comportant un système de d'obturation conforme à l'invention,FIG. 1 represents a schematic view in longitudinal section of a microwave treatment apparatus comprising a shutter system according to the invention,
- la figure 2 est une vue de dessus de l'appareil de la figure 1, le système d'obturation étant en position fermée au-dessus des matras,FIG. 2 is a top view of the apparatus of FIG. 1, the shutter system being in the closed position above the flasks,
- la figure 3 est une vue schématique de dessus de l'appareil de la figure 1, le système d'obturation étant en position ouverte,FIG. 3 is a diagrammatic top view of the apparatus of FIG. 1, the shutter system being in the open position,
- la figure 4 est une vue schématique de détails du bouchon du système d'obturation conforme à l'invention, positionné à l'intérieur d'un matras.- Figure 4 is a schematic view of details of the plug of the closure system according to the invention, positioned inside a flask.
Sur la figure 1 , on a représenté un appareil pour réaliser un traitement en milieu humide sur une pluralité d'échantillons contenue dans une pluralité de matras, ici quatre matras, l'appareil mettant en oeuvre un chauffage par micro-ondes des échantillons.In Figure 1, there is shown an apparatus for carrying out a treatment in a humid environment on a plurality of samples contained in a plurality of flasks, here four flasks, the apparatus employing microwave heating of the samples.
Un tel appareil est décrit structurellement et fonctionnellement dans son ensemble dans les demandes de brevets français FR-2 680 431 et n° 93 157 35 appartenant à la demanderesse. Par conséquent, l'ensemble de l'appareil ne sera pas ici redécrit et la présente description ne porte en détails que sur le système d'obturation d'un tel appareil correspondant à un mode de réalisation particulier de ce dernier.Such an apparatus is described structurally and functionally in as a whole in French patent applications FR-2 680 431 and No. 93 157 35 belonging to the applicant. Consequently, the entire apparatus will not be re-described here and the present description relates in detail only to the shutter system of such an apparatus corresponding to a particular embodiment of the latter.
La cavité d'application 100 ici représentée est de forme cylindrique de révolution d'axe centrale de symétrie Y-Y' et comporte une paroi supérieure 101, une paroi latérale 102 et une paroi inférieure 103. La paroi latérale 102 de la cavité d'application 100 comporte une fenêtre, ici non représentée, transparente au micro-ondes, par laquelle un guide d'ondes (également non représenté) débouche à l'intérieur de ladite cavité. Ce guide d'ondes est raccordé à un générateur de micro-ondes non représenté et transporte les micro-ondes jusqu'à la cavité d'application. La paroi supérieure 101 de la cavité d'application 100 comporte ici quatre ouvertures circulaires 104, dont deux seulement sont représentées, disposées deux à deux de manière symétriquement opposées par rapport à l'axe Y-Y'. Par ailleurs, la cavité d'application 100 porte à l'extérieur sur sa paroi supérieure 101 quatre puits cylindriques identiques 105 dont deux ici sont représentés. Chaque puit cylindrique 105 s'étend vers l'extérieur de la cavité, perpendiculairement à la paroi supérieure 101, à partir de chaque ouverture circulaire 104 prévue dans ladite paroi supérieure 101. La section de chaque puit 105 correspond à la section de chaque ouverture 104 et la hauteur de chaque puit est telle qu'il forme une barrière d'absorption aux micro-ondes afin d'éviter leur propagation vers l'extérieur de la cavité d'application. Les axes X-X' verticaux des puits cylindriques 105 sont parallèles à l'axe Y-Y' et passent par les centres des ouvertures 104.The application cavity 100 shown here is of cylindrical shape of revolution with a central axis of symmetry YY 'and comprises an upper wall 101, a side wall 102 and a lower wall 103. The side wall 102 of the application cavity 100 comprises a window, not shown here, transparent to the microwave, through which a waveguide (also not shown) opens out inside said cavity. This waveguide is connected to a microwave generator (not shown) and transports the microwaves to the application cavity. The upper wall 101 of the application cavity 100 here has four circular openings 104, only two of which are shown, arranged in pairs symmetrically opposite with respect to the axis Y-Y '. Furthermore, the application cavity 100 carries outside on its upper wall 101 four identical cylindrical wells 105, two of which are shown here. Each cylindrical well 105 extends towards the outside of the cavity, perpendicular to the upper wall 101, from each circular opening 104 provided in said upper wall 101. The section of each well 105 corresponds to the section of each opening 104 and the height of each well is such that it forms an absorption barrier to microwaves in order to prevent their propagation towards the outside of the application cavity. The vertical axes X-X 'of the cylindrical wells 105 are parallel to the axis Y-Y' and pass through the centers of the openings 104.
Les échantillons à traiter ici non représentés sont placés dans quatre matras 10, dont deux seulement sont représentés sur la figure 1. Chaque matras 10 est introduit verticalement dans chaque puit 105 vers la cavité d'application 100, via les ouvertures 104 de telle sorte qu'une partie du matras contenant l'échantillon baigne dans ladite cavité. Lorsque les matras sont positionnés dans les puits, les axes X-X' des puits correspondent aux axes X-X' desdit matras. Les matras sont réalisés par exemple en quartz ou en polytétrafluoraéthylène.The samples to be processed here, not shown, are placed in four flasks 10, only two of which are shown in FIG. 1. Each flask 10 is introduced vertically into each well 105 towards the application cavity 100, via the openings 104 so that part of the flask containing the sample bathes in said cavity. When the flasks are positioned in the wells, the axes X-X 'of the wells correspond to the axes X-X' of the said flasks. The matras are produced for example from quartz or polytetrafluoraethylene.
Chaque matras 10 présente une extrémité supérieure ouverte 1 1 positionnée à l'extérieur de chaque puit 105 et permettant l'introduction de l'échantillon à l'intérieur du matras 10. Comme on peut le voir plus en détails sur la figure 4, la surface extérieure 13 de chaque matras 10, à proximité de son ouverture 11, présente une forme conique évasée vers le haut qui prend appui sur le bord de l'ouverture de chaque puit 105. Ainsi le bord de l'ouverture de chaque puit 105 forme un support de chaque matras positionné à l'intérieur de la cavité de l'application 100.Each flask 10 has an open upper end 1 1 positioned outside each well 105 and allowing the introduction of the sample inside the flask 10. As can be seen in more detail in FIG. 4, the outer surface 13 of each flask 10, close of its opening 11, has a conical shape flared upwards which rests on the edge of the opening of each well 105. Thus the edge of the opening of each well 105 forms a support for each flask positioned inside of the application cavity 100.
En outre, l'appareil représenté sur la figure 1 comporte un système d'obturation qui comprend pour chaque matras 10, un bouchon 20 destiné à être enfoncé partiellement dans ledit matras selon l'axe X-X' de façon à obturer son extrémité ouverte 11, et des moyens de retenu aptent à retenir chaque bouchon 20 dans une position d'obturation du matras associé. Ces moyens de retenue sont constitués par un couvercle de fermeture comprenant une surface de butée 30 apte à être positionnée perpendiculairement à l'axe X-X' au-dessus de chaque bouchon 20.In addition, the apparatus shown in FIG. 1 comprises a closure system which comprises, for each flask 10, a plug 20 intended to be partially pressed into said flask along the axis XX 'so as to close its open end 11, and retaining means capable of retaining each plug 20 in a position for closing the associated flask. These retaining means consist of a closure cover comprising an abutment surface 30 capable of being positioned perpendicular to the axis XX ′ above each plug 20.
Comme on peut mieux le voir sur la figure 4, chaque bouchon 20 comporte une tête 21, de forme cylindrique de révolution autour de l'axe X-X', débordante à l'extérieur de chaque matras 10 lorsque ledit bouchon est partiellement enfoncé dans le matras, et un corps 22 s'étendant sensiblement perpendiculairement à ladite tête 21 selon l'axe X-X', engagé à coulissement selon ledit axe X-X' dans le matras 10. Le corps 22 comporte ici à son extrémité libre 25 positionnée à l'intérieur du matras, une jupe 23 périphérique apte à s'appliquer de façon étanche contre la paroi interne 12 du matras associé sous l'effet d'une surpression régnant dans ce dernier par suite du chauffage par micro-ondes de l'échantillon. Plus particulièrement, cette jupe 23 comporte une lèvre 23a annulaire qui s'applique préférentiellement contre la paroi interne 12 du matras 10, sous l'effet de la surpression interne. On remarquera que la jupe 23 munie de sa lèvre 23a présente une forme cylindrique de révolution autour de l'axe X-X', apte à coopérer avec une portion de la paroi interne 12 du matras qui présente une forme conique évasée vers le haut à proximité de son ouverture 11. Cette forme conique de la paroi interne 12 du matras, permet avantageusement d'enlever facilement le bouchon 20 du matras lorsque le chauffage de l'échantillon est terminée. Comme on peut le voir sur les figures 1 et 4, chaque bouchon 20 comporte un conduit axial 24 prévu dans le corps 22 de chaque bouchon qui s'étend sur toute la longueur dudit corps 22 jusque dans la tête 21. Ce conduit axial 24 symétrique de révolution autour de l'axe X-X' est ouvert à l'extrémité libre 25 du corps 22 et est prolongé suivant l'axe X-X' par la jupe 23 au niveau de cette extrémité libre 25. Le conduit axial 24 est raccordé à proximité de son autre extrémité fermée, située dans la tête 21 du bouchon 20, à un dispositif de sécurité 50 (représenté schématiquement sur la figure 1 ). Le raccordement du dispositif de sécurité 50 et du conduit axial 24 est réalisé par un conduit 27 d'axe X i perpendiculaire à l'axe X-X' de sorte que le dispositif de sécurité 50 soit soumis à la surpression régnant à l'intérieur dudit matras par l'intermédiaire dudit conduit axial 24 via le conduit 27 d'axe X ^ Ce dispositif de sécurité est apte à émettre un signal de coupure du chauffage micro-ondes au-dessus d'une surpression déterminée. Le dispositif de sécurité 50 comporte un disque de rupture ici non représenté positionné de façon à obturer ledit conduit 27 d'axe Xj. Ce disque de rupture présente par exemple une résistance à une pression d'environ 40 bars au-dessus de laquelle il se rompt et déclenche l'émission du signal de coupure.As can best be seen in FIG. 4, each plug 20 has a head 21, of cylindrical shape of revolution around the axis XX ′, projecting outside of each flask 10 when said plug is partially inserted in the flask, and a body 22 extending substantially perpendicular to said head 21 along the axis XX ′, engaged in sliding along said axis XX ′ in the flask 10. The body 22 here has at its free end 25 positioned at inside the flask, a peripheral skirt 23 capable of being applied sealingly against the internal wall 12 of the flask associated under the effect of an overpressure prevailing in the latter as a result of the microwave heating of the sample . More particularly, this skirt 23 has an annular lip 23a which is preferably applied against the internal wall 12 of the flask 10, under the effect of the internal overpressure. It will be noted that the skirt 23 provided with its lip 23a has a cylindrical shape of revolution around the axis XX ′, able to cooperate with a portion of the internal wall 12 of the flask which has a conical shape flared upwards at near its opening 11. This conical shape of the internal wall 12 of the flask advantageously allows the plug 20 of the flask to be easily removed when the heating of the sample is finished. As can be seen in Figures 1 and 4, each plug 20 has an axial duct 24 provided in the body 22 of each plug which extends over the entire length of said body 22 as far as the head 21. This symmetrical axial conduit 24 of revolution about the axis XX 'is open at the free end 25 of the body 22 and is extended along the axis XX' by the skirt 23 at this free end 25. The axial conduit 24 is connected near its other closed end, located in the head 21 of the plug 20, to a safety device 50 (shown diagrammatically in FIG. 1). The connection of the safety device 50 and the axial duct 24 is carried out by a duct 27 of axis X i perpendicular to the axis XX 'so that the safety device 50 is subjected to the overpressure prevailing inside said flask via said axial duct 24 via duct 27 of axis X ^ This safety device is capable of emitting a cut-off signal from the microwave heating above a determined overpressure. The safety device 50 comprises a rupture disc, not shown here, positioned so as to close off said conduit 27 of axis Xj. This rupture disc has, for example, a resistance to a pressure of approximately 40 bars above which it ruptures and triggers the emission of the cut-off signal.
Il convient de noter que selon le mode de réalisation représenté sur la figure 4, le bouchon 20 est constitué en deux parties. Une première partie du bouchon 20 comprend la tête 21 et le corps 22 pourvu du conduit axial 24, et une deuxième partie est formée par la jupe périphérique 23 qui se prolonge supérieurement par un manchon 26 destiné à être engagé dans le conduit axial 24 selon l'axe X-X 'pour l' assemblage des deux parties. Une fois assemblé l'axe 28 du manchon 26 de la deuxième partie du bouchon est confondu avec l'axe X-X' du conduit axial 24. Bien entendu on peut envisager que le bouchon 20 soit constitué d'une seule pièce.It should be noted that according to the embodiment shown in Figure 4, the plug 20 is made in two parts. A first part of the plug 20 comprises the head 21 and the body 22 provided with the axial duct 24, and a second part is formed by the peripheral skirt 23 which is extended above by a sleeve 26 intended to be engaged in the axial duct 24 along the 'axis XX' for the assembly of the two parts. Once the axis 28 of the sleeve 26 of the second part of the plug has been assembled, it coincides with the axis XX ′ of the axial duct 24. Of course, it is conceivable that the plug 20 is made in one piece.
Il convient de préciser que lorsque qu'aucune surpression ne régne à l'intérieur du matras 10, la surface inférieure 21a de la tête 21 repose sur le rebord périphérique entourant l'ouverture 11 du matras.It should be noted that when no overpressure reigns inside the flask 10, the lower surface 21a of the head 21 rests on the peripheral rim surrounding the opening 11 of the flask.
Le système d'obturation conforme à l'invention représenté sur les figures 1 à 3, comporte comme cela a déjà été explicité un couvercle comportant une surface de butée 30. Ce couvercle est monté à rotation entre une position fermée et une position ouverte (voir figures 2 et 3) par l'intermédiaire d'un arbre 35, autour de l'axe Y-Y' de la cavité d'application, cette axe Y-Y' étant parallèle à l'axe X-X' des matras 10, sur un support 110 solidaire de la cavité d'application 100 et qui s'étend transversalement entre les puits. L'arbre 35 s'étend selon l'axe Y-Y' entre la surface de butée 30 positionnée perpendiculairement au-dessus des bouchons 20 et un capteur de pression 40 positionné en dessous du support 110 selon l'axe Y-Y'. La surface de butée 30 est reliée mécaniquement au capteur de pression 40.The closure system according to the invention shown in FIGS. 1 to 3 comprises, as has already been explained, a cover comprising a stop surface 30. This cover is mounted for rotation between a closed position and an open position (see Figures 2 and 3) through a shaft 35, around the axis YY 'of the application cavity, this axis YY' being parallel to the axis XX 'of the flasks 10, on a support 110 integral of the application cavity 100 and which extends transversely between the wells. The shaft 35 extends along the axis YY 'between the abutment surface 30 positioned perpendicularly above the plugs 20 and a pressure sensor 40 positioned below the support 110 along the axis Y-Y '. The abutment surface 30 is mechanically connected to the pressure sensor 40.
Comme on peut le voir plus particulièrement sur la figure 1 lorsqu'aucune pression ne régne à l'intérieur desdit matras 10 la surface du butée 30 est positionnée, en position fermée du couvercle (voir figure 2), à une certaine distance des bouchons 20. La position relative de la surface de butée 30 et des bouchons 20 autorise ces derniers à coulisser à l'intérieur des matras selon l'axe X-X' en direction de la surface de butée 30 pour venir en butée contre cette dernière (voir figure 1 ) sous l'effort de poussée induit par la surpression régnant à l'intérieur des matras 10 lors du chauffage des échantillons . Dans cette position de butée de chaque bouchon 20, la jupe périphérique 23 munie de sa lèvre 23a s'applique de manière étanche contre la paroi interne 12 du matras associé . On notera à cet effet, que l'effort de poussée induit par la suppression régnant dans chacun desdits matras est plus importante que l'effort de serrage de la jupe périphérique 23 contre la paroi interne 12 de chaque matras de façon qu'il soit possible d'ouvrir le matras en positionnant le couvercle en position ouvert (voir figure 3) une fois que le chauffage est terminé. Comme on peut le voir également sur la figure 1, la surface de butéeAs can be seen more particularly in FIG. 1 when there is no pressure inside said flasks 10, the surface of the stopper 30 is positioned, in the closed position of the cover (see FIG. 2), at a certain distance from the plugs 20 The relative position of the abutment surface 30 and of the plugs 20 allows the latter to slide inside the flasks along the axis XX 'in the direction of the abutment surface 30 to come into abutment against the latter (see FIG. 1 ) under the thrust force induced by the overpressure prevailing inside the flasks 10 during heating of the samples. In this abutment position of each plug 20, the peripheral skirt 23 provided with its lip 23a is applied sealingly against the internal wall 12 of the associated flask. It will be noted for this purpose that the thrust force induced by the suppression prevailing in each of said flasks is greater than the force for tightening the peripheral skirt 23 against the internal wall 12 of each flask so that it is possible open the flask by positioning the cover in the open position (see Figure 3) once the heating is finished. As can also be seen in Figure 1, the stop surface
30 porte des détecteurs 60 aptent à rentrer en contact avec les bouchons 20 en butée contre ladite surface de butée 30 et destinés à émettre un signal de présence de chaque bouchon 20 contre la surface de butée 30. Ainsi avantageusemenent, il est possible de contrôler la fermeture de chaque matras par l'intermédiaire de ces détecteurs, contrôlant la présence en butée du bouchon 20 contre la surface du butée 30.30 carries detectors 60 capable of coming into contact with the plugs 20 in abutment against said abutment surface 30 and intended to emit a signal of presence of each plug 20 against the abutment surface 30. Thus advantageously, it is possible to control the closure of each flask by means of these detectors, checking the presence of the stopper 20 against the surface of the stopper 30.
Comme on peut le voir plus particulièrement sur les figures 2 et 3 le couvercle et la surface de butée 30 présentent une forme particulière comportant des alvéoles 31, 32, 33, 34 de forme essentiellement circulaire. Selon le mode de réalisation représenté, la surface de butée 30 est pourvue de quatre alvéoles. Chacune des alvéoles de forme circulaire présente un diamètre légèrement supérieur au diamètre d'un matras 10. Les alvéoles 31, 32, 33, 34 sont positionnées deux à deux symétriquement par rapport à l'axe Y-Y'. Lorsque le couvercle est en position ouverte (représentée plus particulièrement à la figure 3 ) chaque matras 10 est positionné dans chaque alvéole 31, 32, 33, 34 de la surface de butée 30 de telle sorte que ladite surface de butée 30 est positionnée de manière décalée par rapport à chacun des matras 10. Ainsi l'ouverture supérieure 11 de chaque matras 10 est libre d'accès pour la mise en place ou l'enlèvement d'un bouchon 20 ou encore pour permettre un fonctionnement ouvert de l'appareil micro-ondes et des matras associés. Ce dernier cas peut être envisagé pour un dégazage préalable des matras au début du chauffage.As can be seen more particularly in FIGS. 2 and 3, the cover and the abutment surface 30 have a particular shape comprising cells 31, 32, 33, 34 of essentially circular shape. According to the embodiment shown, the abutment surface 30 is provided with four cells. Each of the circular-shaped cells has a diameter slightly greater than the diameter of a flask 10. The cells 31, 32, 33, 34 are positioned two by two symmetrically with respect to the axis Y-Y '. When the cover is in the open position (shown more particularly in FIG. 3) each flask 10 is positioned in each cell 31, 32, 33, 34 of the abutment surface 30 so that said abutment surface 30 is positioned offset with respect to each of the flasks 10. Thus the upper opening 11 of each flask 10 is free to access for the establishment or removal of a plug 20 or also for allow open operation of the microwave and associated equipment. The latter case can be envisaged for prior degassing of the flask at the start of heating.
Lorsque le couvercle est en position fermée (voir figure 2), la surface de butée 30 est positionnée dans une position décalée d'un angle α par rapport à la position ouverte du couvercle. Dans cette position fermée, la surface de butée 30 se trouve placée au-dessus de chaque bouchon 20 enfoncé dans chaque matras 10. Ainsi lors de la montée en pression à l'intérieur des matras 10 chaque bouchon 20 vient en butée contre ladite surface de butée 30 et assure une étanchéité au niveau de l'ouverture 11 de chaque matras 10. Comme cela a déjà été explicité, la surface de butée 30 est reliée en dessous du support 110 à un capteur de pression 40. Ce capteur de pression 40 est apte à enregistrer la surpression régnant dans l'ensemble des quatre matras par l'intermédiaire de la surface de butée en appui sur les bouchons 20. Ce capteur de pression fonctionne par traction. En effet les bouchons 20 en appui sur la surface de butée 30 exercent sur la surface de butée 30 une force de traction dirigée vers le haut qui entraîne la compression d'un liquide ou de grains calibrés contenu dans le capteur de pression qui permet de mesurer la somme des pressions régnant dans les matras. On peut ainsi évaluer une valeur moyenne de la pression régnant dans lesdit matras. Un tel capteur est réglé sur environ 10 à 15 bars. Ce capteur permet avantageusement de contrôler et maîtriser la pression à l'intérieur des matras 10 et peut permettre un asservissement de l'appareil en fonction de la pression mesurée.When the cover is in the closed position (see FIG. 2), the abutment surface 30 is positioned in a position offset by an angle α relative to the open position of the cover. In this closed position, the abutment surface 30 is placed above each plug 20 pressed into each flask 10. Thus when the pressure inside the flasks increases, each plug 20 abuts against said surface stop 30 and provides a seal at the opening 11 of each flask 10. As has already been explained, the stop surface 30 is connected below the support 110 to a pressure sensor 40. This pressure sensor 40 is able to record the overpressure prevailing in all four flasks via the abutment surface bearing on the plugs 20. This pressure sensor operates by traction. Indeed, the plugs 20 bearing on the abutment surface 30 exert on the abutment surface 30 a tensile force directed upwards which causes the compression of a liquid or of calibrated grains contained in the pressure sensor which makes it possible to measure the sum of the pressures prevailing in the matras. It is thus possible to evaluate an average value of the pressure prevailing in the said flask. Such a sensor is set to approximately 10 to 15 bars. This sensor advantageously makes it possible to control and control the pressure inside the flasks 10 and can allow the device to be controlled according to the pressure measured.
La présente invention n'est nullement limitée au mode de réalisation décrit et représenté mais l'homme du métier pourra envisager toute variante conforme à son esprit.The present invention is in no way limited to the embodiment described and shown, but a person skilled in the art can envisage any variant in accordance with his spirit.
En effet, on peut envisager un appareil comprenant un nombre supérieur de matras (6, 8, ou 10 matras) comprenant un système d'obturation selon l'invention. Indeed, one can envisage an apparatus comprising a greater number of flasks (6, 8, or 10 flasks) comprising a shutter system according to the invention.

Claims

REVENDICATIONS
1. Système d'obturation d'au moins un matras (10) d'axe longitudinal X-X', qui est ouvert à une première extrémité ( 1 1) destinée à permettre l'introduction d'un échantillon et qui est positionné à l'intérieur d'une cavité d'application de micro-ondes ( 100) en vue du chauffage de l'échantillon, caractérisé en ce qu'il comporte :1. Sealing system for at least one flask (10) of longitudinal axis XX ′, which is open at a first end (1 1) intended to allow the introduction of a sample and which is positioned at the interior of a microwave application cavity (100) for heating the sample, characterized in that it comprises:
- un bouchon (20) destiné à être enfoncé partiellement dans ledit matras ( 10) selon l'axe X-X' de façon à obturer son extrémité ouverte (11),a plug (20) intended to be partially inserted into said flask (10) along the axis XX ′ so as to close off its open end (11),
- des moyens de retenu (30) qui sont montés solidaires d'un support ( 110) faisant partie intégrante de la cavité d'application ( 100), afin de maintenir ledit bouchon (20) dans une position d'obturation du matras associé (10), la partie (22) du bouchon (20) engagée dans ledit matras ( 10) comportant une jupe périphérique (23) apte à s'appliquer de façon étanche contre la paroi interne ( 12) du matras ( 10) sous l'effet d'une surpression régnant dans ce dernier par suite du chauffage par micro-ondes de l'échantillon.- retaining means (30) which are mounted integral with a support (110) forming an integral part of the application cavity (100), in order to maintain said plug (20) in a position for closing the associated flask ( 10), the part (22) of the plug (20) engaged in said flask (10) comprising a peripheral skirt (23) capable of being applied sealingly against the internal wall (12) of the flask (10) under the effect of an overpressure prevailing in the latter as a result of microwave heating of the sample.
2. Système d'obturation selon la revendication 1, caractérisé en ce que les moyens de retenu comprennent une surface de butée (30) apte à être positionnée perpendiculairement à l'axe X-X' au-dessus de chaque bouchon (20), la position relative de la surface de butée (30) et du bouchon (20) autorisant ce dernier à coulisser à l'intérieur dudit matras (10) selon l'axe X-X' en direction de ladite surface de butée (30), pour venir en butée contre cette dernière sous l'effort de poussée induit par la surpression régnant à l'intérieur dudit matras (10) lors du chauffage de l'échantillon.2. obturation system according to claim 1, characterized in that the retaining means comprise an abutment surface (30) capable of being positioned perpendicular to the axis XX 'above each plug (20), the position relative of the abutment surface (30) and of the plug (20) authorizing the latter to slide inside said flask (10) along the axis XX 'in the direction of said abutment surface (30), to come into abutment against the latter under the thrust force induced by the overpressure prevailing inside said flask (10) during heating of the sample.
3. Système d'obturation selon l'une des revendications 1 et 2, caractérisé en ce que la jupe périphérique (23) de chaque bouchon (20) présente une paroi externe de forme cylindrique de révolution autour de l'axe X-X', apte à s'appliquer contre ladite paroi interne ( 12) de forme sensiblement conique dudit matras (10).3. obturation system according to one of claims 1 and 2, characterized in that the peripheral skirt (23) of each plug (20) has an outer wall of cylindrical shape of revolution around the axis XX ' , adapted to be applied against said internal wall (12) of substantially conical shape of said flask (10).
4. Système d'obturation selon l'une quelconque des revendications 1 à4. obturation system according to any one of claims 1 to
3, caractérisé en ce que la jupe périphérique (23) de chaque bouchon (20) est munie d'une lèvre (23a) apte à s'appliquer de manière étanche contre la paroi interne ( 12) du matras associé ( 10) chauffé par micro-ondes, sous l'effet de la surpression interne.3, characterized in that the peripheral skirt (23) of each plug (20) is provided with a lip (23a) capable of being applied in a sealed manner against the internal wall (12) of the associated flask (10) heated by microwave, under the effect of internal overpressure.
5. Système d'obturation selon l'une quelconque des revendications 1 à5. obturation system according to any one of claims 1 to
4, caractérisé en ce que chaque bouchon (20) comporte une tête (21 ) débordante à l'extérieur de chaque matras (10) et un corps (22) s'étendant sensiblement perpendiculairement à ladite tête (21 ), engagé à coulissement selon l'axe X-X' dans ledit matras ( 10) et étant pourvu d'un conduit axial (24) qui est ouvert à l'extrémité libre (25) dudit corps (22), ladite jupe (23) étant positionnée au niveau de ladite extrémité libre (25) dans le prolongement axial dudit conduit (24).4, characterized in that each plug (20) has a head (21) projecting outside of each flask (10) and a body (22) extending substantially perpendicular to said head (21), slidably engaged along the axis XX 'in said flask (10) and being provided with an axial duct (24) which is open at the free end (25) of said body (22 ), said skirt (23) being positioned at said free end (25) in the axial extension of said conduit (24).
6.Système d'obturation selon la revendication 5, caractérisé en ce que le conduit axial (24) prévu dans le corps (22) de chaque bouchon (20) s'étend sur toute la longueur dudit corps (22) jusque dans la tête (21) où il est raccordé à dispositif de sécurité (50) destiné à être soumis à la surpression régnant à l'intérieur dudit matras ( 10) par l'intermédiaire dudit conduit axial (24) et apte à émettre un signal de coupure de chauffage micro-ondes au-dessus d'une surpression déterminée. 6. obturation system according to claim 5, characterized in that the axial duct (24) provided in the body (22) of each plug (20) extends over the entire length of said body (22) up to the head (21) where it is connected to a safety device (50) intended to be subjected to the overpressure prevailing inside said flask (10) via said axial duct (24) and capable of emitting a cut-off signal from microwave heating above a certain overpressure.
7. Système d'obturation selon l'une quelconque des revendications 2 à7. obturation system according to any one of claims 2 to
6, caractérisé en ce qu'il comporte un capteur de pression (40) relié à la surface de butée (30) et apte à enregistrer la surpression régnant à l'intérieur dudit matras ( 10) par l'intermédiaire de ladite surface de butée (30) en appui sur ledit bouchon (20). 6, characterized in that it comprises a pressure sensor (40) connected to the abutment surface (30) and capable of recording the overpressure prevailing inside said flask (10) via said abutment surface (30) resting on said plug (20).
8. Système d'obturation selon l'une quelconque des revendications 2 à8. obturation system according to any one of claims 2 to
7, caractérisé en ce que la surface de butée (30) porte au moins un détecteur (60) apte à rentrer en contact avec chaque bouchon (20) en butée contre ladite surface de butée (30) et à émettre un signal de présence dudit bouchon (20) contre ladite surface de butée (30). 7, characterized in that the abutment surface (30) carries at least one detector (60) capable of coming into contact with each plug (20) abutting against said abutment surface (30) and of emitting a presence signal of said plug (20) against said abutment surface (30).
9. Système d'obturation selon l'une quelconque des revendications 2 à9. obturation system according to any one of claims 2 to
8, caractérisé en ce que la surface de butée (30) est montée à rotation autour d'un axe Y-Y' parallèle à l'axe X-X', sur ledit support ( 110) solidaire de la cavité d'application (100) entre d'une part une position ouverte dans laquelle elle est positionnnée de manière décalée par rapport à chaque matras (10), laissant libre d'accès l'extrémité ouverte dudit matras ( 10) pour la mise en place ou l'enlèvement du bouchon associé (20) ou bien permettre le chauffage dudit matras (10) à l'état ouvert, et d'autre part une position fermée dans laquelle elle est positionnée au-dessus de chaque matras (10) muni du bouchon associé (20) obturant son ouverture (11). 8, characterized in that the abutment surface (30) is mounted for rotation about an axis YY 'parallel to the axis X-X', on said support (110) integral with the application cavity (100) between on the one hand an open position in which it is positioned offset with respect to each flask (10), leaving free access to the open end of said flask (10) for fitting or removing the plug associated (20) or allow the heating of said flask (10) in the open state, and on the other hand a closed position in which it is positioned above each flask (10) provided with the associated plug (20) closing its opening (11).
10. Système d'obturation selon l'une quelconque des revendications 2 à 9, caractérisé en ce qu'il comporte une pluralité de bouchons (20), chacun desdits bouchons (20) étant destiné à être enfoncé dans un matras (10) d'axe X-X', lesdits bouchons (20) étant aptes à venir en butée contre ladite surface de butée (30) positionnée perpendiculairement à l'axe X-X' au-dessus desdits bouchons (10), sous l'effort de poussée induit par la surpression régnant à l'intérieur desdits matras ( 10) lors du chauffage micro-ondes des échantillons.10. obturation system according to any one of claims 2 to 9, characterized in that it comprises a plurality of plugs (20), each of said plugs (20) being intended to be pressed into a flask (10) d 'axis X-X', said plugs (20) being able to abut against said abutment surface (30) positioned perpendicular to the axis XX ' above said plugs (10), under the thrust force induced by the overpressure prevailing inside said flasks (10) during the microwave heating of the samples.
11. Appareil pour réaliser un traitement en milieu humide sur une pluralité d'échantillons contenus dans une pluralité de matras ( 10) d'axes X-X', l'appareil comprenant des moyens pour émettre des micro-ondes à l'intérieur d'une cavité d'application ( 100) d'axe central de symétrie Y-Y', la cavité d'application (100) comportant dans sa paroi supérieure (101) des ouvertures pour l'introduction des matras ( 10) à l'intérieur de la cavité d'application ( 100) parallèlement à l'axe Y-Y', disposés deux à deux de manière symétriquement opposée par rapport à l'axe Y-Y', caractérisé en ce qu'il comporte un système d'obturation selon l'une quelconque des revendications 1 à 10. 11. Apparatus for carrying out a treatment in a humid environment on a plurality of samples contained in a plurality of flasks (10) of axes X-X ', the apparatus comprising means for emitting microwaves inside 'an application cavity (100) with a central axis of symmetry Y-Y', the application cavity (100) comprising in its upper wall (101) openings for the introduction of flasks (10) to the inside the application cavity (100) parallel to the axis Y-Y ', arranged in pairs symmetrically opposite with respect to the axis Y-Y', characterized in that it comprises a system of obturation according to any one of claims 1 to 10.
EP96919884A 1995-05-11 1996-05-09 Flask sealing system and microwave treatment apparatus with such a sealing system Withdrawn EP0770205A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9505594A FR2733923B1 (en) 1995-05-11 1995-05-11 MATTRESS SHUTTERING SYSTEM AND MICROWAVE PROCESSING APPARATUS HAVING SUCH A SHUTTERING SYSTEM
FR9505594 1995-05-11
PCT/FR1996/000698 WO1996035937A1 (en) 1995-05-11 1996-05-09 Flask sealing system and microwave treatment apparatus with such a sealing system

Publications (1)

Publication Number Publication Date
EP0770205A1 true EP0770205A1 (en) 1997-05-02

Family

ID=9478884

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96919884A Withdrawn EP0770205A1 (en) 1995-05-11 1996-05-09 Flask sealing system and microwave treatment apparatus with such a sealing system

Country Status (7)

Country Link
US (1) US5932817A (en)
EP (1) EP0770205A1 (en)
JP (1) JPH10503029A (en)
KR (1) KR970705016A (en)
CA (1) CA2194780A1 (en)
FR (1) FR2733923B1 (en)
WO (1) WO1996035937A1 (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6534140B2 (en) * 1999-03-01 2003-03-18 Cem Limited, L.L.C. Pressure vessel with composite sleeve
US6571648B2 (en) * 2001-03-22 2003-06-03 Kansas Department Of Transportation Method of accelerated aging of neat asphalt binder using microwave radiation process
US7307248B2 (en) * 2003-12-09 2007-12-11 Cem Corporation Method and apparatus for microwave assisted high throughput high pressure chemical synthesis
US8739609B2 (en) * 2009-03-27 2014-06-03 Ofi Testing Equipment, Inc. Test sample heating apparatus and method
CN105064840B (en) * 2015-06-30 2017-03-01 浙江吉利汽车研究院有限公司 A kind of arrangements for automotive doors locking button and the mounting structure of bracing wire
CN106867620B (en) * 2017-04-12 2023-03-24 太原科技大学 Microwave desulfurization intelligent integrated experimental system for high-sulfur coal

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2299401A (en) * 1941-03-26 1942-10-20 William L Melton Electrical oil heating device
US3635370A (en) * 1970-08-11 1972-01-18 Sorvall Inc Ivan Centrifuge tube closure assembly
US5230865A (en) * 1989-09-08 1993-07-27 Cem Corporation Ventable rupture diaphragm-protected container for heating contained materials by microwave radiation
CA1337342C (en) * 1989-09-08 1995-10-17 Wyatt P. Hargett Ventable rupture diaphragm-protected container for heating contained materials by microwave radiation
DE4013817C1 (en) * 1990-04-30 1991-04-11 Samaro Engineering Und Handels Ag, Rueti, Ch
US5407641A (en) * 1990-10-25 1995-04-18 Helmut Katschnig Microwave apparatus, and container for use in a microwave apparatus
DE4223116A1 (en) * 1992-04-30 1993-11-04 Mikrowellen Labor Systeme DEVICE FOR THE EVAPORATION TREATMENT OF PREFERRED LIQUIDS, IN PARTICULAR REAGENTS, OR FOR THE PREPARATION OR ANALYSIS OF SAMPLING MATERIAL
US5542576A (en) * 1992-05-05 1996-08-06 Arment; Elton D. Apparatus for sealing friction resealable containers during air transport
DE4300957A1 (en) * 1993-01-15 1994-07-21 Anton Paar Kg Graz Sealing device for microwave treatment vessel
US5427741A (en) * 1993-05-19 1995-06-27 Cem Corporation Pressure resistant reinforcing means for containers for materials to be microwave heated
DE9311661U1 (en) * 1993-08-04 1993-12-02 Berghof Labor- und Automationstechnik GmbH, 72800 Eningen Pressure digestion tank for microwave heating in element trace analysis
FR2714468B1 (en) * 1993-12-28 1996-04-26 Prolabo Sa Apparatus for treatment in a humid environment simultaneously on a plurality of samples and use of said apparatus.
US5496110A (en) * 1994-04-04 1996-03-05 Geier; James W. Appparatus for mixing and extracting samples

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9635937A1 *

Also Published As

Publication number Publication date
CA2194780A1 (en) 1996-11-14
US5932817A (en) 1999-08-03
KR970705016A (en) 1997-09-06
JPH10503029A (en) 1998-03-17
WO1996035937A1 (en) 1996-11-14
FR2733923A1 (en) 1996-11-15
FR2733923B1 (en) 1997-08-01

Similar Documents

Publication Publication Date Title
EP0293290B1 (en) Closure device for containers
FR2478435A1 (en) APPARATUS FOR GASIFIER BEVERAGES
EP1117454A1 (en) Disposable injection device designed to be pre-filled
EP0462861A1 (en) Method for packaging a product in a container, ensuring product preservation during storage and the corresponding packaging unit
EP0538094A1 (en) Metal container which can be partially opened by tearing along a line of weakness
EP1208861A1 (en) Protecting device for a syringe needle
WO2007034043A1 (en) Device for filling an aerosol container with liquid, filling installation adapted to receive such a device and aerosol cap and container equipped with such a filling device
EP0581632B1 (en) Filler pipe for fuel tank
WO1996035937A1 (en) Flask sealing system and microwave treatment apparatus with such a sealing system
FR2540754A1 (en) DEVICE FOR CLEANING A FILLING HEAD WITHOUT DISASSEMBLING THE SAME
CA2010347C (en) Viscous fluid dispenser
EP1296878A1 (en) Closure system for a reservoir of a freeze-dried product dispensing device
FR2487321A1 (en) CARTRIDGE CUTTER
EP0466564B1 (en) Dismountable vessel supporting an internal pressure
FR2562667A1 (en) Combined sealing and retention device for testing tubes by pressurised fluid
EP2813834A1 (en) Device for sampling solids from a sealed chamber and method for using such a device
FR2572719A1 (en) Resealing stopper, particularly for gassy beverages
FR2706313A1 (en) Fire protection device for vehicles equipped with a fuel tank
EP0047217B1 (en) Overpressure indicating valve for containers
EP0041034B1 (en) Delivery system for a pressurized gas reservoir such as a cartridge
FR2836461A1 (en) Pyrotechnic fluid disperser, e.g. for spoiling stolen banknotes, has chamber with outer apertures and graduated seals
EP0147250B1 (en) Confinement vessel for dangerous, especially radioactive products
LU81988A1 (en) VALVE BODY FOR AEROSOLS
WO1994007754A2 (en) Closing device for a tank or a housing
FR2717778A1 (en) Stopper with degassing system

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

17P Request for examination filed

Effective date: 19970505

17Q First examination report despatched

Effective date: 20010611

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20011023