WO1997044109A1 - Device and installation for microwave extracting of organic compounds from a sample - Google Patents

Device and installation for microwave extracting of organic compounds from a sample Download PDF

Info

Publication number
WO1997044109A1
WO1997044109A1 PCT/FR1997/000883 FR9700883W WO9744109A1 WO 1997044109 A1 WO1997044109 A1 WO 1997044109A1 FR 9700883 W FR9700883 W FR 9700883W WO 9744109 A1 WO9744109 A1 WO 9744109A1
Authority
WO
WIPO (PCT)
Prior art keywords
solvent
container
reservoir
extraction
cartridge
Prior art date
Application number
PCT/FR1997/000883
Other languages
French (fr)
Inventor
Jean-Louis Di Martino
Maria Dolorès LUQUE DE CASTRO
Luis Enrique GARCIA AYUSO
Original Assignee
Societe Prolabo
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 Societe Prolabo filed Critical Societe Prolabo
Priority to CA002256032A priority Critical patent/CA2256032A1/en
Priority to EP97925106A priority patent/EP0907394A1/en
Priority to JP09541714A priority patent/JP2000510765A/en
Publication of WO1997044109A1 publication Critical patent/WO1997044109A1/en

Links

Classifications

    • 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
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0211Solvent extraction of solids in combination with an electric or magnetic field
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0215Solid material in other stationary receptacles
    • B01D11/0219Fixed bed of solid material
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/14Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation

Definitions

  • the present invention relates generally to the extraction of organic compounds present in samples, and more particularly to a device for extracting, via a solvent, organic compounds from a sample, coupled to a container containing said solvent and subjected to microwave heating.
  • the invention also relates to a Soxlhet type extraction installation of organic compounds from a sample, which comprises such an extraction device.
  • the extraction under microwave heating of organic compounds from a sample is carried out according to an extraction method of the Soxtec type, according to which the extraction solvent and the sample to be treated are placed in the bottom of a container, which is connected in the upper part to a cooling system, said container being subjected to microwave heating for a determined period so that the organic compounds present in the sample are extracted in the solvent.
  • the part of the solvent which evaporates under the microwave heating recondenses on contact with the refrigerant and thus falls back to the bottom of the container where the sample and the solvent containing the extracted compounds are located. .
  • the present invention provides a new microwave-assisted extraction device which makes it possible to lighten the abovementioned extraction process by eliminating the filtration step and by reducing the time devoted to the step of reconcentrating the extract.
  • the invention provides a new extraction device via a solvent for organic compounds in a sample, coupled to a container containing said solvent and subjected to microwave heating.
  • This device comprises: - an elongated member carrying at one end engaged in the container a cartridge containing the sample to be treated, a cylindrical wall closed above, which surrounds a part of said elongated member emerging from the container so that an annular passage vapors is delimited between them, the lower part of said cylindrical wall opening tightly into the container, a solvent tank having an upper opening for the installation of a refrigerant system or a vapor suction system ,
  • connection conduit which extends from the interior of the tank in a downwardly inclined direction, towards said elongated member to open into said annular passage of vapors and come into contact with said elongated member.
  • the term “refrigerant system” is understood here to mean a conventional system cooled by a refrigerant fluid such as water, or an electronic Peltier effect system.
  • a refrigerant fluid such as water
  • an electronic Peltier effect system the use of the cartridge makes it possible to eliminate the step of filtration of the solvent containing the extract in which the sediment was found when a microwave extraction was carried out according to the aforementioned prior art.
  • the elongate member is movably mounted to slide along its vertical axis inside said container. The vertical movement of raising and lowering of said elongated member can be carried out according to the invention automatically.
  • the solvent can be evaporated in the device according to the invention, with or without removing the cartridge from said container, simply by raising said elongated member so that the cartridge is no longer immersed in the solvent comprising the extracted compounds, then heating said solvent so as to evaporate it and to refocus the extract.
  • Solvent vapors can be removed via an extractor hood positioned in the upper opening of said tank.
  • the use of the device according to the invention allows a saving of time of approximately 1 h 30 min compared to the extraction time according to the abovementioned conventional microwave extraction method.
  • the elongated member can be slid into said container, so as to position the sediment contained in the cartridge after extraction above the solvent containing the extracted compounds, then makes it possible to carry out rinsing the sediment while continuing to heat after total extraction of the compounds, said solvent so that it continues to evaporate and recondense while passing through the sediment contained in the cartridge.
  • provision may be made for the cylindrical wall and the connection duct to form a single piece.
  • the reservoir and the connection conduit form a single piece.
  • said cylindrical wall and the container form a single piece.
  • Said single piece constituting the reservoir and the connection conduit can then advantageously be in the form of an elbow, the upper part of the elbow constituting said reservoir and the lower part of the elbow constituting said connection conduit.
  • the elongated member is then a hollow rod.
  • the solvent is evaporated by heating it under the action of a micro field. -waves, is assisted by a flow of nitrogen introduced directly into the solvent via the internal conduit of the rod.
  • the reservoir has at its bottom a tap or a solenoid valve for the recovery outside of the solvent present in said reservoir.
  • the elongated member is a solid rod or a wire.
  • a wire instead of a solid rod as an elongated member may be advantageous for the production of a device according to the invention operating automatically, since the raising and lowering of the wire can easily be automated using a winding system of said wire.
  • a solenoid valve is useful in an automated device according to the invention.
  • the solvent used in the reservoir can be recovered and recycled for later extraction.
  • the cylindrical wall has an upper end edge which delimits an opening in which a closure plug fits in which said rod is mounted in leaktight manner.
  • the member extends the cylindrical wall, the reservoir and the connection conduit are made of glass.
  • the present invention also provides a Soxlhet type extraction installation of organic compounds from a sample, which comprises a container containing an extraction solvent, heated by conventional heating means.
  • This installation is characterized in that it comprises means for emitting microwaves in an application cavity delimited by an upper wall, a side wall and a lower wall, the upper wall of said cavity being provided with an opening. , bordered by a chimney forming a barrier to the propagation towards the outside of microwaves, for the introduction into said application cavity of a flask coupled to an extraction device according to the invention, so that the upper part of said cylindrical wall connected by said conduit for connection to said reservoir of said extraction device, is located outside said microwave application cavity, and said lower wall of said cavity comprising an orifice, bordered a chimney forming a barrier to the propagation to the outside of microwaves, allowing the passage of a first external tube which connects the bottom of said flask to said solvent container, this first external tube having a siphon shape, a second external tube being provided for connecting the reservoir of said extraction device to the solvent container.
  • traditional heating is meant here any kind of heating which is not a microwave heating of the electric or gas heating type.
  • the installation according to the invention advantageously makes it possible to better control the extraction operation by varying the traditional heating and the microwave heating independently as well as the solvent used.
  • traditional heating makes it possible, among other things, to heat solvents which may be more or less transparent to the microwave field.
  • FIG. 1 is a longitudinal sectional view of a first embodiment of an extraction device according to the invention coupled to a container
  • - Figures 2a to 2c schematically show a variant of the first embodiment of the device represents in FIG. 1, at three successive stages of an extraction process
  • FIGS. 3a to 3c show diagrammatically at three different stages of an extraction process
  • a second embodiment of the extraction device according to the 'invention
  • FIG. 5 is a schematic representation of an installation according to the present invention.
  • a a represents an extraction device 100, via a solvent, of organic compounds from a sample.
  • This extraction device 100 is coupled to a container 1 intended to contain said solvent and to be subjected to microwave heating.
  • the extraction device 100 comprises an elongated member of axis X, here a rod 110 vertically engaged inside the container 1 along its axis. This rod 110 door at one end engaged in the container 1, a cartridge 120 containing the sample to be treated.
  • the cartridge 120 is an extraction cartridge made of cellulose or any other suitable porous material. It is fixed by means of a support 111 mounted at the end of the rod 110. This support 111 is produced for example from polytetrafluoroethylene. A locking system 112 is engaged on the rod 110 so as to secure the cartridge 120 to the support 111. According to an alternative embodiment not shown, it is possible to provide that the cartridge is secured to the end of the rod by a magnet system , such a magnet system is advantageous in a device according to the invention operating automatically, because it allows the automatic installation and removal of the cartridge.
  • said extraction device 100 has a cylindrical wall 130 which surrounds a part of the rod 110 which emerges from the container 1 so that an annular vapor passage 131 is delimited between said cylindrical wall and said rod.
  • lugs 133 are provided to keep the rod 110 centered inside said cylindrical wall 130.
  • This cylindrical wall 130 has, at the top, an end edge which delimits an opening 132 This opening 132 is hermetically closed by means of a rode stopper made of polytetrafluoroethylene for example. Inside this rode stopper, the rod 110 is engaged so that it is movably mounted to slide inside the container 1 along its axis X.I1 notes that the upward and downward movement of the rod along its axis X ⁇ ans the container, can be automated. To this end, the lapped bushing 160 has a seal for guiding the rod 110.
  • the cylindrical wall 130 has at its lower end an opening which opens into the interior of the container 1.
  • the adjustment of the cylindrical wall 130 has the interior of the container 1 is made in a sealed manner.
  • the extraction device 100 also includes a solvent tank 140 comprising an upper opening 141 in which a running-in 143 is positioned for the installation of a refrigerant system or a vapor suction system.
  • the refrigerant system is a refrigerant system such as water or an automatic Peltier effect system.
  • the reservoir 140 has at its bottom a tap 142 for the recovery outside of the solvent present in said reservoir 140.
  • a solenoid valve in place of the tap 142.
  • a connection duct 150 is provided which extends from the inside of the reservoir 140 in a direction Y inclined downward relative to the axis X of the rod 110, in the direction of the rod 110, to open out. in said annular vapor passage 131 and come into contact with said rod 110.
  • the cylindrical wall 1J0 comprises at the level of this connection duct 150 a widening for allowing part of the duct 150 to extend inside said annular passage of the vapors 131 and to come into contact with said rod 110 .
  • the cylindrical wall 130 and the connection conduit 150 form a single piece.
  • the reservoir and the connection conduit form a single piece, and that the cylindrical wall and the container form a single piece.
  • FIGS. 2a to 2c three successive stages of a process for extracting organic compounds have been shown, here polycyclic aromatic compounds contained in a sample, using an alternative embodiment of the extraction device 100 shown in Figure 1.
  • the container 1 and the cylindrical wall 130 form a single piece, the reservoir 140 and the connection conduit also forming a single piece.
  • FIG. 2a shows the actual extraction step using said device 100.
  • a microwave field with a power for example equal to 90 W is applied to the container 1 which contains a solvent S extraction and the rod 110 is positioned in the low position so that the cartridge 120 is immersed in said solvent S.
  • the solvent Under the action of the microwave field, the solvent vaporizes and the solvent vapors propagate to the reservoir 140 where, in contact with the refrigerant 144, they recondense. The recondensed droplets are recovered in the reservoir 140.
  • the solvent is vaporized either by direct absorption by the latter of microwave energy if said solvent is polar, or, if it is not sufficiently polar, by heat conduction via an element heated by the microwave energy, such as the container, the sample or any other element capable of heating under the direct action of microwaves.
  • the valve 142 of the reservoir 140 is then in the closed position.
  • the solvent flows along the rod 110 to descend into the cartridge 120 via a central conduit 111 'provided in the locking system 112 and the support 111 , and flow through the porous wall of said cartridge, into the bottom of container 1.
  • the rod 110 is positioned in the high position so that the cartridge 120 is above the solvent S and we continue to apply at the bottom of the container 1, the microwave field of the same power, of so that the solvent continues to vaporize and recondense on contact with the refrigerant 144 in the reservoir 140 with its tap 142 closed.
  • the solvent droplets recondensed and recovered in the tank, slide along the rod and rinse the sediment present in the raised cartridge 120.
  • the cartridge is placed in a basket with a sealed wall, fixed at the end of the rod, so that it remains between said sealed wall and said cartridge. , a gap in which the solvent flows through the cartridge, said basket comprising in the upper part a system for discharging solvent in the event of an overflow.
  • Figure 2c shows the next step which is a step of reconcentrating the extract in the container.
  • the cartridge 120 is always positioned in the high position, that is to say above the solvent.
  • the tap 142 is then opened and a microwave field of the same power is applied to the bottom of the container 1.
  • the solvent vaporizes and recondenses in the reservoir 140 under the action of the refrigerant 144, then flows via the tap 142 through a tube 2 connected to said tap, so as to be collected in a graduated container 3.
  • the rod, the reservoir, the cylindrical wall and the connection conduit are made either of glass, or of polytetrafluoroethylene or else of quartz for example.
  • the glass rod is a solid rod.
  • the solid rod is replaced by a wire, which can be automatically wound and unrolls outside the device to allow it to descend and rise ⁇ ans said container.
  • the adaptation of the refrigerant system 144 to the running-in provided in the upper opening of the tank must be such that good tightness is observed and the refrigerant is not in contact with the walls of the solvent tank.
  • FIGS. 3a to 3c three stages of operation of a second embodiment have been shown in the extraction device 100 according to the invention.
  • the upper part of the elbow constitutes the reservoir 140 and the lower part of the elbow constitutes the conduit of connection 150.
  • the reservoir 140 does not have a tap at its bottom.
  • the rod 110 is a hollow rod.
  • the cylindrical wall 130 and the container 101 form a single piece.
  • these two elements are two different parts coupled together.
  • FIG. 3a shows the actual extraction of the polycyclic organic compounds contained in the matrix positioned in the cartridge 120, under the action of the microwave field applied to the bottom of the container 1 which contains the cartridge 120 positioned in position low at the end of the rod 110 so that it bathes in the solvent S.
  • the microwave field is for example of a power of 30 W.
  • the solvent S vaporizes and the solvent vapors rise in the reservoir 140 or they recondense.
  • the recondensed solvent droplets then fall via the connection duct 150 into the container, flowing along the rod 110 to pass through the cartridge 120 and reach the bottom of the container.
  • the rod 110 is raised in the high position so that the cartridge 120 is placed above the quantity of solvent S contained in the bottom of container 1, while the solvent field S at the bottom of container 1 is continued to apply the microwave field.
  • This step shown in Figure 3b is the rinsing step. Under the action in the microwave field, the heated solvent S evaporates and rises to the reservoir 140 via the connection conduit 150.
  • the solvent droplets recondensed via the refrigerant 144 slide via the connection duct 150, along the rod 110 and rinse the sediment located in the raised cartridge 120, before falling back into the bottom of the container 1.
  • the cartridge 120 is then removed from the container 1.
  • a microwave field is applied to the bottom of the container 1 and a flow of nitrogen is introduced from the inside of the rod 110 according to arrow A.
  • the solvent vapors formed under the microwave heating are evacuated towards the connection duct 150 and sucked in according to arrow B with the aid of an extractor hood positioned in the upper opening of the tank.
  • Such a magnetic stirring bar allows homogenization of the sample and of the solvent during the extraction step.
  • the contact and exchange surface between the sample containing the compounds to be extracted and the solution is increased during the extraction step.
  • the duration of the extraction is reduced while maintaining a good extraction yield.
  • Agitation advantageously avoids the possible phenomena of over-boiling of the heated solvent during extraction, such over-boiling causing a O 97/44109 PC17FR97 / 00883 sudden unwanted rise of the solvent in the container.
  • the magnetic bar can advantageously absorb a non-negligible amount of microwave energy and heat by conduction a solvent more or less transparent to microwaves.
  • This mstai-ation comprises a container 1001 in the form of a balloon containing an extraction solvent heated by conventional heating means 1002.
  • conventional cnauffage means means an electric or gas heating plate for example.
  • This installation 1000 further comprises means 1003 for emitting microwaves, for example a magnetron, in a cavity 1100 for applying microwaves.
  • This application cavity 1100 is delimited by an upper wall 1110, a cylindrical side wall 1120 and a lower wall 1130.
  • the upper wall 1110 of said cavity 1100 is provided with an opening 1111 which is bordered by a chimney 1112 whose height H depends on the section of the opening 1111 and on the frequency of emission of microwaves in said cavity , is such that said chimney forms a barrier to the propagation of microwaves out of the cavity.
  • This opening 1111 allows the introduction into said application cavity 1100 of a flask 1 coupled to an extraction device 100 according to the invention.
  • this extraction device 100 is that shown more particularly in FIGS. 2a to 2c.
  • the lower part 1130 of said microwave application cavity 1100 includes an orifice 1131 also bordered by a chimney 1132 whose height H which is a function of the frequency of emission of the microwaves and of the section of the orifice 1131, is such that said chimney forms a barrier to the propagation of microwaves towards the outside of the cavity.
  • the orifice 1131 allows the passage of a first external tube 1004 which connects the bottom of the flask 1 to said container 1001 containing the solvent.
  • this first outer tubu_ re 1004 has the shape of a siphon.
  • This second external tube fits on the valve 142 of the reservoir 140 and opens into the interior of the solvent container 1001.
  • the operating mode of this installation is as follows.
  • the solvent in the solvent container 1001 is heated, which evaporates and circulates in the second connection tube 1005 to reach the reservoir 140 where it recondenses when it comes into contact. refrigerant 144.
  • the solvent in this flask vaporizes again and is recondensed in the reservoir 140 before flowing through the connection duct 150 and the rod 110 in the bottom of the flask 1 while crossing the cartridge 120.
  • the part of the solvent loaded with extracted compounds which does not vaporize flows from the bottom of the flask 1 to the first connection tubing 1004 until the level in this tubing rises.
  • the level of the solvent in the tubing increases until it reaches the elbow of the siphon and then falls back into the solvent container 1001.
  • the extraction is carried out by means of a vaporized solvent, recon ⁇ ensed then revaporized and recondensed.
  • Two sources of heat are used, a traditional source and a source of heat under microwaves, to carry out the extraction.
  • Heating the microwave solvent that passes through the cartridge increases the speed of extraction of comDosés. Thanks to this installation, it is possible to better control the extraction operation by varying the traditional heating, the microwave heating and the solvent used. For a given microwave power, by choosing a solvent more or less transparent to microwaves, it is possible to more or less heat said solvent during its passage through the microwave cavity and by this means, vary the time and quality of extraction of the sample placed in the cartridge.

Abstract

The invention features a device (100) for extracting organic compounds from a sample, coupled with a receptacle (1) containing a solvent and subjected to microwave heating. An elongated means bears at one end engaged in the receptacle (1) a cartridge (120) containing the sample to be treated, a cylindrical wall (130) encloses the said elongated means that emerges from the receptacle (1) such that a ring-shaped steam passage (131) is defined between them, and opens in sealed manner into the receptacle (1). A solvent reservoir (140) comprises an upper aperture (141) for fitting a refrigerating system or a closed hood. A connecting conduit (150) extends from the reservoir (140) along an inclined direction (Y), towards the said means into the ring-shaped steam passage (131) and comes in contact with the said means.

Description

DISPOSITIF ET INSTALLATION D'EXTRACTION SOUS MICRO-ONDES DE COMPOSES ORGANIQUES D'UN ECHANTILLON. La présente invention concerne de manière générale l'extraction de composés organiques présents dans des échantillons, et plus particulièrement un dispositif d'extraction par l'intermédiaire d'un solvant de composés organiques d'un échantillon, couplé à un récipient contenant ledit solvant et soumis à un chauffage micro¬ ondes. L'invention concerne également une installation d'extraction du type Soxlhet de composés organiques d'un échantillon, qui comprend un tel dispositif d'extraction. Actuellement, l'extraction sous chauffage micro¬ ondes de composés organiques d'un échantillon, est réalisée selon une méthode d'extraction du type Soxtec, selon laquelle on place le solvant d'extraction et l'échantillon à traiter dans le fond d'un récipient, qui est raccordé en partie supérieure à un système réfrigérant, ledit récipient étant soumis à un chauffage micro-ondes pendant une durée déterminée afin que les composés organiques présents dans l'échantillon soient extraits dans le solvant. DEVICE AND INSTALLATION FOR MICROWAVE EXTRACTION OF ORGANIC COMPOUNDS FROM A SAMPLE. The present invention relates generally to the extraction of organic compounds present in samples, and more particularly to a device for extracting, via a solvent, organic compounds from a sample, coupled to a container containing said solvent and subjected to microwave heating. The invention also relates to a Soxlhet type extraction installation of organic compounds from a sample, which comprises such an extraction device. Currently, the extraction under microwave heating of organic compounds from a sample is carried out according to an extraction method of the Soxtec type, according to which the extraction solvent and the sample to be treated are placed in the bottom of a container, which is connected in the upper part to a cooling system, said container being subjected to microwave heating for a determined period so that the organic compounds present in the sample are extracted in the solvent.
Pendant toute la durée de l'extraction, la partie du solvant qui s'évapore sous le chauffage micro-ondes se recondense au contact du réfrigérant et retombe ainsi dans le fond du récipient où se trouvent l'échantillon et le solvant contenant les composés extraits.During the entire extraction period, the part of the solvent which evaporates under the microwave heating recondenses on contact with the refrigerant and thus falls back to the bottom of the container where the sample and the solvent containing the extracted compounds are located. .
Lorsque l'extraction proprement dite est terminée, vient alors l'étape de filtration afin de séparer le sédiment d'échantillon du mélange constitué par l,e solvant et les composés extraits, puis l'étape de reconcentration de l'extrait par évaporation du solvant.When the actual extraction is complete, there comes the filtration step in order to separate the sample sediment from the mixture consisting of the solvent and the extracted compounds, then the step of reconcentrating the extract by evaporation of the solvent.
La présente invention propose un nouveau dispositif d'extraction assisté par micro-ondes qui permet d'alléger le procédé d'extraction précité en éliminant l'étape de filtration et en diminuant le temps consacré à l'étape de reconcentration de l'extrait.The present invention provides a new microwave-assisted extraction device which makes it possible to lighten the abovementioned extraction process by eliminating the filtration step and by reducing the time devoted to the step of reconcentrating the extract.
Plus particulièrement, l' invention propose un nouveau dispositif d'extraction par l'intermédiaire d'un solvant de composés organiques d'un échantillon, couplé à un récipient contenant ledit solvant et soumis à un chauffage micro-ondes.More particularly, the invention provides a new extraction device via a solvent for organic compounds in a sample, coupled to a container containing said solvent and subjected to microwave heating.
Ce dispositif comprend : - un organe de forme allongée portant à une extrémité engagée dans le récipient une cartouche renfermant l'échantillon à traiter, une paroi cylindrique fermée supérieurement, qui entoure une partie dudit organe allongé émergeante du récipient de sorte qu'un passage annulaire des vapeurs est délimité entre eux, la partie inférieure de ladite paroi cylindrique débouchant de manière étanche dans le récipient, un réservoir à solvant comportant une ouverture supérieure pour la mise en place d'un système réfrigérant ou d'un système d'aspiration des vapeurs,This device comprises: - an elongated member carrying at one end engaged in the container a cartridge containing the sample to be treated, a cylindrical wall closed above, which surrounds a part of said elongated member emerging from the container so that an annular passage vapors is delimited between them, the lower part of said cylindrical wall opening tightly into the container, a solvent tank having an upper opening for the installation of a refrigerant system or a vapor suction system ,
- un conduit de raccordement qui s'étend à partir de l'intérieur du réservoir suivant une direction inclinée vers le bas, vers ledit organe allongé pour déboucher dans ledit passage annulaire des vapeurs et venir en contact dudit organe allongé.- A connection conduit which extends from the interior of the tank in a downwardly inclined direction, towards said elongated member to open into said annular passage of vapors and come into contact with said elongated member.
On entend ici par système réfrigérant, un système classique à refroidissement par un fluide réfrigérant tel que l'eau, ou un système électronique à effet Peltier. Ainsi, selon l'invention, l'utilisation de la cartouche permet d'éliminer l'étape de filtration du solvant contenant l'extrait dans lequel se trouvait le sédiment lorsqu'on effectuait une extraction micro-ondes selon la technique antérieure précitée. Selon une caractéristique particulièrement avantageuse du dispositif conforme à la présente invention, l'organe allongé est monté mobile à coulissement selon son axe vertical à l'intérieur dudit récipient . Le mouvement vertical de montée et de descente dudit organe allongé peut être réalisé selon l'invention de manière automatique.The term “refrigerant system” is understood here to mean a conventional system cooled by a refrigerant fluid such as water, or an electronic Peltier effect system. Thus, according to the invention, the use of the cartridge makes it possible to eliminate the step of filtration of the solvent containing the extract in which the sediment was found when a microwave extraction was carried out according to the aforementioned prior art. According to a particularly advantageous characteristic of the device according to the present invention, the elongate member is movably mounted to slide along its vertical axis inside said container. The vertical movement of raising and lowering of said elongated member can be carried out according to the invention automatically.
Ainsi, lorsque l'étape d'extraction proprement dite est terminée, l' évaporation du solvant peut être réalisée dans le dispositif selon l'invention, avec ou sans retirer la cartouche dudit récipient, simplement en remontant ledit organe allongé de façon que la cartouche ne baigne plus dans le solvant comprenant les composés extraits, en chauffant alors ledit solvant de manière à l'évaporer et à reconcentrer l'extrait.Thus, when the actual extraction step is completed, the solvent can be evaporated in the device according to the invention, with or without removing the cartridge from said container, simply by raising said elongated member so that the cartridge is no longer immersed in the solvent comprising the extracted compounds, then heating said solvent so as to evaporate it and to refocus the extract.
Les vapeurs de solvant peuvent être évacuées par l'intermédiaire d'une hotte aspirante positionnée dans l'ouverture supérieure dudit réservoir. L'utilisation du dispositif selon l'invention, permet un gain de temps d'environ 1 h 30 mn par rapport au temps d'extraction selon la méthode d'extraction sous micro-ondes classique précitée.Solvent vapors can be removed via an extractor hood positioned in the upper opening of said tank. The use of the device according to the invention allows a saving of time of approximately 1 h 30 min compared to the extraction time according to the abovementioned conventional microwave extraction method.
De plus, le fait que, selon l'invention, l'organe allongé puisse être coulissé dans ledit récipient, de manière à positionner le sédiment contenu dans la cartouche après extraction au-dessus du solvant contenant les composés extraits, permet alors d'effectuer un rinçage du sédiment en continuant de chauffer après extraction totale des composés, ledit solvant de manière qu'il continue à s'évaporer et se recondenser en traversant le sédiment contenu dans la cartouche.In addition, the fact that, according to the invention, the elongated member can be slid into said container, so as to position the sediment contained in the cartridge after extraction above the solvent containing the extracted compounds, then makes it possible to carry out rinsing the sediment while continuing to heat after total extraction of the compounds, said solvent so that it continues to evaporate and recondense while passing through the sediment contained in the cartridge.
Selon un mode de réalisation du dispositif conforme à l'invention, il peut être prévu que la paroi cylindrique et le conduit de raccordement forment une seule pièce.According to one embodiment of the device according to the invention, provision may be made for the cylindrical wall and the connection duct to form a single piece.
Selon un autre mode de réalisation du dispositif conforme à l'invention, le réservoir et le conduit de raccordement forment une seule pièce. Dans ce cas, il peut être prévu également que ladite paroi cylindrique et le récipient forment une seule pièce.According to another embodiment of the device according to the invention, the reservoir and the connection conduit form a single piece. In this case, it can also be provided that said cylindrical wall and the container form a single piece.
Ladite pièce unique constituant le réservoir et le conduit de raccordement, peut se présenter alors avantageusement sous la forme de coude, la partie supérieure du coude constituant ledit réservoir et la partie inférieure du coude constituant ledit conduit de raccordement . Selon ce mode de réalisation précité, l'organe allongé est alors une tige creuse.Said single piece constituting the reservoir and the connection conduit, can then advantageously be in the form of an elbow, the upper part of the elbow constituting said reservoir and the lower part of the elbow constituting said connection conduit. According to this aforementioned embodiment, the elongated member is then a hollow rod.
Ainsi, selon ce mode de réalisation, comme cela sera décrit plus en détail ultérieurement, lors de l'étape de reconcentration de l'extrait, l' évaporation du solvant réalisée par chauffage de celui-ci sous l'action d'un champ micro-ondes, est assistée par un flux d'azote introduit directement dans le solvant via le conduit interne de la tige. Selon un autre mode de réalisation du dispositif conforme à la présente invention, le réservoir comporte dans son fond un robinet ou une électrovanne pour la récupération à l'extérieur du solvant présent dans ledit réservoir. Dans ce cas, l'organe allongé est une tige pleine ou encore un fil.Thus, according to this embodiment, as will be described in more detail later, during the step of reconcentration of the extract, the solvent is evaporated by heating it under the action of a micro field. -waves, is assisted by a flow of nitrogen introduced directly into the solvent via the internal conduit of the rod. According to another embodiment of the device according to the present invention, the reservoir has at its bottom a tap or a solenoid valve for the recovery outside of the solvent present in said reservoir. In this case, the elongated member is a solid rod or a wire.
En effet, selon ce mode de réalisation précité, l'intervention d'un flux d'azote lors de l'étape de reconcenrtration de l'extrait par évaporation totale du solvant, peut être abandonnée et il n'est plus alors nécessaire d'avoir une tige creuse.In fact, according to this aforementioned embodiment, the intervention of a flow of nitrogen during the step of reconcentration of the extract by total evaporation of the solvent can be abandoned and it is no longer necessary to have a hollow stem.
L'utilisation d'un fil au lieu d'une tige pleine en tant qu'organe allongé, peut être avantageuse pour la réalisation d'un dispositif selon l'invention fonctionnant de manière automatique, car la montée et la descente du fil peuvent facilement être automatisées à l'aide d'un système à enroulement dudit fil.The use of a wire instead of a solid rod as an elongated member may be advantageous for the production of a device according to the invention operating automatically, since the raising and lowering of the wire can easily be automated using a winding system of said wire.
De plus, une électrovanne est utile dans un dispositif automatise selon l'invention. Avantageusement, grâce au robinet ou à l' électrovanne on peut récupérer le solvant utilisé se trouvant dans le réservoir et le recycler pour une extraction ultérieure.In addition, a solenoid valve is useful in an automated device according to the invention. Advantageously, using the tap or the solenoid valve, the solvent used in the reservoir can be recovered and recycled for later extraction.
Selon une caractéristique du dispositif conforme à l'invention, la paroi cylindrique comporte un bord d'extrémité supérieur qui délimite une ouverture dans laquelle vient s'adapter un bouchon de fermeture dans lequel est montée de manière étanche ladite tige. Selon une variante de réalisation de l'invention, l'organe allonge la paroi cylindrique, le réservoir et le conduit de raccordement sont réalises en verre.According to a characteristic of the device according to the invention, the cylindrical wall has an upper end edge which delimits an opening in which a closure plug fits in which said rod is mounted in leaktight manner. According to an alternative embodiment of the invention, the member extends the cylindrical wall, the reservoir and the connection conduit are made of glass.
La présente invention propose également une installation d'extraction du type Soxlhet de composes organiques d'un échantillon, qui comprend un récipient contenant un solvant d'extraction, chauffe par des moyens de chauffage traditionnel.The present invention also provides a Soxlhet type extraction installation of organic compounds from a sample, which comprises a container containing an extraction solvent, heated by conventional heating means.
Cette installation est caractérisée en ce qu'elle comporte des moyens pour émettre des micro-ondes dans une cavité d'application délimitée par une paroi supérieure, une paroi latérale et une paroi inférieure, la paroi supérieure de ladite cavité étant pourvue d'une ouverture, bordée d'une cheminée formant barrière à la propagation vers l'extérieur des micro-ondes, pour l'introduction dans ladite cavité d'application d'un matras couple à un dispositif d'extraction selon l'invention, de telle sorte que la partie supérieure de ladite paroi cylindrique raccordée par ledit conduit de raccordement audit réservoir dudit dispositif d'extraction, se situe a l'extérieur de ladite cavité d'application des micro-ondes, et ladite paroi inférieure de ladite cavité comprenant un orifice, borde d'une cheminée formant barrière a la propagation vers l'extérieur des micro-ondes, autorisant le passage d'une première tubulure extérieure qui raccorde le fond dudit matras audit récipient de solvant, cette première tubulure extérieure présentant une forme de siphon, une deuxième tubulure extérieure étant prévue pour raccorder le réservoir dudit dispositif d'extraction au récipient de solvant.This installation is characterized in that it comprises means for emitting microwaves in an application cavity delimited by an upper wall, a side wall and a lower wall, the upper wall of said cavity being provided with an opening. , bordered by a chimney forming a barrier to the propagation towards the outside of microwaves, for the introduction into said application cavity of a flask coupled to an extraction device according to the invention, so that the upper part of said cylindrical wall connected by said conduit for connection to said reservoir of said extraction device, is located outside said microwave application cavity, and said lower wall of said cavity comprising an orifice, bordered a chimney forming a barrier to the propagation to the outside of microwaves, allowing the passage of a first external tube which connects the bottom of said flask to said solvent container, this first external tube having a siphon shape, a second external tube being provided for connecting the reservoir of said extraction device to the solvent container.
On entend ici par chauffage traditionnel, toute sorte de chauffage qui ne soit pas un cnauffage micro¬ ondes du type chauffage électrique ou a gaz. L'installation selon l'invention, permet avantageusement de mieux contrôler l'opération d'extraction en faisant varier le chauffage traditionnel et le chauffage micro-ondes de manière indépendante ainsi que le solvant utilise. En effet, le chauffage traditionnel permet entre autre de chauffer des solvants qui peuvent être plus ou moins transparents au champs micro-ondes .By traditional heating is meant here any kind of heating which is not a microwave heating of the electric or gas heating type. The installation according to the invention advantageously makes it possible to better control the extraction operation by varying the traditional heating and the microwave heating independently as well as the solvent used. Indeed, traditional heating makes it possible, among other things, to heat solvents which may be more or less transparent to the microwave field.
Pour une puissance donnée des micro-ondes en choisissant un solvant plus ou moins transparent aux micro-ondes, il est possible de chauffer plus ou moins ledit solvant lors de son passage dans la cavité d'application des micro-ondes et par ce biais, faire varier le temps et la qualité d'extraction de l'échantillon placé dans la cartouche du dispositif d'extraction selon l'invention.For a given microwave power by choosing a more or less transparent solvent for microwaves, it is possible to more or less heat said solvent during its passage through the microwave application cavity and through this, varying the time and quality of extraction of the sample placed in the cartridge of the extraction device according to the invention.
La description qui va suivre en regard des dessins annexés, donnés à titre d'exemples non limitatifs, fera bien comprendre en quoi consiste l'invention et comment elle peut être réalisée.The description which follows with reference to the appended drawings, given by way of nonlimiting examples, will make it clear what the invention consists of and how it can be implemented.
Sur les dessins annexés :In the accompanying drawings:
- la figure 1 est une vue en coupe longitudinale d'un premier mode de réalisation d'un dispositif d'extraction selon l'invention couplé à un récipient, - les figures 2a à 2c, représentent schematiquement une variante du premier mode de réalisation du dispositif représente sur la figure 1, à trois étapes successives d'un procédé d'extraction, les figures 3a a 3c représentent schematiquement à trois étapes différentes d'un procédé d'extraction, un deuxième mode de réalisation du dispositif d'extraction selon l'invention,- Figure 1 is a longitudinal sectional view of a first embodiment of an extraction device according to the invention coupled to a container, - Figures 2a to 2c, schematically show a variant of the first embodiment of the device represents in FIG. 1, at three successive stages of an extraction process, FIGS. 3a to 3c show diagrammatically at three different stages of an extraction process, a second embodiment of the extraction device according to the 'invention,
- la figure 5 est une représentation schématique d'une installation conforme à la présente invention. Sur la figure 1, on a représente un dispositif d'extraction 100 par l'intermédiaire d'un solvant, de composés organiques d'un échantillon. Ce dispositif d'extraction 100 est couplé a un récipient 1 destine a contenir ledit solvant et à être soumis a un chauffage micro-ondes.- Figure 5 is a schematic representation of an installation according to the present invention. In FIG. 1, a a represents an extraction device 100, via a solvent, of organic compounds from a sample. This extraction device 100 is coupled to a container 1 intended to contain said solvent and to be subjected to microwave heating.
Le dispositif d'extraction 100 comprend un organe allongé d'axe X, ici une tige 110 engagée verticalement à l'intérieur du récipient 1 selon son axe. Cette tige 110 porte à une extrémité engagée dans le récipient 1, une cartouche 120 renfermant l'échantillon a traiter.The extraction device 100 comprises an elongated member of axis X, here a rod 110 vertically engaged inside the container 1 along its axis. This rod 110 door at one end engaged in the container 1, a cartridge 120 containing the sample to be treated.
La cartouche 120 est une cartouche d'extraction en cellulose ou en tout autre matériau poreux adéquat. Elle est fixée par l'intermédiaire d'un support 111 monté à l'extrémité de la tige 110. Ce support 111 est réalisé par exemple en polytétrafluoréthylène. Un système de verrouillage 112 est engagé sur la tige 110 de manière à solidariser la cartouche 120 au support 111. Selon une variante de réalisation non représentée, on peut prévoir que la cartouche soit solidarisée à l'extrémité de la tige par un système a aimants, un tel système à aimants est avantageux dans un dispositif selon l'invention fonctionnant de manière automatique, car il permet la mise en place et l'enlèvement automatiques de la cartouche.The cartridge 120 is an extraction cartridge made of cellulose or any other suitable porous material. It is fixed by means of a support 111 mounted at the end of the rod 110. This support 111 is produced for example from polytetrafluoroethylene. A locking system 112 is engaged on the rod 110 so as to secure the cartridge 120 to the support 111. According to an alternative embodiment not shown, it is possible to provide that the cartridge is secured to the end of the rod by a magnet system , such a magnet system is advantageous in a device according to the invention operating automatically, because it allows the automatic installation and removal of the cartridge.
En outre, ledit dispositif d'extraction 100 comporte une paroi cylindrique 130 qui entoure une partie de la tige 110 qui émerge du récipient 1 de sorte qu'un passage annulaire de vapeur 131 est délimite entre ladite paroi cylindrique et ladite tige.In addition, said extraction device 100 has a cylindrical wall 130 which surrounds a part of the rod 110 which emerges from the container 1 so that an annular vapor passage 131 is delimited between said cylindrical wall and said rod.
Sur la face interne de la paroi cylindrique 130, il est prévu des ergots 133 pour maintenir la tige 110 centrée à l'intérieur de ladite paroi cylindrique 130. Cette paroi cylindrique 130 présente en partie supérieure un bord d'extrémité qui délimite une ouverture 132. Cette ouverture 132 est fermée hermétiquement par l'intermédiaire d'un bouchon rode réalisé en polytétrafluoréthylène par exemple. A l'intérieur de ce bouchon rode, est engagée la tige 110 de façon a ce qu'elle soit montée mobile a coulissement a l'intérieur du récipient 1 selon son axe X.I1 a note que le mouvement de montée et de descente de la tige selon son axe X αans le récipient, peut être automatise. Le boucnon rodé 160 comporte a cet effet, un joint pour le guidage de la tige 110.On the internal face of the cylindrical wall 130, lugs 133 are provided to keep the rod 110 centered inside said cylindrical wall 130. This cylindrical wall 130 has, at the top, an end edge which delimits an opening 132 This opening 132 is hermetically closed by means of a rode stopper made of polytetrafluoroethylene for example. Inside this rode stopper, the rod 110 is engaged so that it is movably mounted to slide inside the container 1 along its axis X.I1 notes that the upward and downward movement of the rod along its axis X αans the container, can be automated. To this end, the lapped bushing 160 has a seal for guiding the rod 110.
La paroi cylindrique 130 comporte a son extrémité inférieure une ouverture qui débouche a l'intérieur du récipient 1. L'ajustement de la paroi cylindrique 130 a l'intérieur du récipient 1 est réalisé de manière etanche .The cylindrical wall 130 has at its lower end an opening which opens into the interior of the container 1. The adjustment of the cylindrical wall 130 has the interior of the container 1 is made in a sealed manner.
Le dispositif d'extraction 100 comporte également un réservoir 140 à solvant comprenant une ouverture supérieure 141 dans lequel est positionné un rodage 143 pour la mise en place d'un système réfrigérant ou d'un système d'aspiration des vapeurs.The extraction device 100 also includes a solvent tank 140 comprising an upper opening 141 in which a running-in 143 is positioned for the installation of a refrigerant system or a vapor suction system.
Le système réfrigérant est un système à fluide réfrigérant tel que l'eau ou un système automatique à effet Peltier.The refrigerant system is a refrigerant system such as water or an automatic Peltier effect system.
Selon le mode de réalisation représenté sur la figure 1, le réservoir 140 comporte dans son fond un robinet 142 pour la récupération à l'extérieur du solvant présent dans ledit réservoir 140. En variante, on peut prévoir dans un but d'automatisation du fonctionnement dudit dispositif, une électrovanne à la place du robinet 142.According to the embodiment shown in FIG. 1, the reservoir 140 has at its bottom a tap 142 for the recovery outside of the solvent present in said reservoir 140. As a variant, provision may be made for the purpose of automating the operation of said device, a solenoid valve in place of the tap 142.
Il est prévu un conduit de raccordement 150 qui s'étend à partir αe l'intérieur du réservoir 140 suivant une direction Y inclinée vers le bas par rapport à l'axe X de la tige 110, en direction de la tige 110, pour déboucher dans ledit passage annulaire de vapeur 131 et venir au contact de ladite tige 110.A connection duct 150 is provided which extends from the inside of the reservoir 140 in a direction Y inclined downward relative to the axis X of the rod 110, in the direction of the rod 110, to open out. in said annular vapor passage 131 and come into contact with said rod 110.
A cet effet, la paroi cylindrique 1J0 comporte au niveau αe ce conduit de raccordement 150 un élargissement peur permettre a une partie du conduit 150 de s' étendre a l'intérieur dudit passage annulaire des vapeurs 131 et de venir au contact de ladite tige 110.To this end, the cylindrical wall 1J0 comprises at the level of this connection duct 150 a widening for allowing part of the duct 150 to extend inside said annular passage of the vapors 131 and to come into contact with said rod 110 .
Selon le mode de réalisation représenté sur la figure 1, la paroi cylindrique 130 et le conduit de raccordement 150 forment une seule pièce.According to the embodiment shown in Figure 1, the cylindrical wall 130 and the connection conduit 150 form a single piece.
Bien entendu, selon d'autres variantes explicitées ultérieurement en référence aux figures 2 et 3, il peut être prévu que le réservoir et le conduit de raccordement forment une seule pièce, et que la paroi cylindrique et le récipient forment une seule pièce.Of course, according to other variants explained later with reference to Figures 2 and 3, it can be provided that the reservoir and the connection conduit form a single piece, and that the cylindrical wall and the container form a single piece.
Sur les figures 2a a 2c, on a représenté trois étapes successives d'un procède d'extraction de composés organiques, ici des composes aromatiques polycycliques contenus dans un échantillon, à l'aide d'une variante de réalisation du dispositif d'extraction 100 représenté sur la figure 1.In FIGS. 2a to 2c, three successive stages of a process for extracting organic compounds have been shown, here polycyclic aromatic compounds contained in a sample, using an alternative embodiment of the extraction device 100 shown in Figure 1.
Selon la variante de réalisation représentée sur les figures 2a à 2c, le récipient 1 et la paroi cylindrique 130 forment une seule pièce, le réservoir 140 et le conduit de raccordement formant également une pièce unique.According to the variant embodiment shown in FIGS. 2a to 2c, the container 1 and the cylindrical wall 130 form a single piece, the reservoir 140 and the connection conduit also forming a single piece.
La figure 2a montre l'étape d'extraction proprement dite à l'aide dudit dispositif 100. Lors de cette étape, un champ micro-ondes d'une puissance par exemple égale à 90 W est applique au récipient 1 qui contient un solvant S d'extraction et la tige 110 est positionnée en position basse de sorte que la cartouche 120 baigne dans ledit solvant S.FIG. 2a shows the actual extraction step using said device 100. During this step, a microwave field with a power for example equal to 90 W is applied to the container 1 which contains a solvent S extraction and the rod 110 is positioned in the low position so that the cartridge 120 is immersed in said solvent S.
Sous l'action du champ micro-ondes, le solvant se vaporise et les vapeurs de solvant se propagent jusqu'au réservoir 140 où en contact avec le réfrigérant 144, elles se recondensent. Les gouttelettes recondensées sont récupérées dans le réservoir 140.Under the action of the microwave field, the solvent vaporizes and the solvent vapors propagate to the reservoir 140 where, in contact with the refrigerant 144, they recondense. The recondensed droplets are recovered in the reservoir 140.
La vaporisation du solvant est réalise soit par absorption directe par ce dernier de l'énergie micro¬ ondes si ledit solvant est polaire, soit, si celui-ci n'est pas suffisamment polaire, par conduction de chaleur via un elémert chauffe par l'énergie micro-ondes, tels que le récipient, l'échantillon ou tout autre élément susceptible de chauffer sous l'action directe des micro¬ ondes .The solvent is vaporized either by direct absorption by the latter of microwave energy if said solvent is polar, or, if it is not sufficiently polar, by heat conduction via an element heated by the microwave energy, such as the container, the sample or any other element capable of heating under the direct action of microwaves.
Le robinet 142 du réservoir 140 est alors en position fermée. Ainsi, lorsque le niveau de solvant S dans le réservoir 140 est suffisamment haut, le solvant s'écoule le long de la tige 110 pour redescendre dans la cartouche 120 via un conduit central 111' prévu dans le système de verrouillage 112 et le support 111, et s'écouler au travers αe la paroα poreuse de ladite cartouche, αans le fond du récipient 1.The valve 142 of the reservoir 140 is then in the closed position. Thus, when the level of solvent S in the reservoir 140 is sufficiently high, the solvent flows along the rod 110 to descend into the cartridge 120 via a central conduit 111 'provided in the locking system 112 and the support 111 , and flow through the porous wall of said cartridge, into the bottom of container 1.
Apres l'étape d'extraction, vient l'étape de rinçage du sédiment contenu dans la cartouche. Lors de cette étape, on positionne la tige 110 en position haute de sorte que la cartouche 120 se trouve au-dessus du solvant S et on continue à appliquer au niveau du fond du récipient 1, le champ micro-ondes de même puissance, de sorte que le solvant continue à se vaporiser et à se recondenser au contact du réfrigérant 144 dans le réservoir 140 avec son robinet 142 fermé.After the extraction step, comes the step of rinsing the sediment contained in the cartridge. During this step, the rod 110 is positioned in the high position so that the cartridge 120 is above the solvent S and we continue to apply at the bottom of the container 1, the microwave field of the same power, of so that the solvent continues to vaporize and recondense on contact with the refrigerant 144 in the reservoir 140 with its tap 142 closed.
Les gouttelettes de solvant recondensées et récupérées dans le réservoir, glissent le long de la tige et viennent rincer le sédiment présent dans la cartouche 120 relevée.The solvent droplets recondensed and recovered in the tank, slide along the rod and rinse the sediment present in the raised cartridge 120.
A cet effet, selon une variante de réalisation non représentée, il peut être prévu que la cartouche soit placée dans un panier à paroi étanche, fixé à l'extrémité de la tige, de sorte qu'il subsiste entre ladite paroi étanche et ladite cartouche, un interstice dans lequel s'écoule le solvant qui traverse la cartouche, ledit panier comprenant en partie supérieure un système de déversement de solvant en cas de trop plein. Ainsi, lors de l'étape de rinçage le solvant reste en contact plus longtemps avec ladite cartouche et on améliore le rinçage du sédiment.To this end, according to an alternative embodiment not shown, it can be provided that the cartridge is placed in a basket with a sealed wall, fixed at the end of the rod, so that it remains between said sealed wall and said cartridge. , a gap in which the solvent flows through the cartridge, said basket comprising in the upper part a system for discharging solvent in the event of an overflow. Thus, during the rinsing step the solvent remains in contact longer with said cartridge and the rinsing of the sediment is improved.
La figure 2c représente l'étape suivante qui est une étape de reconcentration de l'extrait se trouvant dans le récipient.Figure 2c shows the next step which is a step of reconcentrating the extract in the container.
Lors de cette étape, la cartouche 120 est toujours positionnée en position haute, c'est-à-dire au-dessus du solvant .During this step, the cartridge 120 is always positioned in the high position, that is to say above the solvent.
On ouvre alors le robinet 142 et on applique un champ micro-ondes de même puissance sur le fond du récipient 1.The tap 142 is then opened and a microwave field of the same power is applied to the bottom of the container 1.
Le solvant se vaporise et se recondense dans le réservoir 140 sous l'action du réfrigérant 144, puis s'écoule via le robinet 142 au travers d'une tubulure 2 raccordée audit robinet, de façon a être récupéré dans un récipient gradué 3.The solvent vaporizes and recondenses in the reservoir 140 under the action of the refrigerant 144, then flows via the tap 142 through a tube 2 connected to said tap, so as to be collected in a graduated container 3.
Lorsque le solvant est totalement évaporé et restent dans le fond du récipient 1 les composés extraits On notera, qu'à l'aide du dispositif 100 représenté sur les figures 2a à 2c avec un réservoir 140 pourvu dans son fond d'un robinet 142, l'opération d' évaporation du solvant pour la reconcentration de l'extrait s'effectue sans retirer la cartouche du récipient.When the solvent is completely evaporated and the bottom of the container 1 remains the extracted compounds It will be noted that, using the device 100 shown in FIGS. 2a to 2c with a reservoir 140 provided at its bottom with a tap 142, the operation of evaporation of the solvent for the reconcentration of the extract s' without removing the cartridge from the container.
L'utilisation du réservoir avec un robinet prévu dans son fond, permet alors de recycler le solvant utilisé pour l'extraction. Il est à noter qu'il n' y a pas de contrôle visuel direct de l' évaporation du solvant dans le récipient.The use of the tank with a tap provided in its bottom, then makes it possible to recycle the solvent used for the extraction. It should be noted that there is no direct visual control of the evaporation of the solvent in the container.
Toutefois, comme le solvant est récupéré dans un récipient gradué 3, si on connaît le volume du solvant introduit initialement dans le récipient, il est possible de connaître approximativement la quantité de solvant évaporée.However, since the solvent is collected in a graduated container 3, if the volume of the solvent initially introduced into the container is known, it is possible to know approximately the quantity of solvent evaporated.
Il est à noter que la tige, le réservoir, la paroi cylindrique et le conduit de raccordement sont réalisés soit en verre, soit en polytétrafluoréthylène ou encore en quartz par exemple. Selon les modes de réalisation des figures 1 et 2, la tige en verre est une tige pleine.It should be noted that the rod, the reservoir, the cylindrical wall and the connection conduit are made either of glass, or of polytetrafluoroethylene or else of quartz for example. According to the embodiments of Figures 1 and 2, the glass rod is a solid rod.
Selon une variante de réalisation non représentée, la tige pleine est remplacée par un fil, qui peut être automatiquement enroulé et déroule a l'extérieur du dispositif pour permettre sa descente et sa montée αans ledit récipient.According to an alternative embodiment not shown, the solid rod is replaced by a wire, which can be automatically wound and unrolls outside the device to allow it to descend and rise αans said container.
L'adaptation du système réfrigérant 144 sur le rodage prévu dans l'ouverture supérieure du réservoir doit être telle qu'une bonne étancheite est respectée et le réfrigérant ne se trouve pas en contact avec les parois du réservoir a solvant.The adaptation of the refrigerant system 144 to the running-in provided in the upper opening of the tank must be such that good tightness is observed and the refrigerant is not in contact with the walls of the solvent tank.
Sur les figures 3a à 3c, on a représenté trois étapes de fonctionnement d'un deuxième mode de réalisation au dispositif d'extraction 100 selon 1' invention. Selon ce mode de réalisation, il est prévu que le réservoir 140 et le conduit de raccordement 150 forment une seule pièce qui se présente sous la forme d'un coude. La partie supérieure du coude constitue le réservoir 140 et la partie inférieure du coude constitue le conduit de raccordement 150. Ici, le réservoir 140 ne comporte pas de robinet dans son fond.In FIGS. 3a to 3c, three stages of operation of a second embodiment have been shown in the extraction device 100 according to the invention. According to this embodiment, provision is made for the reservoir 140 and the connection conduit 150 to form a single piece which is in the form of an elbow. The upper part of the elbow constitutes the reservoir 140 and the lower part of the elbow constitutes the conduit of connection 150. Here, the reservoir 140 does not have a tap at its bottom.
La tige 110 est une tige creuse. La paroi cylindrique 130 et le récipient 101 forment une seule pièce. Bien entendu, selon une variante de réalisation, on peut prévoir que ces deux éléments soient deux pièces différentes couplées entre-elles.The rod 110 is a hollow rod. The cylindrical wall 130 and the container 101 form a single piece. Of course, according to an alternative embodiment, it can be provided that these two elements are two different parts coupled together.
Sur la figure 3a, on a représenté l'extraction proprement dite des composés organiques polycycliques contenus dans la matrice positionnée dans la cartouche 120, sous l'action du champ micro-ondes appliqué au fond du récipient 1 qui contient la cartouche 120 positionnée en position basse au bout de la tige 110 de telle sorte qu'elle baigne dans le solvant S. Le champ micro-ondes est par exemple d'une puissance de 30 W. Sous l'action du chauffage micro¬ ondes, le solvant S se vaporise et les vapeurs de solvant montent dans le réservoir 140 ou elles se recondensent. Les gouttelettes de solvant recondensées retombent alors via le conduit de raccordement 150 dans le récipient en coulant le long de la tige 110 peur passer au travers de la cartouche 120 et arriver jusqu'au fond du récipient.FIG. 3a shows the actual extraction of the polycyclic organic compounds contained in the matrix positioned in the cartridge 120, under the action of the microwave field applied to the bottom of the container 1 which contains the cartridge 120 positioned in position low at the end of the rod 110 so that it bathes in the solvent S. The microwave field is for example of a power of 30 W. Under the action of microwave heating, the solvent S vaporizes and the solvent vapors rise in the reservoir 140 or they recondense. The recondensed solvent droplets then fall via the connection duct 150 into the container, flowing along the rod 110 to pass through the cartridge 120 and reach the bottom of the container.
A la fin de cette étape d' extraction proprement dite, comme le montre plus particulièrement la figure 3b, la tige 110 est relevée en position haute de sorte que la cartouene 120 se place au-dessus de la quantité de solvant S contenue dans le fond du récipient 1, alors que l'on continue d'appliquer au solvant S se trouvant dans le fond du récipient 1 le champ micro-ondes. Cette étape représentée sur la figure 3b, est l'étape de rinçage. Sous l'action au champ micro-ondes, le solvant S chauffé s'évapore et monte jusque dans le réservoir 140 via le conduit de raccordement 150.At the end of this extraction step proper, as shown more particularly in FIG. 3b, the rod 110 is raised in the high position so that the cartridge 120 is placed above the quantity of solvent S contained in the bottom of container 1, while the solvent field S at the bottom of container 1 is continued to apply the microwave field. This step shown in Figure 3b is the rinsing step. Under the action in the microwave field, the heated solvent S evaporates and rises to the reservoir 140 via the connection conduit 150.
Les gouttelettes de solvant recondensées par l'intermédiaire du réfrigérant 144 glissent via le conduit de raccordement 150, le long de la tige 110 et viennent rincer le sédiment se trouvant dans la cartouche 120 relevée, avant de retomber dans le fond du récipient 1. A la fin de cette étape de rinçage, contrairement à la variante de réalisation représentée sur la figure 2, la cartouche 120 est alors retirer du récipient 1.The solvent droplets recondensed via the refrigerant 144 slide via the connection duct 150, along the rod 110 and rinse the sediment located in the raised cartridge 120, before falling back into the bottom of the container 1. At the end of this rinsing step, unlike the alternative embodiment shown in FIG. 2, the cartridge 120 is then removed from the container 1.
Vient alors l'étape de reconcentration de l'extrait représentée sur la figure 3c, la tige 110 ne comportant plus à son extrémité engagée dans le récipient 1, la cartouche.Then comes the step of reconcentrating the extract shown in FIG. 3c, the rod 110 no longer comprising at its end engaged in the container 1, the cartridge.
Lors de cette étape de reconcentration de l'extrait, on applique un champ micro-ondes sur le fond de récipient 1 et on introduit par l'intérieur de la tige 110 selon la flèche A, un flux d'azote.During this step of reconcentrating the extract, a microwave field is applied to the bottom of the container 1 and a flow of nitrogen is introduced from the inside of the rod 110 according to arrow A.
Ainsi, les vapeurs de solvant formées sous le chauffage micro-ondes, sont évacuées vers le conduit de raccordement 150 et aspirées selon la flèche B à l'aide d'une hotte aspirante positionnée dans l'ouverture supérieure du réservoir.Thus, the solvent vapors formed under the microwave heating, are evacuated towards the connection duct 150 and sucked in according to arrow B with the aid of an extractor hood positioned in the upper opening of the tank.
L' évaporation assistée par flux d'azote permet de reconcentrer l'extrait E directement à l'intérieur du récipient et l'on supprime alors l'étape de reconcentration par évaporateur rotatif effectué à l'aide d'un dispositif selon l'état de la technique.The evaporation assisted by nitrogen flow makes it possible to reconcentrate the extract E directly inside the container and the step of reconcentration by rotary evaporator carried out using a device according to the state is then eliminated. of technique.
On notera que dans les modes de réalisation présentés sur les figures 1, 2a a 2c et 3a a 3c, il peut être prévu avantageusement un oarreau en matériau magnétique positionné soit dans le fond du récipient (1) , soit dans la cartouche (120) . Ce oarreau magnétique est agite par l'intermédiaire d'un système d'agitation par attraction magnétique placé en-dessous du récipient (1) .It will be noted that in the embodiments presented in FIGS. 1, 2a to 2c and 3a to 3c, it can advantageously be provided with a bar of magnetic material positioned either in the bottom of the container (1) or in the cartridge (120) . This magnetic rod is agitated by means of a stirring system by magnetic attraction placed below the container (1).
Un tel barreau magnétique d'agitation permet une homogénéisation de l'échantillon et du solvant pendant l'étape d'extraction. En outre, grâce a l'agitation du barreau magnétique, on augmente durant l'étape d'extraction la surface de contact et d'échange entre l'échantillon contenant les composes a extraire et le soldant. Ainsi, on diminue la durée de l'extraction tout en maintenant un bon rendement d'extraction. L'agitation permet d'éviter avantageusement les phénomènes éventuels de sur-ébullition du solvant chauffe lors de l'extraction, une telle sur-ébullition provoquant une O 97/44109 PC17FR97/00883 brusque remontée malencontreuse du solvant dans le récipient. Le barreau magnétique peut enfin de manière avantageuse absorber une quantité non négligeable d' énergie micro-ondes et chauffer par conduction un solvant plus ou moins transparent aux micro-ondes.Such a magnetic stirring bar allows homogenization of the sample and of the solvent during the extraction step. In addition, thanks to the stirring of the magnetic bar, the contact and exchange surface between the sample containing the compounds to be extracted and the solution is increased during the extraction step. Thus, the duration of the extraction is reduced while maintaining a good extraction yield. Agitation advantageously avoids the possible phenomena of over-boiling of the heated solvent during extraction, such over-boiling causing a O 97/44109 PC17FR97 / 00883 sudden unwanted rise of the solvent in the container. Finally, the magnetic bar can advantageously absorb a non-negligible amount of microwave energy and heat by conduction a solvent more or less transparent to microwaves.
Un test d'extraction avec le deuxième mode de réalisation du dispositif d'extraction (représenté sur les figures 3a à 3c) a été réalisé sur une matrice sédimentaire (SRM 1941a) dont on connaît parfaitement les concentrations en composés aromatiques polycycliques (Papineau, 1995) .An extraction test with the second embodiment of the extraction device (represented in FIGS. 3a to 3c) was carried out on a sedimentary matrix (SRM 1941a) for which the concentrations of polycyclic aromatic compounds are well known (Papineau, 1995 ).
Les résultats sont présentes sur l'histogramme de la figure 4 ou l'on voit apparaître les concentrations certifiées, les concentrations obtenues a l'aide d'un dispositif d'extraction classique par micro-ondes et les concentrations obtenues à l'aide du prototype correspondant au deuxième mode de réalisation du dispositif d'extraction selon l'invention (figures 3a a 3c) . On peut constater sur la figure 4 que le rendement d'extraction des composés recherches est quasiment identique avec les deux dispositifs d'extraction précités .The results are shown on the histogram of FIG. 4 where the certified concentrations appear, the concentrations obtained using a conventional microwave extraction device and the concentrations obtained using the prototype corresponding to the second embodiment of the extraction device according to the invention (Figures 3a to 3c). It can be seen in FIG. 4 that the extraction yield of the researched compounds is almost identical with the two abovementioned extraction devices.
Ainsi, avec le dispositif d'extraction selon l'invention qui permet la mise en oeuvre d'un procède d'extraction allège, l'étape de filtration étant éliminée et l'étape de reconcentration de l'extrait se réalisant en une plus courte durée, on obtient des rendements similaires a ceux obtenus par la méthode d'extraction sous micro-ondes classique.Thus, with the extraction device according to the invention which allows the implementation of a lightened extraction process, the filtration step being eliminated and the step of reconcentrating the extract being carried out in a shorter duration, yields similar to those obtained by the conventional microwave extraction method are obtained.
Sur la figure 5, on a représente une installation 1000 d'extraction de type Soxlhet de composes organiques d'un échantillon.In Figure 5, there is shown an installation 1000 of Soxlhet type extraction of organic compounds from a sample.
Cette mstai-ation comprend un récipient 1001 se présentant sous la forre d'un ballon contenant un solvant d' extraction chauffe par des moyens de chauffage traditionnel 1002. On entend par moyens de cnauffage traditionnel, une plaque chauffante électrique ou à gaz par exemple. Cette installation 1000 comporte en outre des moyens 1003 pour émettre des micro-ondes, par exemple un magnétron, dans une cavité d'application 1100 des micro-ondes. Cette cavité d'application 1100 est délimitée par une paroi supérieure 1110, une paroi latérale 1120 cylindrique et une paroi inférieure 1130.This mstai-ation comprises a container 1001 in the form of a balloon containing an extraction solvent heated by conventional heating means 1002. By conventional cnauffage means means an electric or gas heating plate for example. This installation 1000 further comprises means 1003 for emitting microwaves, for example a magnetron, in a cavity 1100 for applying microwaves. This application cavity 1100 is delimited by an upper wall 1110, a cylindrical side wall 1120 and a lower wall 1130.
La paroi supérieure 1110 de ladite cavité 1100 est pourvue d'une ouverture 1111 qui est bordée d'une cheminée 1112 dont la hauteur H fonction de la section de l'ouverture 1111 et de la fréquence d'émission des micro- ondes dans ladite cavité, est telle que ladite cheminée forme barrière à la propagation des micro-ondes hors de la cavité.The upper wall 1110 of said cavity 1100 is provided with an opening 1111 which is bordered by a chimney 1112 whose height H depends on the section of the opening 1111 and on the frequency of emission of microwaves in said cavity , is such that said chimney forms a barrier to the propagation of microwaves out of the cavity.
Cette ouverture 1111 permet l'introduction dans ladite cavité d'application 1100 d'un matras 1 couplé à un dispositif d'extraction 100 selon l'invention.This opening 1111 allows the introduction into said application cavity 1100 of a flask 1 coupled to an extraction device 100 according to the invention.
Selon le mode de réalisation représenté, ce dispositif d'extraction 100 est celui représenté plus particulièrement sur les figures 2a à 2c.According to the embodiment shown, this extraction device 100 is that shown more particularly in FIGS. 2a to 2c.
La partie supérieure de la paroi cylindrique 110 du dispositif d'extraction 100, raccordée par ledit conduit de raccordement 150 audit réservoir 1-0, est située à l'extérieur de la cavité d'application, et en particulier à l'extérieur de la cheminée 1112.The upper part of the cylindrical wall 110 of the extraction device 100, connected by said connection duct 150 to said reservoir 1-0, is located outside the application cavity, and in particular outside the fireplace 1112.
La parti inférieure 1130 de ladite cavité d'application des micro-ondes 1100 coτprend un orifice 1131 bordé également d'une cheminée 1132 dont la hauteur H qui est fonction de la fréquence d'émission des micro¬ ondes et de la section de l'orifice 1131, est telle que ladite cheminée forme barrière à la propagation des micro-ondes vers l'extérieur de la cavité. L'orifice 1131 autorise le passage d'une première tubulure extérieure 1004 qui raccorde le fond du matras 1 audit récipient 1001 contenant le solvant.The lower part 1130 of said microwave application cavity 1100 includes an orifice 1131 also bordered by a chimney 1132 whose height H which is a function of the frequency of emission of the microwaves and of the section of the orifice 1131, is such that said chimney forms a barrier to the propagation of microwaves towards the outside of the cavity. The orifice 1131 allows the passage of a first external tube 1004 which connects the bottom of the flask 1 to said container 1001 containing the solvent.
Comme cela est représente sur la figure 5, cette première tubu_-re extérieure 1004 présente la forme d'un siphon.As shown in Figure 5, this first outer tubu_ re 1004 has the shape of a siphon.
En outre, il est prévu entre le réservoir 140 du dispositif d'extraction 100 et le récipient contenant le solvant 1101 une deuxième tubulure extérieure 1005. Cette deuxième tubulure extérieure s'adapte sur le robinet 142 du réservoir 140 et débouche à l'intérieur du récipient à solvant 1001.In addition, there is provided between the reservoir 140 of the extraction device 100 and the container containing the solvent 1101 a second external tube 1005. This second external tube fits on the valve 142 of the reservoir 140 and opens into the interior of the solvent container 1001.
Le mode de fonctionnement de cette installation est le suivant.The operating mode of this installation is as follows.
Par l'intermédiaire de la plaque chauffante 1002, on chauffe le solvant se trouvant dans le récipient à solvant 1001 qui s'évapore et circule dans la deuxième tubulure de raccordement 1005 pour arriver jusqu'au réservoir 140 où il se recondense en venant au contact du réfrigérant 144.Via the heating plate 1002, the solvent in the solvent container 1001 is heated, which evaporates and circulates in the second connection tube 1005 to reach the reservoir 140 where it recondenses when it comes into contact. refrigerant 144.
Lorsque le niveau de solvant dans le réservoir 140 est suffisamment élevé, les gouttelettes de solvant recondensées glissent via le conduit de raccordement 150 le long de la tige 110 de façon à traverser la cartoucheWhen the solvent level in the reservoir 140 is sufficiently high, the recondensed solvent droplets slide via the connection conduit 150 along the rod 110 so as to pass through the cartridge
120 et à remplir le fond du matras 1.120 and fill the bottom of the flask 1.
Le fond du matras 1 étant chauffé par ailleurs par le chauffage micro-ondes dans la cavité d'application des micro-ondes, le solvant se trouvant dans ce matras se vaporise à nouveau et vient se recondenser dans le réservoir 140 avant de recouler via le conduit de raccordement 150 et la tige 110 dans le fond du matras 1 en traversant la cartouche 120.The bottom of the flask 1 being further heated by microwave heating in the microwave application cavity, the solvent in this flask vaporizes again and is recondensed in the reservoir 140 before flowing through the connection duct 150 and the rod 110 in the bottom of the flask 1 while crossing the cartridge 120.
La partie du solvant chargée en composés extraits qui ne se vaporise pas s'écoule du fond du matras 1 vers la première tubulure αe raccordement 1004 jusqu'à ce que le niveau dans cette tubulure monte. Le niveau du solvant dans la tubulure augmente jusqu'à ce qu'elle atteigne le coude du siphon pour retomber alors dans le récipient à solvant 1001.The part of the solvent loaded with extracted compounds which does not vaporize flows from the bottom of the flask 1 to the first connection tubing 1004 until the level in this tubing rises. The level of the solvent in the tubing increases until it reaches the elbow of the siphon and then falls back into the solvent container 1001.
Dans cette installation 1000, l'extraction est réalisée par l'intermédiaire d'un solvant vaporisé, reconαensé puis revaporisé et recondensé. Deux sources de chaleur sont utilisées, une source traditionnelle et une source de chaleur sous micro-ondes, pour réaliser l' extraction.In this installation 1000, the extraction is carried out by means of a vaporized solvent, reconαensed then revaporized and recondensed. Two sources of heat are used, a traditional source and a source of heat under microwaves, to carry out the extraction.
Le chauffage sous micro-ondes du solvant qui traverse la cartouche, permet d'augmenter la rapidité de l'extraction des comDosés . Grâce à cette installation, il est possible de mieux contrôler l'opération d'extraction en faisant varier le chauffage traditionnel, le chauffage micro¬ ondes et le solvant utilisé. Pour une puissance donnée des micro-ondes, en choisissant un solvant plus ou moins transparent aux micro-ondes, il est possible de chauffer plus ou moins ledit solvant lors de son passage dans la cavité micro-ondes et par ce biais, faire varier le temps et la qualité d'extraction de l'échantillon placé dans la cartouche.Heating the microwave solvent that passes through the cartridge, increases the speed of extraction of comDosés. Thanks to this installation, it is possible to better control the extraction operation by varying the traditional heating, the microwave heating and the solvent used. For a given microwave power, by choosing a solvent more or less transparent to microwaves, it is possible to more or less heat said solvent during its passage through the microwave cavity and by this means, vary the time and quality of extraction of the sample placed in the cartridge.
Il est à noter en effet, que le chauffage traditionnel permet de chauffer des solvants plus ou moins transparents aux micro-ondes qui, a priori, seraient plutôt mal chauffés par une seule source de chaleur micro-ondes.It should be noted, in fact, that traditional heating makes it possible to heat more or less transparent solvents in the microwave which, a priori, would be rather badly heated by a single source of microwave heat.
Enfin, grâce à cette installation, on peut piloter l'extraction, en comptant le nombre de déversement de la tubulure en forme de siphon, chaque déversement correspondant à un cycle d'extraction. La présente invention n'est nullement limitée aux modes de réalisation décrits et représentes, mais l'homme du métier pourra y apporter toute variante conforme a son esprit. Finally, thanks to this installation, it is possible to control the extraction, by counting the number of spills of the siphon-shaped tubing, each spill corresponding to an extraction cycle. The present invention is in no way limited to the embodiments described and shown, but a person skilled in the art can make any variant which conforms to his spirit.

Claims

REVENDICATIONS
1.Dispositif (100) d'extraction par l'intermédiaire d'un solvant, de composés organiques d'un échantillon, couplé à un récipient (1) contenant ledit solvant et soumis à un chauffage micro-ondes, caractérisé en ce qu' il comprend :1. Device (100) for extracting, via a solvent, organic compounds from a sample, coupled to a container (1) containing said solvent and subjected to microwave heating, characterized in that He understands :
- un organe de forme allongée, portant à une extrémité engagée dans le récipient (1) une cartouche (120) renfermant l'échantillon à traiter,- an elongated member, carrying at one end engaged in the container (1) a cartridge (120) containing the sample to be treated,
- une paroi cylindrique (130) fermée supérieurement, qui entoure une partie dudit organe allongé émergeante du récipient (1) de sorte qu'un passage annulaire de vapeur (131) est délimité entre eux, la partie inférieure de ladite paroi cylindrique (130) débouchant oe manière étanche dans le récipient (1),- a cylindrical wall (130) closed above, which surrounds a part of said elongated member emerging from the container (1) so that an annular vapor passage (131) is delimited between them, the lower part of said cylindrical wall (130) opening in a sealed manner into the container (1),
- un réservoir (140) a solvant comportant une ouverture supérieure (141) pour la mise en place d'un système réfrigérant ou d'un système d'aspiration des vapeurs,- a solvent tank (140) having an upper opening (141) for the installation of a refrigerant system or a vapor suction system,
- un conduit de raccordement (150) qui s'étend à partir de l'intérieur du réservoir (140) suivant une direction (Y) inclinée vers le bas, vers leαit organe allongé pour déboucher dans ledit passage annulaire de vapeur (131) et venir au contact duαit organe allonge.a connection conduit (150) which extends from the interior of the reservoir (140) in a direction (Y) inclined downward, towards the elongated member to open into said annular vapor passage (131) and come into contact with the elongated organ.
2. Dispositif selon la revendication 1, caractérise en ce que l'organe allonge est morte mobile a coulissement selon son axe vertical (X) a l'intérieur dudit récipient (P . 2. Device according to claim 1, characterized in that the elongate member is dead mobile sliding along its vertical axis (X) inside said container (P.
3. Dispositif selon l'une des revendications 1 ou 2, caractérise en ce que la paroi cylindrique (130) et le conduit de raccordement (150) forment une seule pièce.3. Device according to one of claims 1 or 2, characterized in that the cylindrical wall (130) and the connection conduit (150) form a single piece.
4.Dispositif selon l'une des revendications 1 ou 2, caractérise en ce que le réservoir ( 140) et le conduit de raccordement (150) forment une seule pièce.4.Dispositif according to one of claims 1 or 2, characterized in that the tank (140) and the connection conduit (150) form a single piece.
5. Dispositif selon la revendication 4, caractérisé en ce que ladite paroi cylindrique (130) or le récipient (1) forment une seule pièce. 5. Device according to claim 4, characterized in that said cylindrical wall (130) o r the container (1) form a single piece.
6.Dispositif selon l'une des revendications 4 ou 5, caractérisé en ce que ladite pièce unique constituant le réservoir (140) et le conduit de raccordement (150) est en forme de coude, la partie supérieure du coude constituant ledit réservoir (140) et la partie inférieure du coude constituant ledit conduit de raccordement (150) . 6.A device according to one of claims 4 or 5, characterized in that said single piece constituting the reservoir (140) and the connection conduit (150) is in the form of an elbow, the upper part of the elbow constituting said reservoir (140 ) and the lower part of the elbow constituting said connection conduit (150).
7.Dispositif selon la revendication 6, caractérisé en ce que l'organe de forme allongée est une tige (110) creuse. 7. Device according to claim 6, characterized in that the elongate member is a hollow rod (110).
8.Dispositif selon l'une des revendications 1 à 5, caractérisé en ce que le réservoir (140) comporte dans son fond un robinet ou une électrovanne (142) pour la récupération à l'extérieur du solvant présent dans ledit réservoir (140) . 8. Device according to one of claims 1 to 5, characterized in that the reservoir (140) comprises in its bottom a tap or a solenoid valve (142) for the recovery outside of the solvent present in said reservoir (140) .
9. Dispositif selon la revendication 8, caractérisé en ce que l'organe de forme allongée est une tige (110) pleine .9. Device according to claim 8, characterized in that the elongate member is a rod (110) full.
10. Dispositif selon la revendication 8, caractérisé en ce que l'organe de forme allongée est un fil.10. Device according to claim 8, characterized in that the elongate member is a wire.
11.Dispositif selon l'une des revendications 1 à 9, caractérisé en ce que la paroi cylindrique (130) comporte un bord d'extrémité supérieur qui délimite une ouverture (132) dans laquelle vient s'adapter un bouchon de fermeture ( 160) dans lequel est montée de manière étanche ladite tige (110) .11. Device according to one of claims 1 to 9, characterized in that the cylindrical wall (130) has an upper end edge which delimits an opening (132) in which is fitted a closure plug (160) in which said rod (110) is mounted in leaktight manner.
12. Dispositif selon l'une des revendications 1 à 9 , caractérisé en ce que l'organe allongé, la paroi cylindrique (130), le réservoir (140) et le conduit de raccordement (150) sont réalisés en verre.12. Device according to one of claims 1 to 9, characterized in that the elongated member, the cylindrical wall (130), the reservoir (140) and the connection conduit (150) are made of glass.
13. Dispositif selon l'une des revendications 1 à13. Device according to one of claims 1 to
12, caractérisé en ce qu'il est prévu dans le fond du récipient (1) ou dans la cartouche (120] , un barreau en matériau magnétique agité par l'intermédiaire d'un système d'agitation par attraction magnétique placé en dessous dudit récipient (1) .12, characterized in that there is provided in the bottom of the container (1) or in the cartridge (120], a bar of magnetic material stirred by means of a stirring system by magnetic attraction placed below said container (1).
14. Dispositif selon l'une des revendications 1 à14. Device according to one of claims 1 to
13, caractérisé en ce que la cartouche est placée dans un panier à paroi étanche, de sorte qu'il subsiste entre ladite paroi étanche et ladite cartouche, un interstice dans lequel s'écoule le solvant qui traverse la cartouche, ledit panier étant pourvu en partie supérieure d'un système de déversement du solvant vers ledit récipient en cas de trop plein.13, characterized in that the cartridge is placed in a basket with a tight wall, so that it remains between said sealed wall and said cartridge, a gap in which the solvent flows through the cartridge, said basket being provided at the top with a system for discharging the solvent towards said container in the event of an overflow.
15.Installation (1000) d'extraction de type Soxlhet de composés organiques d'un échantillon, qui comprend un récipient (1001) contenant un solvant d'extraction chauffé par des moyens de chauffage traditionnel (1002), caractérisée en ce qu'elle comporte des moyens (1003) pour émettre des micro-ondes dans une cavité d'application (1100) délimitée par une paroi supérieure15. Installation (1000) of Soxlhet type extraction of organic compounds from a sample, which comprises a container (1001) containing an extraction solvent heated by traditional heating means (1002), characterized in that it comprises means (1003) for emitting microwaves into an application cavity (1100) delimited by an upper wall
(1110) , une paroi latérale (1120) et une paroi inférieure(1110), a side wall (1120) and a bottom wall
(1130) , la paroi supérieure (1110) de ladite cavité (1100) étant pourvue d'une ouverture (1111) , bordée d'une cheminée (1112) formant barrière a la propagation vers l'extérieur des micro-ondes, pour l'introduction dans ladite cavité d'application (1100) d'un matras (1) couple à un dispositif d'extraction (100) selon l'une des revendications 1 à 14, de telle sorte que la partie supérieure de ladite paroi cylindrique (110) raccordée par ledit conduit de raccordement (150 audit réservoir(1130), the upper wall (1110) of said cavity (1100) being provided with an opening (1111), bordered by a chimney (1112) forming a barrier to the propagation towards the outside of microwaves, for the introduction into said application cavity (1100) of a flask (1) coupled to an extraction device (100) according to one of claims 1 to 14, so that the upper part of said cylindrical wall ( 110) connected by said connection conduit (150 to said tank
(140) dudit dispositif d'extraction, se situe a l'extérieur de ladite cavité d'application des micro- ondes (1100), et ladite paroi inférieure (1130) de ladite cavité (1100) comprenant un orifice (1131) , borαe d'une cheminée (1132) formant barrière a la propagation vers l'extérieur des micro-ondes, autorisant le passage d'une première tubulure extérieure (1004j qui raccorde le fond dudit matras (1) audit récipient (1001) de solvant, cette première tubulure extérieure ( 1004) présentant une forme de siphon, une deuxième tubulure extérieure (1005) étant prévue pour raccorder le réservoir (140' dudit dispositif d'extraction (100) au récipient de solvant (1001) . (140) of said extraction device, is located outside of said microwave application cavity (1100), and said bottom wall (1130) of said cavity (1100) comprising an orifice (1131), borαe a chimney (1132) forming a barrier to the propagation towards the outside of microwaves, authorizing the passage of a first external tube (1004j which connects the bottom of said flask (1) to said container (1001) of solvent, this first external tube (1004) having a siphon shape, a second external tube (1005) being provided for connecting the reservoir (140 'of said extraction device (100) to the solvent container (1001).
PCT/FR1997/000883 1996-05-20 1997-05-20 Device and installation for microwave extracting of organic compounds from a sample WO1997044109A1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CA002256032A CA2256032A1 (en) 1996-05-20 1997-05-20 Device and installation for microwave extracting of organic compounds from a sample
EP97925106A EP0907394A1 (en) 1996-05-20 1997-05-20 Device and installation for microwave extracting of organic compounds from a sample
JP09541714A JP2000510765A (en) 1996-05-20 1997-05-20 Apparatus and equipment for extracting organic compounds from samples by adding microwaves

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US1904096P 1996-05-20 1996-05-20
US60/019,040 1996-05-20

Publications (1)

Publication Number Publication Date
WO1997044109A1 true WO1997044109A1 (en) 1997-11-27

Family

ID=21791115

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/FR1997/000883 WO1997044109A1 (en) 1996-05-20 1997-05-20 Device and installation for microwave extracting of organic compounds from a sample

Country Status (5)

Country Link
EP (1) EP0907394A1 (en)
JP (1) JP2000510765A (en)
KR (1) KR20000015867A (en)
CA (1) CA2256032A1 (en)
WO (1) WO1997044109A1 (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2212748A1 (en) * 2003-01-14 2004-07-16 Universidad De Cordoba Device for the microwave-accelerated extraction of components of solid samples and applications thereof
EP1593952A1 (en) * 2004-05-05 2005-11-09 C. Gerhardt Fabrik und Lager chemischer Apparate GmbH & Co. KG Apparatus and method for discontinuous hydrolysis
WO2008089937A2 (en) * 2007-01-22 2008-07-31 Milestone S.R.L. Microwave integrated soxhlet
WO2008089943A1 (en) * 2007-01-22 2008-07-31 Milestone S.R.L. Microwave hydrodiffusion for isolation of natural products
WO2019106313A1 (en) * 2017-12-01 2019-06-06 Université D'avignon Et Des Pays De Vaucluse Device for extracting and separating volatile and non-volatile compounds from a biological material, and associated process
US20210284928A1 (en) * 2016-12-01 2021-09-16 Natural Extraction Systems, LLC Rapid botanical oil distillation device utilizing microwave agent

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100556354B1 (en) * 2002-09-30 2006-03-03 엘지전자 주식회사 refining method for organic matter
JP2007289916A (en) * 2006-03-31 2007-11-08 Tokyo Electric Power Co Inc:The Small extractor
JP4831044B2 (en) * 2007-03-30 2011-12-07 東京電力株式会社 Small extractor for microwave oven
CN101290277B (en) * 2007-04-20 2011-05-11 财团法人食品工业发展研究所 Rapid extraction method utilizing microwave radiation
TW200842336A (en) * 2007-04-26 2008-11-01 Food Industry Res & Dev Inst Microwave accelerating extraction equipment
KR100817536B1 (en) * 2007-10-31 2008-03-27 (주)제네마인 A high performance extractor as possible with ascending and descending extraction
JP4831060B2 (en) * 2007-12-19 2011-12-07 東京電力株式会社 Small extractor for microwave oven
WO2014121814A1 (en) * 2013-02-05 2014-08-14 Foss Analytical Ab Solvent extraction apparatus

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3397115A (en) * 1967-08-07 1968-08-13 Dow Chemical Co Extraction apparatus
FR2252861A1 (en) * 1973-12-04 1975-06-27 Randall Edward Liq and vapour solvent extraction - performed in a single vessel in which the sample container can be positioned above and below solvent surface
US4255386A (en) * 1978-11-30 1981-03-10 The United States Of America As Represented By The Deptartment Of Health, Education And Welfare Method and apparatus for destroying organic matter to facilitate trace inorganic element analysis
US4265860A (en) * 1980-03-27 1981-05-05 J & W Scientific, Incorporated High pressure Soxhlet extractor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3397115A (en) * 1967-08-07 1968-08-13 Dow Chemical Co Extraction apparatus
FR2252861A1 (en) * 1973-12-04 1975-06-27 Randall Edward Liq and vapour solvent extraction - performed in a single vessel in which the sample container can be positioned above and below solvent surface
US4255386A (en) * 1978-11-30 1981-03-10 The United States Of America As Represented By The Deptartment Of Health, Education And Welfare Method and apparatus for destroying organic matter to facilitate trace inorganic element analysis
US4265860A (en) * 1980-03-27 1981-05-05 J & W Scientific, Incorporated High pressure Soxhlet extractor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"Microwave heating accelerates solvent extraction", CHEMICAL ENGINEERING, vol. 102, no. 2, 1 February 1995 (1995-02-01), pages 13, XP000489694 *

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2212748A1 (en) * 2003-01-14 2004-07-16 Universidad De Cordoba Device for the microwave-accelerated extraction of components of solid samples and applications thereof
WO2004062766A1 (en) * 2003-01-14 2004-07-29 Universidad de Córdoba Device for the microwave-accelerated extraction of components of solid samples and applications thereof
EP1593952A1 (en) * 2004-05-05 2005-11-09 C. Gerhardt Fabrik und Lager chemischer Apparate GmbH & Co. KG Apparatus and method for discontinuous hydrolysis
WO2008089937A2 (en) * 2007-01-22 2008-07-31 Milestone S.R.L. Microwave integrated soxhlet
WO2008089943A1 (en) * 2007-01-22 2008-07-31 Milestone S.R.L. Microwave hydrodiffusion for isolation of natural products
EP1955749A1 (en) * 2007-01-22 2008-08-13 Milestone S.r.l. Microwave hydrodiffusion for isolation of natural products
EP1955748A1 (en) * 2007-01-22 2008-08-13 Milestone S.r.l. Microwave integrated soxhlet
WO2008089937A3 (en) * 2007-01-22 2008-09-18 Milestone Srl Microwave integrated soxhlet
US8802021B2 (en) 2007-01-22 2014-08-12 Milestone S.R.L. Microwave integrated Soxhlet
US20210284928A1 (en) * 2016-12-01 2021-09-16 Natural Extraction Systems, LLC Rapid botanical oil distillation device utilizing microwave agent
US11820959B2 (en) * 2016-12-01 2023-11-21 Natural Extraction Systems, LLC Rapid botanical oil distillation device utilizing microwave agent
WO2019106313A1 (en) * 2017-12-01 2019-06-06 Université D'avignon Et Des Pays De Vaucluse Device for extracting and separating volatile and non-volatile compounds from a biological material, and associated process

Also Published As

Publication number Publication date
JP2000510765A (en) 2000-08-22
CA2256032A1 (en) 1997-11-27
EP0907394A1 (en) 1999-04-14
KR20000015867A (en) 2000-03-15

Similar Documents

Publication Publication Date Title
WO1997044109A1 (en) Device and installation for microwave extracting of organic compounds from a sample
CA2019416C (en) Centrifugal separator for congealable liquid, gas-oil for example
EP0180528A2 (en) Method for the medical analysis of a liquid sample by means of at least one liquid reagent, and apparatus for carrying out the method
WO1998057896A1 (en) Installation for producing ozonized water
EP0739483B1 (en) Device for automatically injecting solubilized or diluted products
EP0045247B1 (en) Apparatus for the automatic preparation of samples for analysing
EP2983884A1 (en) Device for treating a solid composite material by solvolysis with a view to extracting fibres from the treated material
EP1144321B1 (en) Method and device for drawing a molten material contained in a crucible
EP3592145A1 (en) System and method for vitrifying a biological substance
BE897901A (en) APPARATUS AND METHOD FOR DEGASSING A LIQUID, PARTICULARLY WATER
CA1251340A (en) Device suitable e.g. for small solid of liquid sample pyrolysis
FR3029629A1 (en) METHOD AND DEVICE FOR SAMPLING SAMPLE IN A LIQUID
EP0017588B1 (en) Electromagnetic device for the separation of inclusions contained in an electrically conductive fluid
FR2709250A1 (en) Device for selecting spermatozoa
FR2570956A1 (en) Process and device allowing two substances to be separated by dissolving
FR2533898A1 (en) Device for the automatic emptying of a container
FR2980262B1 (en) METHOD OF FREEZING A PLURALITY OF PACKAGING TUBES FILLED EACH OF A PREDETERMINED VOLUME OF BIOLOGICAL SUBSTANCE AND SYSTEM FOR IMPLEMENTING SUCH A METHOD
EP0608153A1 (en) Reaction apparatus with automatic dosing system, especially for DNA extraction
FR2691080A1 (en) Superconducting magnetic separator and process for clarifying liquids - used in partic. for removing fine particles from reprocessing liquids, resulting from reprocessing of used nuclear fuel
FR2481325A1 (en) NACELLE USABLE FOR LIQUID-LIQUID MULTILAYER EPITAXIC DEPOSITS AND METHOD OF DEPOSITION INVOLVING SAID NACELLE
WO2005002708A1 (en) Device for the separation of particles contained in a fluid stream and cleaning installation comprising one such separation device
EP4170316A1 (en) Sample collection apparatus and sample collection device
BE516709A (en)
FR2601444A1 (en) Closure for a receptacle fitted with a metering device
FR2545202A1 (en) METHOD AND DEVICE FOR COOLING A MATERIAL AND APPLICATION TO THE PRODUCTION OF REFRACTORY MATERIALS BY TEMPERATURE

Legal Events

Date Code Title Description
WWE Wipo information: entry into national phase

Ref document number: 97195615.4

Country of ref document: CN

AK Designated states

Kind code of ref document: A1

Designated state(s): CA CN JP KR US

AL Designated countries for regional patents

Kind code of ref document: A1

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

DFPE Request for preliminary examination filed prior to expiration of 19th month from priority date (pct application filed before 20040101)
121 Ep: the epo has been informed by wipo that ep was designated in this application
ENP Entry into the national phase

Ref document number: 2256032

Country of ref document: CA

Ref document number: 2256032

Country of ref document: CA

Kind code of ref document: A

WWE Wipo information: entry into national phase

Ref document number: 1019980709417

Country of ref document: KR

WWE Wipo information: entry into national phase

Ref document number: 1997925106

Country of ref document: EP

WWP Wipo information: published in national office

Ref document number: 1997925106

Country of ref document: EP

WWP Wipo information: published in national office

Ref document number: 1019980709417

Country of ref document: KR

WWR Wipo information: refused in national office

Ref document number: 1997925106

Country of ref document: EP

WWW Wipo information: withdrawn in national office

Ref document number: 1997925106

Country of ref document: EP

WWW Wipo information: withdrawn in national office

Ref document number: 1019980709417

Country of ref document: KR