EP1993733B1 - Device, use and method for drawing off a liquid - Google Patents

Device, use and method for drawing off a liquid Download PDF

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Publication number
EP1993733B1
EP1993733B1 EP07731725A EP07731725A EP1993733B1 EP 1993733 B1 EP1993733 B1 EP 1993733B1 EP 07731725 A EP07731725 A EP 07731725A EP 07731725 A EP07731725 A EP 07731725A EP 1993733 B1 EP1993733 B1 EP 1993733B1
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EP
European Patent Office
Prior art keywords
container
needle
liquid
millimeters
blowing means
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EP07731725A
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German (de)
French (fr)
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EP1993733A1 (en
Inventor
Michel Rapaud
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Biomerieux SA
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Biomerieux SA
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/02—Burettes; Pipettes
    • B01L3/021—Pipettes, i.e. with only one conduit for withdrawing and redistributing liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/06—Fluid handling related problems
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/14—Process control and prevention of errors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00—Moving or stopping fluids
    • B01L2400/04—Moving fluids with specific forces or mechanical means
    • B01L2400/0475—Moving fluids with specific forces or mechanical means specific mechanical means and fluid pressure
    • B01L2400/0487—Moving fluids with specific forces or mechanical means specific mechanical means and fluid pressure fluid pressure, pneumatics

Definitions

  • the present invention relates to a device for sampling a liquid in a container, for concentrating the drops of liquid present on the inner wall (s) of the container in the lower part of said container.
  • the present invention also relates to a method of sampling a liquid present in a container using the above device.
  • the present invention finally relates to the use of the above sampling device to control the level of the liquid present in the container.
  • this kind of sampling device simply allows, by contact with the liquid to be taken, either the supply of a liquid of interest that it contains or the withdrawal of another liquid of interest present in a container.
  • Such devices are generally constituted by pipettes or hollow needles associated with pumps. Some more sophisticated allow the cleaning of the outer walls of said pipettes or needles that have been soaked in the liquid taken or having added an additional liquid. This is the case for example in the patent application WO-A-99/27973 filed under priority of November 27, 1997 by the plaintiff.
  • This relates to a method for decontaminating a hollow metal needle for sampling and / or dispensing a contaminating liquid, the needle cooperating with electrical connection means making it possible to establish an electric current in the needle. to decontaminate and preserve the integrity of said needle for reuse. Others are equipped with means avoiding contaminating these outer walls of the sampling elements, as is the case with the patent application.
  • WO-A-99/50674 filed under priority 1 April and 22 June 1998 by the applicant.
  • This application relates to a method of sampling a biological sample via a suction-discharge device, such as a pipette, manual or automatic, incorporated or not to an automaton. But it also relates to a method for detecting the free surface of a biological sample, a sample collection apparatus, such as a pipette, and an apparatus for detecting the free surface of a biological sample.
  • Another problem is the determination of a volume of liquid present in a container. Some checks are sometimes necessary to know exactly the volume of liquid dispensed in a container or series of containers. In this case, it is necessary to know precisely said volume. As a result, the presence of unrecovered or recoverable drop (s) can lead to erroneous values and affect the final result.
  • the present invention proposes to provide a solution to these problems in order to meet the expectations of users.
  • the sampling needle consists of a tube open at both ends; the container for containing the liquid to be taken up consists of a tube of diameter greater than that of the lower end of the needle, open only at its upper end.
  • the blowing means comprise at least one lateral opening to the needle; this / these opening (s) allows (s) sending a flow of air on the inner wall (s) (s) of the container.
  • the sampling needle is in a vertical position.
  • the air flow leaving the lateral openings is oblique and directed from top to bottom.
  • This air flow has an angle relative to the horizontal which is between 10 ° and 80 °, preferably between 20 and 50 °, preferably between 25 and 40 ° and even more preferably 30 °.
  • the blowing means comprise three to twenty, preferably five to twelve and even more preferably eight lateral openings.
  • these lateral openings are radially distributed, positioned in the same plane, preferably horizontally.
  • the sampling device is characterized in that the blowing means comprise a closed sleeve comprising at least one pulsed gas inlet, preferably air.
  • the device is characterized in that the sleeve is a closed tube which wholly or partially surrounds the sampling needle.
  • the three steps of introduction, activation of the blowing means (8) and aspiration are sequential.
  • the introduction step and the activation step of the blowing means are performed simultaneously.
  • the first introduction step and the second activation step are sequential but with a recovery period, the introduction ending when the activation has already begun.
  • sampling device can be used to control the level of the liquid present in a container.
  • figure 11 represents the lower end of the sampling needle according to a second embodiment.
  • the present invention relates to a device for sampling a liquid in a container represented on all Figures 1 to 6 .
  • the Figures 1 to 3 represent the sampling device 1 in the absence of any liquid to be taken.
  • This sampling device 1 is well represented on the Figures 1 and 2 and consists essentially of a sampling needle 4 having a lower free end 5 and an upper end 6, said needle 4 being in a vertical position.
  • a container 3 itself consisting of a tube of diameter greater than that of the lower end 5 of the needle 4, and open at its end upper 11 and closed at its lower end 17, this tube being capable of containing a liquid to be taken.
  • the figure 2 is a sampling device 1 after its introduction along a vertical axis in the container 3, said container 3 of conventional shape having an inner wall 10 and an outer wall, not referenced.
  • the upper end 6 of the sampling needle 4 is connected to suction-discharge means 7 via a hose 13.
  • These means 7, known to those skilled in the art, will not be exposed more before. They may just be constituted by a peristaltic pump, or any other equivalent means, such as time-pressure-depression systems, which are based on the principle of a main reservoir in pressure (or in depression depending on the need of the application whose outlet has a hose provided with a solenoid valve controlled by an electronic device using a time base to perform its switching opening - closing.
  • the initial gas flow therefore comes from the blowing means by the inlet 16, said inlet 16 being connected to the blowing means 8 by a hose 14.
  • the flow of gas from the inlet 16 to the lateral openings 12 is therefore through the closed sleeve 15.
  • the lateral openings 12 are radially implanted on said sleeve 15, in order to improve the efficiency of the device.
  • the assembly of the blowing means therefore consists of the blowing means 8 themselves, the hose 14, the lateral openings 12 and the sleeve 15.
  • Each opening 12 implanted on the sleeve 15 is represented on the detail C of the figure 10 .
  • the diameter 19 of the opening 12 is between 0.1 and 1 millimeter, preferably between 0.3 and 0.6 millimeter, and even more preferably 0.4 millimeter.
  • the pulsed gas flow, according to F4 coming from the openings 12 is in an oblique position relative to the horizontal, and is directed from top to bottom, which makes it possible to concentrate the drops 9 present on the inner and lateral wall 10 (see the figure 4 ), the drops 9 being in a position remote from the lower end 17 of the container 3, and the air flow along F4 directing them towards this lower end 17 of said container 3 as shown in FIGS. Figures 7 to 9 .
  • the angle between the horizontal 20 and the gas flow (F4) coming from the openings 12 is therefore between 10 ° and 80 °, preferably between 20 ° and 50 °, preferably between 25 and 40 °, and even more preferentially 30 °.
  • the sampling device 1 can thus be used to take a liquid 2 contained in a closed container at its upper end, for example by an external aluminum film.
  • the lower free end 5 of the sampling needle 4 is of rounded shape 18 on the outside of the needle 4 so that when the outer film is perforated during the descent of the needle to the container, according to F5 the perforation is clear; this avoids any tearing or punching effect of the outer film.
  • the lower free end 5 of the sampling needle 4 comprises a series of slots 18 arranged radially or radially, the number may vary from 4 to 12 without impacting the sample. In the embodiment this number is 6.
  • the perforation is even sharper; this avoids any tearing or punching effect of the outer film.
  • the sampling with this embodiment is even more effective, because its shape allows the sampling even in tubes, specimen style, the space at the bottom is difficult to access.
  • its outer radius of curvature is adapted to the inner radius of curvature of the bottom of the container.
  • the external radius of curvature of the sampling needle 4 matches the internal radius of curvature of the bottom of the container, that is to say is of slightly smaller radius to allow complete support between the two inner surfaces and external.
  • the diameter of said needle 4 is in the presented embodiment of 3.5 millimeters.
  • Said container 3 can also be directed towards the needle 4 in the direction F6 shown in FIG. figure 6 .
  • the activation of the blowing means 8 causes the creation of a flow of gas along F3 which enters through the inlet 16. This flow of gas flows in the sleeve 15 and leaves it from F4 via the lateral openings 12.
  • the projection of the gas towards the inner wall 10 of the container 3 makes it possible to unhook and thus move, according to F7, and to concentrate towards the lower part 17 of the container 3, the drops of liquid 9 present on said wall 10.
  • the present invention also relates to a sampling method represented on all the Figures 7 to 10 .
  • the step of introducing the needle 4 and the step of activating the blowing means 8 are simultaneous, the descent along F5 of the needle 4 in the container 3 being done at the same time as the arrival of gas, according to F3, in the sleeve 15.
  • the blowing means 8 being always activated.

Abstract

A device for drawing off a liquid from a container comprising a drawing-off needle having a free lower end and an upper end, a suction deliverer connected to the upper end of the needle, and a blower carried by the needle allowing drops of the liquid present on the inside wall(s) of the container in the bottom section of the container to be concentrated.

Description

La présente invention concerne un dispositif de prélèvement d'un liquide dans un récipient, permettant de concentrer les gouttes de liquide présentes sur la ou les paroi(s) intérieure(s) du récipient dans la partie basse dudit récipient.The present invention relates to a device for sampling a liquid in a container, for concentrating the drops of liquid present on the inner wall (s) of the container in the lower part of said container.

La présente invention concerne également un procédé de prélèvement d'un liquide présent dans un récipient utilisant le dispositif ci-dessus.The present invention also relates to a method of sampling a liquid present in a container using the above device.

La présente invention concerne enfin l'utilisation du dispositif de prélèvement ci-dessus afin de contrôler le niveau du liquide présent dans le récipient.The present invention finally relates to the use of the above sampling device to control the level of the liquid present in the container.

Jusqu'à présent ce genre de dispositif de prélèvement permet simplement, par contact avec le liquide à prélever, soit l'apport d'un liquide d'intérêt qu'il contient soit le retrait d'un autre liquide d'intérêt présent dans un récipient.Until now this kind of sampling device simply allows, by contact with the liquid to be taken, either the supply of a liquid of interest that it contains or the withdrawal of another liquid of interest present in a container.

De tels dispositifs sont en général constitués par des pipettes ou des aiguilles creuses associées à des pompes. Certaines plus sophistiquées autorisent le nettoyage des parois extérieures desdites pipettes ou aiguilles qui ont été trempées dans le liquide prélevé ou ayant subi un apport d'un liquide additionnel. C'est le cas par exemple dans la demande de brevet WO-A-99/27973 déposée sous priorité du 27 novembre 1997 par la demanderesse. Celle-ci concerne un procédé de décontamination d'une aiguille creuse métallique destinée au prélèvement et/ou à la distribution d'un liquide contaminateur, l'aiguille coopérant avec des moyens de branchement électrique permettant d'établir un courant électrique dans l'aiguille pour décontaminer et préserver l'intégrité de ladite aiguille en vue de sa réutilisation. D'autres sont équipées de moyens évitant de souiller ces parois extérieures des éléments de prélèvements, comme c'est le cas de la demande de brevet WO-A-99/50674 déposée sous priorité du 1er avril et du 22 juin 1998 par la demanderesse. Cette demande concerne un procédé de prélèvement d'un échantillon biologique par l'intermédiaire d'un appareil d'aspiration - refoulement, tel qu'une pipette, manuel ou automatique, incorporé ou non à un automate. Mais elle concerne également un procédé de détection de la surface libre d'un échantillon biologique, un appareil de prélèvement d'un échantillon, tel qu'une pipette, et un appareil de détection de la surface libre d'un échantillon biologique.Such devices are generally constituted by pipettes or hollow needles associated with pumps. Some more sophisticated allow the cleaning of the outer walls of said pipettes or needles that have been soaked in the liquid taken or having added an additional liquid. This is the case for example in the patent application WO-A-99/27973 filed under priority of November 27, 1997 by the plaintiff. This relates to a method for decontaminating a hollow metal needle for sampling and / or dispensing a contaminating liquid, the needle cooperating with electrical connection means making it possible to establish an electric current in the needle. to decontaminate and preserve the integrity of said needle for reuse. Others are equipped with means avoiding contaminating these outer walls of the sampling elements, as is the case with the patent application. WO-A-99/50674 filed under priority 1 April and 22 June 1998 by the applicant. This application relates to a method of sampling a biological sample via a suction-discharge device, such as a pipette, manual or automatic, incorporated or not to an automaton. But it also relates to a method for detecting the free surface of a biological sample, a sample collection apparatus, such as a pipette, and an apparatus for detecting the free surface of a biological sample.

Toutefois, lorsqu'un liquide est ajouté voire éventuellement retiré d'un récipient, tel qu'un tube, une cavité de plaque de microtitration, des éclaboussures peuvent être générées et des gouttes peuvent ainsi se former sur les parois intérieures de ce récipient. Le problème réside alors dans le fait que ces gouttes contiennent des éléments essentiels qui peuvent être utiles à une réaction biologique ultérieure, et que ces éléments n'étant pas présents dans le liquide présent dans le fond dudit récipient ils ne peuvent pas participer à ladite réaction. Ainsi dans le cas d'acides nucléiques, les quantités de ces acides nucléiques extraits de cellules par lyse ou toute autre technique, sont peu nombreuses. Il est donc souhaitable d'amplifier ces cibles moléculaires en leurs ajoutant des amorces d'amplification et des sondes de détection. Si des gouttes isolées contiennent ne serait-ce qu'une partie de ces éléments biologiques : cibles, amorces et/ou sondes, l'amplification et/ou la réaction de détection qui va/vont suivre sera/seront perturbées. La perturbation sera d'autant plus forte que l'on souhaite effectuer une détection quantitative et pas seulement qualitative de la cible.However, when a liquid is added or possibly removed from a container, such as a tube, a microtiter plate cavity, splashes may be generated and drops may thus be formed on the inner walls of this container. The problem lies in the fact that these drops contain essential elements that may be useful for a subsequent biological reaction, and that these elements are not present in the liquid present in the bottom of said container they can not participate in said reaction. . Thus, in the case of nucleic acids, the quantities of these nucleic acids extracted from cells by lysis or any other technique are few. It is therefore desirable to amplify these molecular targets by adding amplification primers and detection probes. If isolated drops contain even a part of these biological elements: targets, primers and / or probes, the amplification and / or the detection reaction that will / will follow will be / will be disturbed. The disturbance will be even stronger than one wishes to perform a quantitative and not only qualitative detection of the target.

Un autre problème est la détermination d'un volume de liquide présent dans un récipient. Certains contrôles sont nécessaires parfois pour connaître avec exactitude le volume de liquide distribué dans un récipient ou une série de récipients. Dans ce cas, il est nécessaire de connaître avec précision ledit volume. De ce fait la présence de goutte (s) non récupérée(s) ou récupérable(s) peut engendrer des valeurs erronées et affecter le résultat final.Another problem is the determination of a volume of liquid present in a container. Some checks are sometimes necessary to know exactly the volume of liquid dispensed in a container or series of containers. In this case, it is necessary to know precisely said volume. As a result, the presence of unrecovered or recoverable drop (s) can lead to erroneous values and affect the final result.

Aucun document de l'état de la technique ne solutionne ces problèmes.No state-of-the-art document solves these problems.

La présente invention se propose d'apporter une solution à ces problèmes afin de répondre à une attente des utilisateurs.The present invention proposes to provide a solution to these problems in order to meet the expectations of users.

A cet effet, la présente invention concerne un dispositif de prélèvement d'un liquide dans un récipient comprenant :

  • une aiguille de prélèvement comportant une extrémité libre inférieure et une extrémité supérieure,
  • des moyens d'aspiration - refoulement reliés à l'extrémité supérieure de l'aiguille,
  • des moyens de soufflage portés par ladite aiguille permettant de concentrer les gouttes de liquide présentes sur la ou les paroi(s) intérieure(s) du récipient dans la partie basse dudit récipient.
For this purpose, the present invention relates to a device for sampling a liquid in a container comprising:
  • a sampling needle having a lower free end and an upper end,
  • suction-discharge means connected to the upper end of the needle,
  • blowing means carried by said needle for concentrating the drops of liquid present on the inner wall (s) of the container in the lower part of said container.

Selon une première variante de réalisation, l'aiguille de prélèvement est constituée d'un tube ouvert à ses deux extrémités; le récipient destiné à contenir le liquide à prélever est constitué d'un tube de diamètre supérieur à celui de l'extrémité inférieure de l'aiguille, ouvert uniquement à son extrémité supérieure.According to a first variant embodiment, the sampling needle consists of a tube open at both ends; the container for containing the liquid to be taken up consists of a tube of diameter greater than that of the lower end of the needle, open only at its upper end.

Selon une seconde variante, les moyens de soufflage comprennent au moins une ouverture latérale à l'aiguille; cette/ces ouverture(s) permet(tent) l'envoi d'un flux d'air sur la ou les paroi(s) intérieure(s) du récipient.According to a second variant, the blowing means comprise at least one lateral opening to the needle; this / these opening (s) allows (s) sending a flow of air on the inner wall (s) (s) of the container.

Selon une troisième variante de réalisation, l'aiguille de prélèvement est en position verticale.According to a third variant embodiment, the sampling needle is in a vertical position.

Selon un mode de réalisation des deux variantes précédentes de l'invention, le flux d'air sortant des ouvertures latérales est oblique et dirigé du haut vers le bas. Ce flux d'air a un angle par rapport à l'horizontale qui est compris entre 10° et 80°, préférentiellement entre 20 et 50°, préférentiellement entre 25 et 40° et encore plus préférentiellement de 30°.According to one embodiment of the two previous variants of the invention, the air flow leaving the lateral openings is oblique and directed from top to bottom. This air flow has an angle relative to the horizontal which is between 10 ° and 80 °, preferably between 20 and 50 °, preferably between 25 and 40 ° and even more preferably 30 °.

Selon un autre mode de réalisation, les moyens de soufflage comprennent trois à vingt, préférentiellement cinq à douze et encore plus préférentiellement huit ouvertures latérales.According to another embodiment, the blowing means comprise three to twenty, preferably five to twelve and even more preferably eight lateral openings.

Selon encore un autre mode de réalisation, ces ouvertures latérales sont réparties de façon rayonnante, positionnées dans un même plan, préférentiellement horizontal.According to yet another embodiment, these lateral openings are radially distributed, positioned in the same plane, preferably horizontally.

Selon une autre variante de réalisation, le dispositif de prélèvement est caractérisé par le fait que :

  • la distance séparant les ouvertures latérales de la ou des parois intérieures du récipient est comprise entre 30 et 70%, préférentiellement entre 40 et 60% du diamètre de l'aiguille,
  • le diamètre de chaque ouverture est compris entre 3 et 25 %, préférentiellement entre 5 et 15 %, et encore plus préférentiellement égal à 10 % du diamètre de ladite aiguille et/ou
  • l'implantation de chaque ouverture par rapport à l'extrémité libre inférieure de l'aiguille est comprise entre 50 et 150 %, préférentiellement entre 80 et 120 %, et encore plus préférentiellement égale à 100 % du diamètre intérieur dudit récipient.
According to another variant embodiment, the sampling device is characterized in that:
  • the distance separating the lateral openings of the inner wall or walls of the container is between 30 and 70%, preferably between 40 and 60% of the diameter of the needle,
  • the diameter of each opening is between 3 and 25%, preferably between 5 and 15%, and even more preferably equal to 10% of the diameter of said needle and / or
  • the implantation of each opening relative to the lower free end of the needle is between 50 and 150%, preferably between 80 and 120%, and even more preferably equal to 100% of the inner diameter of said container.

Selon un mode de réalisation de la variante précédemment décrite, le dispositif de prélèvement est caractérisé par le fait que :

  • la distance séparant les ouvertures latérales de la ou des parois intérieures du récipient est comprise entre 1 et 10 millimètres, préférentiellement entre 2,5 et 4 millimètres, et encore plus préférentiellement entre 2,75 et 3,
  • le diamètre de chaque ouverture est compris entre 0,1 et 1 millimètre, préférentiellement entre 0,3 et 0,6 millimètre, et encore plus préférentiellement de 0,4 millimètre, et/ou
  • l'implantation de chaque ouverture par rapport à l'extrémité libre inférieure de l'aiguille est comprise entre 3 et 25 millimètres, préférentiellement entre 6 et 15 millimètres, et encore plus préférentiellement de 9 millimètres.
According to one embodiment of the variant described above, the sampling device is characterized in that:
  • the distance separating the lateral openings of the inner wall or walls of the container is between 1 and and 10 millimeters, preferably between 2.5 and 4 millimeters, and even more preferentially between 2.75 and 3,
  • the diameter of each opening is between 0.1 and 1 millimeter, preferably between 0.3 and 0.6 millimeters, and still more preferably of 0.4 millimeters, and / or
  • the implantation of each opening relative to the lower free end of the needle is between 3 and 25 millimeters, preferably between 6 and 15 millimeters, and even more preferably 9 millimeters.

Quelque soit la variante ou le mode de réalisation, le dispositif de prélèvement est caractérisé par le fait que les moyens de soufflage comprennent un manchon fermé comportant au moins une arrivée de gaz pulsé, préférentiellement de l'air.Whatever the variant or embodiment, the sampling device is characterized in that the blowing means comprise a closed sleeve comprising at least one pulsed gas inlet, preferably air.

Dans un cas particulier, le dispositif est caractérisé par le fait que le manchon est un tube fermé qui entoure en tout ou partie l'aiguille de prélèvement.In a particular case, the device is characterized in that the sleeve is a closed tube which wholly or partially surrounds the sampling needle.

La présente invention concerne également un procédé de prélèvement d'un liquide dans un récipient utilisant un dispositif de prélèvement tel que précédemment décrit et comprenant les étapes suivantes :

  • introduction de l'extrémité libre inférieure de l'aiguille de prélèvement dans le récipient,
  • activation des moyens de soufflage permettant de concentrer les gouttes de liquide présentes sur la ou les paroi (s) intérieure(s) du récipient dans la partie basse dudit récipient,
  • aspiration de tout ou partie du liquide présent dans ledit récipient par ladite extrémité libre inférieure de l'aiguille.
The present invention also relates to a method of sampling a liquid in a container using a sampling device as previously described and comprising the following steps:
  • introducing the lower free end of the sampling needle into the container,
  • activation of the blowing means for concentrating the drops of liquid present on the inner wall (s) of the container in the lower part of said container,
  • suction of all or part of the liquid present in said container by said lower free end of the needle.

Selon un premier mode de réalisation, les trois étapes d'introduction, d'activation des moyens de soufflage (8) et d'aspiration sont séquentielles.According to a first embodiment, the three steps of introduction, activation of the blowing means (8) and aspiration are sequential.

Selon un second mode de réalisation, l'étape d'introduction et l'étape d'activation des moyens de soufflage sont réalisées simultanément.According to a second embodiment, the introduction step and the activation step of the blowing means are performed simultaneously.

Selon un troisième mode de réalisation, la première étape d'introduction et la seconde étape d'activation sont séquentielles mais avec une période de recouvrement, l'introduction se terminant quand l'activation a déjà débuté.According to a third embodiment, the first introduction step and the second activation step are sequential but with a recovery period, the introduction ending when the activation has already begun.

Enfin, le dispositif de prélèvement peut être utilisé afin de contrôler le niveau du liquide présent dans un récipient.Finally, the sampling device can be used to control the level of the liquid present in a container.

La présente invention sera décrite en rapport avec les figures ci-jointes données à titre d'exemples indicatifs qui n'ont pas de caractère limitatif mais représentent un mode préférentiel de réalisation de ladite invention.

  • La figure 1 représente une vue schématique en perspective d'un dispositif de prélèvement selon l'invention et d'un récipient susceptible de contenir le liquide à délivrer ou à prélever.
  • La figure 2 représente une vue identique à celle de la figure 1, lorsque le dispositif de prélèvement est connecté aux moyens permettant son bon fonctionnement et lorsqu'il est introduit dans le récipient.
  • La figure 3 représente une vue en coupe longitudinale partielle du dispositif de prélèvement et de son récipient, selon l'invention, selon un axe A-A représenté à la figure 2.
  • La figure 4 représente une vue en coupe d'un récipient destiné à contenir le liquide à prélever.
  • La figure 5 représente un détail B de la figure 3 représentant l'extrémité inférieure de l'aiguille de prélèvement selon un premier mode de réalisation.
  • La figure 6 représente l'introduction de l'extrémité libre inférieure de l'aiguille de prélèvement dans le récipient et l'activation des moyens de soufflage.
  • La figure 7 représente une vue identique à celle de la figure 6, les gouttes de liquide étant déplacées vers la partie basse du récipient sous l'action des moyens de soufflage.
  • La figure 8 représente l'étape d'aspiration par l'aiguille de prélèvement du liquide présent dans le récipient.
  • La figure 9 représente une vue en coupe identique à la figure 8, lorsque la totalité du liquide a été prélevé.
  • La figure 10 représente un détail C de la figure 9.
The present invention will be described with reference to the accompanying figures given as indicative examples which are not limiting but represent a preferred embodiment of said invention.
  • The figure 1 is a schematic perspective view of a sampling device according to the invention and a container capable of containing the liquid to be delivered or taken.
  • The figure 2 represents a view identical to that of the figure 1 , when the sampling device is connected to the means for its proper operation and when it is introduced into the container.
  • The figure 3 represents a partial longitudinal sectional view of the sampling device and its container, according to the invention, along an axis AA represented in FIG. figure 2 .
  • The figure 4 is a sectional view of a container for containing the liquid to be taken.
  • The figure 5 represents a detail B of the figure 3 representing the lower end of the sampling needle according to a first embodiment.
  • The figure 6 represents the introduction of the lower free end of the sampling needle into the container and the activation of the blowing means.
  • The figure 7 represents a view identical to that of the figure 6 , the drops of liquid being displaced towards the lower part of the container under the action of the blowing means.
  • The figure 8 represents the suction step by the sampling needle of the liquid present in the container.
  • The figure 9 represents a sectional view identical to the figure 8 when all of the liquid has been removed.
  • The figure 10 represents a detail C of the figure 9 .

Enfin la figure 11 représente l'extrémité inférieure de l'aiguille de prélèvement selon un second mode de réalisation.Finally, figure 11 represents the lower end of the sampling needle according to a second embodiment.

La présente invention concerne un dispositif de prélèvement d'un liquide dans un récipient représenté sur l'ensemble des figures 1 à 6.The present invention relates to a device for sampling a liquid in a container represented on all Figures 1 to 6 .

Les figures 1 à 3 représentent le dispositif de prélèvement 1 en l'absence de tout liquide à prélever. Ce dispositif de prélèvement 1 est bien représenté sur les figures 1 et 2 et est constitué essentiellement d'une aiguille de prélèvement 4 comportant une extrémité libre inférieure 5 et une extrémité supérieure 6, ladite aiguille 4 étant en position verticale.The Figures 1 to 3 represent the sampling device 1 in the absence of any liquid to be taken. This sampling device 1 is well represented on the Figures 1 and 2 and consists essentially of a sampling needle 4 having a lower free end 5 and an upper end 6, said needle 4 being in a vertical position.

Sur la figure 1 est également représenté séparément du dispositif de prélèvement 1 un récipient 3, lui-même constitué d'un tube, de diamètre supérieur à celui de l'extrémité inférieure 5 de l'aiguille 4, et ouvert à son extrémité supérieure 11 et fermé à son extrémité inférieure 17, ce tube étant susceptible de contenir un liquide à prélever.On the figure 1 is also shown separately from the sampling device 1 a container 3, itself consisting of a tube of diameter greater than that of the lower end 5 of the needle 4, and open at its end upper 11 and closed at its lower end 17, this tube being capable of containing a liquid to be taken.

La figure 2 représente un dispositif de prélèvement 1 après son introduction selon un axe vertical dans le récipient 3, ledit récipient 3 de forme classique comportant une paroi intérieure 10 et une paroi extérieure, non référencée. L'extrémité supérieure 6 de l'aiguille de prélèvement 4 est reliée à des moyens d'aspiration - refoulement 7 par l'intermédiaire d'un flexible 13. Ces moyens 7, connus de l'homme du métier, ne seront pas exposés plus avant. Ils peuvent juste être constitués par une pompe péristaltique, ou tout autre moyen équivalent, tel que les systèmes temps - pression - dépression, qui sont basés sur lé principe d'un réservoir principal en pression (ou en dépression suivant le besoin de l'application dont la sortie possède un tuyau muni d'une électrovanne commandée par un dispositif électronique utilisant une base de temps pour réaliser sa commutation ouverture - fermeture.The figure 2 is a sampling device 1 after its introduction along a vertical axis in the container 3, said container 3 of conventional shape having an inner wall 10 and an outer wall, not referenced. The upper end 6 of the sampling needle 4 is connected to suction-discharge means 7 via a hose 13. These means 7, known to those skilled in the art, will not be exposed more before. They may just be constituted by a peristaltic pump, or any other equivalent means, such as time-pressure-depression systems, which are based on the principle of a main reservoir in pressure (or in depression depending on the need of the application whose outlet has a hose provided with a solenoid valve controlled by an electronic device using a time base to perform its switching opening - closing.

Le dispositif de prélèvement 1 selon l'invention fonctionne selon un mode d'aspiration - refoulement, comme indiqué par les flux F1 (aspiration) et F2 (refoulement) sur la figure 3. Il comprend également des moyens de soufflage 8 situés en position latérale de l'aiguille de prélèvement 4. Ces moyens de soufflage 8 sont constitués d'un manchon 15, l'aiguille 4 étant en position coaxiale et concentrique par rapport au manchon 15. Ledit manchon 15 est, quant à lui, fermé et ne possède que :

  • une ouverture/entrée supérieure 16 qui est reliée, via un flexible 14, aux moyens de soufflage 8, dans lesquels est projeté un flux de gaz pulsé selon F3 et
  • au moins une ouverture latérale 12, en position inférieure par laquelle est projeté un flux de gaz pulsé selon F4, ce gaz pulsé étant préférentiellement de l'air.
The sampling device 1 according to the invention operates according to a suction-discharge mode, as indicated by the flows F1 (suction) and F2 (discharge) on the figure 3 . It also comprises blowing means 8 located in the lateral position of the sampling needle 4. These blowing means 8 consist of a sleeve 15, the needle 4 being in a coaxial and concentric position with respect to the sleeve 15. Ledit sleeve 15 is, in turn, closed and has only:
  • an upper opening / inlet 16 which is connected, via a hose 14, to the blowing means 8, in which a pulsed gas flow is projected according to F3 and
  • at least one lateral opening 12, in the lower position through which is projected a flow of pulsed gas along F4, the pulsed gas is preferably air.

Le flux de gaz initial, selon F3, provient donc des moyens de soufflage par l'entrée 16, ladite entrée 16 étant connectée aux moyens de soufflage 8 par un flexible 14. La circulation de gaz depuis l'entrée 16 jusqu'aux ouvertures latérales 12 se fait donc au travers du manchon fermé 15. Préférentiellement, les ouvertures latérales 12 sont implantées de façon rayonnante sur ledit manchon 15, afin d'améliorer l'efficacité du dispositif. De manière générale, l'ensemble des moyens de soufflage est donc constitué des moyens des soufflage 8 eux-mêmes, du flexible 14, des ouvertures latérales 12 et du manchon 15.The initial gas flow, according to F3, therefore comes from the blowing means by the inlet 16, said inlet 16 being connected to the blowing means 8 by a hose 14. The flow of gas from the inlet 16 to the lateral openings 12 is therefore through the closed sleeve 15. Preferably, the lateral openings 12 are radially implanted on said sleeve 15, in order to improve the efficiency of the device. In general, the assembly of the blowing means therefore consists of the blowing means 8 themselves, the hose 14, the lateral openings 12 and the sleeve 15.

Chaque ouverture 12 implantée sur le manchon 15 est représentée sur le détail C de la figure 10. Le diamètre 19 de l'ouverture 12 est compris entre 0,1 et 1 millimètre, préférentiellement entre 0,3 et 0,6 millimètre, et encore plus préférentiellement de 0,4 millimètre. Le flux de gaz pulsé, selon F4, provenant des ouvertures 12 est en position oblique par rapport à l'horizontale, et est dirigé de haut en bas, ce qui permet de concentrer les gouttes 9 présentes sur la paroi intérieure et latérale 10 (voir la figure 4), les gouttes 9 étant en position éloignée de l'extrémité inférieure 17 du récipient 3, et le flux d'air selon F4 les dirigeant vers cette extrémité inférieure 17 dudit récipient 3 comme représenté aux figures 7 à 9. L'angle existant entre l'horizontale 20 et le flux de gaz (F4) provenant des ouvertures 12 est donc compris entre 10° et 80°, préférentiellement entre 20° et 50°, préférentiellement entre 25 et 40°, et encore plus préférentiellement de 30°.Each opening 12 implanted on the sleeve 15 is represented on the detail C of the figure 10 . The diameter 19 of the opening 12 is between 0.1 and 1 millimeter, preferably between 0.3 and 0.6 millimeter, and even more preferably 0.4 millimeter. The pulsed gas flow, according to F4, coming from the openings 12 is in an oblique position relative to the horizontal, and is directed from top to bottom, which makes it possible to concentrate the drops 9 present on the inner and lateral wall 10 (see the figure 4 ), the drops 9 being in a position remote from the lower end 17 of the container 3, and the air flow along F4 directing them towards this lower end 17 of said container 3 as shown in FIGS. Figures 7 to 9 . The angle between the horizontal 20 and the gas flow (F4) coming from the openings 12 is therefore between 10 ° and 80 °, preferably between 20 ° and 50 °, preferably between 25 and 40 °, and even more preferentially 30 °.

Le dispositif de prélèvement 1 selon l'invention peut ainsi être utilisé pour prélever un liquide 2 contenu dans un récipient fermé à son extrémité supérieure, par exemple par un film externe d'aluminium. Dans ce cas, il est nécessaire de perforer le film externe pour que l'extrémité inférieure 5 de l'aiguille de prélèvement 4 puisse accéder au liquide à prélever 2. Comme l'indique le détail B de la figure 5, l'extrémité libre inférieure 5 de l'aiguille de prélèvement 4 est de forme arrondie 18 sur l'extérieur de l'aiguille 4 afin que lorsque le film externe est perforé lors de la descente de l'aiguille vers le récipient, selon F5, la perforation soit nette ; on évite ainsi tout déchirement ou effet emporte-pièce du film externe.The sampling device 1 according to the invention can thus be used to take a liquid 2 contained in a closed container at its upper end, for example by an external aluminum film. In this case, it is necessary to perforate the outer film so that the lower end 5 of the sampling needle 4 can access the liquid to be taken 2. As indicated in detail B of the figure 5 , the lower free end 5 of the sampling needle 4 is of rounded shape 18 on the outside of the needle 4 so that when the outer film is perforated during the descent of the needle to the container, according to F5 the perforation is clear; this avoids any tearing or punching effect of the outer film.

Selon un second mode de réalisation, comme cela est bien représenté sur la figure 11, l'extrémité libre inférieure 5 de l'aiguille de prélèvement 4 comporte une série de fentes 18 disposées radialement ou de façon rayonnante, dont le nombre peut varier de 4 à 12 sans incidence sur le prélèvement. Dans le mode de réalisation ce nombre est de 6. Ainsi, lorsque le film externe est perforé lors de la descente de l'aiguille vers le récipient, selon F5, la perforation est encore plus nette ; on évite ainsi tout déchirement ou effet emporte-pièce du film externe. De plus le prélèvement avec ce mode de réalisation est encore plus efficace, car sa forme permet le prélèvement même dans des tubes, style éprouvette, dont l'espace situé le plus en bas est difficile d'accès. De manière intéressante, son rayon de courbure externe est adapté le rayon de courbure interne du fond du récipient. Selon une alternative, le rayon de courbure externe de l'aiguille de prélèvement 4 épouse le rayon de courbure interne du fond du récipient, c'est-à-dire est de rayon légèrement inférieur pour permettre un appui complet entre les deux surfaces interne et externe.According to a second embodiment, as is well represented on the figure 11 , the lower free end 5 of the sampling needle 4 comprises a series of slots 18 arranged radially or radially, the number may vary from 4 to 12 without impacting the sample. In the embodiment this number is 6. Thus, when the outer film is perforated during the descent of the needle to the container, according to F5, the perforation is even sharper; this avoids any tearing or punching effect of the outer film. In addition, the sampling with this embodiment is even more effective, because its shape allows the sampling even in tubes, specimen style, the space at the bottom is difficult to access. Interestingly, its outer radius of curvature is adapted to the inner radius of curvature of the bottom of the container. According to an alternative, the external radius of curvature of the sampling needle 4 matches the internal radius of curvature of the bottom of the container, that is to say is of slightly smaller radius to allow complete support between the two inner surfaces and external.

Quel que soit le mode de réalisation de l'aiguille de prélèvement 4, le diamètre de ladite aiguille 4 est sur le mode de réalisation présenté de 3,5 millimètres.Whatever the embodiment of the sampling needle 4, the diameter of said needle 4 is in the presented embodiment of 3.5 millimeters.

Lorsque le dispositif de prélèvement 1 est mis en oeuvre, selon les figures 6 à 9, l'aiguille de prélèvement 4 descend dans le récipient 3 selon la direction F5.When the sampling device 1 is used, according to the Figures 6 to 9 the sampling needle 4 descends into the container 3 in the direction F5.

Ledit récipient 3 peut également être dirigé vers l'aiguille 4 selon la direction F6 représentée sur la figure 6. L'activation des moyens de soufflage 8 entraîne la création d'un flux de gaz selon F3 qui pénètre par l'entrée 16. Ce flux de gaz circule dans le manchon 15 et ressort de celui-ci selon F4 par les ouvertures latérales 12. La projection du gaz vers la paroi intérieure 10 du récipient 3 permet de décrocher et donc de déplacer, selon F7, et de concentrer vers la partie inférieure 17 du récipient 3, les gouttes de liquide 9 présentes sur ladite paroi 10.Said container 3 can also be directed towards the needle 4 in the direction F6 shown in FIG. figure 6 . The activation of the blowing means 8 causes the creation of a flow of gas along F3 which enters through the inlet 16. This flow of gas flows in the sleeve 15 and leaves it from F4 via the lateral openings 12. The projection of the gas towards the inner wall 10 of the container 3 makes it possible to unhook and thus move, according to F7, and to concentrate towards the lower part 17 of the container 3, the drops of liquid 9 present on said wall 10.

La présente invention concerne également un procédé de prélèvement représenté sur l'ensemble des figures 7 à 10.The present invention also relates to a sampling method represented on all the Figures 7 to 10 .

Dans le mode de réalisation représenté à la figure 7, l'étape d'introduction de l'aiguille 4 et l'étape d'activation des moyens de soufflage 8 sont simultanées, la descente selon F5 de l'aiguille 4 dans le récipient 3 se faisant en même temps que l'arrivée de gaz, selon F3, dans le manchon 15. Lorsque l'extrémité inférieure 5 de l'aiguille de prélèvement 4 est en contact avec le liquide 2 présent dans le récipient 3, l'aspiration du liquide 2 par l'aiguille de prélèvement 4 débute, selon F1, les moyens de soufflage 8 étant toujours activés.In the embodiment shown at figure 7 , the step of introducing the needle 4 and the step of activating the blowing means 8 are simultaneous, the descent along F5 of the needle 4 in the container 3 being done at the same time as the arrival of gas, according to F3, in the sleeve 15. When the lower end 5 of the sampling needle 4 is in contact with the liquid 2 present in the container 3, the suction of the liquid 2 by the sampling needle 4 begins. according to F1, the blowing means 8 being always activated.

Lorsque la totalité du liquide 2 présent initialement dans le récipient 3 a été prélevé par l'aiguille 4, selon F1, les moyens de soufflage 8 sont désactivés, l'aiguille de prélèvement 4 étant toujours positionnée dans ledit récipient 3.When all of the liquid 2 initially present in the container 3 has been taken by the needle 4, along F1, the blowing means 8 are deactivated, the sampling needle 4 always being positioned in said container 3.

REFERENCESREFERENCES

  • 1 - Dispositif de prélèvement1 - Sampling device
  • 2 - Liquide2 - Liquid
  • 3 - Récipient3 - Container
  • 4 - Aiguille de prélèvement4 - Sampling needle
  • 5 - Extrémité libre inférieure de l'aiguille (4)5 - Lower free end of the needle (4)
  • 6 - Extrémité supérieure de l'aiguille (4)6 - Upper end of the needle (4)
  • 7 - Moyens d'aspiration - refoulement7 - Means of aspiration - repression
  • 8 - Moyens de soufflage8 - Means of blowing
  • 9 - Gouttes de liquide 2 présentes sur la paroi intérieure 10 du récipient 39 - Drops of liquid 2 present on the inner wall 10 of the container 3
  • 10 - Paroi(s) intérieure(s) du récipient 310 - Inside wall (s) of container 3
  • 11 - Extrémité supérieure du récipient 311 - Upper end of the container 3
  • 12 - ouverture latérale à l'aiguille12 - lateral opening with the needle
  • 13 - Flexible connectant les moyens d'aspiration - refoulement 7 avec l'extrémité supérieure 6 de l'aiguille 413 - Hose connecting the suction means - discharge 7 with the upper end 6 of the needle 4
  • 14 - Flexible connectant les moyens de soufflage 8 avec l'entrée de gaz (air) 1614 - Hose connecting the blowing means 8 with the gas inlet (air) 16
  • 15 - Manchon15 - Sleeve
  • 16 - Entrée de gaz (air) dans le manchon 1516 - Gas (air) inlet in the sleeve 15
  • 17 - Extrémité inférieure du récipient 317 - Bottom end of container 3
  • 18 - Arrondi présent à l'extrémité inférieure 5 de l'aiguille 418 - Rounded present at the lower end 5 of the needle 4
  • 19 - Diamètre de chaque ouverture 1219 - Diameter of each opening 12
  • 20 - Angle entre le flux d'air F4 généré par les ouvertures 12 et l'horizontale20 - Angle between the air flow F4 generated by the openings 12 and the horizontal
  • 21 - Fentes de l'extrémité inférieure 5 de l'aiguille 421 - Slots of the lower end 5 of the needle 4
  • F1 - Aspiration du liquide 2 par l'aiguille 4F1 - Suction of liquid 2 by needle 4
  • F2 - Refoulement du liquide 2 par l'aiguille 4F2 - Delivery of liquid 2 by needle 4
  • F3 - Arrivée de gaz (air) dans le manchon 15 provenant des moyens de soufflage 8F3 - Gas (air) inlet in the sleeve 15 from the blowing means 8
  • F4 - Flux de gaz (air) provenant de l'ouverture 12F4 - Gas (air) flow from the opening 12
  • F5 - Descente de l'aiguille 4 dans le récipient 3F5 - Descent of the needle 4 into the container 3
  • F6 - Montée du récipient 3 vers l'aiguille 4F6 - Raising container 3 to needle 4
  • F7 - Déplacement d'une goutte 9 le long d'une paroi 10 sous l'effet du flux selon F3F7 - Displacement of a drop 9 along a wall 10 under the effect of the flow according to F3

Claims (18)

  1. Device for drawing off (1) a liquid (2) from a container (3) comprising:
    - a drawing-off needle (4) having a free lower end (5) and an upper end (6),
    - suction-delivery means (7) connected to the upper end (6) of the needle (4), characterized by
    - blowing means (8) carried by said needle (4) allowing the drops (9) of liquid (2) present on the inside wall(s) (10) of the container (3) in the bottom section of said container (3) to be concentrated.
  2. Device according to Claim 1, characterized in that the needle (4) consists of a tube open at both its ends (5 and 6), and in that the container (3) consists of a tube of greater diameter open only at its upper end (11).
  3. Device according to either of Claims 1 and 2, characterized in that the blowing means (8) comprise at least one side opening (12) to the needle (4) allowing an air stream (F4) to be sent over the inside wall(s) (10) of the container (3).
  4. Device according to any one of Claims 1 to 3, characterized in that the drawihg-off needle (4) is in a vertical position.
  5. Device according to either of Claims 3 and 4, characterized in that the air stream (F4) is oblique and is directed from the top downward.
  6. Device according to any one of Claims 3 to 5, characterized in that the air stream (F4) has an angle (20) relative to the horizontal which is between 10° and 80°, preferably between 20° and 50°, preferably between 25 and 40°, and more preferably still 30°
  7. Device according to any one of Claims 3 to 6, characterized in that the blowing means (8) comprise three to twenty, preferably five to twelve and more preferably still eight side openings (12).
  8. Device according to Claim 7, characterized in that the side openings (12) are radiating.
  9. Device according to either of Claims 7 and 8 characterized in that the side openings (12) are positioned in the same, preferably horizontal, plane.
  10. Device according to any one of Claims 3 to 9, characterized in that:
    - the distance separating the side openings (12) from the inside wall (s) of the container (3) is between 30 and 70%, preferably between 40 and 60% of the diameter of the needle (4),
    - the diameter (19) of each opening (12) is between 3 and 25%, preferably between 5 and 15%, and more preferably still equal to 10% of the diameter of said needle (4) and/or
    - the position of each opening (12) relative to the free lower end (5) of the needle (4) is between 50 and 150%, preferably between 80 and 120%, and more preferably still equal to 100% of the diameter of said needle (4).
  11. Device according to Claim 10, characterized in that:
    - the distance separating the side openings (12) of the inside wall(s) of the container (3) is between 1 and 10 millimeters, preferably between 2.5 and 4 millimeters, and more preferably still between 2.75 and 3 millimeters,
    - the diameter (19) of each opening (12) is between 0.1 and 1 millimeter, preferably between 0.3 and 0.6 millimeter, and more preferably still 0.4 millimeter, and/or
    - the position of each opening (12) relative to the free lower end (5) of the needle (4) is between 3 and 25 millimeters, preferably between 6 and 15 millimeters, and more preferably still 9 millimeters.
  12. Device according to any one of Claims 1 to 11, characterized in that the blowing means (8) comprise a closed sleeve having at least one pulsed gas, preferably air, inlet.
  13. Device according to Claim 12, characterized in that the sleeve (15) is a closed tube which completely or partially surrounds the drawing-off needle (4).
  14. Method for drawing off a liquid (2) from a container (3) using a device (1) according to any one of Claims 1 to 13, and comprising the following steps:
    - introducing the free lower end (5) of the drawing-off needle (4) into the container (3),
    - activating the blowing means (8) allowing the drops (9) of liquid (2) present on the inside wall (s) (10) of the container (3) in the bottom section of said container (3) to be concentrated, and
    - sucking all or part of the liquid (2) present in said container (3) by said lower end (5) of the needle (4).
  15. Method according to Claim 14, characterized in that the three steps of introduction, activation of the means (8) and suction are sequential.
  16. Method according to Claim 14, characterized in that the first step, of introduction and the second step of activation of the means (8) are simultaneous.
  17. Method according to Claim 14, characterized in that the first step of introduction and the second step of activation of the means (8) are sequential but with an overlapping period, the introduction ending when the activation has already started.
  18. Use of a device for drawing off (1), according to any one of Claims 1 to 13, a liquid (2) from a container (3) so as to control the level of liquid (2) in the container (3).
EP07731725A 2006-03-13 2007-03-12 Device, use and method for drawing off a liquid Active EP1993733B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0602161A FR2898285B1 (en) 2006-03-13 2006-03-13 DEVICE, USE AND METHOD FOR COLLECTING A LIQUID
PCT/FR2007/050909 WO2007104886A1 (en) 2006-03-13 2007-03-12 Device, use and method for drawing off a liquid

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EP1993733A1 EP1993733A1 (en) 2008-11-26
EP1993733B1 true EP1993733B1 (en) 2011-06-29

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EP (1) EP1993733B1 (en)
JP (1) JP4896162B2 (en)
AT (1) ATE514486T1 (en)
ES (1) ES2369050T3 (en)
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Also Published As

Publication number Publication date
WO2007104886A1 (en) 2007-09-20
US7987736B2 (en) 2011-08-02
US20090000693A1 (en) 2009-01-01
ES2369050T3 (en) 2011-11-24
JP4896162B2 (en) 2012-03-14
ATE514486T1 (en) 2011-07-15
FR2898285A1 (en) 2007-09-14
FR2898285B1 (en) 2008-04-18
JP2009530594A (en) 2009-08-27
EP1993733A1 (en) 2008-11-26

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