EP2428272B1 - Procédé de revêtement hyrophobe d'embouts de pipette - Google Patents

Procédé de revêtement hyrophobe d'embouts de pipette Download PDF

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Publication number
EP2428272B1
EP2428272B1 EP11173625.2A EP11173625A EP2428272B1 EP 2428272 B1 EP2428272 B1 EP 2428272B1 EP 11173625 A EP11173625 A EP 11173625A EP 2428272 B1 EP2428272 B1 EP 2428272B1
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EP
European Patent Office
Prior art keywords
pipetting
pipette tip
wetting solution
tip
wetting
Prior art date
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EP11173625.2A
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German (de)
English (en)
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EP2428272A2 (fr
EP2428272A3 (fr
Inventor
Vinzenz Kirste
Renato Nay
Rainer Beckbissinger
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Hamilton Bonaduz AG
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Hamilton Bonaduz AG
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Publication of EP2428272A3 publication Critical patent/EP2428272A3/fr
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/02Burettes; Pipettes
    • B01L3/0275Interchangeable or disposable dispensing tips
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/02Burettes; Pipettes
    • B01L3/021Pipettes, i.e. with only one conduit for withdrawing and redistributing liquids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/12Specific details about manufacturing devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00Additional constructional details
    • B01L2300/16Surface properties and coatings
    • B01L2300/161Control and use of surface tension forces, e.g. hydrophobic, hydrophilic
    • B01L2300/165Specific details about hydrophobic, oleophobic surfaces
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00Additional constructional details
    • B01L2300/16Surface properties and coatings
    • B01L2300/161Control and use of surface tension forces, e.g. hydrophobic, hydrophilic
    • B01L2300/165Specific details about hydrophobic, oleophobic surfaces
    • B01L2300/166Suprahydrophobic; Ultraphobic; Lotus-effect
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05CAPPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C17/00Hand tools or apparatus using hand held tools, for applying liquids or other fluent materials to, for spreading applied liquids or other fluent materials on, or for partially removing applied liquids or other fluent materials from, surfaces
    • B05C17/005Hand tools or apparatus using hand held tools, for applying liquids or other fluent materials to, for spreading applied liquids or other fluent materials on, or for partially removing applied liquids or other fluent materials from, surfaces for discharging material from a reservoir or container located in or on the hand tool through an outlet orifice by pressure without using surface contacting members like pads or brushes
    • B05C17/00503Details of the outlet element

Definitions

  • the present invention relates to a method for the hydrophobic coating of pipette tips for the aspiration and dispensing of pipetting fluid.
  • a pipetting tip thus produced usually extends along a pipetting tip longitudinal axis, wherein a first axial longitudinal end region of the pipetting tip has a pipetting longitudinal end region having a pipetting opening operable by the pipetting fluid, and wherein a second axial longitudinal end region of the pipetting tip opposite the pipetting longitudinal end region in the axial direction is the coupling longitudinal end region a coupling geometry for, preferably detachable, coupling to a coupling counter-geometry of a pipetting device, wherein the pipette tip on its outer side an outer hydrophobia region and on its inner side an inner hydrophobicity each having a square roughness in a range of 100 nm to 1000 nm, preferably from 150 nm to 750 nm, and more preferably from 200 nm to 500 nm, and having a peak-to-peak roughness in
  • Such pipetting tips are for example from the WO 03/013731 A known.
  • the roughness ranges mentioned serve the hydrophobic formation of surfaces by utilizing the so-called “lotus effect", as it is also observed on lotus flowers.
  • hydrophobic formation of surfaces of pipette tips facilitates complete emptying of the pipette tip and thus increases the dimensional accuracy of dispensed liquid quantities. Furthermore, hydrophobic formation of surfaces of pipetting tips also reduces the risk of undesirable contamination of pipetting fluids in case of multiple use of a pipette tip. This problem is also referred to in the literature as "cross contamination". It results from the fact that a remainder of a first pipetting fluid remains adhering to a surface of the pipette tip as a wetting droplet from a previous pipetting operation and can thus enter a subsequently pipetted second pipetting fluid.
  • the WO 03/013731 A discloses for hydrophobic formation of a pipette tip a method which initially provides for providing a polymer surface at the pipetting tip. This can be done by preparing the pipetting tip from a corresponding polymer or by coating a pipetting tip by immersion in a corresponding polymer melt.
  • the polymer surface is dissolved with a solvent which contains undissolved particles, which after the removal of the solvent are at least partially firmly bonded to the polymer surface.
  • the particles are present in the solvent dispersed or suspended at the beginning of the process.
  • the pipette tip thus already contains on its inner side the antibody test substance necessary for the desired blood test for the purpose of simplifying and shortening the specific diagnosis.
  • Said object is achieved according to a first method aspect of the present invention by a method for hydrophobic coating of pipette tips with all features of claim 1. This comprises wetting at least portions of the outside and inside of the pipette tip with a wetting solution.
  • the method of the invention comprises a step of coupling the pipetting tip to a fluid pressure source of variable fluid pressure.
  • a fluid pressure is meant which serves for sucking and discharging pipetting fluid, that is to say a pressure of a working fluid other than the pipetting fluid, as a rule of a gas, in particular of air.
  • the inventive method comprises immersing the coupled pipette tip in the wetting solution, whereby it is possible with the simplest means to wet the outside of the pipette tip depending on the depth of immersion.
  • the method according to the invention comprises the step of aspirating wetting solution into the pipetting tip, whereby the inside of the pipetting tip can be wetted by wetting solution and thus provided with a hydrophobic coating.
  • the areas of the pipette tip wetted with wetting solution form the hydrophobically coated areas of the pipette tip after completion of the process.
  • the inventive method comprises dispensing the aspirated wetting solution, so that the pipetting tip can be made free again after wetting.
  • the method of the invention further comprises the step of evaporating solvent contained in the wetting solution whereby the wetted solution wetted portions of the pipetting tip are dried to form a hydrophobic coating.
  • the pipette tip provided with a hydrophobic coating is usually finished coated.
  • the outer hydrophobicity region should extend in the axial direction less far away from the pipetting opening of the pipette tip than the inner hydrophobic region, it can be provided according to a development of the method according to the invention that the height of the aspirated wetting solution column in the pipette tip differs from the immersion depth of the pipette tip in the wetting solution, preferably exceeds the latter.
  • the provision of the receiving cavity may preferably be effected by coupling such a receiving cavity to a pipetting device.
  • a tube element in particular a glass tube element with a smaller diameter, than at least the portion of the pipetting tip closer to the coupling longitudinal end region is used as the receiving cavity, so that the receiving cavity can be introduced from a coupling longitudinal end of the pipetting tip.
  • the outer hydrophobicity region can therefore have an axial extension length of zero in this case.
  • the pipetting tip can be connected to the receiving cavity in any desired manner, preferably in such a way that the pipetting tip surrounds the receiving cavity from its coupling-side longitudinal end so that when the wetting solution is dispensed from the receiving cavity, an interior region of the pipetting tip is rinsed with a binding solution.
  • the pipette tip can be connected directly to the receiving cavity by the pipette tip is attached to the receiving cavity.
  • the pipetting tip can be indirectly connected to the receiving cavity via the common pipetting device, so that pipetting tip and receiving cavity are connected to the same fluid pressure source.
  • a pipetting device and a reservoir of wetting solution are sufficient.
  • the pipetting device for coupling the receiving cavity must be slightly modified, but this is not absolutely necessary for the use of the present invention.
  • the evaporation of the solvent can advantageously be effected thermally and / or convectively, for example by virtue of the fact that the evaporation step comprises heating the pipetting tip and / or flowing the pipetting tip with a fluid, preferably with a gas, more preferably with air, in particular dry air.
  • the method comprises providing the wetting solution at a temperature in a range of 65 ° C to 85 ° C, preferably in a range of 70 ° C to 80 ° C, more preferably about 75 ° C includes.
  • the wetting solution preferably comprises a polymer or copolymer, particularly preferably a polypropylene-polyethylene copolymer, and a solvent which dissolves the polymer or copolymer contained.
  • a solvent in particular xylene-based solvents have proven to be advantageous.
  • a coating thus obtained leads to a surface roughness in the aforementioned range.
  • the wetting solution has a flow rate of from 0.3 ml / s to 0.7 ml / s, preferably from 0.4 ml / s to 0 , 6 ml / s is dispensed through the pipette tip or / and when the wetting solution at a temperature of 20 ° C to 30 ° C, preferably from 21 ° C to 25 ° C, especially preferably dispensed from 22 ° C to 25 ° C through the pipette tip.
  • the hydrophobic surface area on the outside of the pipette tip differs in terms of its axial length relative to the pipette tip longitudinal axis from the axial extension region of the hydrophobic region on the inside of the pipette tip.
  • the pipette tip can and therefore only needs to be made hydrophobic in those areas in which such a design is actually required.
  • the inside of the pipetting tip is considered to be the side whose surface has a normal vector which has an extension component to the imaginary pipetting tip longitudinal axis. Accordingly, the outside is the side whose surface has a normal vector which has an extension component away from the pipette tip longitudinal axis.
  • the hydrophobic formation of a surface of the pipetting tip assists the complete emptying of the pipetting tip during dispensing
  • the pipetting tip is less, and in some cases even less deeply immersed in a pipetting fluid reservoir, as pipetting fluid is sucked high into the pipetting tip of the pipetting tip, which is bounded by the inside of the pipetting tip.
  • This can be taken into account by the fact that the end of the inner hydrophobic area axially further from the pipetting opening is located further from the pipetting opening than the end of the outer hydrophobic area axially further from the pipetting opening.
  • pipetting therefore suffices, starting from the edge of the pipetting opening on the outside of the pipetting tip, to provide a hydrophobic formation of the surface only over a smaller axial extension length than on the inside of this pipetting tip, in order to ensure that the surfaces wetted by the pipetting fluid are as intended the pipette tip are hydrophobic.
  • the edge of the pipetting opening is made hydrophobic. Since a drop of pipetting fluid which wets the pipetting tip surface extends over a more or less large wetting spot on the pipetting tip surface depending on the wetting properties, it is particularly preferred for the purpose of a complete emptying of the pipetting tip that the outer hydrophobic area be provided and the inner hydrophobicity region forms a contiguous hydrophobicity region over an edge of the pipetting orifice defining a boundary between the outside and the inside of the pipetting tip.
  • the hydrophobic embodiment according to the present application is based on the provision of an initially defined roughness of the corresponding surface areas, the desired surface roughness of injection-molded pipetting tips can be produced by corresponding roughness of the mold cavity surfaces generating the surface regions.
  • the pipetting tip may have a more hydrophobic coating in at least one hydrophobic area of inner hydrophobic area and outer hydrophobic area compared to the material of the uncoated pipetting point.
  • the pipetting device includes a pipetting channel in which the negative pressure and / or overpressure is generated and / or provided, which is required for the aspiration and dispensing of pipetting fluid into and out of a pipetting tip.
  • Aerosol contamination is achieved by sucking vaporized or atomized portions of a pipetting fluid aspirated into the pipette tip from the pipetting fluid into the respectively coupled pipetting channel.
  • the vaporized or atomized pipetting liquid can then undesirably pass from the pipetting channel back into the pipetting fluid receiving space of a pipetting tip during a subsequent pipetting operation and contaminate the pipetting fluid received there. This can be done on the basis of the described pollution mechanism involving the pipette tip separate pipetting even with the one-time use of disposable pipetting tips on one and the same pipetting.
  • the filter is preferably provided closer to the coupling longitudinal end portion than the pipetting longitudinal end portion of the pipetting tip.
  • the filter is preferably made of porous, gas-permeable material, such as a sintered plastic material or fiber tangle, or a combination of such materials.
  • gas-permeable filters substantially more effectively prevent undesired passage of moisture when they are at least partially hydrophobic on their porous surface.
  • this can be achieved particularly advantageously by providing a coating which is more hydrophobic compared to the uncoated material of the filter in at least one section of the filter.
  • the wettability of the filter material and thus also the pore wall of the filter in the coated area drops considerably, which leads to an increase in the wetting angles that can be measured between the filter material and a droplet adhering thereto.
  • the wetting angle increases, one and the same droplets adhering to the filter material project more and more away from it, so that with an increasingly hydrophobic coating of the filter material, a smaller amount of liquid is sufficient to render the filter virtually gas-impermeable by narrowing the flow paths.
  • the applicant reserves the right to seek independent protection regardless of a hydrophobic formation of areas of the pipette tip receiving the filter.
  • Such a filter which is at least partially hydrophobic, can thus also be provided in a pipetting tip which is not designed to be hydrophobic or only on its inside or only on its outside or as described above.
  • the filter is provided in a built-up in the pipette tip preferably at least at that end region with a compared to the material of the uncoated filter more hydrophobic coating, which faces the pipetting.
  • the filter in order to increase the effect of the filter, it is particularly preferred to make the filter completely hydrophobic, in particular to provide it with the abovementioned hydrophobic coating.
  • the pipetting tip described hitherto can preferably be realized in that the uncoated pipetting tip has a plastic material at least on its outside and / or on its inside.
  • the pipetting tip over its entire thickness comprises a uniform plastic material, preferably formed from the plastic material.
  • plastic material a polymer or a copolymer such as polypropylene or / and polyethylene has been found, as well as polyamide. Due to their material properties, these materials are already liquid-repellent on their surface. Likewise, blends of these plastics can be used.
  • the hydrophobic coating has a plastic material, which is preferably compatible with the plastic material of the pipetting tip for easier connection.
  • the pipette tip and the hydrophobic coating on the same plastic material are particularly preferably, the pipette tip and the hydrophobic coating on the same plastic material.
  • a pipetting tip has proved to be particularly advantageous in the experimental operation, which in the uncoated state comprises at least on its area intended for hydrophobic coating polypropylene, preferably made of polypropylene, and wherein the hydrophobic coating comprises a polypropylene-polyethylene copolymer.
  • FIG. 1 For example, a pipetting tip made by a method according to the invention is generally designated 10.
  • the pipetting tip 10 extends along a pipetting tip longitudinal axis L from a pipetting opening 12 to a coupling longitudinal end 14.
  • the pipetting tip 10 comprises a first pipetting longitudinal end region 16 which includes the pipetting opening 12, and further comprises a second coupling longitudinal end region 18 which includes the coupling longitudinal end 14.
  • the coupling longitudinal end region 18 is provided in known manner with a coupling inner geometry 20 for releasable positive engagement with a coupling counter-geometry of a pipetting device (see FIG. 2 ).
  • the coupling internal geometry 20 can have a circumferential groove 22 around the pipetting tip longitudinal axis L, into which, in the coupled state of the pipetting tip 10, an elastomer ring squeezed in the axial direction and thus extended in the radial direction (see FIG FIG. 2 ) can engage positively.
  • a pipetting fluid receiving space 24 is advantageously provided into which pipetting fluid aspirates through the pipetting opening 12 and from which pipetting fluid can be dispensed again via the same route.
  • Pipette tip 10 exemplified is preferably injection molded from polypropylene, as this material is less wettable by water than other materials, which, when dispensing pipetting fluid, typically pipetting fluid, desirably facilitates complete emptying of pipette tip 10.
  • a part of the surface of the pipetting tip 10 is made hydrophobic beyond the hydrophobic basic material properties of the preferably used polypropylene.
  • a portion of the pipette tip surface of the inner side 28 of the pipette tip 10 is hydrophobic as the inner hydrophobic region 26, and further, a portion of the surface of the outer surface 30 of the pipette tip 10 is made hydrophobic as the outer hydrophobic region 32.
  • the inner hydrophobicity region 26 and the outer hydrophobicity region 32 coalesce over the edge 34 of the pipetting orifice 12 to form a unitary contiguous hydrophobic surface region of the pipette tip 12.
  • This has the advantage that the edge 34 of the pipetting orifice wetted with pipetting fluid is particularly frequent 12 is hydrophobic, so that the risk of undesired adhesion of Pipettierfluidtröpfchen is at least reduced.
  • the hydrophobic formation of surface areas of the pipette tip 10 is accomplished by providing a defined roughness, such as by providing a surface having a roughness in the range of 220 to 300 nm and with a peak-to-peak roughness in the range of 3000 to 3300 nm.
  • the pipette tip 10 was advantageously immersed first with its outer hydrophobic area 32 in a wetting solution with a polypropylene-polyethylene copolymer dissolved in a xylene-based solvent, so that the entire outer hydrophobic area 32 was wetted by said wetting solution.
  • wetting solution was aspirated into the pipetting fluid receiving space 24 until the surface of the inner side 28 in the region of the inner hydrophobic region 26 was also wetted with wetting solution.
  • the pipetting tip 10 wetted by a residual wetting solution film, was convectively dried in a gas stream after completion of the dispensing process.
  • the wetting solution provided is effectively used, since it is applied only there on the pipette tip 10, where in the later pipetting is actually needed.
  • the axial extent of the inner hydrophobic region 26 is approximately four times the axial extent of the outer hydrophobic region 32. However, this need not be so.
  • the internal hydrophobicity range may also be twice, three times, five times, or a non-integer multiple of the axial extent of the external hydrophobicity region.
  • the pipetting tip 10 preferably at a region closer to the coupling longitudinal end region 18, may have a filter 36 which reduces the risk of aerosol contamination of the distance between the pipetting tip axially located between it and the coupling longitudinal end 14 10 and thus in particular an aerosol contamination of a coupled to the pipette tip 10 pipetting device is used.
  • the filter 36 can be formed, for example, of porous, gas-permeable material in the dry state, for example of sintered plastic, in particular sintered polypropylene and / or polyethylene, and / or of a fiber entanglement.
  • this may, as in FIG. 1 indicated, at least partially, here: about its half axial total extension, also be formed hydrophobic by wetting with the wetting solution described above.
  • the filter 36 is wetted by the hydrophobic coating advantageously worse than in the uncoated state, resulting in that deposited on the filter material pipetting fluid droplets in the deposited state protrude more strongly from the filter material than if the filter material were uncoated, whereby the precipitate on the filter material unwanted Pipettierfluidtröpfchen faster than in the case of an uncoated filter material to close the pores responsible for the gas permeability of the filter material and a Prevent pipetting fluid passage from the pipetting fluid receiving space 24 to the coupling longitudinal end 14 of the pipette tip 10 out advantageous.
  • the filter 36 is thus more appropriate to refer to as a self-regulating moisture-dependent valve, which allows gas to pass in the dry state and to prevent gas passage in the wet state.
  • FIG. 2 a situation is shown which immediately precedes a coating of a portion of the inner surface of a pipetting tip.
  • FIG. 2 The embodiment of the FIG. 2 will be described below only insofar as they differ from that of the FIG. 1 whose description otherwise expressly refers to.
  • the pipette tip 110 of FIG. 2 corresponds exactly in terms of their shape, the pipette tip 10 of FIG. 1 , with the exceptions that the pipette tip 110 has no hydrophobic coating and no filter is provided.
  • the pipetting tip 110 is shown in a state in which it is coupled to a pipetting channel 140.
  • a conical coupling portion 142 corresponding to the conicity of the coupling inner geometry 120 of the pipette tip 110 can be inserted into the pipette tip 110 in the axial direction from the coupling longitudinal end 114.
  • a relative to the coupling portion 142 axially movable Quetschkolben 144 can be displaced in a conventional manner axially to the coupling portion 142 to thereby squeeze axially between a coupling portion 142 and pinch piston 144 elastomer ring and thereby stretch radially.
  • the elastomeric ring 146 in its crimped state can come into positive engagement with the annular groove 122.
  • a receiving cavity 148 in the form of a glass tube is accommodated on the pipetting channel 140, into which wetting solution 150 has been aspirated through the pipetting channel 40.
  • the pipette tip 110 surrounds the receiving cavity 148 so that it is at least partially received in the pipetting fluid receiving space 124 of the pipetting tip 110.
  • the wetting solution 150 will be dispensed from the receiving cavity 148 by overpressure in the pipetting channel 140 so that it will flush at least one portion of the inner surface 128 of the pipetting tip 110 near the pipetting aperture 112.
  • the wetting solution 150 will also be expelled from the pipetting tip 110 through the pipetting opening 112 so that in the pipetting tip 110 a wetted inner hydrophobing section extending from the edge 134 of the pipetting opening 112 in the axial direction over a certain distance into the pipetting fluid receiving space 124 with a desired roughness, which will be completed after its complete drying.
  • the pipette tip 110 is to be at least partially hydrophobic on its outside 130 at a later time, this can be done by simply dipping the pipetting tip into the corresponding wetting solution and then drying the surface section of the pipetting tip 110 so wetted.
  • filter 36 may be not only partially, but completely hydrophobic, preferably by complete wetting with the corresponding wetting solution.

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  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Devices For Use In Laboratory Experiments (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
  • Sampling And Sample Adjustment (AREA)

Claims (7)

  1. Procédé pour le revêtement hydrophobe de pointes de pipetage (10; 110) comprenant un mouillage d'au moins des régions du côté extérieur (30; 130) et du côté intérieur (28; 128) de la pointe de pipetage (10; 110) avec une solution de mouillage,
    caractérisé en ce qu'il comprend les étapes suivantes:
    - accoupler les pointes de pipetage (10; 110) à une source de pression de fluide avec une pression de fluide variable,
    - plonger la pointe de pipetage (10; 110) accouplée dans la solution de mouillage,
    - aspirer de la solution de mouillage dans la pointe de pipetage (10; 110),
    - dispenser la solution de mouillage aspirée,
    - évaporer du solvant contenu dans la solution de mouillage.
  2. Procédé selon la revendication 1,
    caractérisé en ce que le niveau de la colonne de solution de mouillage aspirée dans la pointe de pipetage (10; 110) est différent de la profondeur d'immersion de la pointe de pipetage (10; 110) dans la solution de mouillage, et la dépasse de préférence.
  3. Procédé pour le revêtement hydrophobe de pointes de pipetage (10; 110) comprenant un mouillage d'au moins des régions du côté intérieur (28; 128) de la pointe de pipetage (10; 110) avec une solution de mouillage,
    caractérisé en ce qu'il comprend les étapes suivantes:
    - Prévoir une cavité de réception (148) différente de la pointe de pipetage (110), de préférence un élément de tube, de manière particulièrement préférée un élément de tube en verre, à un dispositif de pipetage (110),
    - plonger la cavité de réception (148) dans la solution de mouillage,
    - aspirer de la solution de mouillage dans la cavité de réception (148),
    - lier la pointe de pipetage (110) à la cavité de réception (148),
    - dispenser la solution de mouillage aspirée de la cavité de réception (148) à travers la pointe de pipetage (110) et ainsi irriguer une section d'espace de réception de fluide de pipetage à l'intérieur de la pointe de pipetage (110),
    - évaporer du solvant contenu dans la solution de mouillage.
  4. Procédé selon une des revendications 1 à 3,
    caractérisé en ce que l'étape de l'évaporation comprend un réchauffement de la pointe de pipetage (10; 110) ou/et une irrigation de pointe de pipetage (10; 110) avec un fluide, de préférence avec un gaz, de manière particulièrement préférée de l'air, en particulier de l'air sec.
  5. Procédé selon une des revendications 1 à 4,
    caractérisé en ce qu'il comprend prévoir la solution de mouillage avec une température comprise entre 65 °C et 85 °C, de préférence comprise entre 70 °C et 80 °C, de manière particulièrement préférée d'environ 75 °C.
  6. Procédé selon une des revendications 1 à 5,
    caractérisé en ce que la solution de mouillage comprend un polymère ou un copolymère, de préférence un copolymère de polypropylène-polyéthylène, et un solvant dissolvant ce dernier, de préférence sur une base de xylol.
  7. Procédé selon une des revendications 3 à 6, se référant à la revendication 3,
    caractérisé en ce que la solution de mouillage est dispensée à travers la pointe de pipetage (10; 110) avec un débit du flux compris entre 0,3 ml/s et 0,7 ml/s, de préférence entre 0,4 ml/s et 0,6 ml/s ou/et que la solution de mouillage est dispensée à travers la pointe de pipetage (10; 110) avec une température comprise entre 20 °C et 30 °C, de préférence entre 21 °C et 25 °C, de manière particulièrement préférée entre 22 °C et 25 °C.
EP11173625.2A 2010-07-12 2011-07-12 Procédé de revêtement hyrophobe d'embouts de pipette Active EP2428272B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102010031240A DE102010031240A1 (de) 2010-07-12 2010-07-12 Pipettierspitze mit hydrophober Oberflächenausbildung

Publications (3)

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EP2428272A2 EP2428272A2 (fr) 2012-03-14
EP2428272A3 EP2428272A3 (fr) 2015-04-29
EP2428272B1 true EP2428272B1 (fr) 2017-08-23

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US (2) US8753715B2 (fr)
EP (1) EP2428272B1 (fr)
JP (2) JP2012073227A (fr)
DE (1) DE102010031240A1 (fr)
NO (1) NO2428272T3 (fr)

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KR101510823B1 (ko) 2014-04-15 2015-04-13 포항공과대학교 산학협력단 피펫 팁
JP6004149B1 (ja) 2015-03-16 2016-10-05 パナソニック株式会社 ピペットチップ及びピペッティング方法
JP6174182B1 (ja) * 2016-03-22 2017-08-02 キヤノンマシナリー株式会社 分注ノズルおよび分注ノズルの製造方法
MX2020000896A (es) * 2017-08-11 2020-09-10 Neomed Inc Conector para transferencia de fluidos.
FR3077995B1 (fr) 2018-02-20 2020-02-14 Gilson Sas Procede de fluoration d'un filtre d'embout de pipette, embout de pipette, son procede de fabrication et pipette associes
WO2020050234A1 (fr) * 2018-09-03 2020-03-12 京セラ株式会社 Capillaire et pipette
CN112827533B (zh) * 2021-01-08 2022-03-08 青岛大学 一种基于超疏水材料的桌面型微液滴化学反应实验平台

Family Cites Families (37)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2067922A (en) * 1934-08-02 1937-01-19 American Can Co Method of coating cans
US3757585A (en) * 1968-08-16 1973-09-11 Heller Labor Pipette apparatus
US4461328A (en) * 1982-06-04 1984-07-24 Drummond Scientific Company Pipette device
DE3635598A1 (de) * 1986-10-20 1988-05-05 Eppendorf Geraetebau Netheler Pipettiervorrichtung mit einem aufsteckkonus fuer eine pipettenspitze sowie pipettenspitze fuer eine solche pipettiervorrichtung
US5051282A (en) * 1988-04-28 1991-09-24 Fuji Photo Film Co., Ltd. Method and apparatus for water-repellent processing of tube
CA1310519C (fr) * 1988-04-29 1992-11-24 Gerald L. Holbrook Methode de commande par retroaction d'un systeme de transmission automatique electronique
JPH03131351A (ja) * 1989-10-16 1991-06-04 Fuji Photo Film Co Ltd 撥水処理されたピペツトチツプ
US5156811A (en) * 1990-11-07 1992-10-20 Continental Laboratory Products, Inc. Pipette device
JP2641075B2 (ja) * 1990-11-28 1997-08-13 富士写真フイルム株式会社 ピペットチップ
FI925118A0 (fi) * 1992-11-11 1992-11-11 Labsystems Oy Behaollare
US5516564A (en) * 1993-04-28 1996-05-14 Costar Corporation Sterile irradiated hydrophobic pipette tip
JP3387649B2 (ja) * 1994-09-16 2003-03-17 富士写真フイルム株式会社 点着チップ
JPH0889820A (ja) * 1994-09-28 1996-04-09 Sumitomo Bakelite Co Ltd ディスペンサー用チップ及びその製造方法
EP0733404A1 (fr) * 1995-03-24 1996-09-25 Becton, Dickinson and Company Embout de pipette
US5785926A (en) * 1995-09-19 1998-07-28 University Of Washington Precision small volume fluid processing apparatus
JP3185646B2 (ja) * 1996-02-14 2001-07-11 トヨタ自動車株式会社 ノズル細孔内への保護膜形成方法
US7268179B2 (en) * 1997-02-03 2007-09-11 Cytonix Corporation Hydrophobic coating compositions, articles coated with said compositions, and processes for manufacturing same
US6475440B1 (en) * 1998-09-16 2002-11-05 Clontech Laboratories, Inc. Applicator for use in deposition of fluid samples onto a substrate surface
DE29919506U1 (de) * 1999-11-05 2000-02-24 Creavis Tech & Innovation Gmbh Mikrostruktuierte Pipetten als Dosiersysteme
EP1269140A4 (fr) * 2000-03-28 2003-05-02 Caliper Techn Corp Procedes permettant de reduire un report fluidique dans des dispositifs microfluidiques
DE10015380A1 (de) * 2000-03-28 2001-10-11 Nmi Univ Tuebingen Mikrofluidkomponente und Verfahren zur Oberflächenbehandlung einer solchen
DE10138037A1 (de) 2001-08-03 2003-02-20 Creavis Tech & Innovation Gmbh Pipettenspitzen mit teilweise strukturierten Oberflächen mit verbesserten Pipettiereigenschaften
JP2003254876A (ja) * 2002-02-28 2003-09-10 Nitto Denko Corp チップ用フィルターおよびチップ
DE10210668A1 (de) * 2002-03-12 2003-09-25 Creavis Tech & Innovation Gmbh Vorrichtung, hergestellt durch Spritzgussverfahren, zur Aufbewahrung von Flüssigkeiten und Verfahren zur Herstellung dieser Vorrichtung
US20050208676A1 (en) * 2004-03-19 2005-09-22 Espir Kahatt Device for aspirating, manipulating, mixing and dispensing nano-volumes of liquids
JP2005270763A (ja) * 2004-03-24 2005-10-06 Seiko Epson Corp 撥液膜形成方法及び撥液膜形成装置
JP4155218B2 (ja) * 2004-03-30 2008-09-24 株式会社島津製作所 オートサンプラ
JP2005324108A (ja) * 2004-05-13 2005-11-24 Honda Motor Co Ltd 細管内壁の樹脂被覆方法
US20070015276A1 (en) * 2005-06-23 2007-01-18 Bioprocessors Corp. Fluid transfer device
JP2007085930A (ja) * 2005-09-22 2007-04-05 Hitachi High-Technologies Corp 金属製プローブの使用方法及び分析装置
JP2007322148A (ja) * 2006-05-30 2007-12-13 Hitachi High-Tech Science Systems Corp 分注管およびそれを用いた分析装置
EP1795264B1 (fr) * 2006-07-06 2012-08-22 Agilent Technologies, Inc. aiguille hydrofuge
JP2008134154A (ja) * 2006-11-28 2008-06-12 Hitachi High-Tech Science Systems Corp 自動分析装置の分注管
WO2008136318A1 (fr) * 2007-04-26 2008-11-13 Toyo Boseki Kabushiki Kaisha Procédé et réacteur d'amplification d'acide nucléique
EP3756767B1 (fr) * 2007-10-02 2024-05-01 Labrador Diagnostics LLC Dispositifs modulaires a utiliser sur place et leurs utilisations
JP5129729B2 (ja) * 2008-02-08 2013-01-30 富士フイルム株式会社 ピペットチップ
US20090220386A1 (en) 2008-02-29 2009-09-03 Ferri Joseph E Porous Sealing Material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

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DE102010031240A1 (de) 2012-01-12
NO2428272T3 (fr) 2018-01-20
JP6140245B2 (ja) 2017-05-31
EP2428272A2 (fr) 2012-03-14
JP2016047531A (ja) 2016-04-07
EP2428272A3 (fr) 2015-04-29
US20120009100A1 (en) 2012-01-12
US8840957B2 (en) 2014-09-23
US8753715B2 (en) 2014-06-17
JP2012073227A (ja) 2012-04-12
US20130280423A1 (en) 2013-10-24

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