EP1862219B1 - Device for holding a pipette tip and pipetting device - Google Patents
Device for holding a pipette tip and pipetting device Download PDFInfo
- Publication number
- EP1862219B1 EP1862219B1 EP06010976.6A EP06010976A EP1862219B1 EP 1862219 B1 EP1862219 B1 EP 1862219B1 EP 06010976 A EP06010976 A EP 06010976A EP 1862219 B1 EP1862219 B1 EP 1862219B1
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- EP
- European Patent Office
- Prior art keywords
- pipette tip
- coupling element
- sealing
- guide
- coupling
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
-
- 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
- B01L3/0275—Interchangeable or disposable dispensing tips
-
- 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
- B01L2200/0689—Sealing
Definitions
- the invention is in the field of dosing and relates to a device for holding and positioning of pipette tips and a pipette tip.
- Pipette tips are elongate, typically tapered, sleeves having a central passageway along the longitudinal axis for metering small quantities of fluid.
- the pipette tips are pushed at their wider end (coupling end) on a suitable holder of a pipetting device and immersed with its pointed end which is axially opposite the wide end in the medium to be pipetted.
- the pipette tips are for single use, i. that they are thrown away after use.
- Pipetting devices are widely used everywhere where relatively small amounts of liquid (for example in the microliter range) have to be dosed, for example in molecular biology.
- the pipetting device may be manual pipetting devices or pipetting or pipetting robots having a single pipetting unit or a plurality of individual pipetting units operated simultaneously or separately.
- the basic mode of operation of a pipetting device is based on the fact that a defined volume of fluid is displaced eg in a cylinder.
- the cylinder is connected on the output side airtight with the passage opening of the pipette tip, so that the displacement of the fluid volume causes a corresponding volume of the medium to be pipetted is sucked at the tip end of the pipette tip.
- the pipette tip must be securely and tightly connected to the pipetting device. This is required to a greater extent in automatic pipetting machines in which the secure seating and precise positioning of the individual pipette tips can not be checked manually.
- pipetting devices should be as low maintenance and inexpensive to produce.
- a holding device with a rigid sealing bead is in US 2003/0000319 described.
- This sealing bead cooperates in the radial direction with a sealing surface of a pipette tip, wherein the wall thickness of the pipette tip in the region of the sealing surfaces is sufficiently thin to ensure easy stretching when pushed onto the sealing bead.
- a radial seal between pipette tip and fixture is in EP 0 351 574 described.
- the holding device has a cylindrical sealing section which corresponds to a sealing section of the pipette tip, the wall thickness in the area of the pipette tip-side sealing section being smaller and thus flexible compared to adjacent areas. This is achieved by a wall thickness weakening on the inside and outside of the pipette wall.
- a pipette tip with elastic cylindrical sealing portion is also in WO 00/27530 described.
- a pipetting device which has an annular pinch seal for radially sealing the pipette tip.
- a displaceable ferrule is pressed axially on the annular pinch seal and this pressed radially outwardly into an annular groove which is formed on the inner wall of the passage opening of the pipette tip.
- a coupling sleeve with an annular stepped shoulder is arranged upstream of the pinch seal axially in the direction of the pipette tip, which serves for the axial and radial positioning of the pipette tip.
- the pipette tip is held and sealed by the pinch seal, which, however, requires moving elements to operate it. This leads to a higher maintenance and equipment costs.
- the pinch seal is subjected to increased wear due to the required flexing work.
- the coupling element may further comprise at least one guide element arranged on its outer side for aligning the pipette tip laterally with respect to the longitudinal axis.
- a holding element for interacting with holding means of the pipette tip to press the sealing portion of the pipette tip against the axial sealing portion and to position the pipette tip in the axial direction.
- the pipette tip is sealed according to the invention by an axially acting seal on the coupling element.
- the coupling element on an elastic sealing element, against which a sealing portion of the pipette tip can be axially pressed.
- the advantage of an axial seal is that it is significantly less susceptible to wear than a radial seal. A radial seal must be rubbed over an outer peripheral surface of the support until it is sufficiently crimped and sealed, or, as in the pinch seal described above WO 00/62933 , is subjected to a great flexing work. In contrast, in the case of an axial seal, the corresponding sealing section only needs to be pressed against the seal. The holder of the invention is thus considerably more durable and low maintenance.
- the sealing element consists of a material which is more elastic in comparison to the material of the coupling element and has a better elastic deformability.
- the sealing element has an axial sealing section, ie a section accessible from the axial direction, for example an end face against which the sealing section of the pipette tip can be pressed axially.
- Sealing and holding element are designed as separate elements.
- the sealing element seals the pipette tip on the coupling element.
- due to the axial sealing effect it also serves as an axial positioning means.
- the pipette tip is not held or fastened by the seal. This function takes over the holding element, which interacts with an associated holding means on the pipette tip and secures this against axial displacement.
- the sealing portion of the pipette tip is pressed against the axial sealing portion of the sealing element and on the one hand reaches the desired sealing effect and on the other hand defines the axial position of the pipette tip by the holding element and sealing element.
- the holding element allows a detachable connection between coupling element and pipette tip.
- the lateral or radial alignment of the pipette tip on the coupling element is advantageously ensured by cooperation of the holder-side guide element with corresponding guide elements, typically cylindrical surfaces on the inner wall of the pipette tip.
- the separation of sealing and holding function as well as lateral guidance is particularly advantageous in pipetting machines, since it makes it possible to precisely define the axial alignment (z position) through the interaction of the axial seal and holding element. On the other hand, a radial pinch seal could prevent a defined axial positioning. Furthermore, the mounting device according to the invention has a low-wear seal and allows accurate positioning of the pipette tip and their secure support.
- the integrated cylindrical guide surface should preferably run longitudinally parallel to the longitudinal axis. This ensures that the pipette tip assumes a defined radial position in interaction of its guide surface with a guide element of the holder regardless of its axial position. The pipette tip can therefore be pushed onto the holder without the guide surface hindering an axial relative movement of the pipette tip and the holder with respect to one another. The guide surface therefore only results in a radial alignment of the pipette tip without affecting its axial positioning, i. axial and radial alignment are separated.
- the inner wall has in the longitudinal axis direction with respect to the longitudinal axis typically at an angle greater than or equal to 0.2 °, preferably between 0.5 ° and 3 °, in particular between 0.5 ° and 1 °. Due to the relatively low angle, the inner wall is formed as Entformungsschräge for easier removal of the prepared pipette tip from an injection mold at a comparatively small taper of the hollow cross-section.
- the coupling section may furthermore have a first section and a second section axially staggered with respect to the first section in the sliding direction, the first section having a smaller radial extent than the second section.
- the coupling section may have a sealing section between the first and second sections with a sealing surface facing axially in the sliding direction for interacting with a sealing element of the holder and one on the inner wall of the second section arranged holding means for interacting with a holding element of the holder.
- the retaining means may be an undercut formed on the inner wall of the second section.
- the pipette tip is an injection molded part, with the inner walls of the first and second portions being parallel to the longitudinal axis, i. have no draft angles.
- the coupling portion, and in particular the second portion of the pipette tip comprise a region which is made more flexible with respect to the remaining regions of the coupling portion or the second portion and is arranged towards the first axial end. The flexible area facilitates the placement and stripping of the pipette tip from the holder.
- the coupling section or in the second section of the coupling section in the longitudinal direction incisions and to fill them with a second material that is more elastic than the material from which the remaining areas of the coupling portion or of the second section.
- the coupling section therefore consists of different materials.
- the sealing portion may be formed by a shoulder or shoulder between the first and second portions.
- the holding element may be a flexible element, which is suitably mounted on the outside of the coupling element, or integrally formed on the outside or be separately attached to the outside rigid or elastic element, for example, one or more radial projections, which are partially or annular circumferentially distributed.
- a pipetting device with a coupling element and a detachable attachable to the coupling element pipette tip is proposed with a sealing portion, wherein the coupling element has an axially extending longitudinal axis and has a free end, from which the pipette tip on the coupling element in the axial direction pushed is.
- the coupling element further has a sealing element made of an elastic material which has an axial and radially extending sealing section exposed in the axial direction towards the free end of the coupling section.
- the sealing portion of the pipette tip is preferably designed with respect to the longitudinal axis of the coupling element as an axial surface facing in the direction of the coupling element, and can be formed for example by a shoulder.
- the coupling element of the pipetting device may additionally individually or in combination, the properties of the above-described separate coupling element, for example, in view of the properties and the material of the sealing element, the number, design and arrangement of guide elements or the number, design and arrangement of holding elements.
- a pipetting device with a coupling element and a pipette tip detachably attachable to the coupling element wherein the coupling element has at least one guide element arranged on its outside for laterally aligning the pipette tip, and preferably comprises as many guide elements as the pipette tip has guide surfaces.
- the one or more guide element (s) may be formed independently of one another preferably in one piece or in several parts.
- the pipette tip has a longitudinal axis and a coupling section extending in the longitudinal axis for pushing onto the holder.
- the coupling section further has at least one section with an inner wall tapering at least in sections opposite the direction of slipping into which a guide surface which is cylindrical relative to the longitudinal axis is integrated for interacting with the at least one coupling-side guide element.
- the one or more guide element (s) on the coupling element is (are) designed so that each guide element has at least partial surfaces of a cylindrical lateral surface which corresponds in each case to an interacting with the partial surface cylindrical guide surface on the pipette tip.
- the pipette tip can individually or in combination have the properties of the separate pipette tip already described above, for example with regard to the properties, the material, the configuration and arrangement of the inner wall, special sections or holding elements.
- the coupling element of the pipetting device can also here additionally or individually in combination have the properties of the above-described separate coupling element, for example with regard to the number, configuration and arrangement of guide elements.
- the coupling element may comprise a sealing element with properties, configurations and suitable materials already described above and one or more holding elements already described above with regard to number, configuration and arrangement.
- the coupling element can furthermore have at least one holding element arranged on its outside for interacting with at least one holding means of the pipette tip.
- the at least one holding element can be designed to be rigid relative to the at least one holding means.
- the at least one holding element can also be designed to be flexible with respect to the at least one holding means.
- the holder according to the invention has for this purpose a coupling element with a particular cylindrical base body, which comprises an elastic sealing element with axially exposed in the direction of the free end of the holder and at least partially radially extending sealing portion. Against this sealing portion can be pushed axially a corresponding sealing portion of a pipette tip. The sealing effect is achieved by axial pressing against the sealing element.
- the sealing element consists of a fluoroelastomer and can be embodied for example as an O-ring or as an X-ring, where O and X refers to the cross section of the ring material.
- cross sections such as hollow or V cross sections are also possible.
- a material elasticity in cross section is to be achieved, i. the cross section of the sealing element is elastic, in particular deformable in the longitudinal direction of the coupling element, and therefore allows a very good axial sealing effect.
- the coupling element furthermore has at least one guide element for lateral positioning and alignment of the pipette tip with respect to the longitudinal axis of the holder.
- the guide element can be formed radially, preferably with a constant radial extent around the coupling element, wherein it may consist of sub-elements. In this case, the guide element project radially beyond adjacent sections of the outside of the coupling element.
- the guide element thus has a greater radial extent than adjacent portions of the coupling element. This ensures that a radial contact between the coupling element and the pipette tip is produced essentially only via the guide element and thus the guide element determines the lateral or radial position of the pipette tip.
- the guide element bears against the inner wall of the pipette tip, which in turn may have corresponding guide elements or guide surfaces.
- the guide element can be annular.
- the holder-side guide element is, in particular, cylindrical guide surfaces or partial surfaces with respect to the longitudinal axis of the coupling element.
- the lateral guidance and orientation of the pipette tip is independent of axial positioning means.
- the coupling element may have two axially spaced-apart guide elements on its outer side.
- the lateral or radial alignment or positioning of the pipette tip is further improved.
- an improved coaxial alignment of coupling element and pipette tip is achieved, i. that a tilting or oblique holding the pipette tip is prevented on the holder. This is particularly advantageous in pipetting machines with a large number of simultaneously actuated pipette tips, which are arranged in a matrix, for example.
- both guide elements have an axial distance which is at least as great as their greatest radial extent.
- the axial distance of the guide elements is understood to mean the distance between the contact regions or contact edges which are furthest apart from one another.
- the guide elements can define guide rings, which run radially around the coupling element and have a different radial extent or different outer diameters.
- the axial distance is defined by the respective outer edge or outline of the guide surface, ie the outer edges, which are axially farthest from each other.
- the guide rings can be designed either as continuous circumferential rings or as interrupted rings. It is also possible to form a guide ring as a continuous circumferential ring and the other guide ring as a broken ring.
- the guide element or the guide ring or the guide rings may have a certain axial extent, so that thereby guide surfaces are defined whose axial width substantially corresponds to the axial extent of the guide rings and the guide element. It is also possible to reduce the axial extent of the guide element or the guide rings or the extent that a substantially linear contact between the guide element and the pipette tip remains.
- the coupling element has two guide elements with different radial extent or outer diameter, wherein the axial distance of the two guide elements to each other is at least as large as the larger of the two outer diameter.
- the coupling element has a first portion, which is arranged near the free end or at the free end of the coupling element, and a second portion, which is arranged offset axially in the sliding direction to the first portion on.
- the sections are substantially cylindrical.
- Each section may comprise a guide element, wherein in particular the first end facing the free end preferably has at each point a smaller radial extent than the second section. This defines a step between the two sections on which the sealing element can be arranged.
- the sealing element is therefore preferably between the first and second section and projects beyond in the radial direction typically the first portion and the guide element located there, so that a part of the sealing element is freely accessible axially from the free end of the coupling element ago.
- an inner stepped shoulder of the pipette tip can be pressed, which is formed by a radially encircling and axially facing sealing surface.
- the coupling element furthermore has at least one holding element, which is arranged on the outside of the coupling element, interacts with corresponding holding means of the pipette tip and removably fixes the pipette tip.
- the retaining element causes a particular axial fixation, thereby simultaneously the sealing portion of the pipette tip is pressed axially against the axial sealing portion of the coupling element.
- a safe and well-defined axial positioning of the pipette tip is achieved by the interaction of sealing element with sealant on the one hand and holding element and retaining means on the other hand.
- the holding element may be flexible or rigid.
- the retaining element may be a flexible tensioning element, e.g. be a circumferential spring element which is arranged in a located on the outside of the coupling element circumferential recess.
- Flexible holding elements allow the pipette tip to be pushed on or off with little effort.
- flexible holding elements are relatively low wear and relatively fault tolerant because they can compensate for manufacturing tolerances due to their flexibility, for example, the pipette tip partially.
- the holding element may also be rigid and, for example, individual radial elevations, for example, rigid cams, which are preferably distributed annularly around the coupling element.
- a non-annular distribution or a continuous ring are suitable as rigid holding elements. Rigid holding elements have the advantage over flexible holding elements that they allow a more accurate centering of the pipette tip.
- this can engage in a radially circumferential undercut on the pipette tip, which is typically arranged on the inner wall of the passage opening of the pipette tip.
- the holding element is arranged in the direction of sliding behind the guide elements or arranged. This ensures that the sealing element is in front of the retaining element in the direction of the free end of the coupling element and thereby protects the retaining element against accidental contamination with the medium to be pipetted.
- the holding device comprises an axisymmetric, typically substantially cylindrical coupling element 4 with a longitudinal axis 6 and an axially disposed passage opening 5.
- the coupling element has a front free end 8. From the free end 8, a pipette tip 10 can be pushed onto the coupling element 4.
- the pipette tip 10 is formed axially symmetrical and has near its rear end (coupling end and first axial end) 12 a coupling portion 14 which is pushed onto the coupling element 4.
- the pipette tip runs from its coupling section 14 to its - not shown here - front tip end conically and there has a suction port for sucking the medium to be pipetted.
- the pipette tip is typically intended for single use and designed as an injection molded part.
- a suitable material for pipette tips that is easy to process is polypropylene, which is injected in liquid form and optionally with additives (e.g., paint) and / or fillers into a suitable injection mold. After solidification of the polypropylene, the finished pipette tip is ejected from the injection mold and removed if necessary, the gate.
- the coupling element 4 is typically integrally formed from metal and has at its free end 8 a first portion 20.
- a second portion 22 of the coupling element 4 is arranged axially offset in the sliding direction 2 with respect to the first portion 20.
- the first portion 20 preferably has at each point a smaller radial extent than the second portion 22, so that the second, in the sliding direction 2 rear portion 22 projects radially beyond the first portion 20.
- On the outside of each section is in each case a guide element 25, 26 arranged in the form of a circumferential cylindrical guide surface.
- the guide surfaces 25, 26, which extend in the longitudinal direction parallel to the longitudinal axis 6, have a greater radial extent than adjacent regions of the respective sections 20, 22, over which they extend radially.
- the two guide elements 25, 26 have an axial distance d, which is at least as large as the diameter D (radial extent) of the larger of the two guide elements, in this case the second guide member 26.
- the distance d is here by the Distance between the respective outer edges 28, 29 of the guide elements 25, 26 defined. These outer edges form the axial end portions of the contact between the guide elements or guide surfaces 25, 26 and the pipette tip.
- the coupling section 14 of the pipette tip 10 likewise has a first section 40 and a second section 42, wherein the first section 40 has a smaller radial extent (diameter) than the second section 42.
- a step or shoulder 43 is formed between the first and second sections 40, 42, which serves as a sealing surface 43.
- the first and second guide members 25 and 26 are formed substantially the same in the illustrated embodiment. However, it is also possible to give the guide elements each a different shape.
- the guide elements 25, 26 are formed circumferentially and rise with respect to the surrounding outer contour of the respective coupling element side portions 20, 22 in the form of an integrally formed ring with a circumferential guide surface whose cross-section is trapezoidal.
- the sealing element is conveniently a ring seal made of an elastic material.
- fluoroelastomers have been found to be suitable materials since they have high elasticity, longevity, high chemical resistance and low wear.
- the sealing element is designed as a solid, rectangular in cross-section ring. However, it is also possible to use ring seals with circular (O-rings) or X-shaped cross section.
- a sealing element 21 'with an X-shaped cross-section is, for example, in FIG FIG. 4 shown.
- the sealing element 21 ' has four sealing lips, wherein the radially outwardly to the free end 12 facing the sealing lip 23', the axial sealing portion 23, against which the corresponding sealing portion of the pipette tip is pressed.
- sealing element 21 has approximately the same radial extent as the second portion 22 and thereby projects beyond the first portion 20 in the radial direction. Therefore, a sealing portion 23 is axially free toward the open end 8 of the coupling element 4 substantially.
- the sealing portion 23 serves as an axial sealing surface and is pressed axially against the circumferentially formed inner shoulder 43 of the pipette tip 10.
- FIG. 2 recognizable which shows a completely attached to the coupling element 4 pipette tip 10
- the sealing element 21 is only with its axial sealing portion 23 in direct contact with the inner wall of the pipette tip and in particular with the shoulder 43. This will be an axial seal and at the same time a z-orientation reached.
- the z-orientation is further defined by a holding element, which will be described below.
- the sealing element 21 has a slightly smaller outer diameter compared to the inner diameter of the second section 42 of the pipette tip. This ensures that the inner wall of the pipette tip when sliding is not rubbed over the sealing element 21, whereby it is considerably less stressed than radial seals that must be pushed to achieve a sufficient sealing effect rubbing over usually tapered surfaces. Therefore, the maintenance of the inventive axial sealing element 21 is considerably lower.
- a radial contact between coupling element 4 and pipette tip 10 is produced via the coupling element-side guide elements 25 and 26 and via first and second guide surfaces 45 and 46 of the coupling section 14 of the pipette tip 10.
- the pipette tip-side guide surfaces 45, 46 can be formed by the inner walls of the respective sections 40, 42 of the pipette tip 10. However, it is also possible to form raised guide surfaces on the inner wall of the pipette tip.
- Each section of the pipette tip-side coupling section 14 has a guide surface 45, 46 which runs continuously around or consists of circumferentially distributed partial segments whose diameter corresponds to the outer diameter of the respective associated first and second guide elements 25, 26, so that a positive alignment of the pipette tip 10 is achieved.
- the corresponding guide surfaces 45, 46 no draft angles.
- Entformungsschrägen are usually provided on injection molded parts in order to solve this easier of the injection mold can.
- the pipette tip-side guide surfaces extending in the axial direction parallel to the axis 6. This ensures that the radial or lateral orientation of the pipette tip does not depend on how far the pipette tip is pushed onto the coupling element.
- tapered guide surfaces they would be increasingly clamped when sliding the pipette tip on the coupling element on the coupling element and thereby oppose the axial movement of a resistance.
- conical guide surfaces affect the axial alignment and increase the required Aufschiebekraft.
- annular groove 30 for receiving an annular spring 27 is introduced.
- the annular spring 27 serves as a holding element and engages in an undercut 47 on the inside of the second portion 42 of the pipette tip.
- the pipette tip is pushed forward with its rear end 12 on the second guide member 26 and the annular spring 27 until the annular spring 27 snaps into the rear portion 47.
- the pipette tip is positioned axially and fixed on the coupling element.
- Ring spring 27 and undercut 47 make a detachable connection, which is also sufficiently stable to axially push the shoulder 43 against the axial sealing portion 23 and thus seal the pipette tip on the coupling element.
- the ring spring can have a slight screw thread.
- the annular groove 30 is executed in the present embodiment with an inclined inner wall 31 which tapers conically to the front end 8 of the coupling element. This ensures that the annular spring 27 is axially positioned exactly towards the free end 8, since it is slightly compressed radially by the pipette tip, due to the conical inner wall 31 dodges in the direction of abutment surface 50 and pressed against this and positioned. Thus, a frictional connection results from the sealing element 21 via the Pipette-side sealing portion 43 to the undercut 47, which leads the power flow through the annular spring 27 to the stop surface 50. As a result, the pipette tip is securely attached to the coupling element and aligned.
- FIG. 3 Another embodiment shows FIG. 3 ,
- an annular groove arranged in an annular spring rigid cams 57 are used as a holding element, which are distributed uniformly on the circumference of the second portion.
- the cams 57 are integrally formed as a circumferential raised ring which is interrupted by cuts.
- the material stress of the coupling portion of the pipette tip several separate rigid cam are cheaper than a continuous ring, as this would enforce a strong expansion of the rear end 12 of the coupling portion 14 when sliding the pipette tip.
- the cams 57 engage in an undercut 47 at the pipette tip.
- FIGS. 5 to 7 show a further embodiment.
- an annular spring (not shown) is used as a holding element, which is arranged in an annular groove 60 with parallel side walls 61, 62 and V-shaped inner wall 63.
- the annular groove 60 has the advantage that on the one hand the annular spring defined in the axial direction and stored on the other hand is elastically deformable in the radial direction. This facilitates the placement of the pipette tip and leads to a longevity of the annular spring.
- FIGS. 6 and 7 Details of the annular groove 60 and the first and second portions 25, 26 of the coupling element are shown. In addition, these figures show the respective guide elements, as they can be used in the other embodiments.
- the V-shaped inner wall 63 (FIG. FIG. 6 ) comprises two partial surfaces which are at an obtuse angle to each other, wherein these are arranged symmetrically with respect to the axis 6.
- the second guide element 26 projects beyond surrounding regions of the coupling element-side second section 22.
- symmetrically formed start flanks 65, 66 are integrally formed laterally relative to the second guide element 26.
- first section 20 ( FIG. 7 ) is formed axially to the first guide member 25 also has a rear approach flanks 67 and a front cone-shaped insertion bevel 68 for pre-centering the pipette tip.
- the to the free end 8 extending chamfer 68 terminates at an end face 69 on which the through hole 5 ends.
- the coupling elements described above can be arranged on manual pipette holders but also on automatic pipetting machines which have many coupling elements.
- Such automatic pipetting machines also have further components, in particular means for stripping the pipette tips.
- these means comprise a relative to the coupling element in the axial direction movable scraper, which engages behind the rear end 12 of the pipette tip 10 and pushes against the Aufschiebraum 2 from the coupling element.
- FIG. 8 a section 42 of the pipette-side coupling section is shown enlarged.
- This section has a tapered inner wall 70.
- the cone angle (angle between Innwand 70 and longitudinal axis 6) is only a few degrees and is preferably between 0.5 ° and 1 °.
- This slightly conical design is a so-called Entformungsschräge to solve the injection molded part shaped pipette tip easier from the injection mold.
- the outer wall 71 of the coupling portion is also cone-shaped for this reason.
- a cylindrical guide surface 72 is integrated, ie, the guide surface 72 extends in the longitudinal direction parallel to the longitudinal axis 6.
- a shoulder 74 between guide surface 72 and inner wall is formed, the depth of the cone angle and the longitudinal extent of the guide surface 72 depends. It is favorable if the guide surface merges directly into the conical inner wall 70 towards the far end of the cone.
- FIG. 9 shows an embodiment with improved flexibility of the pipette side coupling portion 14.
- the coupling portion 14 (or the second portion of the pipette tip) has longitudinal cuts 82 which are filled with a separate material to form axial soft components.
- the material 82 of the axial soft components 82 is compared to the material 80, of which the main part of the coupling portion 14 is made, elastic and thereby increases the radial flexibility of the coupling portion.
- the incisions 82 can, as in FIG. 9 indicated, pass through the undercut 34 for receiving the coupling element-side holding element.
- an injection molding process can likewise be used.
- the pipette tip furthermore has a section 84 attached to the coupling section 14 and conically tapered in the axial direction, which has an opening for sucking in a medium to be pipetted at its axial end remote from the coupling section 14.
- the pipette tip may be polypropylene and filled with graphite to allow for capacitive level measurements.
- the sealing element may in all embodiments consist of fluoroelastomer, e.g. Viton® or Kalrez® from DuPont. Other elastic materials are also suitable, depending on the medium to be pipetted.
- the coupling elements which are also often referred to as a mandrel, are made of a preferably corrosion-resistant metal, e.g. Stainless steel or other alloys, e.g. Tantalum, titanium or tungsten included.
- Stainless steel or other alloys, e.g. Tantalum, titanium or tungsten included.
- suitable e.g. produce conductive plastic.
- composites of different materials are possible, e.g. Stainless steel with plastic inserts or compounds of different conductive and non-conductive plastics.
- the embodiments described above have in common that they allow the placement and stripping of the pipette tip with relatively little effort. This is achieved on the one hand by the coupling element-side flexible holding elements and on the other by flexible regions of the rear end 12 of the pipette tip.
- all coupling elements on a low-wear or even wear-free seal since the sealing element is designed as an axial sealing element.
- the Guide elements allow accurate radial or lateral (x and y direction) positioning and prevent tilting of the pipette tip.
- the axial positioning (z-direction) is determined on the one hand by the interaction of coupling element-side holding element with pipette tip side holding means and on the other hand by the pressing of the shoulder 43 against the sealing element 21.
- the seal and the attachment are thus spatially and functionally separated from each other and allow a positionally secure attachment of the pipette tip on the coupling element. Both the pipette tip and the coupling element can be produced inexpensively and are robust in use.
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Description
Die Erfindung liegt auf dem Gebiet der Dosiertechnik und betrifft eine Vorrichtung zur Halterung und Positionierung von Pipettenspitzen sowie eine Pipettenspitze.The invention is in the field of dosing and relates to a device for holding and positioning of pipette tips and a pipette tip.
Pipettenspitzen sind langgestreckte, typischerweise konisch zulaufende Hülsen mit einer zentralen, entlang der Längsachse verlaufenden Durchgangsöffnung zum Dosieren von kleinen Flüssigkeitsmengen. Die Pipettenspitzen werden an ihrem breiteren Ende (Koppelende) auf eine geeignete Halterung einer Pipettiervorrichtung geschoben und mit ihrem spitzen Ende, das dem breiten Ende axial gegenüber liegt, in das zu pipettierende Medium getaucht. Typischerweise sind die Pipettenspitzen zum Einmalgebrauch bestimmt, d.h. daß sie nach erfolgter Verwendung weggeworfen werden.Pipette tips are elongate, typically tapered, sleeves having a central passageway along the longitudinal axis for metering small quantities of fluid. The pipette tips are pushed at their wider end (coupling end) on a suitable holder of a pipetting device and immersed with its pointed end which is axially opposite the wide end in the medium to be pipetted. Typically, the pipette tips are for single use, i. that they are thrown away after use.
Große Anwendung finden Pipettiervorrichtungen überall dort, wo relativ kleine Flüssigkeitsmengen (z.B. im Mikroliterbereich) dosiert werden müssen, beispielsweise in der Molekularbiologie. Bei der Pipettiervorrichtung kann es sich um manuelle Pipettiervorrichtungen oder um Pipettierautomaten oder Pipettierroboter handeln, die eine einzelne Pipettiereinheit oder eine Vielzahl von einzelnen Pipettiereinheiten aufweisen, die gleichzeitig oder separat betätigt werden.Pipetting devices are widely used everywhere where relatively small amounts of liquid (for example in the microliter range) have to be dosed, for example in molecular biology. The pipetting device may be manual pipetting devices or pipetting or pipetting robots having a single pipetting unit or a plurality of individual pipetting units operated simultaneously or separately.
Die prinzipielle Funktionsweise einer Pipettiervorrichtung beruht darauf, daß ein definiertes Fluidvolumen z.B. in einem Zylinder verschoben wird. Der Zylinder ist dabei ausgangsseitig luftdicht mit der Durchgangsöffnung der Pipettenspitze verbunden, so daß die Verschiebung des Fluidvolumens dazu führt, daß ein entsprechendes Volumen des zu pipettierenden Mediums am spitzen Ende der Pipettenspitze angesaugt wird. Um ein genaues Dosieren zu gewährleisten, muß die Pipettenspitze sicher und dicht mit der Pipettiervorrichtung verbunden werden. Dies ist in erhöhtem Maße bei Pipettierautomaten erforderlich, bei denen der sichere Sitz und die präzise Positionierung der einzelnen Pipettenspitzen nicht manuell überprüft werden kann. Außerdem sollen Pipettiervorrichtungen möglichst wartungsarm und kostengünstig herstellbar sein.The basic mode of operation of a pipetting device is based on the fact that a defined volume of fluid is displaced eg in a cylinder. The cylinder is connected on the output side airtight with the passage opening of the pipette tip, so that the displacement of the fluid volume causes a corresponding volume of the medium to be pipetted is sucked at the tip end of the pipette tip. To ensure accurate dosing, the pipette tip must be securely and tightly connected to the pipetting device. This is required to a greater extent in automatic pipetting machines in which the secure seating and precise positioning of the individual pipette tips can not be checked manually. In addition, pipetting devices should be as low maintenance and inexpensive to produce.
Es ist eine Reihe von Pipettiervorrichtungen mit Haltevorrichtungen zur Aufnahme von Pipettenspitzen bekannt. So beschreiben beispielsweise
Aufwendig ausgeführte radiale Dichtungen sind auch in
Zur axialen Ausrichtung der Pipettenspitzen, d.h. in z-Richtung, können zusätzlich axiale Ausrichtmittel vorgesehen werden. Diese sind z.B. in
Alle vorgenannten Pipettenspitzen werden durch die Quetschung der umlaufenden Dichtung an der Außenumfangsfläche der Halterung gehalten. Eine Fixierung mit separaten Rastrippen zeigt dagegen
Eine Haltevorrichtung mit einer starren Dichtwulst ist in
Eine radiale Dichtung zwischen Pipettenspitze und Haltevorrichtung ist in
Aus
Vor diesem Hintergrund liegt daher der Erfindung die Aufgabe zugrunde, eine Vorrichtung zur Halterung von Pipettenspitzen bzw. entsprechende Pipettenspitzen bereitzustellen, mit denen ein genaues Dosieren möglich ist und die vorzugsweise im Vergleich zum Stand der Technik verbesserte Produkteigenschaften im Hinblick auf den Verschleiß, die Wartung und die Herstellungskosten aufweisen. Erfindungsgemäß wird daher eine Vorrichtung zur Halterung von Pipettenspitzen mit einem Koppelelement mit einer in axialer Richtung verlaufenden Längsachse vorgeschlagen, welches ein freies Ende aufweist, von dem aus eine Pipettenspitze auf das Koppelelement in axialer Richtung aufschiebbar ist, wobei das Koppelelement aufweist:
- ein Dichtelement aus einem elastischen Material, das einen in axialer Richtung zum freien Ende des Koppelelements hin freiliegenden axialen und sich radial ersteckenden Dichtabschnitt aufweist, gegen den ein Dichtabschnitt der Pipettenspitze zumindest teilweise axial preßbar ist.
- a sealing element made of an elastic material which has an axial and radially ersteckenden sealing portion exposed in the axial direction to the free end of the coupling element, against which a sealing portion of the pipette tip is at least partially axially pressed.
Gemäß einem Aspekt der Erfindung kann das Koppelelement weiterhin zumindest ein an seiner Außenseite angeordnetes Führungselement zum in bezug auf die Längsachse lateralen Ausrichten der Pipettenspitze aufweisen.According to one aspect of the invention, the coupling element may further comprise at least one guide element arranged on its outer side for aligning the pipette tip laterally with respect to the longitudinal axis.
Nach einem weiteren Aspekt der Erfindung kann an der Außenseite des Koppelelements ein Halteelement zum Wechselwirken mit Haltemitteln der Pipettenspitze angeordnet sein, um den Dichtabschnitt der Pipettenspitze gegen den axialen Dichtabschnitt zu pressen und die Pipettenspitze in axialer Richtung zu positionieren.According to a further aspect of the invention may be arranged on the outside of the coupling element, a holding element for interacting with holding means of the pipette tip to press the sealing portion of the pipette tip against the axial sealing portion and to position the pipette tip in the axial direction.
Die Pipettenspitze wird erfindungsgemäß durch eine axial wirkende Dichtung am Koppelelement abgedichtet. Dazu weist das Koppelelement ein elastisches Dichtelement auf, gegen das ein Dichtabschnitt der Pipettenspitze axial gepreßt werden kann. Der Vorteil einer axialen Dichtung ist, daß diese erheblich verschleißärmer als eine radiale Dichtung ist. Eine radiale Dichtung muß reibend über eine Außenumfangsfläche der Halterung geschoben werden, bis sie ausreichend gequetscht ist und damit dichtet, oder, wie bei der weiter oben beschriebenen Quetschdichtung der
Weiterhin sind Dichtung und Halterung bzw. Befestigung in vorteilhafter Weise sowohl räumlich als auch funktionell voneinander getrennt, d.h. Dicht- und Halteelement sind als separate Elemente ausgeführt. Das Dichtelement dichtet die Pipettenspitze am Koppelelement ab. Darüber hinaus dient es, aufgrund der axialen Dichtwirkung, auch als ein axiales Positionierungsmittel. Allerdings wird die Pipettenspitze durch die Dichtung nicht gehalten bzw. befestigt. Diese Funktion übernimmt das Haltelement, welches mit einem zugeordneten Haltemittel an der Pipettenspitze wechselwirkt und diese gegen ein axiales Verschieben sichert. Dabei wird gleichzeitig der Dichtabschnitt der Pipettenspitze gegen den axialen Dichtabschnitt des Dichtelements gepreßt und einerseits die gewünschte Dichtwirkung erreicht und andererseits die axiale Position der Pipettenspitze durch das Halteelement und Dichtelement definiert. Das Halteelement erlaubt eine lösbare Verbindung zwischen Koppelelement und Pipettenspitze.Furthermore, the gasket and fixture are advantageously separated both spatially and functionally, i. Sealing and holding element are designed as separate elements. The sealing element seals the pipette tip on the coupling element. Moreover, due to the axial sealing effect, it also serves as an axial positioning means. However, the pipette tip is not held or fastened by the seal. This function takes over the holding element, which interacts with an associated holding means on the pipette tip and secures this against axial displacement. At the same time the sealing portion of the pipette tip is pressed against the axial sealing portion of the sealing element and on the one hand reaches the desired sealing effect and on the other hand defines the axial position of the pipette tip by the holding element and sealing element. The holding element allows a detachable connection between coupling element and pipette tip.
Schließlich wird in vorteilhafter Weise die laterale oder radiale Ausrichtung der Pipettenspitze am Koppelelement durch Zusammenwirken des halterungsseitigen Führungselements mit entsprechenden Führungselementen, typischerweise Zylinderflächen an der Innenwand der Pipettenspitze, gewährleistet.Finally, the lateral or radial alignment of the pipette tip on the coupling element is advantageously ensured by cooperation of the holder-side guide element with corresponding guide elements, typically cylindrical surfaces on the inner wall of the pipette tip.
Die Trennung von Dichtungs- und Halterungsfunktion sowie lateraler Führung ist insbesondere bei Pipettierautomaten von Vorteil, da sie es ermöglicht, die axiale Ausrichtung (z-Position) durch das Zusammenwirken von axialer Dichtung und Halteelement genau zu definieren. Eine radiale Quetschdichtung könnte dagegen eine definierte axiale Positionierung verhindern. Weiterhin weist die erfindungsgemäße Halterungsvorrichtung eine verschleißarme Dichtung auf und gestattet eine genaue Positionierung der Pipettenspitze sowie deren sichere Halterung.The separation of sealing and holding function as well as lateral guidance is particularly advantageous in pipetting machines, since it makes it possible to precisely define the axial alignment (z position) through the interaction of the axial seal and holding element. On the other hand, a radial pinch seal could prevent a defined axial positioning. Furthermore, the mounting device according to the invention has a low-wear seal and allows accurate positioning of the pipette tip and their secure support.
Die Erfindung betrifft weiterhin eine Pipettenspitze zum Aufsetzen auf eine Halterung, wobei die Pipettenspitze aufweist:
- eine um eine Längsachse verlaufende Mantelfläche;
- einen Koppelabschnitt in der Nähe eines ersten axialen Endes der Pipettenspitze,
- a circumferential surface extending about a longitudinal axis;
- a coupling portion near a first axial end of the pipette tip,
Die integrierte zylindrische Führungsfläche sollte vorzugsweise in Längsrichtung parallel zur Längsachse verlaufen. Dadurch wird erreicht, daß die Pipettenspitze bei Wechselwirkung ihrer Führungsfläche mit einem Führungselement der Halterung unabhängig von ihrer axialen Position eine definierte radiale Position einnimmt. Die Pipettenspitze kann daher auf die Halterung aufgeschoben werden, ohne daß die Führungsfläche eine axiale Relativbewegung von Pipettenspitze und Halterung zueinander behindert. Die Führungsfläche führt daher lediglich zu einer radialen Ausrichtung der Pipettenspitze ohne deren axiale Positionierung zu beeinflussen, d.h. axiale und radiale Ausrichtung sind getrennt.The integrated cylindrical guide surface should preferably run longitudinally parallel to the longitudinal axis. This ensures that the pipette tip assumes a defined radial position in interaction of its guide surface with a guide element of the holder regardless of its axial position. The pipette tip can therefore be pushed onto the holder without the guide surface hindering an axial relative movement of the pipette tip and the holder with respect to one another. The guide surface therefore only results in a radial alignment of the pipette tip without affecting its axial positioning, i. axial and radial alignment are separated.
Die Innenwand weist in Längsachsenrichtung in bezug auf die Längsachse typischerweise einen Winkel größer oder gleich 0,2°, bevorzugt zwischen 0,5° und 3° auf insbesondere zwischen 0,5° und 1° auf. Durch den relativ geringen Winkel wird die Innenwand als Entformungsschräge zum leichteren Entfernen der hergestellten Pipettenspitze aus einer Spritzgußform bei vergleichsweise geringer Verjüngung des Hohlquerschnitts ausgeformt.The inner wall has in the longitudinal axis direction with respect to the longitudinal axis typically at an angle greater than or equal to 0.2 °, preferably between 0.5 ° and 3 °, in particular between 0.5 ° and 1 °. Due to the relatively low angle, the inner wall is formed as Entformungsschräge for easier removal of the prepared pipette tip from an injection mold at a comparatively small taper of the hollow cross-section.
Der Koppelabschnitt kann weiterhin einen ersten Abschnitt und einen zum ersten Abschnitt in Aufschiebrichtung axial versetzt angeordneten zweiten Abschnitt haben, wobei der erste Abschnitt eine kleinere radiale Ausdehnung als der zweite Abschnitt aufweist. Zusätzlich kann der Koppelabschnitt einen Dichtabschnitt zwischen erstem und zweitem Abschnitt mit axial in Aufschiebrichtung weisender Dichtfläche zum Wechselwirken mit einem Dichtelement der Halterung sowie ein an der Innenwand des zweiten Abschnitts angeordnetes Haltemittel zum Wechselwirken mit einem Halteelement der Halterung aufweisen.The coupling section may furthermore have a first section and a second section axially staggered with respect to the first section in the sliding direction, the first section having a smaller radial extent than the second section. In addition, the coupling section may have a sealing section between the first and second sections with a sealing surface facing axially in the sliding direction for interacting with a sealing element of the holder and one on the inner wall of the second section arranged holding means for interacting with a holding element of the holder.
Das Haltemittel kann ein an der Innenwand des zweiten Abschnitts geformter Hinterschnitt sein. Typischerweise ist die Pipettenspitze ein Spritzgußteil, wobei die Innenwände des ersten und zweiten Abschnitts parallel zur Längsachse verlaufen, d.h. keine Entformungsschrägen aufweisen. Weiterhin kann der Koppelabschnitt, und insbesondere der zweite Abschnitt der Pipettenspitze, einen Bereich umfassen, der in bezug auf die übrigen Bereiche des Koppelabschnitts bzw. des zweiten Abschnitts flexibler ausgebildet ist und zum ersten axialen Ende hin angeordnet ist. Der flexible Bereich erleichtert das Aufsetzen und Abstreifen der Pipettenspitze von der Halterung. Um die Flexibilität zu verbessern und gezielt einzustellen ist es möglich, im Koppelabschnitt bzw. im zweiten Abschnitt des Koppelabschnitts in Längsrichtung verlaufende Einschnitte vorzusehen und diese mit einem zweiten Material zu befüllen, das elastischer ist als das Material, aus dem die übrigen Bereiche des Koppelabschnitts bzw. des zweiten Abschnitts bestehen. Der Koppelabschnitt besteht daher aus unterschiedlichen Materialien.The retaining means may be an undercut formed on the inner wall of the second section. Typically, the pipette tip is an injection molded part, with the inner walls of the first and second portions being parallel to the longitudinal axis, i. have no draft angles. Furthermore, the coupling portion, and in particular the second portion of the pipette tip, comprise a region which is made more flexible with respect to the remaining regions of the coupling portion or the second portion and is arranged towards the first axial end. The flexible area facilitates the placement and stripping of the pipette tip from the holder. In order to improve the flexibility and to selectively adjust it is possible to provide in the coupling section or in the second section of the coupling section in the longitudinal direction incisions and to fill them with a second material that is more elastic than the material from which the remaining areas of the coupling portion or of the second section. The coupling section therefore consists of different materials.
Der Dichtabschnitt kann von einer Schulter oder Absatz zwischen erstem und zweitem Abschnitt gebildet werden.The sealing portion may be formed by a shoulder or shoulder between the first and second portions.
Gemäß einem weiteren Aspekt wird weiterhin eine Vorrichtung zur Halterung von Pipettenspitzen mit einem Koppelelement mit einer in axialer Richtung verlaufenden Längsachse vorgeschlagen, welches ein freies Ende aufweist, von dem aus eine Pipettenspitze auf das Koppelelement in axialer Richtung aufschiebbar ist, wobei das Koppelelement an seiner Außenseite aufweist:
- zwei axial voneinander beabstandete Führungselemente, und
- ein in bezug auf die Führungselemente separates Halteelement zum Wechselwirken mit Haltemitteln der Pipettenspitze, um die Pipettenspitze in axialer Richtung zu positionieren.
- two axially spaced guide elements, and
- a separate with respect to the guide elements holding member for interacting with holding means of the pipette tip to position the pipette tip in the axial direction.
Das Halteelement kann ein flexibles Element, das an der Außenseite des Koppelelements geeignet gelagert ist, oder ein integral an der Außenseite angeformtes oder separat an der Außenseite befestigtes starres oder elastisches Element sein, beispielsweise eine oder mehrere radiale Erhebungen, die partiell oder ringförmig umfangsseitig verteilt sind.The holding element may be a flexible element, which is suitably mounted on the outside of the coupling element, or integrally formed on the outside or be separately attached to the outside rigid or elastic element, for example, one or more radial projections, which are partially or annular circumferentially distributed.
Gemäß einem weiteren Aspekt wird eine Pipettiervorrichtung mit einem Koppelelement und einer am Koppelelement lösbar befestigbaren Pipettenspitze mit einem Dichtabschnitt vorgeschlagen, wobei das Koppelelement eine in axialer Richtung verlaufende Längsachse besitzt und ein freies Ende aufweist, von dem aus die Pipettenspitze auf das Koppelelement in axialer Richtung aufschiebbar ist. Das Koppelelement besitzt weiterhin ein Dichtelement aus einem elastischen Material, das einen in axialer Richtung zum freien Ende des Koppelabschnitts hin freiliegenden axialen und sich radial erstreckenden Dichtabschnitt aufweist. Der Dichtabschnitt der Pipettenspitze hingegen ist in Bezug auf die Längsachse des Koppelelementes bevorzugt als axiale Fläche, die in Richtung des Koppelelementes weist, ausgestaltet und kann beispielsweise durch eine Schulter gebildet werden. In gekoppeltem Zustand sollte zumindest ein Teil des Dichtabschnittes des Koppelelementes gegen zumindest einen Teil des Dichtabschnittes der Pipettenspitze axial gepreßt sein. Das Koppelelement der Pipettiervorrichtung kann zusätzlich einzeln oder in Kombination die Eigenschaften des oben bereits beschriebenen separaten Koppelelementes, beispielsweise im Hinblick auf die Eigenschaften und das Material des Dichtelementes, die Anzahl, Ausgestaltung und Anordnung von Führungselementen oder die Anzahl, Ausgestaltung und Anordnung von Halteelementen aufweisen.According to a further aspect, a pipetting device with a coupling element and a detachable attachable to the coupling element pipette tip is proposed with a sealing portion, wherein the coupling element has an axially extending longitudinal axis and has a free end, from which the pipette tip on the coupling element in the axial direction pushed is. The coupling element further has a sealing element made of an elastic material which has an axial and radially extending sealing section exposed in the axial direction towards the free end of the coupling section. The sealing portion of the pipette tip, however, is preferably designed with respect to the longitudinal axis of the coupling element as an axial surface facing in the direction of the coupling element, and can be formed for example by a shoulder. In the coupled state, at least a part of the sealing portion of the coupling element should be axially pressed against at least a portion of the sealing portion of the pipette tip. The coupling element of the pipetting device may additionally individually or in combination, the properties of the above-described separate coupling element, for example, in view of the properties and the material of the sealing element, the number, design and arrangement of guide elements or the number, design and arrangement of holding elements.
Gemäß einem weiteren Aspekt wird eine Pipettiervorrichtung mit einem Koppelelement und einer am Koppelelement lösbar befestigbaren Pipettenspitze vorgeschlagen, wobei das Koppelelement mindestens ein an seiner Außenseite angeordnetes Führungselement zum lateralen Ausrichten der Pipettenspitze aufweist, und vorzugsweise so viele Führungselemente umfaßt, wie die Pipettenspitze Führungsflächen besitzt. Das oder die Führungselement(e) können dabei unabhängig voneinander vorzugsweise einstückig oder mehrteilig ausgebildet sein. Die Pipettenspitze weist eine Längsachse sowie einen in Längsachse verlaufenden Koppelabschnitt zum Aufschieben auf die Halterung auf. Der Koppelabschnitt hat weiterhin mindestens einen Abschnitt mit einer entgegen der Aufschiebrichtung zumindest abschnittsweise konisch zulaufenden Innenwand, in die eine in bezug auf die Längsachse zylindrische Führungsfläche zum Wechselwirken mit dem zumindest einen koppelseitigen Führungselement integriert ist. Das oder die Führungselement(e) am Koppelelement ist (sind) so ausgestaltet, daß jedes Führungselement zumindest Teilflächen einer zylindrischen Mantelfläche aufweist, die jeweils einer mit der Teilfläche wechselwirkenden zylindrischen Führungsfläche an der Pipettenspitze entspricht. Die Pipettenspitze kann zusätzlich einzeln oder in Kombination die Eigenschaften der oben bereits beschriebenen separaten Pipettenspitze, beispielsweise im Hinblick auf die Eigenschaften, das Material, die Ausgestaltung und Anordnung der Innenwand, spezieller Abschnitte oder von Halteelementen aufweisen. Zudem kann das Koppelelement der Pipettiervorrichtung auch hier zusätzlich einzeln oder in Kombination die Eigenschaften des oben bereits beschriebenen separaten Koppelelementes, beispielsweise im Hinblick auf die Anzahl, Ausgestaltung und Anordnung von Führungselementen aufweisen. Zudem kann das Koppelelement ein Dichtelement mit bereits weiter oben beschriebenen Eigenschaften, Ausgestaltungen sowie geeigneten Materialen und ein oder mehrere im Hinblick auf Anzahl, Ausgestaltung und Anordnung bereits oben beschriebene Halteelemente umfassen.According to a further aspect, a pipetting device with a coupling element and a pipette tip detachably attachable to the coupling element is proposed, wherein the coupling element has at least one guide element arranged on its outside for laterally aligning the pipette tip, and preferably comprises as many guide elements as the pipette tip has guide surfaces. The one or more guide element (s) may be formed independently of one another preferably in one piece or in several parts. The pipette tip has a longitudinal axis and a coupling section extending in the longitudinal axis for pushing onto the holder. The coupling section further has at least one section with an inner wall tapering at least in sections opposite the direction of slipping into which a guide surface which is cylindrical relative to the longitudinal axis is integrated for interacting with the at least one coupling-side guide element. The one or more guide element (s) on the coupling element is (are) designed so that each guide element has at least partial surfaces of a cylindrical lateral surface which corresponds in each case to an interacting with the partial surface cylindrical guide surface on the pipette tip. In addition, the pipette tip can individually or in combination have the properties of the separate pipette tip already described above, for example with regard to the properties, the material, the configuration and arrangement of the inner wall, special sections or holding elements. In addition, the coupling element of the pipetting device can also here additionally or individually in combination have the properties of the above-described separate coupling element, for example with regard to the number, configuration and arrangement of guide elements. In addition, the coupling element may comprise a sealing element with properties, configurations and suitable materials already described above and one or more holding elements already described above with regard to number, configuration and arrangement.
Das Koppelelement kann weiterhin mindestens ein an seiner Außenseite angeordnetes Halteelement zum Wechselwirken mit zumindest einem Haltemittel der Pipettenspitze aufweisen. Dabei kann das mindestens eine Haltelement gegenüber dem zumindest einen Haltemittel starr ausgebildet sein. Alternativ kann das mindestens eine Haltelement gegenüber dem zumindest einen Haltemittel auch flexibel ausgebildet sein.The coupling element can furthermore have at least one holding element arranged on its outside for interacting with at least one holding means of the pipette tip. In this case, the at least one holding element can be designed to be rigid relative to the at least one holding means. Alternatively, the at least one holding element can also be designed to be flexible with respect to the at least one holding means.
Im weiteren soll die Erfindung anhand von in Figuren dargestellten Ausführungsbeispielen erläutert werden, aus denen sich weitere Vorteile und Abwandlungen ergeben. Dazu zeigen:
-
eine Schnittansicht einer Halterung mit Koppelelement und Pipettenspitze gemäß einer ersten Ausführungsform;Figur 1 -
eine Schnittansicht einer Halterung mit Koppelelement und aufgeschobener Pipettenspitze gemäß der ersten Ausführungsform;Figur 2 -
Figur 3 eine Schnittansicht einer Halterung mit Koppelelement und aufgeschobener Pipettenspitze gemäß einer zweiten Ausführungsform; -
Figur 4 ein Ausschnitt eines Koppelelements mit X-förmigem Dichtelement; -
eine Schnittansicht einer Halterung mit Koppelelement gemäß einer dritten Ausführungsform;Figur 5 -
einen ersten Ausschnitt vom Koppelelement gemäß drittem Ausführungsbeispiel;Figur 6 -
Figur 7 einen zweiten Ausschnitt vom Koppelelement gemäß drittem Ausführungsbeispiel; -
Figur 8 ein Koppelabschnitt eines ersten Ausführungsbeispiels einer Pipettenspitze; und -
Figur 9 ein zweites Ausführungsbeispiel einer Pipettenspitze.
-
FIG. 1 a sectional view of a holder with coupling element and pipette tip according to a first embodiment; -
FIG. 2 a sectional view of a holder with coupling element and deferred pipette tip according to the first embodiment; -
FIG. 3 a sectional view of a holder with coupling element and deferred pipette tip according to a second embodiment; -
FIG. 4 a section of a coupling element with X-shaped sealing element; -
FIG. 5 a sectional view of a holder with coupling element according to a third embodiment; -
FIG. 6 a first section of the coupling element according to the third embodiment; -
FIG. 7 a second section of the coupling element according to the third embodiment; -
FIG. 8 a coupling portion of a first embodiment of a pipette tip; and -
FIG. 9 A second embodiment of a pipette tip.
Zum sicheren Befestigen und Halten von Pipettenspitzen an Pipettiervorrichtungen bzw. Pipettierautomaten werden spezielle Halterungen verwendet. Die erfindungsgemäße Halterung weist dazu ein Koppelelement mit einem insbesondere zylinderförmigen Grundkörper auf, welches ein elastisches Dichtelement mit axial in Richtung des freien Endes der Halterung freiliegendem und sich zumindest teilweise radial erstreckendem Dichtabschnitt umfaßt. Gegen diesen Dichtabschnitt kann axial ein korrespondierender Dichtabschnitt einer Pipettenspitze geschoben werden. Die Dichtwirkung wird dabei durch axiales Pressen gegen das Dichtelement erreicht. Typischerweise besteht das Dichtelement aus einem Fluorelastomer und kann beispielsweise als O-Ring oder auch als X-Ring ausgeführt sein, wobei sich O und X auf den Querschnitt des Ringmaterials bezieht. Andere Querschnitte, beispielsweise Hohl- oder V-Querschnitte sind ebenfalls möglich. Durch die Wahl des jeweiligen Querschnitts soll eine Materialelastizität im Querschnitt erreicht werden, d.h. der Querschnitt des Dichtelements ist elastisch, insbesondere in Längsrichtung des Koppelelements verformbar, und ermöglicht daher eine sehr gute axiale Dichtwirkung.Special holders are used for secure attachment and holding of pipette tips to pipetting devices or pipetting machines. The holder according to the invention has for this purpose a coupling element with a particular cylindrical base body, which comprises an elastic sealing element with axially exposed in the direction of the free end of the holder and at least partially radially extending sealing portion. Against this sealing portion can be pushed axially a corresponding sealing portion of a pipette tip. The sealing effect is achieved by axial pressing against the sealing element. Typically, the sealing element consists of a fluoroelastomer and can be embodied for example as an O-ring or as an X-ring, where O and X refers to the cross section of the ring material. Other cross sections, such as hollow or V cross sections are also possible. By choosing the respective cross-section, a material elasticity in cross section is to be achieved, i. the cross section of the sealing element is elastic, in particular deformable in the longitudinal direction of the coupling element, and therefore allows a very good axial sealing effect.
Das Koppelelement weist weiterhin zumindest ein Führungselement zum - in bezug auf die Längsachse der Halterung - lateralen Positionieren und Ausrichten der Pipettenspitze auf. Insbesondere kann das Führungselement radial vorzugsweise mit konstanter radialer Ausdehnung um das Koppelelement umlaufend ausgebildet sein, wobei es aus Teilelementen bestehen kann. Dabei kann das Führungselement benachbarte Abschnitte der Außenseite des Koppelelements radial überragen. Das Führungselement hat somit eine größere radiale Ausdehnung als benachbarte Abschnitte des Koppelelements. Damit wird sichergestellt, daß ein radialer Kontakt zwischen Koppelelement und Pipettenspitze im wesentlichen nur über das Führungselement hergestellt wird und damit das Führungselement die laterale bzw. radiale Position der Pipettenspitze bestimmt. Typischerweise liegt das Führungselement an der Innenwand der Pipettenspitze an, die ihrerseits entsprechende Führungselemente bzw. Führungsflächen aufweisen kann. Das Führungselement kann ringförmig sein. Bei dem halterungsseitigen Führungselement handelt es sich insbesondere um in bezug auf die Längsachse des Koppelements zylindrische Führungsflächen oder Teilflächen. Dadurch ist, im Gegensatz zu konischen Flächen, die laterale Führung und Ausrichtung der Pipettenspitze unabhängig von axialen Positionierungsmitteln.The coupling element furthermore has at least one guide element for lateral positioning and alignment of the pipette tip with respect to the longitudinal axis of the holder. In particular, the guide element can be formed radially, preferably with a constant radial extent around the coupling element, wherein it may consist of sub-elements. In this case, the guide element project radially beyond adjacent sections of the outside of the coupling element. The guide element thus has a greater radial extent than adjacent portions of the coupling element. This ensures that a radial contact between the coupling element and the pipette tip is produced essentially only via the guide element and thus the guide element determines the lateral or radial position of the pipette tip. Typically, the guide element bears against the inner wall of the pipette tip, which in turn may have corresponding guide elements or guide surfaces. The guide element can be annular. The holder-side guide element is, in particular, cylindrical guide surfaces or partial surfaces with respect to the longitudinal axis of the coupling element. Thus, unlike conical surfaces, the lateral guidance and orientation of the pipette tip is independent of axial positioning means.
In einer Ausprägung der erfindungsgemäßen Halterung kann das Koppelelement zwei axial voneinander beabstandete Führungselemente an seiner Außenseite aufweisen. Dadurch wird die laterale bzw. radiale Ausrichtung bzw. Positionierung der Pipettenspitze weiter verbessert. Ebenso wird eine verbesserte koaxiale Ausrichtung von Koppelelement und Pipettenspitze erreicht, d.h. daß ein Verkippen oder schräges Halten der Pipettenspitze an der Halterung verhindert wird. Dies ist insbesondere bei Pipettierautomaten mit einer Vielzahl von gleichzeitig betätigten Pipettenspitzen, die beispielsweise matrixartig angeordnet sind, von Vorteil.In one embodiment of the holder according to the invention, the coupling element may have two axially spaced-apart guide elements on its outer side. As a result, the lateral or radial alignment or positioning of the pipette tip is further improved. Likewise, an improved coaxial alignment of coupling element and pipette tip is achieved, i. that a tilting or oblique holding the pipette tip is prevented on the holder. This is particularly advantageous in pipetting machines with a large number of simultaneously actuated pipette tips, which are arranged in a matrix, for example.
Günstig ist, wenn beide Führungselemente einen axialen Abstand haben, der mindestens so groß ist wie deren größte radiale Ausdehnung. Unter axialem Abstand der Führungselemente wird dabei der Abstand der voneinander am weitesten auseinander liegenden Kontaktbereiche oder Kontaktkanten verstanden. Beispielsweise können die Führungselemente Führungsringe definieren, die radial um das Koppelelement verlaufen und eine unterschiedliche radiale Ausdehnung bzw. unterschiedliche Außendurchmesser aufweisen. In diesem-Fall wird der axiale Abstand durch die jeweilige Außenkante oder Außenlinie der Führungsfläche definiert, d.h. die Außenkanten, die axial voneinander am weitesten entfernt sind. Die Führungsringe können dabei wahlweise als durchgängig umlaufende Ringe oder auch als unterbrochene Ringe ausgebildet sein. Es ist ebenfalls möglich, einen Führungsring als durchgängig umlaufenden Ring und den anderen Führungsring als unterbrochenen Ring auszubilden.It is favorable if both guide elements have an axial distance which is at least as great as their greatest radial extent. The axial distance of the guide elements is understood to mean the distance between the contact regions or contact edges which are furthest apart from one another. For example, the guide elements can define guide rings, which run radially around the coupling element and have a different radial extent or different outer diameters. In this case, the axial distance is defined by the respective outer edge or outline of the guide surface, ie the outer edges, which are axially farthest from each other. The guide rings can be designed either as continuous circumferential rings or as interrupted rings. It is also possible to form a guide ring as a continuous circumferential ring and the other guide ring as a broken ring.
Das Führungselement bzw. der oder die Führungsringe können eine gewisse axiale Ausdehnung aufweisen, so daß dadurch Führungsflächen definiert werden, deren axiale Breite im wesentlichen der der axialen Ausdehnung der Führungsringe bzw. des Führungselements entspricht. Es ist ebenfalls möglich, die axiale Ausdehnung des Führungselements bzw. der oder die Führungsringe soweit zu reduzieren, daß ein im wesentlichen linienförmiger Kontakt zwischen Führungselement und Pipettenspitze verbleibt.The guide element or the guide ring or the guide rings may have a certain axial extent, so that thereby guide surfaces are defined whose axial width substantially corresponds to the axial extent of the guide rings and the guide element. It is also possible to reduce the axial extent of the guide element or the guide rings or the extent that a substantially linear contact between the guide element and the pipette tip remains.
Typischerweise hat das Koppelelement zwei Führungselemente mit unterschiedlicher radialer Ausdehnung bzw. Außendurchmesser, wobei der axiale Abstand der beiden Führungselemente zueinander mindestens so groß ist wie der größere der beiden Außendurchmesser.Typically, the coupling element has two guide elements with different radial extent or outer diameter, wherein the axial distance of the two guide elements to each other is at least as large as the larger of the two outer diameter.
In einer weiteren Ausprägung der Erfindung weist das Koppelelement einen ersten Abschnitt, der nahe dem freien Ende bzw. am freien Ende des Koppelelements angeordnet ist, und einen zweiten Abschnitt, der axial in Aufschiebrichtung zum ersten Abschnitt versetzt angeordnet ist, auf. Typischerweise sind die Abschnitte im wesentlichen zylinderförmig. Jeder Abschnitt kann ein Führungselement aufweisen, wobei insbesondere der dem freien Ende zugewandte erste Abschnitt vorzugsweise an jeder Stelle eine kleinere radiale Ausdehnung als der zweite Abschnitt hat. Dadurch wird eine Stufe zwischen den beiden Abschnitten definiert, an der das Dichtelement angeordnet sein kann. Das Dichtelement liegt demnach vorzugsweise zwischen erstem und zweitem Abschnitt und überragt in radialer Richtung typischerweise den ersten Abschnitt und das dort befindliche Führungselement, so daß ein Teil des Dichtelements axial vom freien Ende des Koppelelements her frei zugänglich ist.In a further embodiment of the invention, the coupling element has a first portion, which is arranged near the free end or at the free end of the coupling element, and a second portion, which is arranged offset axially in the sliding direction to the first portion on. Typically, the sections are substantially cylindrical. Each section may comprise a guide element, wherein in particular the first end facing the free end preferably has at each point a smaller radial extent than the second section. This defines a step between the two sections on which the sealing element can be arranged. The sealing element is therefore preferably between the first and second section and projects beyond in the radial direction typically the first portion and the guide element located there, so that a part of the sealing element is freely accessible axially from the free end of the coupling element ago.
Gegen das Dichtelement kann beispielsweise ein innerer Stufenabsatz der Pipettenspitze gedrückt werden, der von einer radial umlaufenden und in axialer Richtung weisenden Dichtungsfläche gebildet wird.For example, against the sealing element, an inner stepped shoulder of the pipette tip can be pressed, which is formed by a radially encircling and axially facing sealing surface.
Das Koppelelement weist weiterhin mindestens ein Halteelement auf, welches an der Außenseite des Koppelelements angeordnet ist, mit korrespondierenden Haltemitteln der Pipettenspitze wechselwirkt und die Pipettenspitze lösbar fixiert. Das Halteelement bewirkt dabei eine insbesondere axiale Fixierung, so daß dadurch gleichzeitig der Dichtabschnitt der Pipettenspitze axial gegen den axialen Dichtabschnitt des Koppelelements gedrückt wird. Außerdem wird durch die Wechselwirkung von Dichtelement mit Dichtmittel einerseits und Halteelement und Haltemittel andererseits eine sichere und genau definierte axiale Positionierung der Pipettenspitze erreicht. Das Halteelement kann flexibel oder starr ausgebildet sein.The coupling element furthermore has at least one holding element, which is arranged on the outside of the coupling element, interacts with corresponding holding means of the pipette tip and removably fixes the pipette tip. The retaining element causes a particular axial fixation, thereby simultaneously the sealing portion of the pipette tip is pressed axially against the axial sealing portion of the coupling element. In addition, a safe and well-defined axial positioning of the pipette tip is achieved by the interaction of sealing element with sealant on the one hand and holding element and retaining means on the other hand. The holding element may be flexible or rigid.
Das Halteelement kann ein flexibles Spannelement, z.B. ein umlaufendes Federelement sein, das in einer an der Außenseite des Koppelelements befindlichen umlaufenden Vertiefung angeordnet ist. Flexible Haltelemente ermöglichen ein Aufschieben bzw. Abstreifen der Pipettenspitze mit geringem Kraftaufwand. Außerdem sind flexible Halteelemente relativ verschleißarm und vergleichsweise fehlertolerant, da sie aufgrund ihrer Flexibilität Fertigungstoleranzen, beispielsweise der Pipettenspitze, teilweise kompensieren können.The retaining element may be a flexible tensioning element, e.g. be a circumferential spring element which is arranged in a located on the outside of the coupling element circumferential recess. Flexible holding elements allow the pipette tip to be pushed on or off with little effort. In addition, flexible holding elements are relatively low wear and relatively fault tolerant because they can compensate for manufacturing tolerances due to their flexibility, for example, the pipette tip partially.
Andererseits kann das Halteelement auch starr ausgebildet sein und beispielsweise einzelne radiale Erhebungen, beispielsweise starre Nocken, aufweisen, die vorzugsweise ringförmig um das Koppelelement verteilt sind. Auch eine nicht ringförmige Verteilung oder ein durchgängiger Ring sind als starre Haltelemente geeignet. Starre Halteelemente haben gegenüber flexiblen Halteelementen den Vorteil, daß sie eine genauere Zentrierung der Pipettenspitze erlauben.On the other hand, the holding element may also be rigid and, for example, individual radial elevations, for example, rigid cams, which are preferably distributed annularly around the coupling element. Also, a non-annular distribution or a continuous ring are suitable as rigid holding elements. Rigid holding elements have the advantage over flexible holding elements that they allow a more accurate centering of the pipette tip.
Unabhängig von der jeweils konkreten Ausgestaltung des Halteelements kann dieses in einen radial umlaufenden Hinterschnitt an der Pipettenspitze eingreifen, der typischerweise an der Innenwand der Durchgangsöffnung der Pipettenspitze angeordnet ist.Regardless of the specific embodiment of the holding element, this can engage in a radially circumferential undercut on the pipette tip, which is typically arranged on the inner wall of the passage opening of the pipette tip.
In einer weiteren Ausprägung der Erfindung ist das Halteelement in Aufschiebrichtung gesehen hinter dem oder den Führungselementen angeordnet. Dadurch wird gewährleistet, daß sich das Dichtelement vor dem Haltelement in Richtung zum freien Ende des Koppelelements befindet und dadurch das Haltelement vor einem versehentlichen Verunreinigen mit dem zu pipettierenden Medium schützt.In a further embodiment of the invention, the holding element is arranged in the direction of sliding behind the guide elements or arranged. This ensures that the sealing element is in front of the retaining element in the direction of the free end of the coupling element and thereby protects the retaining element against accidental contamination with the medium to be pipetted.
Mit Bezug auf
Die Pipettenspitze ist typischerweise zum einmaligen Gebrauch bestimmt und als Spritzgußteil ausgeführt. Ein geeignetes, leicht zu verarbeitendes Material für Pipettenspitzen ist Polypropylen, das in flüssiger Form und wahlweise mit Zusätzen (z.B. Farbe) und/oder Füllstoffen versetzt in eine geeignete Spritzgußform eingespritzt wird. Nach Erstarren des Polypropylens wird die fertige Pipettenspitze aus der Spritzgußform ausgestoßen und falls erforderlich der Anschnitt entfernt.The pipette tip is typically intended for single use and designed as an injection molded part. A suitable material for pipette tips that is easy to process is polypropylene, which is injected in liquid form and optionally with additives (e.g., paint) and / or fillers into a suitable injection mold. After solidification of the polypropylene, the finished pipette tip is ejected from the injection mold and removed if necessary, the gate.
Das Koppelelement 4 ist typischerweise einstückig aus Metall geformt und hat an seinem freiem Ende 8 einen ersten Abschnitt 20. Ein zweiter Abschnitt 22 des Koppelelements 4 ist axial in Aufschiebrichtung 2 in bezug zum ersten Abschnitt 20 versetzt angeordnet. Der erste Abschnitt 20 hat vorzugsweise an jeder Stelle eine geringere radiale Ausdehnung als der zweite Abschnitt 22, so daß der zweite, in Aufschiebrichtung 2 hintere Abschnitt 22 radial den ersten Abschnitt 20 überragt. An der Außenseite jedes Abschnitts ist jeweils ein Führungselement 25, 26 in Form einer umlaufenden zylinderförmigen Führungsfläche angeordnet. Die Führungsflächen 25, 26, die in Längsrichtung parallel zur Längsachse 6 verlaufen, haben eine größere radiale Ausdehnung als benachbarte Bereiche der jeweilige Abschnitte 20, 22, über die sie sich radial erstrecken. Dadurch soll sichergestellt werden, daß die Pipettenspitze 10 radial lediglich mit den Führungsflächen in Kontakt tritt und durch die Wechselwirkung der Führungsflächen mit der Innenwand des Koppelabschnitts 14 die radiale Ausrichtung bzw. Positionierung der Pipettenspitze 10 in bezug auf das Koppelelement 4 definiert wird. Durch die zwei axial gegeneinander versetzt angeordneten Führungselemente 25 und 26 wird gleichzeitig auch ein schräges Aufsetzten der Pipettenspitze 10 bzw. Verkippen derselben auf das Koppelement 4 verhindert. Bevorzugt haben die beiden Führungselemente 25, 26 einen axialen Abstand d, der mindestens so groß ist wie der Durchmesser D (radiale Ausdehnung) des größeren der beiden Führungselemente, hier also des zweiten Führungselements 26. Dadurch wird die koaxiale Ausrichtung der Pipettenspitze 10 am Koppelelement 4 weiter verbessert. Der Abstand d ist hier durch den Abstand der jeweiligen Außenkanten 28, 29 der Führungselemente 25, 26 definiert. Diese Außenkanten bilden die axialen Endbereiche des Kontakts zwischen den Führungselementen bzw. Führungsflächen 25, 26 und der Pipettenspitze.The coupling element 4 is typically integrally formed from metal and has at its free end 8 a
Korrespondierend zum ersten und zweiten Abschnitt 20, 22 des Koppelelements weist der Koppelabschnitt 14 der Pipettenspitze 10 ebenfalls einen ersten Abschnitt 40 und einen zweiten Abschnitt 42 auf, wobei der erste Abschnitt 40 eine geringere radiale Ausdehnung (Durchmesser) als der zweite Abschnitt 42 hat. Dadurch wird eine Stufe bzw. Schulter 43 zwischen erstem und zweitem Abschnitt 40, 42 gebildet, die als Dichtfläche 43 dient.Corresponding to the first and
Das erste und zweite Führungselement 25 und 26 sind im vorgestellten Ausführungsbeispiel im wesentlichen gleich geformt. Es ist allerdings auch möglich, den Führungselementen eine jeweils unterschiedliche Form zu geben. Im vorliegenden Ausführungsbeispiel sind die Führungselemente 25, 26 umlaufend ausgebildet und erheben sich gegenüber der sie umgebenden Außenkontur der jeweiligen kopplungselementseitigen Abschnitte 20, 22 in Form eines integral angeformten Ringes mit umlaufender Führungsfläche, dessen Querschnitt trapezförmig ist.The first and
Zwischen erstem und zweitem Abschnitt 20, 22 verläuft eine radial an der Außenseite des Koppelelements 4 umlaufende Vertiefung oder Hinterschnitt 34, in welcher ein ebenfalls radial umlaufendes Dichtelement 21 sitzt. Das Dichtelement ist günstigerweise eine Ringdichtung aus einem elastischen Material. Als geeignete Materialien haben sich insbesondere Fluoroelastomere herausgestellt, da sie eine hohe Elastizität, Langlebigkeit, hohe chemische Beständigkeit und Verschleißarmut aufweisen. Im vorliegenden Ausführungsbeispiel ist das Dichtelement als massiver, im Querschnitt rechteckiger Ring ausgeführt. Es ist allerdings auch möglich, Ringdichtungen mit kreisförmigem (O-Ringe) oder X-förmigen Querschnitt zu verwenden. Beispielsweise sind Ringdichtungen mit X-förmigen Querschnitt aufgrund der einzelnen Dichtlippen elastischer als O-Dichtungen und führen daher zu einer noch besseren Abdichtung der Pipettenspitze am Koppelelement. Ein Dichtelement 21' mit X-förmigem Querschnitt ist beispielsweise in
Das in
Das Dichtelement 21 hat einen im Vergleich zum Innendurchmesser des zweiten Abschnitts 42 der Pipettenspitze etwas geringeren Außendurchmesser. Dadurch wird sichergestellt, daß die Innenwand der Pipettenspitze beim Aufschieben nicht reibend über das Dichtelement 21 geführt wird, wodurch es erheblich weniger belastet wird als radiale Dichtungen, die zum Erreichen einer ausreichenden Dichtwirkung reibend über üblicherweise konisch zulaufende Flächen geschoben werden müssen. Daher ist auch der Wartungsaufwand für das erfindungsgemäße axiale Dichtelement 21 erheblich geringer.The sealing
Ein radialer Kontakt zwischen Koppelelement 4 und Pipettenspitze 10 wird über die koppelelementseitigen Führungselemente 25 und 26 und über erste und zweite Führungsflächen 45 und 46 des Koppelabschnitts 14 der Pipettenspitze 10 hergestellt. Im einfachsten Fall können die pipettenspitzenseitigen Führungsflächen 45, 46 durch die Innenwände der jeweiligen Abschnitte 40, 42 der Pipettenspitze 10 gebildet werden. Es ist allerdings auch möglich, erhabene Führungsflächen an der Innenwand der Pipettenspitze anzuformen. Jeder Abschnitt des pipettenspitzenseitigen Koppelabschnitts 14 weist eine durchgängig umlaufende bzw. aus umfangsseitig verteilten Teilsegmenten bestehende Führungsfläche 45, 46 auf, deren Durchmesser dem Außendurchmesser des jeweils zugeordneten ersten und zweiten Führungselements 25, 26 entspricht, so daß eine formschlüssige Ausrichtung der Pipettenspitze 10 erreicht wird.A radial contact between coupling element 4 and
Um eine möglichst paßgenaue Ausrichtung zu ermöglichen, weisen die entsprechenden Führungsflächen 45, 46 keine Entformungsschrägen auf. Entformungsschrägen werden üblicherweise an Spritzgußteilen vorgesehen, um diese von der Spritzgußform leichter lösen zu können. Durch den Verzicht auf Entformungsschrägen verlaufen die pipettenspitzenseitigen Führungsflächen in axialer Richtung parallel zur Achse 6. Dadurch wird erreicht, daß die radiale bzw. laterale Ausrichtung der Pipettenspitze nicht davon abhängt, wie weit die Pipettenspitze auf das Koppelelement geschoben wird. Im Falle von konisch zulaufenden Führungsflächen würden diese beim Aufschieben der Pipettenspitze auf das Koppelelement zunehmend am Koppelelement verspannt werden und dadurch der Axialbewegung einen Widerstand entgegensetzen. Somit beeinflussen konische Führungsflächen die axiale Ausrichtung und erhöhen die erforderliche Aufschiebekraft. In Aufschiebrichtung hinter dem zweiten Führungselement 26 ist eine Ringnut 30 zur Aufnahme einer Ringfeder 27 eingebracht. Die Ringfeder 27 dient als Halteelement und greift in einen Hinterschnitt 47 an der Innenseite des zweiten Abschnitts 42 der Pipettenspitze ein. Beim Aufsetzen der Pipettenspitze wird diese mit ihrem hinteren Ende 12 voran über das zweite Führungselement 26 und die Ringfeder 27 geschoben, bis die Ringfeder 27 in den Hinterabschnitt 47 einschnappt. Dadurch wird die Pipettenspitze axial positioniert und am Koppelelement fixiert. Ringfeder 27 und Hinterschnitt 47 stellen eine lösbare Verbindung her, die gleichzeitig ausreichend stabil ist, um die Schulter 43 axial gegen den axialen Dichtabschnitt 23 zu drücken und so die Pipettenspitze am Koppelelement abzudichten. Die Ringfeder kann einen leichten Schraubengang aufweisen.In order to enable the most accurate alignment, the corresponding guide surfaces 45, 46 no draft angles. Entformungsschrägen are usually provided on injection molded parts in order to solve this easier of the injection mold can. By eliminating Entformungsschrägen the pipette tip-side guide surfaces extending in the axial direction parallel to the
Beim Aufschieben der Pipettenspitze kann es zu einer reversiblen leichten Verformung des hinteren Endes 12 der Pipettenspitze kommen, da das hintere Ende beim Passieren der Ringfeder 27 leicht gedehnt wird. Die Pipettenspitze sollte daher an ihrem hinteren Ende bis zu einem gewissen Grade elastisch ausgebildet. Die Elastizität kann durch geeignete Wahl der Materialstärke eingestellt werden. Es ist allerdings auch möglich, die Ringfeder 27 soweit flexibel auszubilden, daß sie beim Aufsetzen der Pipettenspitze nachgibt und beim Passieren des Hinterschnitts 47 in diesen einspringt.When sliding the pipette tip, a reversible slight deformation of the
Die Ringnut 30 ist im vorliegenden Ausführungsbeispiel mit geneigter Innenwand 31 ausgeführt, die konisch auf das vordere Ende 8 des Koppelelements zuläuft. Dadurch wird erreicht, daß die Ringfeder 27 axial in Richtung zum freien Ende 8 hin genau positioniert ist, da sie durch die Pipettenspitze leicht radial zusammengedrückt wird, aufgrund der konischen Innenwand 31 in Richtung Anschlagfläche 50 ausweicht und gegen diese gedrückt und positioniert wird. Somit ergibt sich ein Kraftschluß ausgehend vom Dichtelement 21 über den pipettenseitigen Dichtabschnitt 43 zum Hinterschnitt 47, der den Kraftfluß über die Ringfeder 27 zur Anschlagfläche 50 führt. Dadurch wird die Pipettenspitze sicher am Koppelelement befestigt und ausgerichtet.The
Eine weitere Ausführungsform zeigt
Wie im ersten Ausführungsbeispiel greifen die Nocken 57 in einen Hinterschnitt 47 an der Pipettenspitze ein.As in the first embodiment, the
In
Die V-förmige Innenwand 63 (
Im ersten Abschnitt 20 (
Die vorstehend beschriebenen Koppelemente können an manuellen Pipettenhalterungen aber auch an Pipettierautomaten angeordnet sein, die viele Koppelelemente aufweisen. Derartige Pipettierautomaten weisen weiterhin noch weitere Komponenten auf, insbesondere Mittel zum Abstreifen der Pipettenspitzen. Üblicherweise umfassen diese Mittel einen relativ zum Koppelelement in axialer Richtung bewegbaren Abstreifer, der hinter das hintere Ende 12 der Pipettenspitze 10 eingreift und diese entgegen der Aufschiebrichtung 2 vom Koppelelement schiebt.The coupling elements described above can be arranged on manual pipette holders but also on automatic pipetting machines which have many coupling elements. Such automatic pipetting machines also have further components, in particular means for stripping the pipette tips. Usually, these means comprise a relative to the coupling element in the axial direction movable scraper, which engages behind the
In
Bei allen Ausführungen kann die Pipettenspitze aus Polypropylen bestehen und mit Graphit gefüllt sein, um kapazitive Füllstandsmessungen zu ermöglichen.In all designs, the pipette tip may be polypropylene and filled with graphite to allow for capacitive level measurements.
Das Dichtelement kann bei allen Ausführungsformen aus Fluorelastomer bestehen, z.B. Viton® oder Kalrez® von DuPont. Andere elastische Materialen sind je nach zu pipettierendem Medium ebenfalls geeignet.The sealing element may in all embodiments consist of fluoroelastomer, e.g. Viton® or Kalrez® from DuPont. Other elastic materials are also suitable, depending on the medium to be pipetted.
Die Koppelelemente, die auch häufig als Dorn bezeichnet werden, bestehen aus einem bevorzugt korrosionsbeständigen Metall, z.B. Edelstahl oder anderen Legierungen, die z.B. Tantal, Titan oder Wolfram enthalten. Es ist allerdings auch möglich, die Koppelelemente aus geeignetem, z.B. leitendem Kunststoff herzustellen. Ebenfalls sind Verbunde aus unterschiedlichen Materialien möglich, z.B. Edelstahl mit Kunststoffeinlagen oder Verbindungen von unterschiedlichen, leitenden und nicht-leitenden Kunststoffen.The coupling elements, which are also often referred to as a mandrel, are made of a preferably corrosion-resistant metal, e.g. Stainless steel or other alloys, e.g. Tantalum, titanium or tungsten included. However, it is also possible to use the coupling elements of suitable, e.g. produce conductive plastic. Also composites of different materials are possible, e.g. Stainless steel with plastic inserts or compounds of different conductive and non-conductive plastics.
Den vorstehend beschriebenen Ausführungsformen ist gemein, daß sie das Aufsetzen und Abstreifen der Pipettenspitze mit vergleichsweise geringem Kraftaufwand ermöglichen. Dies wird einerseits durch die koppelelementseitigen flexiblen Halteelemente und andererseits durch flexible Bereiche des hinteren Endes 12 der Pipettenspitze erreicht. Darüber hinaus weisen alle Koppelelemente eine verschleißarme bzw. sogar verschleißfreie Dichtung auf, da das Dichtelement als axiales Dichtelement ausgebildet ist. Die Führungselemente gestatten eine genaue radiale bzw. laterale (x- und y-Richtung) Positionierung und verhindern ein Verkippen der Pipettenspitze. Die axiale Positionierung (z-Richtung) wird einerseits durch das Zusammenspiel von koppelelementseitigem Halteelement mit pipettenspitzenseitigem Haltemittel und andererseits durch das Andrücken der Schulter 43 gegen das Dichtelement 21 festgelegt. Die Dichtung und die Befestigung sind somit räumlich und funktionell voneinander getrennt und ermöglichen eine lagesichere Befestigung der Pipettenspitze am Koppelelement. Sowohl die Pipettenspitze als auch das Koppelelement lassen sich kostengünstig herstellen und sind robust im Gebrauch.The embodiments described above have in common that they allow the placement and stripping of the pipette tip with relatively little effort. This is achieved on the one hand by the coupling element-side flexible holding elements and on the other by flexible regions of the
- 22
- Aufschiebrichtungsliding-on
- 44
- Koppelelementcoupling element
- 55
- DurchgangsöffnungThrough opening
- 66
- Längsachselongitudinal axis
- 88th
- freies Ende des Koppelelementsfree end of the coupling element
- 1010
- Pipettenspitzepipette tip
- 1212
- hinteres Ende der Pipettenspitze / erstes axiales Enderear end of the pipette tip / first axial end
- 1414
- Koppelabschnitt der PipettenspitzeCoupling section of the pipette tip
- 2020
- erster Abschnitt des Koppelelementsfirst section of the coupling element
- 21, 21'21, 21 '
- Dichtelementsealing element
- 2222
- zweiter Abschnitt des Koppelelementssecond section of the coupling element
- 23, 23'23, 23 '
- Dichtabschnittsealing portion
- 2525
- erstes Führungselementfirst guide element
- 2626
- zweites Führungselementsecond guide element
- 2727
- Ringfeder / HalteelementRing spring / retaining element
- 28, 2928, 29
- Außenkanteouter edge
- 3030
- Ringnutring groove
- 3131
- Innenwand der RingnutInner wall of the annular groove
- 3434
- Vertiefung / HinterschnittRecess / undercut
- 4040
- erster Abschnitt der Pipettenspitzefirst section of the pipette tip
- 4242
- zweiter Abschnitt der Pipettenspitzesecond section of the pipette tip
- 4343
- Dichtabschnitt / SchulterSealing section / shoulder
- 4545
- erste Führungsflächefirst guide surface
- 4646
- zweite Führungsflächesecond guide surface
- 4747
- Hinterschnittundercut
- 5050
- Anschlagflächestop surface
- 5757
- Nocken / HalteelementCam / retaining element
- 6060
- Ringnutring groove
- 61, 6261, 62
-
Seitenwände der Ringnut 60Side walls of the
annular groove 60 - 6363
-
Innenwand der Ringnut 60Inner wall of the
annular groove 60 - 65, 66, 6765, 66, 67
- Anlaufflankenstart flanks
- 6868
- Einführschrägechamfer
- 6969
- Stirnflächeface
- 7070
- Innenwandinner wall
- 7171
- Außenwandouter wall
- 7272
- Führungsflächeguide surface
- 7474
- Absatzparagraph
- 8080
- erstes Materialfirst material
- 8282
- zweites Materialsecond material
- 8484
- konischer Abschnittconical section
Claims (29)
- Device for mounting pipette tips, having a coupling element (4) with a longitudinal axis (6) that extends in the axial direction and has a free end (8) from which a pipette tip (10) can be slid onto the coupling element (4) in the axial direction, wherein the coupling element has:- a sealing element (21, 21') made from a resilient material which has an axial, radially extending sealing portion (23, 23') which is exposed in the axial direction towards the free end (8) of the coupling element (4), against which a sealing portion (43) of the pipette tip (10) can be pressed axially at least in part, characterized in thatthe coupling element (4) has at least one holding element (27, 57) arranged on the outside thereof for interacting with holding means (47) of the pipette tip in order to press the sealing portion (43) of the pipette tip (10) against the axial sealing portion (23, 23') and to position the pipette tip in the axial direction, wherein the holding element is a peripheral spring element (27) which is arranged in a peripheral depression (30) located on the outside of the coupling element.
- Device according to Claim 1, characterized in that the coupling element (4) has at least one preferably single-part or multi-part guide element (25, 26) arranged on the outside thereof for aligning the pipette tip (10) laterally.
- Device according to Claim 2, characterized in that the coupling element has two guide elements (25, 26) set axially apart from each other on the outside of the coupling element.
- Device according to Claim 3, characterized in that the guide elements (25, 26) each form a radially encircling guide ring having a predefined radial and preferably a constant radial extension, wherein the guide rings have a different radial extension and are of continuous and/or interrupted construction preferably independently of one another.
- Device according to Claim 3 or 4, characterized in that the guide elements (25, 26) are at a distance (d) from each other, which distance is at least as great as the radial extension (D) of the guide elements or of the larger of the two guide elements.
- Device according to any one of the preceding claims, characterized in that the coupling element (4) has at least one holding element (27, 57) arranged on the outside thereof for interacting with holding means (47) of the pipette tip in order to press the sealing portion (43) of the pipette tip (10) against the axial sealing portion (23, 23') and/or to position the pipette tip in the axial direction.
- Device according to any one of the preceding claims, characterized in that the coupling element (4) has a first portion (20) which is arranged close to the free end (8) of the coupling element and a second portion (22) which is arranged with an axial offset relative to the first portion (20) in the pushing-on direction.
- Device according to Claim 7, characterized in that the first portion (20) has a smaller radial extension than the second portion (22) preferably at each point.
- Device according to Claim 7 or 8, characterized in that one guide element (25, 26) is arranged on each of the first and second portions (20, 22).
- Device according to any one of Claims 7 to 9, characterized in that the sealing element (21, 21') is arranged between the first and second portions (20, 22) .
- Device according to any one of Claims 7 to 10, characterized in that the holding element (27, 57) is arranged on the second portion (22).
- Device according to any one of the preceding claims, characterized in that the sealing element (21, 21') consists of a fluoroelastomer.
- Device according to any one of Claims 6 to 12, characterized in that the holding element is a peripheral spring element (27) which is arranged in a peripheral depression (30) located on the outside of the coupling element.
- Device according to any one of Claims 6 to 12, characterized in that the holding element has one or more radial elevations (57) which are arranged in a partially or annularly encircling manner on the outside of the coupling element and are preferably rigid or flexible.
- Device according to any one of Claims 6 to 14, characterized in that the holding element (27, 57) is arranged behind all guide elements (25, 26) when viewed in the pushing-on direction.
- Device according to any one of the preceding claims, characterized in that the sealing element (21, 21') is elastically deformable in its material cross section.
- Device according to any one of the preceding claims, characterized in that the coupling element (4) has an insertion bevel (68) at its free end (8) for pre-adjusting the pipette tip.
- Use of a pipette tip for placing on the device for mounting according to any one of the preceding claims, wherein the pipette tip has- a longitudinal axis (6); and- a coupling portion (14) extending in the longitudinal axis (6) for pushing onto the mounting, wherein the coupling portion (14) has a first portion (40) and a second portion (42) offset axially with respect to the first portion (40) in the pushing-on direction (2), and the first portion (40) has a smaller radial extension than the second portion (42), and wherein at least one portion (40, 42) has an inner wall (70) at least sections of which taper conically counter to the pushing-on direction (2), in which a guide surface (45, 46, 72) that is cylindrical relative to the longitudinal axis (6) is integrated, characterized by- a sealing portion between the first and the second portions (40, 42) with as sealing surface (43) facing axially in the pushing-on direction (2) for interacting with the sealing element of the mounting.
- Use according to Claim 18, characterized in that the inner wall (70) is aligned at an angle greater than 0.2° and preferably between 0.5° and 3° relative to the longitudinal axis (6) in the direction of the longitudinal axis.
- Use according to Claim 18 or 19, characterized in that each of the first and second portions (40, 42) has conically tapering inner walls, in each of which a cylindrical guide surface (45, 46, 72) is integrated.
- Use according to any one of Claim 18 to 20, characterized in that it has at least one holding means (47) arranged on the inner wall of the second portion (42) for interacting with a holding element of the mounting.
- Use according to Claim 21, characterized in that the holding means (47) is an undercut.
- Use according to any one of Claims 18 to 22, characterized in that the pipette tip is an injection moulded part.
- Use according to any one of Claims 18 to 23, characterized in that coupling portion (14) comprises an end area which is designed to be more flexible than the other areas of the coupling portion (14).
- Use according to any one of Claims 18 to 24, characterized in that the coupling portion (14) is made from a first material (80) and has incisions (82) extending in the longitudinal direction which are filled with a second material that is more resilient than the first material.
- Use according to any one of Claims 18 to 25, characterized in that the sealing section is a shoulder between the first and second portions (40, 42) .
- Pipetting device with(a) a coupling element (4) according to any one of Claims 1 to 17 and(b) a pipette tip (10) which is detachably fastenable to the coupling element (4) having a sealing portion (43) that is embodied as an axial surface facing in the direction of the coupling element (4) relative to the longitudinal axis (6) of the coupling element (4),and wherein in the coupled state at least a part of the sealing portion (23, 23') of the coupling element (4) is pressed axially against at least one part of the sealing portion (43) of the pipette tip (10).
- Use according to any one of claims 18 to 26,- wherein the coupling element (4) has at least one guide element (25, 26) arranged on the outside thereof for aligning the pipette tip (10) laterally, and preferably has as many guide elements (25, 26) as the pipette tip (10) has guide surfaces (45, 46, 72),- wherein the guide element or elements (25, 26) is/are embodied independently of one another, preferably as a single part or as multiple parts- and wherein each guide element (25, 26) has at least partial surfaces of a cylindrical lateral surface, each of which corresponds to a cylindrical guide surface (45, 46, 72) which interacts with the partial surface on the pipette tip (10).
- Pipetting device according to Claim 27, characterized in that the coupling element (4) has at least one holding element (27, 57) arranged on the outside thereof for interacting with at least one holding means (47) of the pipette tip (10), wherein the at least one holding element (27, 57) is designed preferably either rigidly or flexibly relative to the at least one holding means (47).
Priority Applications (12)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP06010976.6A EP1862219B1 (en) | 2006-05-29 | 2006-05-29 | Device for holding a pipette tip and pipetting device |
EP07725637.8A EP2024090B1 (en) | 2006-05-29 | 2007-05-29 | Device for mounting pipette tips, pipette tip, and pipetting device |
PCT/EP2007/004746 WO2007137818A1 (en) | 2006-05-29 | 2007-05-29 | Device for mounting pipette tips, pipette tip, and pipetting device |
BRPI0712522-4A BRPI0712522B1 (en) | 2006-05-29 | 2007-05-29 | Pipette tip for placement on a rack, and pipetting device |
ES07725637T ES2886457T3 (en) | 2006-05-29 | 2007-05-29 | Device for holding pipette tips, pipette tip, as well as pipetting device |
DK07725637.8T DK2024090T3 (en) | 2006-05-29 | 2007-05-29 | PIPETTE TIPS, PIPETTE TIP AND PIPETTING DEVICE |
US12/302,749 US8512650B2 (en) | 2006-05-29 | 2007-05-29 | Device for mounting pipette tips, pipette tip, and pipetting device |
JP2009512480A JP5511375B2 (en) | 2006-05-29 | 2007-05-29 | Pipette tip loading device, pipette tip, and pipette drive device |
KR1020087031523A KR101159885B1 (en) | 2006-05-29 | 2007-05-29 | Device for mounting pipette tips, pipette tip, and pipetting device |
EP21169623.2A EP3885046A1 (en) | 2006-05-29 | 2007-05-29 | Device for holding pipette tips and usage of the device |
CN2007800253319A CN101484242B (en) | 2006-05-29 | 2007-05-29 | Device for mounting pipette tips, pipette tip, and pipetting device |
RU2008151740/05A RU2424851C2 (en) | 2006-05-29 | 2007-05-29 | Pipette tip fastener, pipette tip, pipette doser |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP06010976.6A EP1862219B1 (en) | 2006-05-29 | 2006-05-29 | Device for holding a pipette tip and pipetting device |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1862219A1 EP1862219A1 (en) | 2007-12-05 |
EP1862219B1 true EP1862219B1 (en) | 2018-02-07 |
Family
ID=37043865
Family Applications (3)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP06010976.6A Active EP1862219B1 (en) | 2006-05-29 | 2006-05-29 | Device for holding a pipette tip and pipetting device |
EP07725637.8A Active EP2024090B1 (en) | 2006-05-29 | 2007-05-29 | Device for mounting pipette tips, pipette tip, and pipetting device |
EP21169623.2A Pending EP3885046A1 (en) | 2006-05-29 | 2007-05-29 | Device for holding pipette tips and usage of the device |
Family Applications After (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP07725637.8A Active EP2024090B1 (en) | 2006-05-29 | 2007-05-29 | Device for mounting pipette tips, pipette tip, and pipetting device |
EP21169623.2A Pending EP3885046A1 (en) | 2006-05-29 | 2007-05-29 | Device for holding pipette tips and usage of the device |
Country Status (10)
Country | Link |
---|---|
US (1) | US8512650B2 (en) |
EP (3) | EP1862219B1 (en) |
JP (1) | JP5511375B2 (en) |
KR (1) | KR101159885B1 (en) |
CN (1) | CN101484242B (en) |
BR (1) | BRPI0712522B1 (en) |
DK (1) | DK2024090T3 (en) |
ES (1) | ES2886457T3 (en) |
RU (1) | RU2424851C2 (en) |
WO (1) | WO2007137818A1 (en) |
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US9486803B2 (en) * | 2010-01-22 | 2016-11-08 | Biotix, Inc. | Pipette tips |
-
2006
- 2006-05-29 EP EP06010976.6A patent/EP1862219B1/en active Active
-
2007
- 2007-05-29 JP JP2009512480A patent/JP5511375B2/en active Active
- 2007-05-29 CN CN2007800253319A patent/CN101484242B/en active Active
- 2007-05-29 RU RU2008151740/05A patent/RU2424851C2/en active
- 2007-05-29 BR BRPI0712522-4A patent/BRPI0712522B1/en active IP Right Grant
- 2007-05-29 EP EP07725637.8A patent/EP2024090B1/en active Active
- 2007-05-29 WO PCT/EP2007/004746 patent/WO2007137818A1/en active Application Filing
- 2007-05-29 EP EP21169623.2A patent/EP3885046A1/en active Pending
- 2007-05-29 KR KR1020087031523A patent/KR101159885B1/en active IP Right Grant
- 2007-05-29 DK DK07725637.8T patent/DK2024090T3/en active
- 2007-05-29 US US12/302,749 patent/US8512650B2/en active Active
- 2007-05-29 ES ES07725637T patent/ES2886457T3/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0351574A2 (en) * | 1988-07-21 | 1990-01-24 | Eppendorf-Netheler-Hinz Gmbh | Removable pipette tip shaped as a container adapted to the shape of a receiving piece, especially a tapered pipette end |
DE19917375A1 (en) * | 1999-04-16 | 2000-11-02 | Hamilton Bonaduz Ag Bonaduz | Pipette tip, pipetting device and combination of pipette tip and pipetting device |
Also Published As
Publication number | Publication date |
---|---|
EP2024090B1 (en) | 2021-06-30 |
EP1862219A1 (en) | 2007-12-05 |
WO2007137818A1 (en) | 2007-12-06 |
BRPI0712522B1 (en) | 2018-08-07 |
RU2424851C2 (en) | 2011-07-27 |
KR20090027671A (en) | 2009-03-17 |
EP2024090A1 (en) | 2009-02-18 |
ES2886457T3 (en) | 2021-12-20 |
JP5511375B2 (en) | 2014-06-04 |
JP2009538725A (en) | 2009-11-12 |
US8512650B2 (en) | 2013-08-20 |
EP3885046A1 (en) | 2021-09-29 |
DK2024090T3 (en) | 2021-09-20 |
US20100196210A1 (en) | 2010-08-05 |
RU2008151740A (en) | 2010-07-10 |
CN101484242B (en) | 2012-11-28 |
BRPI0712522A2 (en) | 2012-09-04 |
KR101159885B1 (en) | 2012-06-26 |
CN101484242A (en) | 2009-07-15 |
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