EP1514027B1 - Hochdruck-kleinvolumen-verdrängerpumpe - Google Patents

Hochdruck-kleinvolumen-verdrängerpumpe Download PDF

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Publication number
EP1514027B1
EP1514027B1 EP03727124A EP03727124A EP1514027B1 EP 1514027 B1 EP1514027 B1 EP 1514027B1 EP 03727124 A EP03727124 A EP 03727124A EP 03727124 A EP03727124 A EP 03727124A EP 1514027 B1 EP1514027 B1 EP 1514027B1
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EP
European Patent Office
Prior art keywords
piston
pump
sealing
displacement chamber
sealing surfaces
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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EP03727124A
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English (en)
French (fr)
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EP1514027A2 (de
Inventor
Fritz Gyger
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Gyger Fritz
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Individual
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Publication of EP1514027A2 publication Critical patent/EP1514027A2/de
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Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04BPOSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B11/00Equalisation of pulses, e.g. by use of air vessels; Counteracting cavitation
    • F04B11/005Equalisation of pulses, e.g. by use of air vessels; Counteracting cavitation using two or more pumping pistons
    • F04B11/0075Equalisation of pulses, e.g. by use of air vessels; Counteracting cavitation using two or more pumping pistons connected in series
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04BPOSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B53/00Component parts, details or accessories not provided for in, or of interest apart from, groups F04B1/00 - F04B23/00 or F04B39/00 - F04B47/00
    • F04B53/14Pistons, piston-rods or piston-rod connections
    • F04B53/144Adaptation of piston-rods
    • F04B53/147Mounting or detaching of piston rod
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04BPOSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B53/00Component parts, details or accessories not provided for in, or of interest apart from, groups F04B1/00 - F04B23/00 or F04B39/00 - F04B47/00
    • F04B53/16Casings; Cylinders; Cylinder liners or heads; Fluid connections
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04BPOSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B53/00Component parts, details or accessories not provided for in, or of interest apart from, groups F04B1/00 - F04B23/00 or F04B39/00 - F04B47/00
    • F04B53/16Casings; Cylinders; Cylinder liners or heads; Fluid connections
    • F04B53/162Adaptations of cylinders
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04BPOSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B53/00Component parts, details or accessories not provided for in, or of interest apart from, groups F04B1/00 - F04B23/00 or F04B39/00 - F04B47/00
    • F04B53/16Casings; Cylinders; Cylinder liners or heads; Fluid connections
    • F04B53/162Adaptations of cylinders
    • F04B53/164Stoffing boxes
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04BPOSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B2201/00Pump parameters
    • F04B2201/02Piston parameters
    • F04B2201/0201Position of the piston
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F05INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
    • F05CINDEXING SCHEME RELATING TO MATERIALS, MATERIAL PROPERTIES OR MATERIAL CHARACTERISTICS FOR MACHINES, ENGINES OR PUMPS OTHER THAN NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES
    • F05C2203/00Non-metallic inorganic materials
    • F05C2203/08Ceramics; Oxides
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F05INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
    • F05CINDEXING SCHEME RELATING TO MATERIALS, MATERIAL PROPERTIES OR MATERIAL CHARACTERISTICS FOR MACHINES, ENGINES OR PUMPS OTHER THAN NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES
    • F05C2225/00Synthetic polymers, e.g. plastics; Rubber
    • F05C2225/04PTFE [PolyTetraFluorEthylene]
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F05INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
    • F05CINDEXING SCHEME RELATING TO MATERIALS, MATERIAL PROPERTIES OR MATERIAL CHARACTERISTICS FOR MACHINES, ENGINES OR PUMPS OTHER THAN NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES
    • F05C2225/00Synthetic polymers, e.g. plastics; Rubber
    • F05C2225/12Polyetheretherketones, e.g. PEEK

Definitions

  • the present invention refers to pumps according to the preamble of claim 1. Furthermore, the invention refers to adjusting methods and to applications of such pumps.
  • a current construction comprises two positive displacement pump units arranged in series.
  • the fist unit is the feed pump, which aspirates the liquid at low pressure, e.g. at ambient pressure, and delivers it to the second unit, the storage pump, at operating pressure.
  • the storage pump essentially operates in a push-pull relationship with the first unit. It delivers a liquid flow while the first unit aspirates the liquid and stores the surplus while the first unit is expelling the working medium at the operating pressure. This allows achieving a regular flow with low pulsation.
  • the pistons are made of mechanically resistant materials, more particularly ceramic (preferred), crystalline and/or mineral materials, which are guided in stone bearings, i.e. ruby, sapphire, synthetic corundum, or ceramic bearings. Tightness is ensured by piston seals that are open towards the working volume. Thus, since the working medium under pressure accesses the outside of the sealing lip, the latter is pressed against the piston surface by the working pressure, thereby providing the corresponding sealing effect by itself. In order to ensure the required pressure resistance and chemical inertness, the parts in contact with the working medium are made of high-grade materials, metals, and precious stones. Thus, the use of titanium is current practice, for example.
  • the pistons are driven by camshafts acting on the rear end of the pistons in combination with resilient restoring elements.
  • the compressibility of the liquids becomes noticeable, so that a pump of this kind can be adjusted for minimum compressibility only at a given pressure by mutually adjusting the sequences of movements of the two pump units.
  • An additional difficulty is that the dead space of such pumps is relatively large compared to the dispensing volume of approx. 0.01 to 0.05 cm 3 (10 to 50 microliters) per stroke in gradient applications, so that the dead space may even be greater than the dispensing volume.
  • the large dead space is mainly a result of the minimal distance of the piston from the bottom of the displacement chamber and of the piston seal.
  • the dead space affects the gradient capability, i.e. it determines the minimal dispensing rate at which a working medium of changing composition can still be delivered by the pump without being substantially mixed.
  • a large dead space contains correspondingly large quantities of the working medium that also have to be exchanged to avoid mixing in gradient operation.
  • the pumps are subject to aging, thereby requiring maintenance. Due to the stringent requirements especially in the assembly, this must be done by a specialist.
  • Suitable pumps are e.g. known from ( EP-A-0 898 077 ; US-A-3 981 620 or DE-A-43 08 467 ).
  • the particularity of these pumps is that they are composed of disk-shaped functional blocks that are clamped together in a clamping device. The fact that the junctions extend between the blocks eliminates the need for external connecting ducts.
  • a problematic zone with regard to tolerances in assembly consists in small misalignments or angular deviations of the connecting elements required at the inlets and outlets of the pump units, i.e. at the access points of the working medium.
  • a connecting piece in the form of a so-called cartridge is inserted between the connecting element and the access.
  • a cartridge may essentially have the form of a pipe section (coupling sleeve) or e.g. comprise a check valve ("valve cartridge").
  • a second object of the present invention is to provide a pump of this kind that reduces the influence of construction tolerances on the dispensing quality.
  • Another object consists in controlling and/or reducing the influence of the dead space.
  • a pump attaining the first object is given by claim 1.
  • the further claims define preferred embodiments of the pump, methods of adjusting the pump, applications of the pump and chromographic devices including the pump.
  • the involved pairs of surfaces are designed as a combination of a cambered (convex, spherical) and a concave conical surface.
  • a misalignment between the medium inlet and the connecting element results in a slightly canted fit of the cartridge.
  • the mentioned design nevertheless provides a circular contact line and a regular contact pressure.
  • the involved pairs of surfaces may be formed not only on the mentioned parts but also on the corresponding part and on a sealing body (a capsule).
  • the cambered surface will preferably be provided on the capsule.
  • Another aspect of the invention is to provide the possibility of adjusting the dead space and furthermore a general reduction thereof.
  • One measure to this effect is a construction of the displacement chamber and/or of the piston that allows the adjustment of a minimum dead space or of a dead space resulting in an optimum behavior of the pump at the desired operating pressure. It is therefore suggested, on one hand, to make the total length of the piston adjustable by dividing it into the proper piston and a piston rod. The connection between the piston and the piston rod is adjustable in length, thereby allowing an adjustment providing a minimum distance of the piston from the bottom of the displacement chamber.
  • the distance may even be set to zero if in order to avoid damages, the bottom of the chamber is formed of an insert that is sufficiently incompressible under operating pressure but nevertheless capable of yielding enough to prevent damages when hit by the piston.
  • Another approach consists in providing an opposed piston whose front end essentially forms the chamber bottom, thereby making the chamber bottom adjustable.
  • novel constructions of the seals between the piston and the displacement chamber also provide a reduction of the dead space.
  • the classic piston seal comprises a spiral spring enclosed in the piston seal and surrounding the sealing lip. Particularly the interior of the spiral spring causes a large dead space.
  • a laterally open spring element is suggested.
  • the aperture allows a filling body to be inserted in the spring element such that the major part of the cavity within the spring element is filled.
  • the spring element is essentially in the form of a band-shaped element surrounding the sealing lip.
  • the latter is a spiral of a spring-elastic material, particularly metal.
  • the flat shape of the spring element allows a small cross-section of the internal wall of the displacement chamber also in the area of the seal, thereby keeping the dead space small.
  • Figs. 1 and 2 show sectional views of head 1 of a HPLC pump designed according to the invention.
  • the elements that are not represented are realized according to the prior art.
  • the piston assemblies for feed pump device 3 (feed pump) and storage pump device 4 (storage pump), replacing the undivided pistons of the prior art are formed of respective pistons 7, 8 and piston rods 11, 12.
  • the piston rods are guided in high-grade linear guides in the enclosure of the driving unit, more particularly in linear ball bearings (not shown). Bearings of this kind are known per se in the art.
  • respective sleeves 15, 16 are fixedly fitted on hard material bars 19, 20, i.e. bars of a mechanically resistant material (e.g. ceramic). Sleeves 15, 16 are closed at their rear ends.
  • respective steel balls 25 e.g. of hardened steel
  • Balls 25 provide a defined contact in the center of the hard material bars, on one hand, and on the other hand, an annular contact on the bottom of bores 26 whose shape is conical due to the shape of the tips of usual drills.
  • Sleeves 15, 16 are seated in location holes 28 in the ends of piston rods 11, 12.
  • a spring 32 is inserted in a smaller location hole 30 in the bottom of location hole 28, the free end of the spring resting on the bottom 23 of sleeve 16.
  • Each one of piston rods 11, 12 is surrounded by a set collar 36.
  • Each set collar 36 comprises a set screw 38 in a thread 39, the end of the screw contacting sleeve 15, 16 through a bore 40 in piston rod 11, 12.
  • the pistons 7, 8 are thus capable of being locked in the respective piston rod by fastening screw 38.
  • Screw 38 of storage pump 4 is accessible from the outside through an aperture 42 in the enclosure of pump head 1.
  • bore 31 in piston rod 11 is internally threaded to receive a threaded stem 33 attached to sleeve 15.
  • a precise adjustment of the piston length is thus possible through a rotation of threaded stem 33.
  • a locking device is required here too, e.g. a set collar 36 with a set screw 38.
  • the adjustment of the dead space in the assembled state is obtained by varying the displacement chamber, for which purpose a solution will be indicated below.
  • Both hard material bars 19, 20 extend into the proper displacement chamber 47 through a conventional piston seal 44, a stone bearing 46 (e.g. of synthetic precious stone such as ruby) and finally through a piston seal according to the invention that provides a reduced dead space.
  • Chamber 47 is formed of a highly resistant and chemically inert material, e.g. of titanium.
  • Outlet 112 of feed pump 3 is connected to inlet 115 of storage pump 4 by a known flexible conduit 114 having a small internal volume.
  • Conduit 114 is tightly fastened to the connections 100 by screwed joints known per se .
  • the dispensing piston is shown with a first embodiment 48 of a piston seal of the invention that is illustrated on an enlarged scale in Fig. 3 .
  • It is essentially formed of a sealing body 50 of essentially L-shaped cross-section, one leg 52 of which forms a sleeve-shaped sealing lip in which hard material bar 19 resp. 20 of a piston 7 resp. 8 is insertable.
  • the sealing lip is surrounded by a spring 54 in such manner that the spiral turns themselves wind around the sealing lip.
  • this allows a relatively narrow design of internal wall 56 around seal 48 as compared to the environment of the conventional piston seal 44, thereby providing a considerable reduction of the dead space.
  • Displacement chamber 47 of feed pump 3 is open at the bottom and closed by means of an opposed piston 58 whose front end forms the (movable) bottom of the displacement chamber.
  • Opposed piston 58 is also made of titanium.
  • Opposed piston 58 extends through a sealing bushing 60 retained by a clamping sleeve 62 in an enlarged portion 64 of displacement chamber bore 57. It is also possible to provide a screwed attachment both of sleeve 62 in enlarged portion 64 and of opposed piston 58 in sleeve 62 to allow a displacement of the opposed piston by rotation thereof and thus a variation of the displacement chamber volume.
  • Fig. 11 shows a seal 64 of the prior art that may be inserted instead of sealing bushing 60 and results in a reduced dead space. Since opposed piston 58 is not moved in operation and only rarely otherwise, the requirements with regard to this seal are substantially less stringent.
  • Seal 64 comprises a seal body 65 with a sealing lip 66 that is pressed against opposed piston 58 (not shown). The contact pressure is initially provided by embedded O-ring 67 and in operation by the internal pressure of the pump acting upon O-ring 67 and on the sealing lip.
  • Possible materials for the seal body are pressure-resistant materials that are chemically inert under the operating conditions, such as PTFE, in particular.
  • a corresponding elastomer will be selected for the O-ring, e.g. KALREZ (DuPont). Seals of this kind are known per se .
  • FIG. 4 An enlarged view of the applied piston seal 70 is shown in Fig. 4 and the special spring element in Fig. 5 .
  • Sealing element 72 of the piston seal is C-shaped in cross-section, and so is spring element 74.
  • a thickened or cambered portion 75 is formed at the end of internal sealing lip 73.
  • the internal surface 76 of spring element 74 and its curved portion 77 are divided by multiple slots 79. Depending on the desired rigidity, the slots also divide external surface 81, the rigidity decreasing with the width of remaining lands 82. Curved portion 77 describes an angle that is a little smaller than 180°, so that the internal surface is slightly biased inwards.
  • spring element 74 is arranged in sealing element 72 with the cross-sections extending in parallel, and an annular filling body 83 is inserted in the resulting annular gap.
  • the filling body consists of a material that is chemically inert to the working medium and substantially incompressible under working pressure.
  • the filling body is so dimensioned that it largely fills out the interior of the spring element, i.e. at least half of it, preferably at least 90% and more preferably at least 99%. Basically, is should be as voluminous as possible, however without reducing the spring action of the spring element below the required level.
  • the dead space caused by the seal is substantially reduced while maintaining the same mounting dimensions as in the case of a conventional piston seal.
  • the storage pump also comprises an arrangement for adjusting the dead space that includes the adjusting device between piston 8 and piston rod 16 as well as an insert 87 in displacement chamber 89.
  • the material of insert 87 is chosen such that a contact between hard material bar 20 and insert 87 is possible without causing damages.
  • a material will be chosen that is inert to the working medium and substantially incompressible under operating pressure while still being slightly deformable by the mechanically resistant material.
  • the circumference of the front ends of hard material bars 19, 20 is rounded to avoid damages of the seals and guides when they are inserted in the displacement chambers.
  • the material of insert 87 is capable of a certain adaptation to this rounded edge, thereby additionally reducing the dead space.
  • Displacement chambers 47, 89 are located in bores of a pump block 91.
  • displacement chambers 47, 89 comprise a groove 93 in which a pin 94 engages.
  • Displacement chambers 47, 89 are followed by an extension ring 95 which is fixed in block extension 96 by a threaded ring 97.
  • Block extension 96 is screwed to block 91.
  • an elastomer preferably the synthetic material PTFE (polytetrafluorethylene) may be used, particularly PTFE reinforced with graphite fibers, which offers an increased wear, pressure, and temperature resistance.
  • PTFE polytetrafluorethylene
  • PEEK polyetherether ketone
  • feed pump and the storage pump may also be identical in design.
  • both pumps may be provided with the same inventive piston seals of either type.
  • the feed pump may comprise a closed displacement chamber with an insert 87, i.e. it may be designed like the described storage pump and conversely, the storage pump may be designed like the described feed pump. It is thereby possible to adjust the dead space of the feed pump to nearly zero, which is optimal in almost all operating conditions. A subsequent adjustment of the opposed piston in the storage pump allows to minimize the pulsation, i.e. to adjust the pump to the working pressure and to the compressibility of the working medium.
  • the adjustment of a determined dead space at the bottom of the displacement chamber, or in the extreme case of a dead space reduced to nearly zero, is always effected by first moving the respective piston to the upper dead center, i.e. by moving the drive to the position of maximum penetration of the piston into the displacement chamber, while the corresponding set screw is loosened.
  • the hard material bar of the piston now contacts insert 87.
  • Set screw 38 is tightened, whereby the dead space is adjusted to minimum.
  • the dead space may subsequently be enlarged to a desired amount by retracting the opposed piston.
  • a further basic aspect with regard to the quality of a pump of this kind is tightness. It will be noted that minimal leakage, which is not detectable externally due to the small volumes of e.g. substantially less than 0.001 cm 3 (1 microliter), may already influence the result. In this respect, the sealing of the various connections against the displacement chambers constitutes a problem of utmost importance.
  • the cartridges may simply represent passages (see Fig. 7 , cartridge 101), or e.g. check valves 102 as provided according to Figs. 1 and 2 at the inlet 111 and outlet 112 of the feed pump.
  • one of the sealing surfaces of a junction is cambered, more particularly in a convex spherical shape, and the respective corresponding surface has a concave conical shape.
  • a circular contact line is still obtained, and thus also a substantially constant contact pressure.
  • a metallic sealing membrane 117 is preferably interposed, preferably one of titanium because of its contact with the working medium, or of a synthetic material, particularly of PEEK.
  • the rounded sealing surfaces are provided on the connecting elements and on the displacement chambers and the conical ones on cartridges 102.
  • the inverse arrangement is also possible.
  • the described construction also avoids leaks due to angular deviations between the parts to be joined.
  • one 120 of the two sealing surfaces, or possibly both sealing surfaces in the case of two sealing surfaces with an interposed membrane, particularly metallic ones, may have steps 121 formed thereon (see Fig. 9 ).
  • the result is a stepped sealing action or a plurality of line contacts, thereby further improving the sealing effect.
  • Another useful solution consists in providing concentric grooves 123 ( Fig. 10 ).
  • FIG. 12 and 13 A further preferred embodiment of the junctions for the connection of a capillary conduit without additional functions is shown in Figs. 12 and 13 .
  • Conduit 114 is made of titanium and is welded to an end piece 130.
  • Connecting piece 100 is in the form of a threaded collar that is displaceable on the capillary conduit.
  • the passage for conduit 114 through connecting piece 100 is enlarged at its inner end 132 to leave room for the weld seam 134.
  • Sealing surface 136 of end piece 130 is designed as described above so as to ensure a perfect seal also in the case of a misalignment.
  • the embodiment using a sealing capsule or the embodiment using a sealing membrane may be chosen.
  • the threaded collar is screwed into the pump enclosure in a known manner.
  • the contact surfaces 138 between end piece 130 and connecting piece 100 have complementary cambered, conical, or similar shapes to provide a self-centering action when the connecting piece is screwed into the pump enclosure. However, contact surfaces 138 do not have a sealing function.
  • Connecting piece 100 is made of PEEK or of steel. Compared to the first described embodiment, this solution eliminates two sealing surfaces as well as the dead space caused by the channel in the empty cartridge, whose diameter is relatively large, and around the additional threaded collars screwed into connecting pieces 100.
  • Fig. 13 shows a connecting conduit 114 whose ends are provided with the above-mentioned connecting devices.
  • the two threaded collars 100 Prior to the welding of the second one of end pieces 130, the two threaded collars 100 have to be slipped on conduit 114.
  • the operation of bending conduit 114 to the required shape, e.g. the shape of a U, may take place afterwards.
  • each one of the measures leads to in increased quality of the pump, they may also serve to simplify maintenance, i.e. particularly to reduce the skills required of the technician. Thus, in particular, maintenance can be carried out on site by the user without accepting losses in quality.
  • the connecting elements may also be flanged to the pump body or fastened in another manner. However, they are preferably removable for uncomplicated maintenance and repair.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Details Of Reciprocating Pumps (AREA)
  • Reciprocating Pumps (AREA)
  • Diaphragms For Electromechanical Transducers (AREA)
  • Compressors, Vaccum Pumps And Other Relevant Systems (AREA)

Claims (23)

  1. Pumpe (1) zur Förderung genau bestimmter kleiner Flüssigkeitsströme bei hohen Drücken, insbesondere von Strömen bis maximal 5 cm3/min (5 ml/min) und/oder bei Drücken von mindestens 100 bar, wobei die Pumpe mindestens eine Pumpeinrichtung (3; 4) aufweist, die einen in einer Verdrängerkammer (47; 89) bewegbaren Kolben (7; 8) umfasst, an wenigstens einer Arbeitsmediumzugangsbohrung der Pumpeinrichtung eine lösbare Anschlussanordnung (100, 101; 100, 102; 100, 130) vorhanden ist, die wenigstens ein Dichtflächenpaar aufweist, die einen gegenüber dem Arbeitsmedium dichten Übergang bilden, dadurch gekennzeichnet, dass im Zentrum der Dichtflächen jeweils eine Öffnung eines Kanals für das Arbeitsmedium vorhanden ist, die eine Dichtfläche der Paare von Dichtflächen im wesentlichen kalottenförmig und konvex und die andere im wesentlichen konkav und kegelförmig ausgebildet ist, so dass auch bei nicht genau fluchtender Anordnung der Kanalöffnungen eine ringförmige Kontaktlinie zwischen den beiden Dichtflächen vorliegt.
  2. Pumpe gemäss Anspruch 1, dadurch gekennzeichnet, dass zwischen den Dichtflächen mindestens eines Paares von Dichtflächen, bevorzugt aller derartiger Paare, eine Dichtung (117) angeordnet ist, insbesondere in Form eines membranartigen Elements aus Metall oder einem hoch druckfesten Kunststoff, bevorzugt aus PEEK.
  3. Pumpe (1) gemäss Anspruch 1, dadurch gekennzeichnet, dass mindestens ein erstes und ein zweites Paar von Dichtflächen vorhanden und zwischen den beiden Paaren von Dichtflächen ein Dichtkörper (119) angeordnet ist, an dem die jeweils innere Dichtfläche der beiden Dichtflächenpaare ausgebildet ist und der aus einem formstabilen, hoch druckfesten Kunststoff, bevorzugt aus PEEK, besteht.
  4. Pumpe (1) gemäss einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass mindestens ein erstes und drittes Paar von Dichtflächen vorhanden ist, wovon die beiden inneren, jeweils dem anderen Paar zugewandten Dichtflächen an einem Verbindungskörper (101, 102) ausgebildet sind, der zwischen den beiden anderen, äusseren Dichtflächen der beiden Paare angeordnet ist, so dass die beiden Dichtflächenpaare je einen dichten Übergang zum Verbindungskörper darstellen.
  5. Pumpe gemäss einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass zusätzlich zu einem Dichtflächenpaar ein Paar (138) aus einer ersten und einer zweiten Kontaktfläche vorhanden ist, wobei die erste und die zweite Kontaktfläche aneinander anliegen, die erste Kontaktfläche und die eine der Dichtflächen an einem zweiten Verbindungskörper (130) in der Anschlussanordung (100, 130) ausgebildet sind und der zweite Verbindungskörper zwischen der zweiten Kontaktfläche und der anderen der Dichtflächen gehalten ist und mit einer Leitung (114) für das Arbeitsmedium fest verbunden ist, wobei die Leitung in den Kanal mündet, dessen Öffnung sich in der Dichtfläche am zweiten Verbindungskörper befindet.
  6. Pumpe gemäss Anspruch 5, dadurch gekennzeichnet, dass die Kontaktflächen (138) gewölbt und komplementär zueinander ausgebildet sind, um eine Zentrierung des zweiten Verbindungskörpers (130) in der zweiten Kontaktfläche zu bewirken.
  7. Pumpe gemäss einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass mindestens in einem der ersten Dichtflächenpaare, bevorzugt in allen ersten Dichtflächenpaaren, mindestens eine der Dichtflächen (120) eine konzentrisch stufenförmige Oberfläche (121) aufweist, um eine Mehrzahl Dichtlinien zu erhalten.
  8. Pumpe (1) gemäss einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, dass der Kolben wenigstens eine vorderste, den Kolben gegen die Verdrängerkammer abdichtende erste Dichtung (70) aufweist und die erste Dichtung ein Dichtelement (72) mit einer den Kolben umfassenden Dichtlippe (73) aufweist, dass die erste Oberfläche der Dichtlippe mittels eines federelastischen Elements (74), das an der gegenüberliegenden zweiten Oberfläche der Dichtlippe anliegt, gegen den Kolben vorgespannt ist, wobei die zweite Oberfläche mit der Verdrängerkammer in Verbindung steht, und dadurch, dass das Dichtelement (72) und das Federelement einen im wesentlichen C-förmigen Querschnitt aufweisen und darin ein unter den Betriebsbedingungen im wesentlichen inkompressibler Füllkörper (83) angeordnet ist, um das von der Dichtung herrührende Totvolumen der Pumpeinrichtung zu vermindern.
  9. Pumpe gemäss Anspruch 8, dadurch gekennzeichnet, dass die Breite des Schlitzes des C-Profils im wesentlichen gleich der Höhe des Inneren des C ist, so dass der Füllkörper (83) axial in das Federelement (74) einschiebbar ist und den Innenraum des C wenigstens zum überwiegenden Teil, bevorzugt nahezu vollständig, ausfüllt.
  10. Pumpe gemäss einem der Ansprüche 1 bis 9, dadurch gekennzeichnet, dass der Kolben wenigstens eine vorderste, den Kolben gegen die Verdrängerkammer abdichtende zweite Dichtung (48) aufweist, dass die zweite Dichtung eine den Kolben umfassende Dichtlippe (52) aufweist, deren erste Oberfläche mittels eines federelastischen Elements (54), das an deren gegenüberliegender zweiter Oberfläche anliegt, gegen den Kolben vorgespannt ist, wobei die zweite Oberfläche mit der Verdrängerkammer in Verbindung steht, und dass das Federelement im wesentlichen die Form eines geschlossenen federelastischen Bandes aufweist, das mit seiner Innenseite an der zweiten Oberfläche der Dichtlippe anliegt, und dass die Innenwand der Verdrängungskammer mit geringem Abstand zur Aussenfläche des Federelements ausgeführt ist, um das von der Dichtung herrührende Totvolumen der Pumpeinrichtung zu vermindern.
  11. Pumpe (1) gemäss Anspruch 10, dadurch gekennzeichnet, dass das bandartige Federelement (54) im wesentlichen aus einer Spirale aus federelastischem Material besteht, wobei die Spiralwindungen um die Dichtlippe (52) verlaufen.
  12. Pumpe (1) gemäss einem der Ansprüche 1 bis 11, dadurch gekennzeichnet, dass der Kolben über eine Kolbenstange (11; 12) mit dem Pumpantrieb in Wirkverbindung steht, der Kolben über eine Kolbenjustiereinrichtung (15, 28, 31, 33, 36, 38; 16, 28, 30, 32, 36, 38) mit der Kolbenstange verbunden ist, und die Kolbenjustiereinrichtung zwischen Kolben und Kolbenstange in der Länge verstellbar ausgeführt ist, um die Gesamtlänge der Anordung von Kolben und Kolbenstange an die Distanz zwischen Antrieb und Verdrängerkammerboden und damit das Totvolumen einstellen zu können.
  13. Pumpe (1) gemäss Anspruch 12, dadurch gekennzeichnet, dass der Kolben (7; 8) an der Kolbenstange (11; 12) längsbeweglich angeordnet ist.
  14. Pumpe gemäss einem der Ansprüche 12 bis 13, dadurch gekennzeichnet, dass die Kolbenjustiereinrichtung (15, 28, 31, 33, 36, 38; 16, 28, 30, 32, 36, 38) mit einem Klemmmittel (36, 38) ausgestattet ist, um den Kolben (7; 8) in einer bestimmten Position gegenüber der Kolbenstange (11; 12) feststellen zu können.
  15. Pumpe (1) gemäss einem der Ansprüche 12 bis 14, dadurch gekennzeichnet, dass in der Kolbenjustiereinrichtung (15, 28, 31, 33, 36, 38; 16, 28, 30, 32, 36, 38) ein Federmittel (32) zwischen Kolben (7; 8) und Kolbenstange (11; 12) angeordnet ist, so dass eine Verkürzung der Gesamtlänge der Anordnung aus Kolben und Kolbenstange gegen die Rückstellkraft des Federelements erfolgt.
  16. Pumpe (1) gemäss einem der Ansprüche 12 bis 15, dadurch gekennzeichnet, dass in der Verdrängerkammer (89) als Verdrängerkammerboden ein Körper (87) vorhanden ist, der aus einem unter Betriebsdruck der Pumpe höchstens vernachlässigbar kompressiblen, jedoch hinreichend elastischeren Material als der Kolben besteht und den Querschnitt der Verdrängerkammer vollständig ausfüllt, so dass der Kolben (8) bis auf eine beliebig geringe Distanz zum Verdrängerkammerboden am oberen Totpunkt einstellbar ist, insbesondere bis auf ein im wesentlichen nicht mehr vorhandenes Totvolumen, ohne dass die Gefahr einer Beschädigung des Kolbens bei einem Kontakt mit dem Verdrängerkammerboden während des Einstellungsvorganges oder des Betriebes besteht.
  17. Pumpe (1) gemäss einem der Ansprüche 14 bis 16, dadurch gekennzeichnet, dass der Kolben (7; 8) einen stabförmigen Kolbenteil (19; 20) aus einem Hartmaterial, insbesondere aus Keramik, kristallinem und/oder mineralischem Material, aufweist, dessen Hinterende in einer Aufnahme in einer Hülse (15; 16) gefasst ist, so dass das Klemmmittel (38, 39) im wesentlichen punktförmig auf der Hülse aufsetzbar und diese damit in der Kolbenstange (11; 12) fixierbar ist ohne das Risiko einer Beschädigung des durch das Klemmmittel stabförmigen Kolbenteils.
  18. Pumpe (1) gemäss einem der Ansprüche 1 bis 17, dadurch gekennzeichnet, dass der Boden der Verdrängerkammer mindestens einer Pumpeinrichtung im wesentlichen aus dem Vorderende eines Gegenkolbens (58) gebildet ist, der in der Verdrängerkammer verschiebbar ist, so dass das Totvolumen der Pumpeinrichtung einstellbar ist.
  19. Pumpe (1) gemäss Anspruch 18, dadurch gekennzeichnet, dass der Gegenkolben (58) mit einer Verstelleinrichtung mit Positionsanzeigeeinrichtung versehen ist, um das Totvolumen in der Verdrängerkammer von aussen erkennbar, insbesondere ablesbar, einstellen zu können.
  20. Pumpe mit mindestens einer ersten (7) und einer zweiten (8) Pumpeinrichtung bestehend aus Verdrängerkammer (47; 89) und Kolben (7; 8), wobei die der ersten Pumpanordnung nachgeschaltete Pumpe als Speichereinrichtung der Pulsation der ersten Pumpeinrichtung betreibbar ist und die Pumpeinrichtungen jeweils gemäss einem der Ansprüche 1 bis 19 ausgebildet sind.
  21. Verfahren zum Einstellen des Totvolumens in einer Pumpe (1) gemäss einem der Ansprüche 12 bis 19, dadurch gekennzeichnet, dass die Kolbenstange (11; 12) auf den oberen Totpunkt gestellt wird, der Kolben (7; 8) bis zum gewünschten Totvolumen in die Verdrängerkammer vorgeschoben wird und der Kolben in der Kolbenstange durch Betätigen einer Feststelleinrichtung (38) der Kolbenjustiereinrichtung festgestellt wird.
  22. Verwendung der Pumpe gemäss Anspruch 18 oder 19 oder gemäss Anspruch 20, soweit von einem der Ansprüche 18 bis 19 abhängig, dadurch gekennzeichnet, dass der Gegenkolben (58) entsprechend dem vorgesehenen Betriebsdruck verstellt wird, um eine geringe Pulsation zu erreichen.
  23. Hochdruckchromatographievorrichtung, insbesondere für HPLC, mit einer Pumpe gemäss einem der Ansprüche 1 bis 20 als Mediumpumpe.
EP03727124A 2002-06-19 2003-06-18 Hochdruck-kleinvolumen-verdrängerpumpe Expired - Lifetime EP1514027B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP03727124A EP1514027B1 (de) 2002-06-19 2003-06-18 Hochdruck-kleinvolumen-verdrängerpumpe

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
EP02405509 2002-06-19
EP02405509A EP1375921A1 (de) 2002-06-19 2002-06-19 Hochdruck-Kleinvolumen-Verdrängerpumpe
PCT/CH2003/000394 WO2004001228A2 (en) 2002-06-19 2003-06-18 High-pressure small volume pump
EP03727124A EP1514027B1 (de) 2002-06-19 2003-06-18 Hochdruck-kleinvolumen-verdrängerpumpe

Publications (2)

Publication Number Publication Date
EP1514027A2 EP1514027A2 (de) 2005-03-16
EP1514027B1 true EP1514027B1 (de) 2011-12-07

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EP02405509A Withdrawn EP1375921A1 (de) 2002-06-19 2002-06-19 Hochdruck-Kleinvolumen-Verdrängerpumpe
EP03727124A Expired - Lifetime EP1514027B1 (de) 2002-06-19 2003-06-18 Hochdruck-kleinvolumen-verdrängerpumpe

Family Applications Before (1)

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EP02405509A Withdrawn EP1375921A1 (de) 2002-06-19 2002-06-19 Hochdruck-Kleinvolumen-Verdrängerpumpe

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EP (2) EP1375921A1 (de)
CN (1) CN100406734C (de)
AT (1) ATE536477T1 (de)
AU (1) AU2003233907A1 (de)
CA (1) CA2485552C (de)
DE (1) DE60326841D1 (de)
EA (1) EA009029B1 (de)
WO (1) WO2004001228A2 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102011056094A1 (de) 2011-12-06 2013-06-06 Dionex Softron Gmbh Schaltventil, insbesondere für das Schalten eines unter hohem Druck stehenden Fluids

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2733664A (en) * 1956-02-07 saalfrank
US2346964A (en) * 1940-08-26 1944-04-18 Omega Machine Company Positive displacement pump
US2841092A (en) * 1955-08-09 1958-07-01 Milton Roy Co High-pressure pump
US3981620A (en) * 1972-03-06 1976-09-21 Waters Associates, Inc. Pumping apparatus
US4045343A (en) * 1975-11-10 1977-08-30 Varian Associates, Inc. High pressure liquid chromatography system
US4592558A (en) * 1984-10-17 1986-06-03 Hydril Company Spring ring and hat ring seal
US4706970A (en) * 1984-11-14 1987-11-17 Polydyne Industries, Inc. Flexible ring seal with insert in circumferentially extending channel
DE4308467A1 (de) 1992-10-28 1994-05-05 Herbert Dr Funke Hochdruckpumpe zur Flüssigkeits-Feindosierung
CH688919A5 (de) * 1994-04-13 1998-05-29 Cryomec Ag Triebwerk einer Kolbenpumpe für cryogene Anwendungen.
US5799953A (en) * 1995-05-25 1998-09-01 American Variseal Capped spring-energized seal
GB9717564D0 (en) * 1997-08-20 1997-10-22 Hydrair Ltd Pump for shear sensitive material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102011056094A1 (de) 2011-12-06 2013-06-06 Dionex Softron Gmbh Schaltventil, insbesondere für das Schalten eines unter hohem Druck stehenden Fluids
EP2602518A1 (de) 2011-12-06 2013-06-12 Dionex Softron GmbH Schaltventil, insbesondere für das Schalten eines unter hohem Druck stehenden Fluids
DE102011056094B4 (de) * 2011-12-06 2014-05-28 Dionex Softron Gmbh Schaltventil, insbesondere für das Schalten eines unter hohem Druck stehenden Fluids
US9133944B2 (en) 2011-12-06 2015-09-15 Dionex Softron Gmbh Switching valve to control a fluid subject to high pressure

Also Published As

Publication number Publication date
DE60326841D1 (de) 2009-05-07
EP1375921A1 (de) 2004-01-02
EA200401530A1 (ru) 2006-10-27
ATE536477T1 (de) 2011-12-15
CN1662745A (zh) 2005-08-31
WO2004001228A3 (en) 2004-03-04
EP1514027A2 (de) 2005-03-16
EA009029B1 (ru) 2007-10-26
AU2003233907A1 (en) 2004-01-06
CA2485552C (en) 2011-08-23
AU2003233907A8 (en) 2004-01-06
WO2004001228A2 (en) 2003-12-31
CN100406734C (zh) 2008-07-30
CA2485552A1 (en) 2003-12-31

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