EP0584277A4 - Centrifuge tube adapter. - Google Patents

Centrifuge tube adapter.

Info

Publication number
EP0584277A4
EP0584277A4 EP19920913835 EP92913835A EP0584277A4 EP 0584277 A4 EP0584277 A4 EP 0584277A4 EP 19920913835 EP19920913835 EP 19920913835 EP 92913835 A EP92913835 A EP 92913835A EP 0584277 A4 EP0584277 A4 EP 0584277A4
Authority
EP
European Patent Office
Prior art keywords
adapter
segment
segments
rotor
inboard
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.)
Granted
Application number
EP19920913835
Other languages
German (de)
French (fr)
Other versions
EP0584277B1 (en
EP0584277A1 (en
Inventor
William Andrew Romanuaskas
Thomas Edward Sheeran Jr
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sorvall Products LP
Original Assignee
EI Du Pont de Nemours and Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by EI Du Pont de Nemours and Co filed Critical EI Du Pont de Nemours and Co
Publication of EP0584277A1 publication Critical patent/EP0584277A1/en
Publication of EP0584277A4 publication Critical patent/EP0584277A4/en
Application granted granted Critical
Publication of EP0584277B1 publication Critical patent/EP0584277B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B04CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04BCENTRIFUGES
    • B04B5/00Other centrifuges
    • B04B5/04Radial chamber apparatus for separating predominantly liquid mixtures, e.g. butyrometers
    • B04B5/0407Radial chamber apparatus for separating predominantly liquid mixtures, e.g. butyrometers for liquids contained in receptacles
    • B04B5/0414Radial chamber apparatus for separating predominantly liquid mixtures, e.g. butyrometers for liquids contained in receptacles comprising test tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B04CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04BCENTRIFUGES
    • B04B5/00Other centrifuges
    • B04B5/04Radial chamber apparatus for separating predominantly liquid mixtures, e.g. butyrometers
    • B04B5/0407Radial chamber apparatus for separating predominantly liquid mixtures, e.g. butyrometers for liquids contained in receptacles
    • B04B2005/0435Radial chamber apparatus for separating predominantly liquid mixtures, e.g. butyrometers for liquids contained in receptacles with adapters for centrifuge tubes or bags

Definitions

  • the present invention relates to an adapter for holding a centrifuge tube in a centrifuge rotor cavity, and in particular, to an adapter having two segments, the segments being in some cases joined by a hinge, the hinge axis extending perpendicular to the axis of the adapter.
  • a device known as a tube adapter When the shape and size of a centrifuge tube does not closely conform to the shape and size of the rotor cavity in which it is to be disposed a device known as a tube adapter is usually employed.
  • the tube adapter has an interior cavity having a shape and size which closely conforms to the shape and size of the centrifuge tube being adapted.
  • the exterior shape and size of the adapter closely conforms to the shape and size of the rotor cavity in which the tube is to be used.
  • the adapter serves to support a tube within the cavity in which it is received and thus serves to prevent deformation of the tube during centrifugation.
  • an adapter formed of a single unitary member is the device disclosed in United States Patent 4,304,356 (Chulay et al.). This adapter supports only the neck region of the centrifuge tube and is fabricated of a material having a lower density than the liquid being carried therein to prevent bottoming of the adapter in the rotor cavity in the event of tube rupture.
  • an adapter formed of two piece construction is the device shown in United States Patent 3,674,197 (Mitchell et al.), assigned to the assignee hereof.
  • This adapter comprises two discrete segments, each of which has an indentation therein. When joined the indentations form a recess for receiving a collapsible bag during centrifugation.
  • the adapter disclosed in this patent includes aperture(s) through which tubes from the bag exit the adapter. Thus, the possibility exists that the bag may extrude through these 3 apertures if the adapter were to undergo centrifugation in a vertical angle rotor.
  • An adapter arrangement formed of two discrete adapter 5 segments and useful to support the capped end of a centrifuge tube is available as part of the Nalgene Ultra-Lok Tube System sold by Fisher Scientific Incorporated.
  • United States Patent 4,692,137 discloses a 0 tube adapter having two segments which are hinged along the lateral edges of the segments.
  • the hinge axes align in parallel relationship to the axis of the cavity in which the adapter is received.
  • the disposition of hinges along the lateral edges of the segments is believed disadvantageous in that such a 5 disposition may interfere with the insertion or removal of the adapter into or from the rotor cavity.
  • the present invention relates to an adapter having an axis therethrough for supporting a centrifuge tube within a cavity in a centrifuge rotor.
  • the cavity itself has an axis therethrough.
  • the axis of the adapter may, in use, align in parallel relationship with the axis of the cavity.
  • the adapter comprises a first and a second adapter segment, each segment having an exterior surface and a mating surface thereon. Each segment has an indentation in the mating surface thereof.
  • the segments may be connected by at least one hinge that supports the segments for relative pivotal movement about a hinge axis from an open to a mated position.
  • the hinge axis extends perpendicular to the axis of the adapter.
  • the indentation in each segment is shaped such that when the segments are in the mated position the recess is sized to closely correspond to the configuration of at least the neck of the tube.
  • at least one of the segments has a feature on the mating surface thereof that projects into the indentation therein.
  • the indentation in each segment is shaped such that when the segments are in the mated position the recess so defined is sized to closely correspond to the size and configuration of the centrifuge tube over its entire length.
  • the present invention relates to an adapter for supporting a closed centrifuge tube having a predetermined size and configuration within a cavity in a vertical angle centrifuge rotor.
  • the rotor is rotatable to a predetermined maximum speed.
  • the adapter has a central axis extending therethrough that, in use, aligns in parallel relationship both with the axis of the rotor cavity in which the adapter is disposed and with the axis of rotation of the vertical angle rotor.
  • the adapter comprises a first and a second adapter segment, each of which has an exterior surface and a mating surface thereon. Each segment has an indentation in the mating surface thereof.
  • the indentations are shaped such that when the segments are joined along their mating surfaces the indentations cooperate to define a recess able to totally surround a centrifuge tube disposed therein.
  • Each adapter segment is fabricated of a material that has sufficient strength to withstand the vertical forces created by the pressure of a liquid under centrifugation.
  • each adapter segment defines a predetermined angle with respect to a plane that is normal to a plane containing the line of action along which the adapter segments are joined. Inclination of the mating surfaces of the adapter segments allows the same to displace relative to each other to totally fill the rotor cavity in which they are disposed without any separation being defined between the segments. Inclined mating surfaces may be provided on any of the adapter segments disclosed in the present application.
  • the present invention relates to an adapter for supporting a closed centrifuge tube in which at least one of the. adapter segments has an effective weight sufficient to balance forces created by the pressure of a liquid carried in the tube under centrifugation that act transversely to the central axis.
  • the one segment is disposed closer to the axis of rotation so that the mating surfaces of the adapter segments lie in a plane that is perpendicular to a radius of the rotor extending through the cavity.
  • the weight of the one segment while under centrifugation is sufficient to maintain the mating surfaces of the adapter segments in contacting relationship with each other.
  • Suitable keying may be provided to identify the one segment having the predetermined effective weight.
  • Figure 1 is a perspective view of an adapter according to a first embodiment of the present invention for supporting the neck region of a centrifuge tube of the type in which a portion of the tube neck has a constricted region thereon when capped, the adapter being shown in the open position;
  • Figure 2 is a fragmentary elevation view, in section, of the tube adapter of Figure 1 in use and supporting the neck portion of a centrifuge tube in a fixed angle rotor cavity;
  • Figure 3 a perspective view of an adapter according to a second embodiment of the present invention for supporting the full length of a centrifuge tube within a rotor cavity, the adapter being shown in the open position;
  • Figure 4 is a fragmentary elevation view, in section, of the tube adapter of Figure 3 in use and supporting a centrifuge tube over its entire axial length in a fixed angle rotor cavity;
  • Figure 5 is a perspective view similar to Figure 3 of a modification of the embodiment of the tube adapter there shown for use with an open top tube;
  • Figure 6 is a fragmentary elevation view, in section, of the centrifuge tube adapter of Figure 5 in use and supporting a centrifuge tube over its entire axial length in a fixed angle rotor cavity;
  • Figure 7A is a perspective view of an adapter in accordance with another aspect of the present invention used to support a closed tube within the cavity of a vertical angle rotor, the adapter segments being independent of each other, while Figure 7B is a modification of the embodiment of adapter shown in Figure 7A in which the adapter segments are hinged;
  • Figure 8 is a fragmentary elevational view of an adapter shown in either Figure 7A or 7B in use and supporting a centrifuge tube over its entire axial length in a vertical angle centrifuge rotor cavity, with a portion of the tube being broken away;
  • Figures 9A and 9B are sectional views taken along section lines 9A-9A, 9B-9B in Figure 8 showing the inclination of the mating surfaces of the adapter segments, the view of Figure 9A illustrating the relationship of the adapter segments with respect to each other, with respect to the tube received in the adapter, and with respect to the rotor cavity in which the adapter is placed while rotor is at rest while the view of Figure 9B shows the relationship of the adapter segments with respect to each other, with respect to the tube received in the adapter, and with respect to the rotor cavity in which the adapter is placed when the rotor is rotating;
  • Figure 10 is a perspective view of an adapter in accordance with yet another aspect of the present invention used to support a closed tube within the cavity of a vertical angle rotor;
  • Figure HA is a side sectional view of an adapter of Figure 10 in use and supporting a centrifuge tube over its entire axial length in a vertical angle centrifuge rotor cavity
  • Figures 11B and 11C are, respectively, sectional views of the adapter as shown in Figure 11A taken along section lines 11B-11B and 11C-11C;
  • Figure 12A is a perspective view of a modification of the embodiment of the adapter shown in Figures 10 and 11 with the inboard adapter segment having a keying configuration thereon, while Figure 12B is a side sectional view of the adapter of Figure 12A with the adapter segments joined together;
  • Figure 13 is a perspective view of another modification of the embodiment of the adapter shown in Figures 10 and 11;
  • Figure 14 is an enlarged view of a portion of the perspective view of Figure 13 illustrating a hinge arrangement useful with the modified adaptor shown therein;
  • Figure 15 is an enlarged view of the inboard segment of the modified adaptor shown in Figure 13 taken along view lines 15-15 therein;
  • Figure 16 is a side sectional view of an adapter of Figure 10 in use and supporting a centrifuge tube over its entire axial length in a vertical angle centrifuge rotor cavity.
  • FIG. 1 is an exploded perspective view of an adapter, generally indicated by the reference character 10, according to a first embodiment of the present invention.
  • the adapter 10 in accordance with this embodiment is useful for supporting a centrifuge tube T of the type having a body portion B with a closed end C, the body B tapering through a transition region R to a narrowed neck region N.
  • the neck N serves as the liquid port through which a liquid under test may be loaded into the tube T.
  • the tube T is capped at least one portion D of the neck N becomes radially inwardly constricted, thereby forming a constricted region in the neck of the tube.
  • the capping assembly disclosed in United States Patent 4,552,278 (Romanauskas) is used to cap the tube, so that the neck N of the tube has a corrugated configuration imparted thereto.
  • the corrugated configuration has at least one and optionally a plurality of circumferentially extending corrugations formed in the neck N. It should be understood that any other capping arrangement may be used, so long as any form of constricted region is imparted to the configuration of the neck N.
  • the adapter 10 is comprised of a first adapter segment 12 and an identical second adapter segment 14.
  • Each segment 12, 14 has an exterior surface 16 and a planar mating surface 18 thereon.
  • the exterior surface 16 of each segment is defined by a generally cylindrical lateral surface portion 20 and a planar upper surface portion 22.
  • an enlarged collar 24 is disposed intermediate the lateral surface portion 20 and the upper surface portion 22.
  • the configuration and size of the adjacent lateral surface portions 20 closely corresponds to the configuration and diameter of a rotor cavity 40 in which the adapter 10 is used.
  • the upper surface portions 22 of the conjoined segments are accessible when the adapter 10 is received in the rotor cavity 40.
  • the segments 12 and 14 are connected and supported for relative pivotal movement with respect to each other by at least one hinge 26.
  • the hinge 26 may take the form of a live hinge bridging the upper surface portions 22 of the segments 12, 14, or may, if desired, take the form of a coined hinge.
  • live hinge refers to a hinge type, typically made of a polypropylene material, which must be flexed or bent before the plastic is cooled or permanently set. Such hinges are complete without secondary operations.
  • coined hinge refers to a hinge that is cold-formed, usually by a stamping operation. The stamping operation creates a narrower and a thinner flexing region which defines a hinge.
  • the axis 26A of the hinge 26 that is, the axis about which occurs the relative pivotal motion of the segments, extends perpendicular to the axis 10A of the adapter 10. This relationship of the hinge axis 26 A to the axis 10A of the adapter 10 is best illustrated in Figure 2.
  • each of the adapter segments 12, 14 has an indentation 28 therein.
  • the indentation 28 in each segment 12, 14 corresponds to the size and contour of at least a portion of the tube T.
  • the indentations 28 therein cooperate to define a recess 30 ( Figure 2) that corresponds to the size and shape of at least a predetermined portion of the tube T that is received therein.
  • At least one but preferably both indentations 28 contains a feature 34, in the form of a circumferentially extending ridge, that corresponds in size and is located complementarity to the position of the constriction D in the neck N of the tube.
  • the adapter 10 shown in Figures 1 and 2 is especially useful when the diameter of body B of the tube T is equal to the diameter of a cavity 40 in a centrifuge rotor 42, but the overall length L of the tube T is less than the axial length of the cavity.
  • the rotor cavity 40 has an axis 40A therethrough that aligns in parallel relationship with the axis 10A of the adapter 10 when the same is disposed therein.
  • the adapter 10 defined by the mated segments 12, 14 serves to support the neck N and the transition region R of the tube T within the cavity 40.
  • the tube T is inserted into one of the segments 12, 14, so that the feature 34 on the segment(s) is received within the constricted region D in the neck N of the tube T when the segments are in the mated position.
  • the segments 12, 14 are then pivoted about the hinge axis 26A to place the mating surfaces 18 thereon in abutting contact. This closes the adapter 10 around the tube T and thus permits the tube T to be manipulated by manipulation of the adapter 10.
  • the tube T and the adapter 10 are then axially inserted into the cavity 40. In the preferred instance the tube T bottoms against the closed end of the cavity 40.
  • the axial length of the adapter 10 is selected such that when the tube T is received in the cavity 40, the upper surface portions 22 on the segments 12, 14 are accessible to a user.
  • the hinge 26 may be formed so as to define a useful lifting appliance, as shown in Figure 2.
  • a user grasps the hinge 26 and lifts the tube from the cavity 40.
  • the feature 34 in such an instance defines a lifting surface which acts against the material of the tube in the constricted region D in the neck N thereof, and thus serves to transmit the lifting force to the tube T to withdraw the same from the cavity.
  • the tube T may be withdrawn without unduly agitating the separation within the tube T.
  • the rotor 42 may have a shoulder 44 defined about the mouth of the cavity 40.
  • the shoulder 44 is preferably located on the rotor 42 at a position that is axially beneath the collars 24 on the segments 12, 14 when the adapter is received within the cavity, thereby to guard against the possibility that tube rupture will permit the adapter 10 to enter into the cavity 40.
  • the segments 12, 14 with the hinge 26 therebetween are preferably integrally formed from a suitable material, such as polypropylene.
  • a suitable material such as polypropylene.
  • the segments 12, 14 may be otherwise fabricated from one or more pieces, using other manufacturing techniques and other materials, and assembled to define the adapter 10. Similar techniques may be used to form any other embodiment of the adapter illustrated and discussed herein.
  • the adapter 10' shown in Figures 3 and 4 finds utility.
  • the recess 30' ( Figure 4) formed by the cooperative association of the indentations 28' in the mated adapter segments 12', 14' is configured to correspond to the size and shape of the tube T over the entire axial length L' thereof.
  • the segments 12', 14' are each provided with an axial extension 36 having a bottom wall 38.
  • the bottom wall 38 need not completely close the bottom of the adapter 12', 14', as is illustrated, but may only partly close the same.
  • the presence of the extension 36 and the bottom wall 38 permit the recess 30' defined when the segments 12', 14' are joined to receive the entire axial length L' of the tube T.
  • Figure 4 illustrates this embodiment of the invention in use.
  • the closed end C of the tube T is contacted by the interior surface of the bottom wall 38.
  • the indentations 28' in the segments 12', 14 * are placed such that the tube T lies as close to the bottom of the rotor cavity 40, thereby to maximize the centrifugal force imposed on the liquid sample.
  • the feature 34 present in the embodiment of Figure 1 is not required, since the requisite lifting force transmission surface is defined by the bottom wall 38 operating against the bottom end C of the tube T.
  • the collar 24 may be eliminated.
  • Figure 5 illustrates an adapter 10" that defines a modification of the embodiment of the invention shown in Figure 3.
  • the tube T" has the form of a test tube, with no constriction present to define a neck.
  • the segments 12", 14" are modified to exhibit indentations 28" similar to those shown in Figure 3, but which correspond in size and shape to the test tube T" over the entire axial length L" thereof.
  • the hinge between the segments is disposed on the upper surface portion of the exterior surface of the adapter segments. Such a disposition is believed advantageous in that it locates the hinge at a position where the hinge does not interfere with the receipt of the adapter within the rotor cavity. At the same time the hinge defines a useful lifting appliance.
  • the adapter previously illustrated and discussed may find utility in the environment of a vertical angle rotor, such a utilization may typically require the provision of a suitable capping arrangement to prevent tube failure.
  • the capping arrangement is required in the case that the adapter does not completely surround the tube, such as shown in Figures 1 and 2.
  • a capping arrangement is also required if the adapter does completely surround the tube, as shown in Figures 3 through 6, but does not have sufficient strength to withstand the vertical force due to liquid pressure under centrifugation.
  • FIGS. 7A and 7B illustrate such an adapter in accordance with another aspect of the present invention.
  • Figure 7A illustrates an unhinged embodiment of the vertical angle rotor adapter, while Figure 7B shows a hinged embodiment thereof.
  • the vertical angle rotor adapter shown in Figures 7A and 7B is generally indicated by the reference character 10 3 and is generally similar to the adapters 10' and 10" discussed in connection with Figures 3 and 5 in the sense that the adapter 10 3 is arranged to totally surround the tube T disposed there within.
  • the adapter 10 3 comprises a first adapter segment 12 3 and a second adapter segment 14 3 .
  • Each segment 12 3 , 14 3 has an exterior surface 16 3 thereon.
  • the exterior surface 16 3 of each segment 12 3 , 14 3 is defined by a. generally cylindrical lateral surface portion 20 3 and a planar upper surface portion 223.
  • the adapter segment 12 3 has a planar mating surface 18 3 thereon while the adapter segment 14 3 has a planar mating surface 19 3 thereon.
  • the mating surfaces 18 3 and 19 3 on the segments 12 3 and 14 3 are angled with respect to a predetermined reference plane, to be defined.
  • the inclination of the mating surfaces 18 3 and 19 3 on the segments 12 3 and 14 3 , respectively, is believed best seen in Figures 9A and 9B. It should be understood that the mating surfaces of the adapter segments in any of the embodiments shown in Figures 1 through 6 may also be inclined in the manner shown in Figures 9A and 9B.
  • each of the adapter segments 12 3 and 14 3 each have an indentation 28 3 therein.
  • the indentation 28 3 in each segment 12 3 and 14 3 corresponds to the size and shape of the entire axial length L of the tube T.
  • the indentations 28 3 therein cooperate to define a recess 30 3 ( Figure 8) that corresponds to the size and shape of the entire axial length of the tube T ( Figures 1 and 8) that is received therein.
  • the indentations 28 3 in each segment are shaped such that when the segments 12 3 and 14 3 are joined along their respective mating surfaces 18 3 and 19 3 the indentations 28 3 in each segment cooperate to define a recess 30 3 able to totally surround a centrifuge tube T disposed therein.
  • Figure 8 illustrates the adapter 10 3 in accordance with this aspect of the present invention in use in the environment of a vertical angle centrifuge rotor 42 v .
  • the axis of each cavity 40 v is parallel or approaching parallel (with an inclination angle of not more than fifteen (15) degrees) to the axis of rotation A of the rotor.
  • the adapter 10 3 has a central axis 10 3 A that, in use, aligns with the axis of the cavity 40 v in which it is disposed and with the axis of rotation A of the vertical angle rotor 42 v .
  • the segments 12 3 , 14 3 are independent of each other. These segments 12 3 , 14 3 may be joined by moving each segment toward the other along a line of action 48 thereby to bring the mating surfaces 12 3 , 14 3 thereof in abutting contact.
  • line of action is meant to denote that direction of motion which joins the segments 12 3 , 14 3 such that, in a given predetermined plane perpendicular to the central axis 10 ⁇ simultaneous contact of both sides of the segments 12 3 , 14 3 occurs.
  • the segments 12 3 , 14 3 are connected and supported for relative pivotal movement with respect to each other by at least one hinge 26 3 .
  • the pivotal axis 26 3 A ( Figure 8) of the hinge 26 3 that is, the axis about which occurs the relative pivotal motion of the segments 12 3 , 14 3 , extends perpendicular to the axis 10 3 A of the adapter 10 3 .
  • the hinge 26 3 may take the form of a live hinge bridging the upper surface portions 22 3 of the segments 12 3 , 14 3 , or may, if desired, take the form of a coined hinge.
  • the segments 12 3 , 14 3 may also be joined by moving each segment toward the other along the line of action 48.
  • the line of action 48 also lies in the plane perpendicular to the pivotal axis 26 3 A of the hinge 26 3 .
  • the inclination of the surfaces 18 3 , 19 3 may be most clearly seen. (Sectioning of the adapter has been omitted from Figures 9A and 9B for clarity of illustration).
  • the segments 12 3 , 14 3 may expand during centrifugation to fill the entirety of the rotor cavity 40 v .
  • any variations in the size of the various cavities 40 v in a given rotor, variations in cavity size from rotor to rotor, and variations in the thickness of the segments from adapter to adapter may be accommodated without breaking the total containment of the tube T by the adapter.
  • the radial distance Ri measured between the central axis 10 3 A and the interior surface of the adapter segment 14 3 in the region of the indentation 28 3 therein is less than the radial distance R2 measured between the central axis 10 3 A and the interior surface of the adapter segment 12 3 in the region of the indentation 28 3 therein.
  • the radial distance R3 as the distance between the central axis 10 3 and the exterior surface of the adapter segment 14 3 in the region of the indentation 28 3 therein and the radial distance R2 as the distance between the central axis 10 3 and the exterior surface of the adapter segment 12 3 in the region of the indentation 28 3 therein.
  • the thickness of the segment 12 3 is equal to the difference between the distances R4 and R2, while thickness of the segment 14 3 is equal to the difference between the distances R3 and Ri.
  • the arc length of the inner surface of the segment 14 3 i.e., the distance between the points 50-50 in a plane perpendicular to the adapter axis 10 3 A (the plane of Figure 9A) plus the arc length of the inner surface of the segment 12 3 (i.e., the distance between the points 52-52) in the same plane must equal the circumference of the inside of the adapter in a plane perpendicular to the adapter axis 10 3 A in the case when the adapter of the smallest segment thickness is conformed to the largest rotor cavity, as illustrated in Figure 9B.
  • the magnitude of angles of inclination of the surfaces may be measured by reference to a reference plane 54.
  • the reference plane 54 is that plane that contains both the vertical central axis 10 3 of the adapter 10 3 and at least one of the inwardly projecting corners 50 of the adapter segment 14 3 .
  • the reference plane 54 may be defined as the plane that is normal to the line of action 48 (superimposed on Figure 9A) along which the segments 12 3 , 14 3 are joined together.
  • the inclination of the surfaces 18 3 and 19 3 lies in the range of angles from about 10 to about 80 degrees.
  • each angle is forty five (45) degrees.
  • the surfaces 18 3 and 19 3 are shown as being inclined to the same degree (i.e., the angles of the surfaces 18 3 and 19 3 with respect to the reference plane 54 are equal), such is not necessarily required. It is only necessary that the inclination of the surfaces 18 3 and 19 3 be such that the segments are maintained in mutual contact if they expand during centrifugation to fill the cavity 40 v . It should also be noted that the segments 12 3 and 14 3 may be other than circular, and can be ellipsoidal, if desired.
  • An adapter in accordance with this embodiment of the present invention may be fabricated from any suitable material so long as the resulting adapter has sufficient strength (as that term is defined herein).
  • the material of choice must exhibit other desirable properties, such as appropriate ultimate strength, appropriate modulus of elasticity, suitable chemical compatibility with any liquid sample being centrifuged and ability to withstand autoclaving.
  • Suitable plastic materials include polypropylene, polyamide, acetal, polyphenylene oxide, polyvinyl choloride, polycarbonate or polyethylene.
  • Other plastic or metallic materials either homogeneous (neat) or fiber reinforced) with similar or better mechanical and chemical properties for the application under consideration may also be used.
  • the adapter may be formed in any convenient manner consistent with the material selected, such as molding, machining, casting or forging.
  • the adapter 10 3 hi order to support a tube T in a vertical angle rotor without the assistance of the restraining force provided by a capping mechanism, the adapter 10 3 must exhibit sufficient strength to absorb the forces imposed on the tube T by the pressure of the liquid therein.
  • "sufficient strength" means that the adapter must be able to withstand the forces imposed on it during centrifugation without failing or deforming to the extent that the tube carried therein ruptures.
  • Whether a given adapter is of sufficient strength, and thus falls within the scope of the claims of the present invention, can be determined from various readily ascertainable operating parameters of the vertical angle rotor in which the adapter is to be used and the application to which the adapter is to be put. These parameters are the specific weight of the liquid sample within the tube received by adapter, the radius Ri which represents the minimum distance to the sample from the axis A of rotation ( Figure 8), the diameter D 0 ( Figure 8) of the rotor cavity, the thickness of the adapter segment, the inside diameter of the tube, and the speed of rotation of the vertical angle rotor.
  • P is the pressure (psi)
  • is the rotational velocity of the rotor (radians per second)
  • g is acceleration due to gravity (inches per second 2 )
  • is the specific weight of the sample (Lb per inch 3 )
  • R 0 is the distance to the point of interest x where the pressure value is desired from the center of rotation (inches)
  • Rj is the minimum distance to the sample from the axis A of rotation (inches).
  • the total vertical force Fv that the adapter must withstand is then found by integrating this pressure function over the circular cross sectional area of the inside of the tube.
  • the average stress in the wall of the adapter can be determined in accordance with the relationship: Fv
  • D 0 is the diameter of the rotor cavity
  • Dj is the inside diameter of the adapter when operating at speed, which equals the diameter of the rotor cavity minus the thickness of each of the segments of the adapter ( Figure 9B).
  • the modulus of elasticity of that material may be readily obtained.
  • An estimation of the vertical deformation of the adapter may be found by multiplying the initial length of the adapter by the average stress divided by the modulus of elasticity of the adapter material. If the average stress calculated in Equation (2) is less than the ultimate strength of the adapter material, and the predicted deformation is less than the deformation that will cause first leakage in the tube carried within the adapter, then the given adapter is to be construed to have sufficient strength for at least one operating cycle, and therefore falls within the contemplation of the present invention. The determination of sufficient strength as set forth above under operating conditions will verify both the analysis and the conclusion of the sufficiency of strength of the adapter.
  • the adapter heretofore described in connection with Figures 7A through 9B for use primarily in a vertical angle rotor is fabricated of a material and in a manner such that the adapter, while under centrifugation, has sufficient strength to withstand the vertical forces Fv (that is, forces that act parallel to the central axis of the adapter). Vertical stresses in the tube T are therefore minimized.
  • Angled mating edges on the adapter segments are provided to prevent a separation from forming between the segments in response to the radial expansion of the tube under pressure. The prevention of such a separation insures that the tube is supported about the entirety of its circumference such that the possibility of tube failure is minimized.
  • the adapter may be designed and fabricated such that, under centrifugation, the body force of one adapter segment is sufficient to balance the force created by the pressure of a liquid carried in the tube under centrifugation that acts transversely to the central axis.
  • the preferred form of such an adapter when in use must be disposed within a cavity of a rotor in an orientation such that the mating surfaces of the adapter segments lie in a plane that is substantially perpendicular to a radius of the rotor extending through the cavity.
  • FIG 10 illustrates a preferred arrangement of a split adapter 10 4 for use in a vertical angle rotor in accordance with this embodiment of the present invention.
  • the structure of the adapter 10 4 is generally similar to the adapter 10' shown and discussed in connection with Figures 3A and 3B and to the adapter 10 3 shown and discussed in connection with Figures 7A and 7B in the sense that the adapter 10 4 , like the adapters 10' and 10 3 , is arranged to totally surround a tube T disposed there within.
  • the adapter 10 4 includes a first adapter segment 12 4 and a second adapter segment 14 4 .
  • Each segment 12 4 , 14 4 has an exterior surface 16 4 and a mating surface 18 4 thereon.
  • the exterior surface 16 4 of each segment 12 4 , 14 4 is defined by a generally cylindrical lateral surface portion 20 4 and a planar upper surface portion 22 4 .
  • the exterior surface 16 4 of each segment 12 4 , 14 4 is sized and shaped for close fitting receipt within the cavity 40 v of a vertical angle rotor 42 v ( Figures 11A through 11C).
  • Each segment 12 4 , 14 4 is provided with an indentation 28 4 in the mating surface 18 4 thereof.
  • the indentation 28 4 in each segment 12 4 , 14 4 is shaped so that when the segments 12 4 and 14 4 arc joined along their mating surfaces 18 4 the indentations 28 4 cooperate to define a recess 30 4 able to totally surround a centrifuge tube T disposed therein.
  • the adapter 10 4 has a central axis lO- ⁇ A extending therethrough ( Figure 11 A). As will be discussed later, the recess 30 4 may be inclined with respect to the central axis lCHA and remain within the contemplation of this invention.
  • an adapter 10 4 in accordance with this embodiment of the present invention may be provided with a hinge on the upper surface 22 4 of the segments, similar to the embodiment shown in Figure 7B. If a hinge is provided, the pivotal axis of the hinge extends perpendicular to the axis of the adapter. As discussed earlier, the hinge may take the form of a live hinge or a coined hinge.
  • At least one of the segments of the adapter 10 4 must have a predetermined effective weight under centrifugation that is sufficient to prevent separation of the adapter segments.
  • the effective weight of the adapter segment is defined as the weight of the segment at sea level multiplied by the g (gravity) force imposed on the segment when the same is rotated at a predetermined operating speed with the center of mass of the segment lying a predetermined radial distance from an axis of rotation.
  • the 14 4 has at least one, but preferably, a pair of resilient extensions 58 4 , 60 4 , respectively, thereon.
  • the resilient extensions 58 4 , 60 4 are flexibly mounted, as by hinging, to the outside surface 16 4 of the segment along a line of bending 62 4 .
  • the resilient extensions 58 4 , 60 4 are biased to flare outwardly from the adapter segment, and are bendable along the line of bending 62 4 to close inwardly toward the lateral surface portion 20 4 of the outside surface 16 4 of the segment to which they are attached. In the closed position the resilient extensions 58 4 , 60 4 are in contact with the lateral surface portion 20 4 of the outside surface 16 4 of the segment to which they are attached.
  • each extension is tapered, as at 64 4 . It should be noted that when the adapter segments 12 4 , 14 4 are mated the edges of resilient extensions 58 4 , 60 4 are circumferentially spaced a slight distance apart, thereby to provide sufficient clearance to accommodate the flexing motion of the resilient extensions 58 4 , 60 4 during insertion into the rotor cavity.
  • each extension 58 4 , 60 4 serves to frictionally interact with the boundaries of a rotor cavity 42 v ( Figure 11 A through 11C) to prevent rotation of the adapter 10 4 about its axis lO- ⁇ A with respect to the body of the rotor 40 v thereby to maintain the adapter 10 4 in a predetermined angular orientation within the cavity during operation of the rotor.
  • FIGS 11A through 11C illustrate the adapter 10 4 of Figure 10 in use in a cavity 40 v of a vertical angle centrifuge rotor 42 v . Sectioning of the adapter has been omitted from Figure 11C for clarity of illustration.
  • the segment for example, the segment 12 4
  • the other segment 14 4 which lies farther from the axis of rotation 10A is termed the "outboard" segment.
  • the inboard segment 12 4 must have an effective weight sufficient to balance the force FT created by the pressure of a liquid carried in the tube under centrifugation that acts transversely to the central axis lCHA of the adapter 10 4 . Such an arrangement precludes separation of the adapter segments 12 4 , 14 4 during centrifugation.
  • the mating surfaces 18 4 of the adapter segments 12 4 , 14 4 are disposed so as to lie in a plane 68 ( Figure HA) that is substantially perpendicular to a radius of the rotor 42 v extending through the cavity 40 v .
  • the plane 68 is the plane of Figure 11B.
  • the recess 30 4 may be arranged within the adapter 10 4 such that an axis extending centrally through the recess 30 4 of the adapter 10 4 is offset radially with respect to the axis KHA of the adapter 10 4 .
  • the recess 30 4 is not concentric with the generally cylindrical lateral surface portion 20 4 of the adapter 10 4 . If so offset it its preferred that the recess 30 4 be displaced radially outwardly with respect to the axis 10 of the adapter 10 4 .
  • Such an arrangement may be utilized to increase the effective weight of the inboard segment 12 4 and/or to dispose the sample to higher g-forces resulting from the increased radial distance to the sample.
  • the inboard adapter segment 12 4 has an effective weight sufficient for the purpose of containing the transverse force FT, and thus fall within the scope of the claims of the present invention, can be determined from consideration of the identical operating parameters as previously developed and described in connection with the "sufficient strength" determination for accommodation of the vertical force Fv.
  • the pressure P across the diameter of the tube is defined by Equation (1).
  • the value of the pressure P ranges from zero at the inboard edge of the tube to a maximum value at the farthest radial location of the liquid sample from the axis of rotation of the rotor.
  • the inboard segment 12 4 of the adapter 10 4 is subjected to a radially inwardly directed force FT that results from liquid pressure in the inboard half of the tube.
  • the magnitude of this radially inwardly directed force FT is determined by integrating the component of the pressure function defined by Equation (1) that is parallel to a radial line through the center of mass of the inboard segment 12 4 over the surface area of the indentation 28 4 of the adapter segment 12 4 .
  • An adapter 10 4 having segments 12 4 , 14 4 in accordance with this embodiment of the invention may be fabricated from any suitable material so long as the resulting adapter segment 12 4 has sufficient effective weight (as that term is defined herein) and exhibits suitable chemical compatibility with any liquid sample being centrifuged. It should preferably have the ability to withstand sterilization, as by autoclaving.
  • Suitable plastic materials include polypropylene, polyamide, acetal, polyphenylene oxide, polyvinyl choloride, polycarbonate or polyethylene.
  • Other plastic or metallic materials either homogeneous (neat) or fiber reinforced
  • the adapter may be formed in any convenient manner consistent with the material selected, such as molding, machining, casting or forging.
  • both the segments 12 4 , 14 4 may be substantially identical in weight or they may be substantially different in weight, so long as the inboard adapter segment has the requisite effective weight to completely contain the tube T during operation of the rotor.
  • the adapter 10 4 also be fabricated of a material that has sufficient strength to withstand the vertical force Fv due to liquid pressure under centrifugation, as discussed in connection with Figures 7 A through 9B.
  • the adapter 10 4 is not able to withstand the vertical force Fv, then a separate capping arrangement on the rotor is required.
  • the inboard segment 12 4 By providing the inboard segment 12 4 having a -suitable effective weight the mating surfaces on the inboard and outboard segments remain in contact during operation of the rotor and no gap therebetween may form.
  • the tube T is thus completely contained within the conjoined adapter segments during operation of the rotor, and the possibility of tube failure due to extrusion into a gap is precluded.
  • the present embodiment carries the additional benefit of minimizing circumferential stress in the tube caused by the pressure of the liquid, therefore further reducing the possibility of tube failure. Since the effective weight of the inboard segment of the adapter is at least as great as the transverse force due to pressure FT, the inboard segment limits expansion of tube. Greater tube reliability over a greater range of tube, adapter and cavity tolerances is thus produced.
  • the adapter 10 4 must be disposed in the cavity 40 v of the rotor 42 v in an orientation which substantially aligns the line of action 48 of closure of the adapter segments 12 4 , 14 4 with a radial line extending from the axis of rotation of the rotor to the center of the cavity 40 v in which the adapter is disposed and which places the mating surfaces 18 4 of the adapter segments 12 4 , 14 4 in the plane 68 ( Figure HA) that is perpendicular to the radius extending through the cavity 40 v .
  • the segments 12 4 , 14 4 may be keyed in a fashion to be described.
  • both segments 12 4 , 14 4 have the requisite effective weight sufficient to ensure complete containment of the tube in the adapter recess, then either segment may assume the position of the inboard segment.
  • the adapter may be inserted into the cavity in either of two different orientations and the desired performance will occur.
  • the keying can be implemented by providing any suitable distinctive physical feature on the adapter, such as a visually distinctive marking or a distinctive shape. Should only one segment 12 4 exhibit the requisite effective weight then a form of keying is necessary which both: (1) identifies that segment as the inboard segment; and (2) aligns the mating surfaces 18 4 of the adapter segments 12 4 , 14 4 in the plane 68.
  • FIG. 12A and 12B A particular modified configuration of an adapter 10 4 in which only one segment 12 4 exhibits the requisite effective weight is illustrated in Figures 12A and 12B.
  • the inboard adapter segment 12 4 has a distinctive configuration imparted thereto in the form of the fiat surfaces 68 4 provided on the exterior surface 16 4 of the segment 12 4 .
  • the cavity 40 v into which the adapter 10 4 of Figure 12 is insertable is correspondingly shaped, thus to ensures that the adapter 10 4 is properly received into the rotor 42 v .
  • a portion of the upper surface 22 4 of the inboard segment 12 4 is removed to define a channel 70 4 therein.
  • the mating surfaces 18 4 on the inboard segment 12 4 are flush with the boundaries of the channel 70 4 .
  • the upper surface 22 4 of the outboard segment 14 4 is provided with a projecting flange 72 4 that is shaped in correspondence to the channel 70 4 .
  • the mating surfaces 18 4 on the outboard segment 14 4 are arranged to slidably engage the corresponding mating surfaces 18 4 on the inboard segment 12 4 .
  • the undersurface of the flange 72 4 has a pocket 76 4 therein that accepts the upper capped end of the tube T.
  • This structure defines a compact, cartridge-like adapter 10 4 for the tube T.
  • the tube T is retained in the outboard segment 14 4 with the capped end of the tube T received in the pocket 76 4 therein. This disposition is believed to facilitate handling of the tube T.
  • Such an adapter may be useful in converting a vertical angle rotor to a rotor having a "near vertical" cavity orientation.
  • the mating surfaces of the segments in such a case will lie in a plane that contains the axis of the recess, said plane also being inclined with respect to the axis of the adapter. These mating surfaces of such an adapter need not, therefore, align with the plane perpendicular to a radius extending from the axis of rotation of the rotor through the center of the cavity, as is the case in connection with the preferred embodiment of this aspect of the invention as shown in Figures 10 through 12.
  • FIGs 13, 14, 15 and 16 illustrate another modified configuration for a compact, cartridge-like adapter 10 4 similar to that shown in Figures 12A and 12B.
  • the adaptor 10 4 includes adapter segments 12 4 , 14 4 , each of which has an exterior surface 16 4 and a mating surface 18 4 thereon.
  • the exterior surface 16 4 has a cylindrical configuration similar to the adaptor of Figure 11C (without the resilient extensions 58 4 and 60 4 ) and is thus insertable in a correspondingly shaped cylindrical rotor cavity 40 v ( Figure 16).
  • the mating surfaces 18 4 include those planar surfaces of the adapter segments 12 4 , 14 4 that align in the plane 68 (perpendicular to the radius of the rotor 42 4 ) when the adapter is received within the rotor, as well as planar lateral surfaces that extend generally perpendicular thereto.
  • the former are indicated in the Figures by the characterl8 4 and 18 4 ' respectively.
  • the mating surface 18 4 in each segment is provided with an indentation 28 4 that cooperate to define a recess 30 4 sized to accept a centrifuge tube T therein.
  • in the adapter 10 4 of Figures 13 through 16 only one segment, e. g., the inboard segment 12 4 , exhibits the requisite effective weight to insure that the mating surfaces 18 4 on the inboard segment 12 4 and the outboard segment 14 4 remain in contact during operation of the rotor so that no gap therebetween may form.
  • a portion of the upper surface 22 4 of the outboard segment 14 4 is removed to define the channel 70 4 therein.
  • the upper surface 22 4 of the inboard segment 12 4 is provided with the projecting flange 72 4 that is shaped in correspondence to the channel 70 4 .
  • the lateral portions 18 4 ' of the mating surfaces 18 4 on the inboard segment 12 4 are arranged to slidably engage the corresponding lateral portions 18 4 ' of the mating surfaces 18 4 ' on the outboard segment 14 4 .
  • the undersurface of the flange 72 4 may have a pocket 76 4 therein that accepts the upper capped end of the tube T.
  • the projecting flange 72 4 on the upper surface 22 4 of the inboard segment 12 4 has gripping serrations 80 4 provided thereon. These gripping serrations 80 4 facilitate manipulations of the segments.
  • the presence of the serrations 80 4 serves as a visual indicator key which both identifies the inboard segment and aligns the mating surfaces 18 4 of the adapter segments 12 4 , 14 4 in the plane 68.
  • a portion 82 4 of the flange 72 4 also projects forward!
  • the segments 12 4 , 14 4 may be hinged. Since the serrated flange 72 4 is located at the upper end of the cartridge adaptor 10 4 a more convenient form of hinge arrangement 26 4 is shown in Figures 13 and 14.
  • the hinge arrangement 26 4 includes a pair of stub-like axles 86 4 disposed opposed lateral surface portions 18 4' of the mating surface 18 4 of the inboard segment 12 4 .
  • the hinge arrangement 26 4 further includes a pair of trunnion recesses 88 4 provided on the opposed confronting lateral surface portions 18 4 ' of the mating surface 18 4 of the outboard segment 14 4 .
  • the stub-like axles 86 4 on the inboard segment 12 4 snappingly engage into the trunnion recesses 88 4 on the outboard segment 14 4 .
  • the axis 26 A 4 of the hinge 26 4 is perpendicular to the axis of the adapter 10 4 and supports the relative pivotal movement, about the hinge axis 26A 4 of the segment 12 4 , 14 4 with respect to the other from an open to a mated position.
  • the adapter 10 4 of Figures 13-16 may be fabricated of the same material as used for the adapter 10 4 of Figures 12 A, 12B.
  • Such an adapter may be useful in converting a vertical angle rotor to a rotor having a "near vertical" cavity orientation.
  • the mating surfaces of the segments in such a case will lie in a plane that contains the axis of the recess, said plane also being inclined with respect to the axis of the adapter.

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Abstract

An adapter for a centrifuge tube (T) comprises two segments (124)(144) that may be hinged along a hinge axis that extends perpendicular to the axis of the adapter.

Description

TITLE
CENTRIFUGE TUBE ADAPTER
CROSS REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of application Serial Number 07/695,871, filed May 6, 1991 (IP-0805-B), which is itself a a continuation-in-part of application Serial Number 07/552,631, filed July 13, 1990 (IP-0805-A), which is itself a continuation-in-part of application Serial Number 07/432,646, filed November 7, 1989 (IP-0805), all in the names of Romanauskas and Sheeran and all assigned to the assignee of the present invention.
BACKGROUND OFTHE INVENTION
Field of the Invention The present invention relates to an adapter for holding a centrifuge tube in a centrifuge rotor cavity, and in particular, to an adapter having two segments, the segments being in some cases joined by a hinge, the hinge axis extending perpendicular to the axis of the adapter.
Description of the Prior Art In the operation of a centrifuge it is important that the size and shape of the tube in which a liquid sample is carried closely conforms to the size and shape of the cavity in the centrifuge rotor in which the tube is received. During centrifugation the centrifugal force exerted on the tube itself and the liquid therein acts to deform the centrifuge tube. A centrifuge tube which does not closely conform to the rotor cavity may thus be deformed to the point of rupture. Even if the tube does not rupture the deformation may make the tube difficult to remove from the rotor cavity. Moreover, even if the deformed tube is removable from the rotor, the return of the tube to its undeformed shape may agitate the contents of the tube to an extent that destroys the sample separation.
When the shape and size of a centrifuge tube does not closely conform to the shape and size of the rotor cavity in which it is to be disposed a device known as a tube adapter is usually employed. The tube adapter has an interior cavity having a shape and size which closely conforms to the shape and size of the centrifuge tube being adapted. The exterior shape and size of the adapter closely conforms to the shape and size of the rotor cavity in which the tube is to be used. The adapter serves to support a tube within the cavity in which it is received and thus serves to prevent deformation of the tube during centrifugation.
Exemplary of an adapter formed of a single unitary member is the device disclosed in United States Patent 4,304,356 (Chulay et al.). This adapter supports only the neck region of the centrifuge tube and is fabricated of a material having a lower density than the liquid being carried therein to prevent bottoming of the adapter in the rotor cavity in the event of tube rupture.
Exemplary of an adapter formed of two piece construction is the device shown in United States Patent 3,674,197 (Mitchell et al.), assigned to the assignee hereof. This adapter comprises two discrete segments, each of which has an indentation therein. When joined the indentations form a recess for receiving a collapsible bag during centrifugation. The adapter disclosed in this patent includes aperture(s) through which tubes from the bag exit the adapter. Thus, the possibility exists that the bag may extrude through these 3 apertures if the adapter were to undergo centrifugation in a vertical angle rotor.
An adapter arrangement formed of two discrete adapter 5 segments and useful to support the capped end of a centrifuge tube is available as part of the Nalgene Ultra-Lok Tube System sold by Fisher Scientific Incorporated.
United States Patent 4,692,137 (Anthony) discloses a 0 tube adapter having two segments which are hinged along the lateral edges of the segments. The hinge axes align in parallel relationship to the axis of the cavity in which the adapter is received. The disposition of hinges along the lateral edges of the segments is believed disadvantageous in that such a 5 disposition may interfere with the insertion or removal of the adapter into or from the rotor cavity.
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0 United States Patent 3,998,383 (Romanauskas et al.) and
United States Patent 4,015,775 (Rohde), both assigned to the assignee of the present invention, disclose centrifuge rotors of the vertical angle type. In such a rotor the axis of the rotor cavities is substantially parallel to the axis of rotation. When 5 using a vertical angle rotor it is necessary that a cap be provided at the mouth of each cavity to impose a vertical restraining force on the tube disposed in the cavity. Even though the tube may be disposed in an adapter received within the cavity, without such a capping arrangement the possibility 0 exists that the pressure of the liquid during centrifugation may rupture the tube. United States Patent 3,998,383 (Romanauskas et al.) exemplifies a typical capping arrangement for a vertical angle rotor. Such capping arrangements must be individually threaded into the rotor body. Moreover, in order to provide proper support it is necessary that the capping arrangement be in intimate contact with the tube. Improper assembly can thus lead to the possibility of tube rupture and/or cap failure. For these reasons such capping arrangements are believed disadvantageous.
In view of the foregoing it is believed advantageous to provide an adapter for use in a vertical angle rotor that eliminates the necessity of a capping mechanism for the rotor cavity.
SUMMARY OFTHE INVENΗQN
The present invention relates to an adapter having an axis therethrough for supporting a centrifuge tube within a cavity in a centrifuge rotor. The cavity itself has an axis therethrough. The axis of the adapter may, in use, align in parallel relationship with the axis of the cavity. The adapter comprises a first and a second adapter segment, each segment having an exterior surface and a mating surface thereon. Each segment has an indentation in the mating surface thereof. The segments may be connected by at least one hinge that supports the segments for relative pivotal movement about a hinge axis from an open to a mated position. The hinge axis extends perpendicular to the axis of the adapter.
When in the mated position the mating surfaces of the segments are in contacting relationship and the indentations therein cooperate to define a recess having a predetermined shape. In one embodiment of the adapter of the present invention, used with a centrifuge tube having a body with a neck thereon in which a portion of the neck has a constricted region when the tube is capped, the indentation in each segment is shaped such that when the segments are in the mated position the recess is sized to closely correspond to the configuration of at least the neck of the tube. In this embodiment at least one of the segments has a feature on the mating surface thereof that projects into the indentation therein. When the segments are in the mated position and the neck of the tube is received within the adapter the feature is received within the constricted region of the neck of the tube. A collar may be provided to prevent the bottoming of the tube in the cavity.
In another embodiment of the adapter of the present invention the indentation in each segment is shaped such that when the segments are in the mated position the recess so defined is sized to closely correspond to the size and configuration of the centrifuge tube over its entire length.
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In another aspect the present invention relates to an adapter for supporting a closed centrifuge tube having a predetermined size and configuration within a cavity in a vertical angle centrifuge rotor. The rotor is rotatable to a predetermined maximum speed. The adapter has a central axis extending therethrough that, in use, aligns in parallel relationship both with the axis of the rotor cavity in which the adapter is disposed and with the axis of rotation of the vertical angle rotor. The adapter comprises a first and a second adapter segment, each of which has an exterior surface and a mating surface thereon. Each segment has an indentation in the mating surface thereof. The indentations are shaped such that when the segments are joined along their mating surfaces the indentations cooperate to define a recess able to totally surround a centrifuge tube disposed therein. Each adapter segment is fabricated of a material that has sufficient strength to withstand the vertical forces created by the pressure of a liquid under centrifugation. Thus, use of an adapter in accordance with this aspect of the present invention permits a tube to be centrifuged in a vertical angle centrifuge rotor without the necessity of a capping mechanism being placed in the rotor cavity.
In still another aspect the mating surface on each adapter segment defines a predetermined angle with respect to a plane that is normal to a plane containing the line of action along which the adapter segments are joined. Inclination of the mating surfaces of the adapter segments allows the same to displace relative to each other to totally fill the rotor cavity in which they are disposed without any separation being defined between the segments. Inclined mating surfaces may be provided on any of the adapter segments disclosed in the present application.
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In still another aspect the present invention relates to an adapter for supporting a closed centrifuge tube in which at least one of the. adapter segments has an effective weight sufficient to balance forces created by the pressure of a liquid carried in the tube under centrifugation that act transversely to the central axis. In use, with the adapter inserted into a cavity of a rotor, the one segment is disposed closer to the axis of rotation so that the mating surfaces of the adapter segments lie in a plane that is perpendicular to a radius of the rotor extending through the cavity. In such a disposition the weight of the one segment while under centrifugation is sufficient to maintain the mating surfaces of the adapter segments in contacting relationship with each other. Suitable keying may be provided to identify the one segment having the predetermined effective weight. BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be more fully understood from the following detailed description thereof, taken in connection with the accompanying drawings, which form a part of this application and in which:
Figure 1 is a perspective view of an adapter according to a first embodiment of the present invention for supporting the neck region of a centrifuge tube of the type in which a portion of the tube neck has a constricted region thereon when capped, the adapter being shown in the open position;
Figure 2 is a fragmentary elevation view, in section, of the tube adapter of Figure 1 in use and supporting the neck portion of a centrifuge tube in a fixed angle rotor cavity;
Figure 3 a perspective view of an adapter according to a second embodiment of the present invention for supporting the full length of a centrifuge tube within a rotor cavity, the adapter being shown in the open position;
Figure 4 is a fragmentary elevation view, in section, of the tube adapter of Figure 3 in use and supporting a centrifuge tube over its entire axial length in a fixed angle rotor cavity;
Figure 5 is a perspective view similar to Figure 3 of a modification of the embodiment of the tube adapter there shown for use with an open top tube;
Figure 6 is a fragmentary elevation view, in section, of the centrifuge tube adapter of Figure 5 in use and supporting a centrifuge tube over its entire axial length in a fixed angle rotor cavity; Figure 7A is a perspective view of an adapter in accordance with another aspect of the present invention used to support a closed tube within the cavity of a vertical angle rotor, the adapter segments being independent of each other, while Figure 7B is a modification of the embodiment of adapter shown in Figure 7A in which the adapter segments are hinged;
Figure 8 is a fragmentary elevational view of an adapter shown in either Figure 7A or 7B in use and supporting a centrifuge tube over its entire axial length in a vertical angle centrifuge rotor cavity, with a portion of the tube being broken away;
Figures 9A and 9B are sectional views taken along section lines 9A-9A, 9B-9B in Figure 8 showing the inclination of the mating surfaces of the adapter segments, the view of Figure 9A illustrating the relationship of the adapter segments with respect to each other, with respect to the tube received in the adapter, and with respect to the rotor cavity in which the adapter is placed while rotor is at rest while the view of Figure 9B shows the relationship of the adapter segments with respect to each other, with respect to the tube received in the adapter, and with respect to the rotor cavity in which the adapter is placed when the rotor is rotating;
Figure 10 is a perspective view of an adapter in accordance with yet another aspect of the present invention used to support a closed tube within the cavity of a vertical angle rotor;
Figure HA is a side sectional view of an adapter of Figure 10 in use and supporting a centrifuge tube over its entire axial length in a vertical angle centrifuge rotor cavity, while Figures 11B and 11C are, respectively, sectional views of the adapter as shown in Figure 11A taken along section lines 11B-11B and 11C-11C; and
Figure 12A is a perspective view of a modification of the embodiment of the adapter shown in Figures 10 and 11 with the inboard adapter segment having a keying configuration thereon, while Figure 12B is a side sectional view of the adapter of Figure 12A with the adapter segments joined together;
Figure 13 is a perspective view of another modification of the embodiment of the adapter shown in Figures 10 and 11;
Figure 14 is an enlarged view of a portion of the perspective view of Figure 13 illustrating a hinge arrangement useful with the modified adaptor shown therein;
Figure 15 is an enlarged view of the inboard segment of the modified adaptor shown in Figure 13 taken along view lines 15-15 therein;
Figure 16 is a side sectional view of an adapter of Figure 10 in use and supporting a centrifuge tube over its entire axial length in a vertical angle centrifuge rotor cavity.
PETAI EP PESCRIPTIQN OF THE INVENTION
Throughout the following detailed description, similar reference numerals refer to similar elements in all Figures of the drawings. Superscripted numerals generally relate to corresponding functional elements or features throughout all of the Figures of the drawings.
Figure 1 is an exploded perspective view of an adapter, generally indicated by the reference character 10, according to a first embodiment of the present invention. The adapter 10 in accordance with this embodiment is useful for supporting a centrifuge tube T of the type having a body portion B with a closed end C, the body B tapering through a transition region R to a narrowed neck region N. The neck N serves as the liquid port through which a liquid under test may be loaded into the tube T. When the tube T is capped at least one portion D of the neck N becomes radially inwardly constricted, thereby forming a constricted region in the neck of the tube. Preferably the capping assembly disclosed in United States Patent 4,552,278 (Romanauskas) is used to cap the tube, so that the neck N of the tube has a corrugated configuration imparted thereto. The corrugated configuration has at least one and optionally a plurality of circumferentially extending corrugations formed in the neck N. It should be understood that any other capping arrangement may be used, so long as any form of constricted region is imparted to the configuration of the neck N.
The adapter 10 is comprised of a first adapter segment 12 and an identical second adapter segment 14. Each segment 12, 14 has an exterior surface 16 and a planar mating surface 18 thereon. The exterior surface 16 of each segment is defined by a generally cylindrical lateral surface portion 20 and a planar upper surface portion 22. In the preferred instance an enlarged collar 24 is disposed intermediate the lateral surface portion 20 and the upper surface portion 22. When the segments 12, 14 are mated together the mating surfaces 18 thereof are joined in abutting contact. As will become clearer herein the member so produced has an axis 10A (best seen in Figure 2) extending therethrough. As is best seen in Figure 2 the configuration and size of the adjacent lateral surface portions 20 closely corresponds to the configuration and diameter of a rotor cavity 40 in which the adapter 10 is used. The upper surface portions 22 of the conjoined segments are accessible when the adapter 10 is received in the rotor cavity 40.
The segments 12 and 14 are connected and supported for relative pivotal movement with respect to each other by at least one hinge 26. The hinge 26 may take the form of a live hinge bridging the upper surface portions 22 of the segments 12, 14, or may, if desired, take the form of a coined hinge. The term "live hinge" refers to a hinge type, typically made of a polypropylene material, which must be flexed or bent before the plastic is cooled or permanently set. Such hinges are complete without secondary operations. The term "coined hinge" refers to a hinge that is cold-formed, usually by a stamping operation. The stamping operation creates a narrower and a thinner flexing region which defines a hinge. These forms of hinges are defined in the Handbook of Plastics and Elastomers, McGraw-Hill Book Company 1975, (Charles A. Harper, Editor) at page 12-9.
However formed, in accordance with the present invention the axis 26A of the hinge 26, that is, the axis about which occurs the relative pivotal motion of the segments, extends perpendicular to the axis 10A of the adapter 10. This relationship of the hinge axis 26 A to the axis 10A of the adapter 10 is best illustrated in Figure 2.
The mating surface 18 of each of the adapter segments 12, 14 has an indentation 28 therein. The indentation 28 in each segment 12, 14 corresponds to the size and contour of at least a portion of the tube T. Thus, when the segments 12, 14 are mated, the indentations 28 therein cooperate to define a recess 30 (Figure 2) that corresponds to the size and shape of at least a predetermined portion of the tube T that is received therein. In the embodiment of Figure 1, in which the adapter 10 is configured and sized to support only the neck N and the transition region R of the tube T, at least one but preferably both indentations 28 contains a feature 34, in the form of a circumferentially extending ridge, that corresponds in size and is located complementarity to the position of the constriction D in the neck N of the tube.
The adapter 10 shown in Figures 1 and 2 is especially useful when the diameter of body B of the tube T is equal to the diameter of a cavity 40 in a centrifuge rotor 42, but the overall length L of the tube T is less than the axial length of the cavity. The rotor cavity 40 has an axis 40A therethrough that aligns in parallel relationship with the axis 10A of the adapter 10 when the same is disposed therein. In use, as is best seen in connection with Figure 2, the adapter 10 defined by the mated segments 12, 14 serves to support the neck N and the transition region R of the tube T within the cavity 40.
To mount the tube T in the cavity, the tube T is inserted into one of the segments 12, 14, so that the feature 34 on the segment(s) is received within the constricted region D in the neck N of the tube T when the segments are in the mated position. The segments 12, 14 are then pivoted about the hinge axis 26A to place the mating surfaces 18 thereon in abutting contact. This closes the adapter 10 around the tube T and thus permits the tube T to be manipulated by manipulation of the adapter 10. The tube T and the adapter 10 are then axially inserted into the cavity 40. In the preferred instance the tube T bottoms against the closed end of the cavity 40.
The axial length of the adapter 10 is selected such that when the tube T is received in the cavity 40, the upper surface portions 22 on the segments 12, 14 are accessible to a user. The hinge 26 may be formed so as to define a useful lifting appliance, as shown in Figure 2. Thus, to withdraw the tube T at the end of a centrifugation run, a user grasps the hinge 26 and lifts the tube from the cavity 40. It should be appreciated from the foregoing that the feature 34 in such an instance defines a lifting surface which acts against the material of the tube in the constricted region D in the neck N thereof, and thus serves to transmit the lifting force to the tube T to withdraw the same from the cavity. The tube T may be withdrawn without unduly agitating the separation within the tube T.
In some cases the rotor 42 may have a shoulder 44 defined about the mouth of the cavity 40. The shoulder 44 is preferably located on the rotor 42 at a position that is axially beneath the collars 24 on the segments 12, 14 when the adapter is received within the cavity, thereby to guard against the possibility that tube rupture will permit the adapter 10 to enter into the cavity 40.
The segments 12, 14 with the hinge 26 therebetween are preferably integrally formed from a suitable material, such as polypropylene. Of course, the segments 12, 14 may be otherwise fabricated from one or more pieces, using other manufacturing techniques and other materials, and assembled to define the adapter 10. Similar techniques may be used to form any other embodiment of the adapter illustrated and discussed herein.
For those instances wherein the diameter of the tube T is less than the corresponding diameter of the cavity 40 the adapter 10' shown in Figures 3 and 4 finds utility. In this embodiment of the invention the recess 30' (Figure 4) formed by the cooperative association of the indentations 28' in the mated adapter segments 12', 14' is configured to correspond to the size and shape of the tube T over the entire axial length L' thereof. For this purpose the segments 12', 14' are each provided with an axial extension 36 having a bottom wall 38. The bottom wall 38 need not completely close the bottom of the adapter 12', 14', as is illustrated, but may only partly close the same. The presence of the extension 36 and the bottom wall 38 permit the recess 30' defined when the segments 12', 14' are joined to receive the entire axial length L' of the tube T.
Figure 4 illustrates this embodiment of the invention in use. When the tube T is received in the recess 30' the closed end C of the tube T is contacted by the interior surface of the bottom wall 38. Preferably the indentations 28' in the segments 12', 14* are placed such that the tube T lies as close to the bottom of the rotor cavity 40, thereby to maximize the centrifugal force imposed on the liquid sample. It should also be noted that in this embodiment of the invention the feature 34 present in the embodiment of Figure 1 is not required, since the requisite lifting force transmission surface is defined by the bottom wall 38 operating against the bottom end C of the tube T. It is also noted that in this embodiment of the invention the collar 24 may be eliminated.
Figure 5 illustrates an adapter 10" that defines a modification of the embodiment of the invention shown in Figure 3. In this embodiment, the tube T" has the form of a test tube, with no constriction present to define a neck. In this instance, the segments 12", 14" are modified to exhibit indentations 28" similar to those shown in Figure 3, but which correspond in size and shape to the test tube T" over the entire axial length L" thereof.
In whatever one of the embodiments used, the hinge between the segments is disposed on the upper surface portion of the exterior surface of the adapter segments. Such a disposition is believed advantageous in that it locates the hinge at a position where the hinge does not interfere with the receipt of the adapter within the rotor cavity. At the same time the hinge defines a useful lifting appliance.
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Although the adapter previously illustrated and discussed may find utility in the environment of a vertical angle rotor, such a utilization may typically require the provision of a suitable capping arrangement to prevent tube failure. The capping arrangement is required in the case that the adapter does not completely surround the tube, such as shown in Figures 1 and 2. However, a capping arrangement is also required if the adapter does completely surround the tube, as shown in Figures 3 through 6, but does not have sufficient strength to withstand the vertical force due to liquid pressure under centrifugation.
As outlined earlier, a capping arrangement may be viewed as disadvantageous for various reasons. Accordingly, it is believed desirable to provide an adapter able to support a closed tube T in a vertical angle rotor without the necessity of a capping arrangement. Figures 7A and 7B illustrate such an adapter in accordance with another aspect of the present invention. Figure 7A illustrates an unhinged embodiment of the vertical angle rotor adapter, while Figure 7B shows a hinged embodiment thereof.
The vertical angle rotor adapter shown in Figures 7A and 7B is generally indicated by the reference character 103 and is generally similar to the adapters 10' and 10" discussed in connection with Figures 3 and 5 in the sense that the adapter 103 is arranged to totally surround the tube T disposed there within. The adapter 103 comprises a first adapter segment 123 and a second adapter segment 143. Each segment 123, 143 has an exterior surface 163 thereon. The exterior surface 163 of each segment 123, 143 is defined by a. generally cylindrical lateral surface portion 203 and a planar upper surface portion 223.
In accordance with the embodiment of the invention shown in Figures 7A and 7B the adapter segment 123 has a planar mating surface 183 thereon while the adapter segment 143 has a planar mating surface 193 thereon. For a reason which is explained more fully herein the mating surfaces 183 and 193 on the segments 123 and 143, respectively, are angled with respect to a predetermined reference plane, to be defined. The inclination of the mating surfaces 183 and 193 on the segments 123 and 143, respectively, is believed best seen in Figures 9A and 9B. It should be understood that the mating surfaces of the adapter segments in any of the embodiments shown in Figures 1 through 6 may also be inclined in the manner shown in Figures 9A and 9B.
The mating surfaces 183 and 193 of each of the adapter segments 123 and 143, respectively, each have an indentation 283 therein. The indentation 283 in each segment 123 and 143 corresponds to the size and shape of the entire axial length L of the tube T. Thus, when the segments 123 and 143 are mated the indentations 283 therein cooperate to define a recess 303 (Figure 8) that corresponds to the size and shape of the entire axial length of the tube T (Figures 1 and 8) that is received therein. That is to say, the indentations 283 in each segment are shaped such that when the segments 123 and 143 are joined along their respective mating surfaces 183 and 193 the indentations 283 in each segment cooperate to define a recess 303 able to totally surround a centrifuge tube T disposed therein.
Figure 8 illustrates the adapter 103 in accordance with this aspect of the present invention in use in the environment of a vertical angle centrifuge rotor 42 v. In such a rotor the axis of each cavity 40v is parallel or approaching parallel (with an inclination angle of not more than fifteen (15) degrees) to the axis of rotation A of the rotor. As seen from Figure 8 the adapter 103 has a central axis 103A that, in use, aligns with the axis of the cavity 40v in which it is disposed and with the axis of rotation A of the vertical angle rotor 42v.
In the embodiment of the invention shown in Figure 7A the segments 123, 143 are independent of each other. These segments 123, 143 may be joined by moving each segment toward the other along a line of action 48 thereby to bring the mating surfaces 123, 143 thereof in abutting contact. As used herein the term "line of action" is meant to denote that direction of motion which joins the segments 123, 143 such that, in a given predetermined plane perpendicular to the central axis 10^ simultaneous contact of both sides of the segments 123, 143 occurs.
In Figure 7B the segments 123, 143 are connected and supported for relative pivotal movement with respect to each other by at least one hinge 263. The pivotal axis 263 A (Figure 8) of the hinge 263, that is, the axis about which occurs the relative pivotal motion of the segments 123, 143, extends perpendicular to the axis 103A of the adapter 103. As discussed earlier the hinge 263 may take the form of a live hinge bridging the upper surface portions 223 of the segments 123, 143, or may, if desired, take the form of a coined hinge. Accordingly the segments 123, 143, as shown in the embodiment of Figure 7B may also be joined by moving each segment toward the other along the line of action 48. In the embodiment of Figure 7B it is noted that the line of action 48 also lies in the plane perpendicular to the pivotal axis 263A of the hinge 263. With reference to the sectional views of Figures 9A and 9B, the inclination of the surfaces 183, 193 may be most clearly seen. (Sectioning of the adapter has been omitted from Figures 9A and 9B for clarity of illustration). When the segments 123, 143 are joined, the tube T is totally surrounded by the adapter 103. By inclining the mating surfaces 183, 193 the segments 123, 143 may expand during centrifugation to fill the entirety of the rotor cavity 40 v. Thus, any variations in the size of the various cavities 40v in a given rotor, variations in cavity size from rotor to rotor, and variations in the thickness of the segments from adapter to adapter may be accommodated without breaking the total containment of the tube T by the adapter.
It is also clear from Figure 9A that when the segments
123, 143 are mated the interior surface of the interior recess 303 of the adapter 103 is interrupted by the inwardly projecting corners 50 on the mating surface 193 of the segment 143. The corners 50 lie inwardly of the corresponding corners 52 defined on the mating surface 123. The radial distance Ri measured between the central axis 103A and the interior surface of the adapter segment 143 in the region of the indentation 283 therein is less than the radial distance R2 measured between the central axis 103A and the interior surface of the adapter segment 123 in the region of the indentation 283 therein. For reference purposes it is convenient at this point to define the radial distance R3 as the distance between the central axis 103 and the exterior surface of the adapter segment 143 in the region of the indentation 283 therein and the radial distance R2 as the distance between the central axis 103 and the exterior surface of the adapter segment 123 in the region of the indentation 283 therein. The thickness of the segment 123 is equal to the difference between the distances R4 and R2, while thickness of the segment 143 is equal to the difference between the distances R3 and Ri. To accommodate the instance where the rotor cavity 40v is at its largest possible tolerance and the thickness of the segments of the adapter are at their smallest possible tolerance, the arc length of the inner surface of the segment 143 (i.e., the distance between the points 50-50) in a plane perpendicular to the adapter axis 103A (the plane of Figure 9A) plus the arc length of the inner surface of the segment 123 (i.e., the distance between the points 52-52) in the same plane must equal the circumference of the inside of the adapter in a plane perpendicular to the adapter axis 103A in the case when the adapter of the smallest segment thickness is conformed to the largest rotor cavity, as illustrated in Figure 9B.
The magnitude of angles of inclination of the surfaces may be measured by reference to a reference plane 54. The reference plane 54 is that plane that contains both the vertical central axis 103 of the adapter 103 and at least one of the inwardly projecting corners 50 of the adapter segment 143. Alternatively, the reference plane 54 may be defined as the plane that is normal to the line of action 48 (superimposed on Figure 9A) along which the segments 123, 143 are joined together. Measured with respect to the reference plane 54 the inclination of the surfaces 183 and 193 lies in the range of angles from about 10 to about 80 degrees. Preferably, each angle is forty five (45) degrees.
It should be noted that although the surfaces 183 and 193 are shown as being inclined to the same degree (i.e., the angles of the surfaces 183 and 193 with respect to the reference plane 54 are equal), such is not necessarily required. It is only necessary that the inclination of the surfaces 183 and 193 be such that the segments are maintained in mutual contact if they expand during centrifugation to fill the cavity 40v. It should also be noted that the segments 123 and 143 may be other than circular, and can be ellipsoidal, if desired.
An adapter in accordance with this embodiment of the present invention may be fabricated from any suitable material so long as the resulting adapter has sufficient strength (as that term is defined herein). The material of choice must exhibit other desirable properties, such as appropriate ultimate strength, appropriate modulus of elasticity, suitable chemical compatibility with any liquid sample being centrifuged and ability to withstand autoclaving. Suitable plastic materials include polypropylene, polyamide, acetal, polyphenylene oxide, polyvinyl choloride, polycarbonate or polyethylene. Other plastic or metallic materials (either homogeneous (neat) or fiber reinforced) with similar or better mechanical and chemical properties for the application under consideration may also be used. The adapter may be formed in any convenient manner consistent with the material selected, such as molding, machining, casting or forging.
hi order to support a tube T in a vertical angle rotor without the assistance of the restraining force provided by a capping mechanism, the adapter 103 must exhibit sufficient strength to absorb the forces imposed on the tube T by the pressure of the liquid therein. Thus, as the term is used herein, "sufficient strength" means that the adapter must be able to withstand the forces imposed on it during centrifugation without failing or deforming to the extent that the tube carried therein ruptures.
Whether a given adapter is of sufficient strength, and thus falls within the scope of the claims of the present invention, can be determined from various readily ascertainable operating parameters of the vertical angle rotor in which the adapter is to be used and the application to which the adapter is to be put. These parameters are the specific weight of the liquid sample within the tube received by adapter, the radius Ri which represents the minimum distance to the sample from the axis A of rotation (Figure 8), the diameter D0 (Figure 8) of the rotor cavity, the thickness of the adapter segment, the inside diameter of the tube, and the speed of rotation of the vertical angle rotor.
The pressure at any location across the diameter of the tube in which the liquid sample is disposed is
ω2 P = o ( Ro2 - Ri2) (1 )
2g
where P is the pressure (psi), ω is the rotational velocity of the rotor (radians per second), g is acceleration due to gravity (inches per second2), α is the specific weight of the sample (Lb per inch3), R0 is the distance to the point of interest x where the pressure value is desired from the center of rotation (inches), and Rj is the minimum distance to the sample from the axis A of rotation (inches).
The total vertical force Fv that the adapter must withstand is then found by integrating this pressure function over the circular cross sectional area of the inside of the tube.
Knowing the adapter dimensions and the force Fy, the average stress in the wall of the adapter can be determined in accordance with the relationship: Fv
S = (2)
(π/4 )( Do2 - Di2)
where s is the stress (psi), Fv is the force (Lbf)
D0 is the diameter of the rotor cavity, and Dj is the inside diameter of the adapter when operating at speed, which equals the diameter of the rotor cavity minus the thickness of each of the segments of the adapter (Figure 9B).
Based on the identity of the material used in the given adapter, the modulus of elasticity of that material may be readily obtained. An estimation of the vertical deformation of the adapter may be found by multiplying the initial length of the adapter by the average stress divided by the modulus of elasticity of the adapter material. If the average stress calculated in Equation (2) is less than the ultimate strength of the adapter material, and the predicted deformation is less than the deformation that will cause first leakage in the tube carried within the adapter, then the given adapter is to be construed to have sufficient strength for at least one operating cycle, and therefore falls within the contemplation of the present invention. The determination of sufficient strength as set forth above under operating conditions will verify both the analysis and the conclusion of the sufficiency of strength of the adapter.
It should be understood that it is within the contemplation of this invention to use an adapter in accordance herewith to support a tube or a predetermined portion thereof within a swinging bucket, thereby making the use of the adapter in accordance with this invention amenable for use in the environment of a swinging bucket rotor.
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To recapitulate, the adapter heretofore described in connection with Figures 7A through 9B for use primarily in a vertical angle rotor is fabricated of a material and in a manner such that the adapter, while under centrifugation, has sufficient strength to withstand the vertical forces Fv (that is, forces that act parallel to the central axis of the adapter). Vertical stresses in the tube T are therefore minimized. Angled mating edges on the adapter segments (Figures 7A and 9A) are provided to prevent a separation from forming between the segments in response to the radial expansion of the tube under pressure. The prevention of such a separation insures that the tube is supported about the entirety of its circumference such that the possibility of tube failure is minimized.
As yet another alternative embodiment of the present invention, the adapter may be designed and fabricated such that, under centrifugation, the body force of one adapter segment is sufficient to balance the force created by the pressure of a liquid carried in the tube under centrifugation that acts transversely to the central axis. As will be developed, when in use the preferred form of such an adapter must be disposed within a cavity of a rotor in an orientation such that the mating surfaces of the adapter segments lie in a plane that is substantially perpendicular to a radius of the rotor extending through the cavity. In such an orientation the line of action of closure of the preferred form of such an adapter aligns with a radial line extending from the axis of rotation of the rotor to the center of the cavity in which the adapter is disposed. Figure 10 illustrates a preferred arrangement of a split adapter 104 for use in a vertical angle rotor in accordance with this embodiment of the present invention. The structure of the adapter 104 is generally similar to the adapter 10' shown and discussed in connection with Figures 3A and 3B and to the adapter 103 shown and discussed in connection with Figures 7A and 7B in the sense that the adapter 104, like the adapters 10' and 103, is arranged to totally surround a tube T disposed there within.
Structurally, the adapter 104 includes a first adapter segment 124 and a second adapter segment 144. Each segment 124, 144 has an exterior surface 164 and a mating surface 184 thereon. The exterior surface 164 of each segment 124, 144 is defined by a generally cylindrical lateral surface portion 204 and a planar upper surface portion 224. The exterior surface 164 of each segment 124, 144 is sized and shaped for close fitting receipt within the cavity 40v of a vertical angle rotor 42v (Figures 11A through 11C).
Each segment 124, 144 is provided with an indentation 284 in the mating surface 184 thereof. The indentation 284 in each segment 124, 144 is shaped so that when the segments 124 and 144 arc joined along their mating surfaces 184 the indentations 284 cooperate to define a recess 304 able to totally surround a centrifuge tube T disposed therein. The adapter 104 has a central axis lO-^A extending therethrough (Figure 11 A). As will be discussed later, the recess 304 may be inclined with respect to the central axis lCHA and remain within the contemplation of this invention.
The mating surfaces 184 of the segments 124, 144 need not be angled with respect to the reference plane as discussed previously in connection with Figures 9 A, 9B, although they may be so aπanged if desired. Alternatively or additionally, it should be noted that an adapter 104 in accordance with this embodiment of the present invention may be provided with a hinge on the upper surface 224 of the segments, similar to the embodiment shown in Figure 7B. If a hinge is provided, the pivotal axis of the hinge extends perpendicular to the axis of the adapter. As discussed earlier, the hinge may take the form of a live hinge or a coined hinge.
In accordance with this embodiment of the invention, at least one of the segments of the adapter 104 must have a predetermined effective weight under centrifugation that is sufficient to prevent separation of the adapter segments. The effective weight of the adapter segment is defined as the weight of the segment at sea level multiplied by the g (gravity) force imposed on the segment when the same is rotated at a predetermined operating speed with the center of mass of the segment lying a predetermined radial distance from an axis of rotation.
At least one, but preferably, both of the segments 124,
144 has at least one, but preferably, a pair of resilient extensions 584, 604, respectively, thereon. In the preferred case the resilient extensions 584, 604 are flexibly mounted, as by hinging, to the outside surface 164 of the segment along a line of bending 624. The resilient extensions 584, 604 are biased to flare outwardly from the adapter segment, and are bendable along the line of bending 624 to close inwardly toward the lateral surface portion 204 of the outside surface 164 of the segment to which they are attached. In the closed position the resilient extensions 584, 604 are in contact with the lateral surface portion 204 of the outside surface 164 of the segment to which they are attached. The lower end of each extension is tapered, as at 644. It should be noted that when the adapter segments 124, 144 are mated the edges of resilient extensions 584, 604 are circumferentially spaced a slight distance apart, thereby to provide sufficient clearance to accommodate the flexing motion of the resilient extensions 584, 604 during insertion into the rotor cavity. As will become clearer herein each extension 584, 604 serves to frictionally interact with the boundaries of a rotor cavity 42v (Figure 11 A through 11C) to prevent rotation of the adapter 104 about its axis lO-^A with respect to the body of the rotor 40v thereby to maintain the adapter 104 in a predetermined angular orientation within the cavity during operation of the rotor.
Figures 11A through 11C illustrate the adapter 104 of Figure 10 in use in a cavity 40v of a vertical angle centrifuge rotor 42 v. Sectioning of the adapter has been omitted from Figure 11C for clarity of illustration. When disposed in the rotor 42 v the segment (for example, the segment 124) which lies closer to the axis of rotation A of the rotor is termed the "inboard" segment. The other segment 144 which lies farther from the axis of rotation 10A is termed the "outboard" segment. The inboard segment 124 must have an effective weight sufficient to balance the force FT created by the pressure of a liquid carried in the tube under centrifugation that acts transversely to the central axis lCHA of the adapter 104. Such an arrangement precludes separation of the adapter segments 124, 144 during centrifugation. When properly positioned in the cavity 40v of the rotor 42 v the mating surfaces 184 of the adapter segments 124, 144 are disposed so as to lie in a plane 68 (Figure HA) that is substantially perpendicular to a radius of the rotor 42 v extending through the cavity 40v. The plane 68 is the plane of Figure 11B.
It should be noted that in some instances the recess 304 may be arranged within the adapter 104 such that an axis extending centrally through the recess 304 of the adapter 104 is offset radially with respect to the axis KHA of the adapter 104. In such an arrangement the recess 304 is not concentric with the generally cylindrical lateral surface portion 204 of the adapter 104. If so offset it its preferred that the recess 304 be displaced radially outwardly with respect to the axis 10 of the adapter 104. Such an arrangement may be utilized to increase the effective weight of the inboard segment 124 and/or to dispose the sample to higher g-forces resulting from the increased radial distance to the sample.
Whether the inboard adapter segment 124 has an effective weight sufficient for the purpose of containing the transverse force FT, and thus fall within the scope of the claims of the present invention, can be determined from consideration of the identical operating parameters as previously developed and described in connection with the "sufficient strength" determination for accommodation of the vertical force Fv.
As earlier noted the pressure P across the diameter of the tube is defined by Equation (1). The value of the pressure P ranges from zero at the inboard edge of the tube to a maximum value at the farthest radial location of the liquid sample from the axis of rotation of the rotor. The inboard segment 124 of the adapter 104 is subjected to a radially inwardly directed force FT that results from liquid pressure in the inboard half of the tube. The magnitude of this radially inwardly directed force FT is determined by integrating the component of the pressure function defined by Equation (1) that is parallel to a radial line through the center of mass of the inboard segment 124 over the surface area of the indentation 284 of the adapter segment 124. So long as the effective weight of the inboard segment 124 is equal to or greater than the force FT due to liquid pressure, then centrifugal force effects acting on the inboard segment 124 cause the mating surfaces 184 of the adapter segments 124, 144 to remain in contacting relationship. The adapter 104 will thus maintain complete containment of the tube during operation of the rotor. An adapter 104 having segments 124, 144 in accordance with this embodiment of the invention may be fabricated from any suitable material so long as the resulting adapter segment 124 has sufficient effective weight (as that term is defined herein) and exhibits suitable chemical compatibility with any liquid sample being centrifuged. It should preferably have the ability to withstand sterilization, as by autoclaving. Suitable plastic materials include polypropylene, polyamide, acetal, polyphenylene oxide, polyvinyl choloride, polycarbonate or polyethylene. Other plastic or metallic materials (either homogeneous (neat) or fiber reinforced) with similar or better mechanical and chemical properties for the application under consideration may also be used. The adapter may be formed in any convenient manner consistent with the material selected, such as molding, machining, casting or forging.
It should be understood that both the segments 124, 144 may be substantially identical in weight or they may be substantially different in weight, so long as the inboard adapter segment has the requisite effective weight to completely contain the tube T during operation of the rotor.
Although not required of this embodiment, it is preferred that the adapter 104 also be fabricated of a material that has sufficient strength to withstand the vertical force Fv due to liquid pressure under centrifugation, as discussed in connection with Figures 7 A through 9B. Of course, if the adapter 104 is not able to withstand the vertical force Fv, then a separate capping arrangement on the rotor is required.
By providing the inboard segment 124 having a -suitable effective weight the mating surfaces on the inboard and outboard segments remain in contact during operation of the rotor and no gap therebetween may form. The tube T is thus completely contained within the conjoined adapter segments during operation of the rotor, and the possibility of tube failure due to extrusion into a gap is precluded. The present embodiment carries the additional benefit of minimizing circumferential stress in the tube caused by the pressure of the liquid, therefore further reducing the possibility of tube failure. Since the effective weight of the inboard segment of the adapter is at least as great as the transverse force due to pressure FT, the inboard segment limits expansion of tube. Greater tube reliability over a greater range of tube, adapter and cavity tolerances is thus produced.
As previously mentioned, the adapter 104 must be disposed in the cavity 40v of the rotor 42v in an orientation which substantially aligns the line of action 48 of closure of the adapter segments 124, 144 with a radial line extending from the axis of rotation of the rotor to the center of the cavity 40 v in which the adapter is disposed and which places the mating surfaces 184 of the adapter segments 124, 144 in the plane 68 (Figure HA) that is perpendicular to the radius extending through the cavity 40 v. To meet this need, the segments 124, 144 may be keyed in a fashion to be described.
If both segments 124, 144 have the requisite effective weight sufficient to ensure complete containment of the tube in the adapter recess, then either segment may assume the position of the inboard segment. Thus, the adapter may be inserted into the cavity in either of two different orientations and the desired performance will occur.
The keying can be implemented by providing any suitable distinctive physical feature on the adapter, such as a visually distinctive marking or a distinctive shape. Should only one segment 124 exhibit the requisite effective weight then a form of keying is necessary which both: (1) identifies that segment as the inboard segment; and (2) aligns the mating surfaces 184 of the adapter segments 124, 144 in the plane 68.
A particular modified configuration of an adapter 104 in which only one segment 124 exhibits the requisite effective weight is illustrated in Figures 12A and 12B. In this modification the inboard adapter segment 124 has a distinctive configuration imparted thereto in the form of the fiat surfaces 684 provided on the exterior surface 164 of the segment 124. The cavity 40v into which the adapter 104 of Figure 12 is insertable is correspondingly shaped, thus to ensures that the adapter 104 is properly received into the rotor 42v.
In addition, a portion of the upper surface 224 of the inboard segment 124 is removed to define a channel 704 therein. The mating surfaces 184 on the inboard segment 124 are flush with the boundaries of the channel 704. The upper surface 224 of the outboard segment 144 is provided with a projecting flange 724 that is shaped in correspondence to the channel 704. In addition, the mating surfaces 184 on the outboard segment 144 are arranged to slidably engage the corresponding mating surfaces 184 on the inboard segment 124. The undersurface of the flange 724 has a pocket 764 therein that accepts the upper capped end of the tube T.
This structure defines a compact, cartridge-like adapter 104 for the tube T. When the segments are separated, the tube T is retained in the outboard segment 144 with the capped end of the tube T received in the pocket 764 therein. This disposition is believed to facilitate handling of the tube T. As briefly noted earlier, it may be desirable in some instances to orient the indentations within each adapter segment such that a central axis through the recess formed when the segments are joined is inclined to the axis of the adapter. Such an adapter may be useful in converting a vertical angle rotor to a rotor having a "near vertical" cavity orientation. The mating surfaces of the segments in such a case will lie in a plane that contains the axis of the recess, said plane also being inclined with respect to the axis of the adapter. These mating surfaces of such an adapter need not, therefore, align with the plane perpendicular to a radius extending from the axis of rotation of the rotor through the center of the cavity, as is the case in connection with the preferred embodiment of this aspect of the invention as shown in Figures 10 through 12. It should be understood, however, that so long as the effective weight of the inboard segment while under centrifugation is sufficient to maintain the mating surfaces of the adapter segments in contacting relationship with each other, such a modified "near vertical" adapter lies within the contemplation of the present invention as defined by the appended claims.
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Figures 13, 14, 15 and 16 illustrate another modified configuration for a compact, cartridge-like adapter 104 similar to that shown in Figures 12A and 12B. The adaptor 104 includes adapter segments 124, 144, each of which has an exterior surface 164 and a mating surface 184 thereon. When the segments 124, 144 of the adaptor 104 are conjoined the exterior surface 164 has a cylindrical configuration similar to the adaptor of Figure 11C (without the resilient extensions 584 and 604) and is thus insertable in a correspondingly shaped cylindrical rotor cavity 40v (Figure 16). Simlar to the case shown in Figures 12A and 12B, the mating surfaces 184 include those planar surfaces of the adapter segments 124, 144 that align in the plane 68 (perpendicular to the radius of the rotor 424) when the adapter is received within the rotor, as well as planar lateral surfaces that extend generally perpendicular thereto. The former are indicated in the Figures by the characterl84 and 184' respectively. The mating surface 184 in each segment is provided with an indentation 284 that cooperate to define a recess 304 sized to accept a centrifuge tube T therein. As is also the case with the arrangement of Figures 12A, 12B, in the adapter 104 of Figures 13 through 16 only one segment, e. g., the inboard segment 124, exhibits the requisite effective weight to insure that the mating surfaces 184 on the inboard segment 124 and the outboard segment 144 remain in contact during operation of the rotor so that no gap therebetween may form.
In the arrangement of Figures 13 through 16 a portion of the upper surface 224 of the outboard segment 144 is removed to define the channel 704 therein. The upper surface 224 of the inboard segment 124 is provided with the projecting flange 724 that is shaped in correspondence to the channel 704. The lateral portions 184' of the mating surfaces 184 on the inboard segment 124 are arranged to slidably engage the corresponding lateral portions 184' of the mating surfaces 184' on the outboard segment 144. The undersurface of the flange 724 may have a pocket 764 therein that accepts the upper capped end of the tube T. Thus, when the segments 124, 144 are separated a tube T is retained in the inboard segment 124
The projecting flange 724 on the upper surface 224 of the inboard segment 124 has gripping serrations 804 provided thereon. These gripping serrations 804 facilitate manipulations of the segments. In addition the presence of the serrations 804 serves as a visual indicator key which both identifies the inboard segment and aligns the mating surfaces 184 of the adapter segments 124, 144 in the plane 68. As perhaps best seen in Figure 15 a portion 824 of the flange 724 also projects forward! y thereby to overhang exterior surface 164 on the inboard segment 124- As is seen in Figure 16 when the adaptor 10 is received within the cavity 40v of the vertical rotor 42v the forwardly projecting portion 824 abuts against a shelf 45v that is formed about the mouth of the cavity on the inboard side thereof. It should abe understood by those skilled in the art that an adapter as shown in Figures 10 through 16 can also be used in rotors other than vertical rotors.
As briefly noted earlier, the segments 124, 144 may be hinged. Since the serrated flange 724 is located at the upper end of the cartridge adaptor 104 a more convenient form of hinge arrangement 264 is shown in Figures 13 and 14. The hinge arrangement 264 includes a pair of stub-like axles 864 disposed opposed lateral surface portions 184' of the mating surface 184 of the inboard segment 124. The hinge arrangement 264 further includes a pair of trunnion recesses 884 provided on the opposed confronting lateral surface portions 184' of the mating surface 184 of the outboard segment 144. The stub-like axles 864 on the inboard segment 124 snappingly engage into the trunnion recesses 884 on the outboard segment 144. The axis 26 A4 of the hinge 264 is perpendicular to the axis of the adapter 104 and supports the relative pivotal movement, about the hinge axis 26A4 of the segment 124, 144 with respect to the other from an open to a mated position.
The adapter 104 of Figures 13-16 may be fabricated of the same material as used for the adapter 104 of Figures 12 A, 12B. In connection with the arrangement of Figures 12A, 12B as well as Figures 13-16 it should be understood that in some instances it may be desirable to orient the indentations within each adapter segment such that a central axis through the recess formed when the segments are joined is inclined to the axis of the adapter. Such an adapter may be useful in converting a vertical angle rotor to a rotor having a "near vertical" cavity orientation. The mating surfaces of the segments in such a case will lie in a plane that contains the axis of the recess, said plane also being inclined with respect to the axis of the adapter. These mating surfaces of such an adapter need not, therefore, align with the plane perpendicular to a radius extending from the axis of rotation of the rotor through the center of the cavity, as is the case in connection with the preferred embodiment of this aspect of the invention as shown in Figures 10 through 12. It should be understood, however, that so long as the effective weight of the inboard segment while under centrifugation is sufficient to maintain the mating surfaces of the adapter segments in contacting relationship with each other, such a modified "near vertical" adapter lies within the contemplation of the present invention as defined by the appended claims.
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Those skilled in the art, having the benefit of the teachings of the present invention may impart numerous modifications thereto. It should be understood that such modifications are also to be construed to lie within the scope of the present invention, as defined by the appended claims.

Claims

WHAT IS CLAIMED IS:
1. An adapter for supporting a closed centrifuge tube within a cavity of a centrifuge rotor, the adapter comprising: a first, inboard, adapter segment and a second, outboard, adapter segment, each segment having an exterior surface and a mating surface thereon, each segment having an indentation in the mating surface thereof, the indentation in each segment being shaped such that when the segments are joined along their mating surfaces the indentations cooperate to define a recess able to totally surround a centrifuge tube disposed therein, the adapter having a central axis extending therethrough, at least the first, inboard, segment of the adapter having an effective weight sufficient to balance forces created by the pressure of a liquid carried in the tube under centrifugation that act transversely to the central axis, so that, in use with the adapter inserted into a cavity of a rotor with the mating surfaces of the adapter segments being in contacting relationship with each other, the effective weight of the inboard segment while under centrifugation is sufficient to maintain the mating surfaces of the adapter segments in such contacting relationship.
2. The adapter of claim 1 wherein the outboard segment has a predetermined effective weight, and wherein the effective weight of the inboard segment is different from the effective weight of the outboard segment.
3. The adapter of claim 2 wherein the effective weight of the inboard segment is greater than the effective weight of the outboard segment.
4. The adapter of claim 1 wherein the outboard segment has a predetermined effective weight, and wherein the effective weight of the inboard segment is the same as the effective weight of the outboard segment.
5. The adapter of claim 2 wherein one of the segments has a distinctive feature thereon.
6. The adapter of claim 5 wherein the distinctive feature is a visual feature.
7. The adapter of claim 5 wherein the distinctive feature is the shape of the segment.
8. The adapter of claim 5 wherein the distinctive feature is on the inboard segment.
9. The adapter of claim 8 wherein the distinctive feature is a visual marking.
10. The adapter of claim 8 wherein the inboard segment has a predetermined shape, and wherein the distinctive feature is the shape of the inboard segment.
11. The adapter of claim 1 wherein one of the segments has a distinctive feature thereon.
12. The adapter of claim 11 wherein the distinctive feature is a visual marking.
13. The adapter of claim 11 wherein the distinctive feature is the shape of the segment.
14. The adapter of claim 11 wherein the distinctive feature is on the inboard segment. 15. The adapter of claim 14 wherein the distinctive feature is a visual feature.
16. The adapter of claim 14 wherein the inboard segment has a predetermined shape, and wherein the distinctive feature is the shape of the inboard segment.
17. The adapter of claim 1 wherein the cavity of the rotor is circular and wherein each of the segments has an exterior surface thereon, at least one of the segments has at least a first resilient extension thereon, the resilient extension being biased to flare outwardly from the adapter segment, the resilient extension being bendable with respect to the adapter segment from the flared position to a second position in which the extension contacts against the exterior surface of the segment on which it is disposed, when the adapter is disposed in a rotor, the extension frictionally interacts with the boundaries of a rotor cavity to prevent rotation of the adapter about its axis with respect to the body of the rotor, thereby to maintain the adapter in a predetermined angular orientation within the cavity during operation of the rotor.
18. The adapter of claim 17 wherein the extension is hinged to the segment along a line of bending disposed on the exterior surface of the segment.
19. The adapter of claim 18 wherein the extension has a tapered portion thereon.
20. The adapter of claim 1 wherein inboard segment has an exterior surface thereon, the exterior surface having at least one planar keying region defined thereon. 21. The adapter of claim 20 wherein both the inboard segment and the outboard segment have an upper surface thereon, the inboard segment having a channel formed through the upper surface thereon, the outboard segment having a flanged shaped in correspondence to the channel disposed on the upper surface thereof, the flange having a pocket formed therein , the pocket being sized to receive the end of a tube received within the adapter.
22. The adapter of claim 1 wherein the centrifuge rotor is a vertical angle rotor, and wherein the adapter segments are fabricated of a material that has sufficient strength to withstand the vertical forces created by the pressure of a liquid under centrifugation.
23. The adapter of claim 1 further comprising at least one hinge connecting the segments and supporting the relative pivotal movement, about a hinge axis, of at least one segment with respect to the other from an open to a mated position, the hinge axis extending perpendicular to the axis of the adapter.
24. The adapter of claim 1 wherein the outboard segment has a predetermined effective weight, and wherein the effective weight of the outboard segment is greater than the effective weight of the inboard segment.
25. The adapter of claim 23 wherein the hinge comprises a pair of axles formed at the lower end of one segment and a pair of trunnion recesses formed at a corresponding location on the other segment.
26. The adapter of claim 22 further comprising at least one hinge connecting the segments and supporting the relative pivotal movement, about a hinge axis, of at least one segment with respect to the other from an open to a mated position, the hinge axis extending perpendicular to the axis of the adapter, the hinge comprising a pair of axles formed at the lower end of one segment and a pair of trunnion recesses formed at a corresponding location on the other segment.
27. The adapter of claim 1 wherein the inboard segment has a flange and the outboard segment has a channel therein sized to receive the flange, the flange having serrations thereon.
28. The adapter of claim 27 wherein the flange on the inboard segment has overhanging projection thereon adapted to seat against a shelf provided in a centrifuge rotor.
EP92913835A 1991-05-06 1992-05-06 Centrifuge tube adapter Expired - Lifetime EP0584277B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US69587191A 1991-05-06 1991-05-06
US695871 1991-05-06
PCT/US1992/003813 WO1992019382A1 (en) 1991-05-06 1992-05-06 Centrifuge tube adapter

Publications (3)

Publication Number Publication Date
EP0584277A1 EP0584277A1 (en) 1994-03-02
EP0584277A4 true EP0584277A4 (en) 1994-11-30
EP0584277B1 EP0584277B1 (en) 1998-01-28

Family

ID=24794774

Family Applications (1)

Application Number Title Priority Date Filing Date
EP92913835A Expired - Lifetime EP0584277B1 (en) 1991-05-06 1992-05-06 Centrifuge tube adapter

Country Status (5)

Country Link
EP (1) EP0584277B1 (en)
JP (1) JP2777283B2 (en)
CA (1) CA2102320A1 (en)
DE (1) DE69224289T2 (en)
WO (1) WO1992019382A1 (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5295943A (en) * 1989-11-07 1994-03-22 E. I. Du Pont De Nemours And Company Adapter for holding a pair of centrifuge tubes
US5935052A (en) * 1993-05-27 1999-08-10 Sorvall Products, L.P. Adapter for centrifuge tube
JP2011125813A (en) * 2009-12-18 2011-06-30 National Cancer Center Centrifugal separation container, adapter for retaining position of centrifugal separation container and centrifugal separation implement
DE102014008445A1 (en) * 2014-06-06 2015-12-17 Thermo Electron Led Gmbh Adapter for a sample container of a centrifuge as well as adapter group and centrifuging system
JP6431438B2 (en) * 2015-04-28 2018-11-28 株式会社フコク Adapter for maintaining the position of centrifuge containers

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3674197A (en) * 1970-09-08 1972-07-04 Sorvall Inc Ivan Washing means for flexible bags in split enclosures
US4306676A (en) * 1980-04-17 1981-12-22 Beckman Instruments, Inc. Tube holder for centrifuge rotor
US4692137A (en) * 1985-04-03 1987-09-08 Beckman Instruments, Inc. Split tube centrifuge rotor adapter

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
No further relevant documents disclosed *
See also references of WO9219382A1 *

Also Published As

Publication number Publication date
WO1992019382A1 (en) 1992-11-12
EP0584277B1 (en) 1998-01-28
CA2102320A1 (en) 1992-11-07
JP2777283B2 (en) 1998-07-16
DE69224289T2 (en) 1998-09-10
DE69224289D1 (en) 1998-03-05
EP0584277A1 (en) 1994-03-02
JPH06511187A (en) 1994-12-15

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