EP0056609A2 - Tube séparateur pour la séparation par centrifugation - Google Patents

Tube séparateur pour la séparation par centrifugation Download PDF

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Publication number
EP0056609A2
EP0056609A2 EP82100181A EP82100181A EP0056609A2 EP 0056609 A2 EP0056609 A2 EP 0056609A2 EP 82100181 A EP82100181 A EP 82100181A EP 82100181 A EP82100181 A EP 82100181A EP 0056609 A2 EP0056609 A2 EP 0056609A2
Authority
EP
European Patent Office
Prior art keywords
separating
separating element
tube according
tube
separating tube
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
EP82100181A
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German (de)
English (en)
Other versions
EP0056609B1 (fr
EP0056609A3 (en
Inventor
Uwe Werner Dr. Ballies
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Individual
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Individual
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Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to AT82100181T priority Critical patent/ATE6993T1/de
Publication of EP0056609A2 publication Critical patent/EP0056609A2/fr
Publication of EP0056609A3 publication Critical patent/EP0056609A3/de
Application granted granted Critical
Publication of EP0056609B1 publication Critical patent/EP0056609B1/fr
Expired legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5021—Test tubes specially adapted for centrifugation purposes
    • B01L3/50215—Test tubes specially adapted for centrifugation purposes using a float to separate phases

Definitions

  • the invention relates to a separation tube for the centrifugal separation of a liquid containing at least two components, in which a separating element with a top and bottom surface is arranged, which consists of elastic material, preferably non-elastic plastic, the specific weight of which lies between those of the components to be separated and which In the idle state, the cross-section of the separating tube is blocked.
  • Such a separating tube is already known from DE-OS 27 11 336, in which an essentially cylindrical separating element made of polystyrene is arranged in a separating tube made of plastic.
  • the diameter of the separating tube widens somewhat due to compression, while the shape of the separating element made of hard plastic does not change.
  • This creates an annular gap between the separating element and the inner wall of the separating tube, so that the separating element is moved towards the bottom of the separating tube under the influence of the centrifugal force.
  • the lighter component enters through the annular gap into the space above the separating element, which is deposited on the heavier component.
  • the inner wall of the separating tube fits tightly against the Separating element and closes the annular gap, so that a. complete separation of the two components is achieved and maintained.
  • a disadvantage of the known separating tube is that it must not be made of a material that does not expand in the radial direction during centrifugation, so that glass tubes separate for this.
  • a separating tube of the type mentioned above which is characterized in that the center of gravity of the separating element is arranged eccentrically with respect to its axis and that the separating element can be tilted in the separating tube due to its shape only during centrifugation in such a way that a gap arises between the largest circumference of the separating element and the inner wall of the separating tube.
  • the separating element tilts in the separating tube during centrifuging and thus forms a gap through which the lighter component can pass from the underside of the separating element to the top thereof.
  • the separating element has the shape of an asymmetrical truncated cone, the largest diameter D 1 of which is twice as large as its smallest diameter D 2 , and a generatrix of the separating element which is perpendicular to both the largest diameter D 1 and the smallest diameter D 2 connects two diameters D 1 and D 2 .
  • a separating element is trapezoidal in cross section or in view.
  • the center of gravity of the separating element is eccentric with respect to the axis of the separating tube, so that the separating element is tilted during centrifugation in such a way that the center of gravity moves to the central axis M of the separating tube.
  • the separating element touches the inner wall of the separating tube with two diametrically opposite points and forms two crescent-shaped gaps for the passage of the component to be separated. A tilting over of the separating element is prevented by a point of the bottom surface touching the wall of the separating tube in an extreme position.
  • the separating element has the shape of a cylindrical section with a circular shape ger top surface, which runs perpendicular to the generatrix of the cylinder section and shuts off the diameter of the separating tube in the idle state.
  • the cylinder section has a smaller circumference than a semicircle, so that the separating element can tilt when centrifuging.
  • the underside of the top surface is preferably beveled toward the bottom surface of the separating element, so that no air remains trapped under the separating element.
  • a separating wall is provided on the underside of the free top surface, which has an edge which, when the separating element is in the rest position, runs at an angle to the wall of the separating tube. In an extreme position of the separating element, this edge of the dividing wall touches the wall of the separating tube and prevents a further tilting or rotating movement.
  • the separating element is conical with a spherical shell-shaped bottom surface, the height of the cone attached to the spherical shell surface being less than half the diameter of the separating tube. If the cone points upwards during centrifugation, the center of gravity lies above and has the largest diameter of the separating element thereby an unstable position so that it will turn around and bring the cone tip down.
  • the separating element is molded onto a piston rod via a predetermined breaking point, so that it can be used like a syringe piston before centrifuging.
  • the piston rod is broken off, for which purpose, in the case of a conical separating element, two annular beads arranged at a distance from one another are additionally formed on the inner wall of the separating tube, namely in the vicinity of its upper end. These ring beads form a counter bearing for breaking off the piston rod.
  • the wall of the separating tube forms this counter bearing.
  • the tilting or the rotational movement of the separating element is further supported by the fact that in particularly preferred embodiments at least one buoyancy chamber is provided, which includes air before centrifuging in the rest position of the separating element.
  • the buoyancy chamber is preferably arranged in a region diametrically opposite the center of gravity, so that the buoyancy force supports the action of the centrifugal force acting in the center of gravity during the rotation of the separating element.
  • the inclination of the buoyancy chamber wall is selected so that air can be enclosed in the idle state, but this completely exits the buoyancy chamber during centrifugation, so that after centrifugation there is no air in the area of the separating layer of the two components and adversely affects them.
  • a separating tube 2 is shown in the figures in a horizontal position, as is often used in centrifuges.
  • the separating tube 2 consists, for example, of plastic or glass and is initially closed with a sealing plug 4, a separating element 6 in the form of an asymmetrical body with an eccentric center of gravity S being attached to the underside of the sealing plug 4 via a connecting element 8.
  • the two components or phases to be separated are represented by lines or dots, the lines indicating the liquid phase and the dots indicating a heavier, for example solid phase, dispersed therein.
  • the connecting element 8 is, for example, an adhesive layer whose bond with the separating element 6 is broken up by the action of the centrifugal force.
  • the separating element 6 shown in FIGS. 1 to 9 has a circular top surface 7 and a likewise circular bottom surface 5, which lie in mutually parallel planes.
  • the circular top surface 7 has the same outside diameter D 1 as the inside diameter of the separating tube 2, while the diameter D 2 of the bottom surface 5 is half the size of the top surface diameter D 1 .
  • the distance between the bottom surface 5 and the top surface 7 corresponds to the height of the separating element 6, which has the shape of a rectangular trapezoid in section. 1, a generatrix of the separating element 6 lies against the wall of the separating tube 2, while the diametrically opposite generatrix, which connects the top surface 7 to the bottom surface 5, runs from the inner wall of the separating tube 2 to the separating tube axis M. Due to the shape of the separating element 6, its center of gravity S does not lie in the separating tube axis M, but is arranged eccentrically with respect to this by the amount e.
  • the separating element shown in FIG. 1 also has in its half opposite the center of gravity S at least one buoyancy chamber 10 which encloses air L in the idle state according to FIG. 1.
  • Fig. 2 shows the state which arises after a certain period of action of the centrifugal force, whereby has separated the separating element 6 from the connecting element 8 and the two phases have already been partially separated by the gap f between the separating element 6 and the tube wall by tilting the separating element.
  • This tilting or rotating of the separating element 6 is achieved in that, on the one hand, the centrifugal force acting in the center of gravity S tries to rotate the center of gravity S into the separating tube axis M.
  • the rotational movement is indicated by arrow A.
  • a buoyancy force acting in the buoyancy chamber 10 acts in the opposite direction to the action of the centrifugal force, so that a rotating twin is created which supports the rotational movement of the separating element 6 in the direction of arrow A.
  • the separating element 6 is supported on two diametrically opposite points on the inner wall of the separating tube 2, which lie on the circumference of the top surface 7 in the normal plane running through the separating tube axis M on the cutting or drawing plane.
  • the liquid phase passes the separating element 6, which slides in the direction of the tube bottom and finally floats on the heavier phase according to FIG it through knife of the separating tube 2 is blocked.
  • the air L enclosed in the buoyancy chamber 10 before centrifugation has completely escaped during centrifugation, so that in the end position according to FIG. 3 no force counteracts the restoring buoyancy force of the heavier phase. In addition, no air is trapped in the buoyancy chamber 10 which could adversely affect the heavier phase.
  • the separating element 6 can be made from any material, in particular plastic. It can be solid, hollow or filled with additional weights.
  • the buoyancy chamber 10 can be open towards the circumference of the separating element 6. In another embodiment, the buoyancy chamber is closed and contains granules as an additional buoyancy body.
  • a separating element made of glass-hard, light plastic, for example made of polystyrene is preferably used, which has a specific weight of-1.045, i.e. is lighter than the erythrocyte layer with a specific weight of-1.09 and somewhat heavier than the plasma - or serum layer, the specific weight of which is ⁇ 1.04 to 1.045.
  • Fig. 4 illustrates the effect and arrangement of the buoyancy chamber 10 based on five positions of the separation elements 6 during centrifugation, which are shown one above the other in a separating tube 2 for reasons of clarity.
  • a normal N is assumed on the separating tube 2 or on the separating tube axis M, with respect to which, on the one hand, the angle of the chamber wall inclination ⁇ IV and the surface inclination ⁇ IV is indicated.
  • the separating element 6 hangs on the sealing plug 4 by means of the connecting element 8. Its cover surface 7 is parallel to the normal N of the separating tube 2, so that the inclination of the cover surface ß I with respect to the normal N 0 0 is.
  • the buoyancy chamber 10 is filled with air L I. Furthermore, liquid W I is also partly located in the buoyancy chamber 10, specifically the position of the liquid level is determined by the upper right edge of the buoyancy chamber 10 in FIG. 41.
  • the buoyancy chamber 10 is shaped so that it can be demoulded to the right at an angle during the shaping. For this purpose, the chamber opening must have at least the same diameter as the rest of the chamber in order to be able to use an undivided molded body. In the case of a buoyancy chamber with a smaller chamber opening than the inner chamber diameter, it is necessary to use a divided molded body in the production of the separating element.
  • Fig. 4II shows the position of the separating element 6 after the start of centrifuging, a gap f II being formed by rotation in the direction of arrow A II .
  • this is a counter clockwise rotation.
  • Some of the air L II enclosed in the buoyancy chamber 10 can now escape through the gap f II , while liquid W II flows into the buoyancy chamber 10.
  • the chamber wall inclination ⁇ II is smaller than in Fig. 41, while the cover surface inclination ⁇ II has increased.
  • the separating element 6 is rotated by pivoting in the direction of arrow A III to such an extent that the inclination of the chamber wall has reached a negative range with respect to the normal N.
  • the liquid W III flowing into the buoyancy chamber 10 has displaced the entire air L III and the previous buoyancy due to the air L in the right half of the separating element 6 has been eliminated.
  • the surface inclination ⁇ III is greatest, while the chamber wall inclination ⁇ III has its greatest negative value of, for example, 5 to 20 °, preferably 10.
  • FIGS. 5 to 7 show the absolute position of the separating tube 2 in a centrifuge, the same parts again being provided with the same reference numerals.
  • FIG. 5 shows the suspended separating tube 2 before centrifuging, the axis of the centrifuge being designated C.
  • the speed of the centrifuge v 0.
  • FIG. 6 shows the separating tube 2 during centrifuging at rotational speeds v II-IV , which corresponds to the separating element positions II-IV in FIG. 4.
  • FIG. 7 shows the end position of the separating tube 2, which is reached at the highest centrifuging speed v V and which corresponds to the position of the separating element in FIG. 4V.
  • Fig. 8 shows a perspective view of the separating element 6, in which the top surface 7 with its diameter D1 and the bottom surface 5 with its diameter D 2 are clearly recognizable.
  • a predetermined breaking point 16 is formed in the center of the circular, flat cover surface 7, by means of which the separating element 6 connects to a piston rod 15 indicated in FIG. 9.
  • the separation tube axis M. passes the center of the circular bottom surface 5 with respect to the center of the top surface 7 to D 1/4 offset, that is to say half the radius of the top surface 7, so that in the top view, the bottom surface 5 extends from an edge of the top surface 7 to the predetermined breaking point 16 lying in its center. This results in the shape of a right-angled trapezoid, which can be seen in FIG. 9, with a generatrix running parallel to the wall of the separating tube 2.
  • the separating element 6 can also be used as a piston for sucking up blood, for which purpose it is molded onto a piston rod 15 via a predetermined breaking point 16. After the blood has been drawn up into the separating tube 2, which for this purpose is provided on its underside with a closable cannula cone 18, which is not shown in this figure, but can be seen in FIG. 10, the piston rod 15 is turned clockwise in FIG. 9 broken off, the separating element 6 being supported on the wall of the separating tube 2.
  • the separating element 6 ' also has at least one buoyancy chamber 10, which is shown in FIG. 10 by a partial section is recognizable.
  • the buoyancy chamber 10 is indicated by dashed lines in FIG. 11. 10 has on its bottom a cannula cone 18 through which blood or the liquid to be separated can be sucked.
  • the piston rod 15 is broken off in the manner described above and the separating tube 2 is closed on its upper side with an overlapping sealing plug 4'. Furthermore, the cannula cone 18 is likewise closed by a cover cap which is known per se but is omitted for reasons of clarity.
  • FIG. 11 shows the broken-off separating element 6 'in the starting position and the sealing plug 4', which is provided with a conical depression corresponding to the top surface 7 '.
  • FIGS. 12 and 13 show a further embodiment of the separating element, the same parts again being provided with the same reference symbols.
  • the modified separating element bears the reference symbol 6 ".
  • the separating element 6" has a circular cover surface 7, to which a cylinder section 11 is connected.
  • the circumference of the cylinder section 11 is shorter than half a circle, so that the greatest width of the cylinder section 11 is less than the diameter of the top surface 7 and thus the separation tube 2. This allows the separating element 6 "to be tilted in the separating tube 2, specifically counterclockwise in FIG. 13.
  • FIG. 13 shows the separating element 6 "in section, it being seen that the underside 9 of the top surface 7 extends inclined from the wall of the separating tube 2 to the bottom surface 5" of the separating element 6 "and an angle of, for example, 5 to 20 with the top surface 7 °, preferably 10 °.
  • air trapped under the top surface 7 can escape when the separating element 6 "is tilted from the underside 9 of the separating element 6" of the separating tube 2 ends and thus prevents the separating element 6 "from tipping over during centrifugation.
  • the separating element 6 "thus has approximately the outline shape of the separating element 6 shown in FIGS. 1 to 9.
  • the separating element 6" is in turn molded onto a piston rod 15 via a predetermined breaking point 16 and can be removed from it by kinking the piston rod 15 after being pulled up blood or the fluid to be separated.
  • This breaking off takes place in Fig. 13 by moving the piston rod 15 clockwise, so that the cylinder section 11 is supported on the wall of the separating tube 2 and forms a counter bearing.
  • FIGS. 14 to 16 show a further embodiment of the invention with a conical separating element 6 ′′ ′, the tip of which is in turn molded onto a breakable piston rod 15 via a predetermined breaking point 16.
  • the same parts are again provided with the same reference numerals in these figures
  • the separating element 6 "'thus has a conical top surface 7"', the largest outside diameter of which corresponds to the inside diameter of the separating tube 2.
  • the conical top surface 7 '" is followed by a curved bottom surface 5"', which in the embodiment shown is a spherical section
  • the largest diameter of the spherical section D 1 is indicated in dashed lines in FIG. 14 and corresponds to the inside diameter of the separating tube 2.
  • the height of the top surface cone from its base containing the diameter D 1 to the tip formed by the predetermined breaking point 16 is slightly less than half the inside diameter D 1 of the separation tube 2, so that the separation element 6 '"after breaking off of the piston rod 15 during centrifugation according to FIG.
  • At least one buoyancy chamber 10 ''' is also arranged eccentrically in the curved bottom surface 5'', so that the center of gravity S is again eccentric with respect to the separating tube axis M.
  • FIG. 15 shows the separating element 6"' which has tipped over after being broken off, with the curved base surface 5 "'now pointing upwards. Since the buoyancy chamber 10'" is also open at the top, there is no air locked in.
  • two ring beads 20 and 21 are provided at the upper end of the separating tube 2, which are spaced apart from one another in such a way that they clamp the separating element 6'" on the circumference.
  • the outer annular bead 20 is larger in the radial direction of the separating tube 2, so that pulling out of the separating element 6 '"from the separating tube 2 is substantially hindered.
  • the inner annular bead 21, on the other hand, is somewhat smaller, so that the separating element 6'" overlaps when pulled up can move this ring bead.
  • the two annular beads 20 and 21 form a counter bearing for the separating element 6 '"for breaking off the piston rod 15.
  • the separating element 6'" is in the position indicated by dash-dotted lines in FIG. 14.
  • the outer and inner annular beads 20 and 21 are arranged at one end of the separating tube 2, in which case a sealing plug which surrounds the separating tube 2 on the outside is selected.
  • a sealing plug which surrounds the separating tube 2 on the outside is selected.
  • the two annular beads are at a distance from the end of the separating tube, so that it can be closed by one of the sealing plugs 4 and 4 'shown in the previous figures.
  • FIG. 16 shows a perspective view of the conical separating element 6 '"broken off from the piston rod, the edge of the buoyancy chamber 10'" also being recognizable.
  • the separating element according to FIGS. 14 to 16 is a solid body without a buoyancy chamber, the turning or overturning of the separating element taking place solely due to its unstable position after the piston rod has broken off.
  • the separating element has approximately the shape according to FIG. 15, its top surface being curved and its bottom surface being conical.
  • the arched top surface is connected via a connecting element to a plug or via a connecting element before centrifuging a predetermined breaking point is formed on a piston rod.
  • This separating element with a curved top surface and a conical bottom surface can in turn also have one or more buoyancy chambers, from which the previously enclosed air can reliably escape during centrifugation. Appropriate embodiments for the buoyancy chambers are described with reference to Figures 1 to 11.
  • the separating element in a view triangular or trapezoidal in the case of a separating tube which is quadrilateral in cross-section, so that again the entire cross-section of the separating tube is shut off in the idle state, while the separating element is tilted and thus a gap is formed during centrifugation .

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Hematology (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Centrifugal Separators (AREA)
  • Measurement Of The Respiration, Hearing Ability, Form, And Blood Characteristics Of Living Organisms (AREA)
EP82100181A 1981-01-21 1982-01-13 Tube séparateur pour la séparation par centrifugation Expired EP0056609B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT82100181T ATE6993T1 (de) 1981-01-21 1982-01-13 Trennroehrchen fuer die zentrifugaltrennung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3101733 1981-01-21
DE3101733A DE3101733C2 (de) 1981-01-21 1981-01-21 Trennelement in einem Trennröhrchen zur Zentrifugaltrennung

Publications (3)

Publication Number Publication Date
EP0056609A2 true EP0056609A2 (fr) 1982-07-28
EP0056609A3 EP0056609A3 (en) 1982-12-08
EP0056609B1 EP0056609B1 (fr) 1984-04-11

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EP82100181A Expired EP0056609B1 (fr) 1981-01-21 1982-01-13 Tube séparateur pour la séparation par centrifugation

Country Status (4)

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US (1) US4364832A (fr)
EP (1) EP0056609B1 (fr)
AT (1) ATE6993T1 (fr)
DE (2) DE3101733C2 (fr)

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DE8910591U1 (de) * 1989-09-05 1989-12-21 Walter Sarstedt Geräte und Verbrauchsmaterial für Medizin und Wissenschaft, 5223 Nümbrecht Blutserumgewinnungsvorrichtung
DE4332189A1 (de) * 1993-09-22 1995-03-23 Braun Melsungen Ag Blutentnahmevorrichtung
US5575778A (en) * 1994-09-21 1996-11-19 B. Braun Melsungen Ag Blood-taking device
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US9757721B2 (en) 2015-05-11 2017-09-12 Biomet Biologics, Llc Cell washing plunger using centrifugal force

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DE4332189A1 (de) * 1993-09-22 1995-03-23 Braun Melsungen Ag Blutentnahmevorrichtung
EP0847726A1 (fr) 1993-09-22 1998-06-17 B. Braun Melsungen Ag Dispositif de prise de sang
US5575778A (en) * 1994-09-21 1996-11-19 B. Braun Melsungen Ag Blood-taking device
US9339741B2 (en) 2008-07-21 2016-05-17 Becton, Dickinson And Company Density phase separation device
CN104190487A (zh) * 2009-05-15 2014-12-10 贝克顿·迪金森公司 密度相分离装置
CN104190487B (zh) * 2009-05-15 2016-12-07 贝克顿·迪金森公司 密度相分离装置
US10343157B2 (en) 2009-05-15 2019-07-09 Becton, Dickinson And Company Density phase separation device
US10376879B2 (en) 2009-05-15 2019-08-13 Becton, Dickinson And Company Density phase separation device
US10413898B2 (en) 2009-05-15 2019-09-17 Becton, Dickinson And Company Density phase separation device
US10456782B2 (en) 2009-05-15 2019-10-29 Becton, Dickinson And Company Density phase separation device

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DE3260096D1 (en) 1984-05-17
ATE6993T1 (de) 1984-04-15
US4364832A (en) 1982-12-21
DE3101733A1 (de) 1982-08-05
EP0056609B1 (fr) 1984-04-11
DE3101733C2 (de) 1982-10-14
EP0056609A3 (en) 1982-12-08

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