EP0056609B1 - Tube séparateur pour la séparation par centrifugation - Google Patents

Tube séparateur pour la séparation par centrifugation Download PDF

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Publication number
EP0056609B1
EP0056609B1 EP82100181A EP82100181A EP0056609B1 EP 0056609 B1 EP0056609 B1 EP 0056609B1 EP 82100181 A EP82100181 A EP 82100181A EP 82100181 A EP82100181 A EP 82100181A EP 0056609 B1 EP0056609 B1 EP 0056609B1
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EP
European Patent Office
Prior art keywords
separating
separating tube
separating member
separating element
tube according
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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.)
Expired
Application number
EP82100181A
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German (de)
English (en)
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EP0056609A2 (fr
EP0056609A3 (en
Inventor
Uwe Werner Dr. Ballies
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Individual
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Individual
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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
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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 again lies closely against the separating element and closes the annular gap, so that a complete separation of the two components is achieved and is 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 which is characterized in that the center of gravity of the separating element is arranged eccentrically with respect to the separating tube axis in the idle state, and that the separating element can only be tilted in the separating tube due to its shape during centrifugation in such a way that there is a gap 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 get from the underside of the separating element to its upper side.
  • the separating element has the shape of an asymmetrical truncated cone, the largest diameter 0 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 0 1 and the smallest diameter D 2 connects both diameters 0 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 cover surface that runs perpendicular to the generating section of the cylindrical section and blocks 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 cover 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 the largest diameter of the separating element and this has an unstable position, so that it will turn around and bring the cone tip down.
  • the separating element is formed on 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 additional annular beads arranged at a distance from one another 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 rotary 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 it emerges entirely from the buoyancy chamber during centrifugation, so that after centrifugation there is no air in the region 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 0 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 that occurs after a certain time of action of the centrifugal force, wherein the separating element 6 has detached from the connecting element 8 and already a partial separation of the two phases through the gap f between the separating element 6 and the tube wall by tilting the separating element is done.
  • 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. 3 and is rotated back into the starting position by the buoyancy when immersed in the heavier phase, in which it blocks the diameter of the separation tube 2.
  • 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 on the basis of five positions of the separating element 6 during centrifuging, which are shown one above the other in a separating tube 2 for reasons of clarity.
  • a normal N to the separating tube 2 or to the separating tube axis M is assumed, with respect to which the angle of the chamber wall inclination ⁇ IV and the top surface inclination ⁇ IV is indicated.
  • the separating element 6 hangs on the plug 4 by means of the connecting element 8. Its cover surface 7 lies parallel to the normal N of the separating tube 2, so that the inclination of the cover surface ⁇ 1 with respect to the normal N 0 ° is.
  • the buoyancy chamber 10 is filled with air L. Furthermore, liquid W 1 is also partially 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 in such a way that it can be demolded to the right 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. 411 shows the position of the separating element 6 after the start of centrifuging, a gap f ll being formed by rotation in the direction of the arrow A ll . In Fig. 411, this is a counterclockwise rotation. Part of the air L ll enclosed in the buoyancy chamber 10 can now escape through the gap f ll , while liquid W ll flows into the buoyancy chamber 10.
  • the chamber wall inclination ⁇ ll is smaller than in FIG. 41, while the cover surface inclination ⁇ ll has increased.
  • the separating element 6 is rotated by pivoting in the direction of arrow A 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 flowing into the buoyancy chamber 10 has displaced all of the air L and the previous buoyancy through the air L in the right half of the separating element 6 has been eliminated.
  • the top 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. 6 shows the separation tube 2 during centrifugation at revolution speeds v,). jv , which corresponds to the separator 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 Vv 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 D 1 and the bottom surface 5 with its diameter D 2 can be clearly recognized.
  • 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 separating tube axis M runs through the center of the top surface 7 and thus also through the predetermined breaking point 16.
  • the center of the circular bottom surface 5 is offset by D i / 4 with respect to the center of the top surface 7, i.e. by 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 the suction of blood, for which purpose it is molded on 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 bent by turning it 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 can be seen in FIG. 10 by a partial section.
  • 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.
  • 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 of the separating 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 °.
  • a partition 12 is also provided under the free cover surface 7, the lower edge 13 of which is at a distance from the wall 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.
  • 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 ′, 6 ′′, the tip of which is in turn molded onto a breakable piston rod 15 via a predetermined breaking point 16.
  • the conical separating element 6 ', 6 "thus has a conical top surface 7', 7", the largest outside diameter of which corresponds to the inside diameter of the separating tube 2.
  • the conical top surface 7 ', 7 is followed by a curved bottom surface 5', 5", which is a spherical section in the embodiment shown.
  • the largest diameter of the spherical section is 0 1 indicated by dashed lines in Fig.
  • 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 inner diameter D 1 of the separation tube 2, so that the Separating element 6 ', 6 "after being broken off from the piston rod 15 during centrifugation according to FIG is also again eccentric with respect to the separating tube axis M.
  • air can be enclosed in the buoyancy chamber 10 ', 10 ", which assists the separating element 6', 6" from tipping over during centrifugation.
  • annular beads 20 and 21 are provided at the upper end of the separating tube 2, which are spaced from one another such that they clamp the separating element 6', 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 ', 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', 6 "when pulling up over this ring bead.
  • the two ring beads 20 and 21 form a counter bearing for the separating element .6 ', 6 "for breaking off the piston rod 15.
  • the separating element 6', 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 that surrounds the separating tube 2 on the outside is selected.
  • a sealing plug that 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 ', 6 "broken off from the piston rod, the edge of the buoyancy chamber 10', 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 curved top surface in one embodiment is connected to a sealing plug via a connecting element before centrifuging, or is molded onto a piston rod via a predetermined breaking point.
  • 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 the case of a separating tube which is quadrangular in cross section in a view, triangular or trapezoidal, so that again the entire cross section of the separating tube is shut off in the idle state, while during centrifuging the separating element is tilted and thus a gap is formed .

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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)

Claims (12)

1. Tube séparateur pour la séparation centrifuge d'un liquide contenant au moins deux composants, dans lequel est disposé un élément séparateur comportant une surface de recouvrement (7) et une surface de fond (5), qui se compose d'un matériau non élastique, de préférence une matière plastique non élastique dont le poids spécifique est compris entre ceux des composants à séparer et qui obture dans la condition de repos la section du tube séparateur, caractérisé en ce que, dans la condition de repos, le centre de gravité (S) de l'élément séparateur (6, 6', 6") est disposé excentriquement par rapport à l'axe (M) du tube séparateur et en ce que l'élément séparateur (6, 6', 6") peut être basculé, du fait de sa forme et seulement pendant la centrifugation, dans le tube séparateur (2) de telle sorte qu'il s'établisse un intervalle (f) entre la périphérie la plus grande (Di) de l'élément séparateur (6, 6', 6") et la paroi intérieure du tube séparateur (2).
2. Tube séparateur selon la revendication 1, caractérisé en ce que l'élément séparateur (6) a la forme d'un tronc de cône asymétrique dont le diamètre maximal (D1) a une dimension double de son diamètre minimal (D2) et en ce qu'une génératrice de l'élément séparateur (6) orientée perpendiculairement d'une part au diamètre maximal (D1) et d'autre part au diamètre minimal (D2) relie les deux diamètres (Di et D2) (figures 1-11
3. Tube séparateur selon la revendication 1, caractérisé en ce que l'élément séparateur (6") a la forme d'une partie de cylindre à surface de recouvrement de forme circulaire (7), en dessous de l'extrémité libre de laquelle il est prévu une paroi séparatrice (12) empêchant un basculement de l'élément séparateur (6") (figures 12 et 13).
4. Tube séparateur selon la revendication 3, caractérisé en ce que le côté inférieur (9) de la surface de recouvrement (7) est incliné depuis son extrémité libre jusqu'à la surface de fond (5") de l'élément séparateur (6") (figures 12 et 13).
5. Tube séparateur selon la revendication 1, caractérisé en ce que l'élément séparateur (6, 6") a la forme d'un cône à surface de fond arrondie (5', 5") (figures 14 à 16).
6. Tube séparateur selon l'une des revendications 1 ou 2, caractérisé en ce que l'élément séparateur (6, 6") comporte une surface de recouvrement de forme conique (7') (figures 10 et 11).
7. Tube séparateur selon l'une des revendications 1 à 6, caractérisé en ce que l'élément séparateur (6, 6', 6") est muni d'une zone de rupture imposée (16) sur une tige de piston (15).
8. Elément séparateur selon la revendication 7, caractérisé en ce que la zone de rupture de consigne (16) est disposée sur la surface de recouvrement plane (7) de l'élément séparateur (6) qui possède le diamètre maximal (D,) (figures 8-9 et 12-13).
9. Tube séparateur selon la revendication 7, caractérisé en ce que la zone de rupture imposée (16) est située au sommet de la surface de recouvrement de forme conique (7', 7") (figures 10-11 et 14-16).
10. Tube séparateur selon la revendication 5, caractérisé en ce que la zone de rupture imposée (16) est formée sur la surface de fond arrondie (5', 5").
11. Tube séparateur selon l'une des revendications 1 à 6, caractérisé en ce que l'élément séparateur (6, 6', 6") comporte au moins une chambre de sustentation disposée excentriquement (10).
12. Tube séparateur selon l'une des revendications 1 à 10, caractérisé en ce que l'élément séparateur (6, 6', 6") est formé de polystyrène.
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
DE3101733A DE3101733C2 (de) 1981-01-21 1981-01-21 Trennelement in einem Trennröhrchen zur Zentrifugaltrennung
DE3101733 1981-01-21

Publications (3)

Publication Number Publication Date
EP0056609A2 EP0056609A2 (fr) 1982-07-28
EP0056609A3 EP0056609A3 (en) 1982-12-08
EP0056609B1 true 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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DE3260096D1 (en) 1984-05-17
DE3101733C2 (de) 1982-10-14
EP0056609A2 (fr) 1982-07-28
EP0056609A3 (en) 1982-12-08
DE3101733A1 (de) 1982-08-05
ATE6993T1 (de) 1984-04-15
US4364832A (en) 1982-12-21

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