EP0322548A1 - Bottle stopper for freeze-drying - Google Patents

Bottle stopper for freeze-drying Download PDF

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Publication number
EP0322548A1
EP0322548A1 EP88118843A EP88118843A EP0322548A1 EP 0322548 A1 EP0322548 A1 EP 0322548A1 EP 88118843 A EP88118843 A EP 88118843A EP 88118843 A EP88118843 A EP 88118843A EP 0322548 A1 EP0322548 A1 EP 0322548A1
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EP
European Patent Office
Prior art keywords
pin
longitudinal axis
transverse plane
shank
section
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
EP88118843A
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German (de)
French (fr)
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EP0322548B1 (en
Inventor
Rik Schrooten
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Helvoet Pharma NV
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Helvoet Pharma NV
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Publication date
Application filed by Helvoet Pharma NV filed Critical Helvoet Pharma NV
Priority to AT88118843T priority Critical patent/ATE91470T1/en
Publication of EP0322548A1 publication Critical patent/EP0322548A1/en
Application granted granted Critical
Publication of EP0322548B1 publication Critical patent/EP0322548B1/en
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D39/00—Closures arranged within necks or pouring openings or in discharge apertures, e.g. stoppers
    • B65D39/0005—Closures arranged within necks or pouring openings or in discharge apertures, e.g. stoppers made in one piece
    • B65D39/0023—Plastic cap-shaped hollow plugs
    • 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
    • B01L3/508—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above
    • B01L3/5082—Test tubes per se
    • B01L3/50825—Closing or opening means, corks, bungs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D51/00—Closures not otherwise provided for
    • B65D51/002—Closures to be pierced by an extracting-device for the contents and fixed on the container by separate retaining means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D51/00—Closures not otherwise provided for
    • B65D51/24—Closures not otherwise provided for combined or co-operating with auxiliary devices for non-closing purposes
    • B65D51/241—Closures not otherwise provided for combined or co-operating with auxiliary devices for non-closing purposes provided with freeze-drying means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D2539/00—Details relating to closures arranged within necks or pouring openings or in discharge apertures, e.g. stoppers
    • B65D2539/001—Details of closures arranged within necks or pouring opening or in discharge apertures, e.g. stoppers
    • B65D2539/005—Details of closures arranged within necks or pouring opening or in discharge apertures, e.g. stoppers provided with slits or gaps for increasing the elasticity

Definitions

  • the invention relates to a freeze-drying stopper made of rubber-elastic material, consisting of a spigot intended for insertion into the container neck to be sealed and a flange which is formed integrally with the spigot and protrudes radially above said essentially circular disk, the longitudinal axis of which flange coincides with that of the spigot, which spigot contains a cavity surrounding the pin longitudinal axis, which is open to the free pin end face and extends to a central closed wall part of the flange, the pin containing a first portion of its axial length, which extends radially between one of the pins and the pin extends outwardly projecting boundary surface of the flange and a second transverse plane perpendicular to the pin longitudinal axis and has a closed outer circumferential surface, the maximum diameter of which is slightly larger than the inside diameter of the container neck and adjusts itself contains the second section adjoining the second section, the outer envelope surface of which has essentially the same diameter as the first section and which contains at
  • freeze-drying stopper of this type the spigot is designed over practically its entire length as an essentially tubular body with an almost constant wall thickness, i. H. the laterally delimiting inner wall surface of its central cavity is approximately a cylindrical surface.
  • freeze-drying stoppers in which only the first section of the axial length of the journal adjacent to the flange has the shape of a tubular body, a plurality of pins projecting from one another at the end of this body, the axes of which are parallel to the journal. Longitudinal axis are directed, the diameter of which approximately corresponds to the wall thickness of the body and from each of which protrudes a retractable or disengageable by bending the pin locking element.
  • Frozen food (in particular a medicament), which is contained in a container and is sealed with one of the plugs explained above, is usually removed by piercing the flange of the plug with a cannula and introducing liquid into the container and the solution or suspension with the stopper held down with the cannula. If the cannula is not positioned exactly in the center of the flange and practically parallel to the longitudinal axis of the plug pushed in, there is a risk that the cannula tip hits the inner side wall surface, which can clog the cannula or punch out particles from the material of the pin. It is also disadvantageous that, of the known plugs, a considerable residual volume of solution or suspension that cannot be removed with the cannula remains in the container.
  • the object of the invention is to develop a freeze-drying stopper of the type mentioned in such a way that the possibility of the cannula tip hitting the lateral inner wall surface is greatly reduced or less care is required when puncturing the cannula and that other requirements are also met to a freeze-drying stopper, in particular with regard to low residual volume, inexpensive manufacture, adequate tightness and easy handling in the course of the freeze-drying process.
  • the inner wall surface laterally delimiting the cavity lies completely outside a cone, the axis of which is the longitudinal axis of the pin, the tip of which lies in the first plane and the tip angle in degrees is greater than one according to the formula -39 + 75 x lg (D) is calculated value, where in the formula "lg” means the decimal logarithm and "D" the maximum diameter of the first section of the pin measured in millimeters.
  • the inner wall surface of the central wall part of the flange, which axially delimits the cavity is essentially flat in a surface area surrounding the longitudinal axis of the journal, and this area lies in a transverse plane perpendicular to the longitudinal axis of the journal, which is close to the first Transverse plane runs, the inner wall surface laterally delimiting the cavity starting from the surface area surrounding the longitudinal axis of the pin and increasing in diameter as the free end face of the pin approaches.
  • the area of the outer surface of the central wall part of the flange which surrounds the longitudinal axis of the plug is advantageously delimited from the remaining peripheral surface area by a circular arrangement of projections which is concentric with the longitudinal axis of the plug, thereby marking the puncture site for the cannula and in connection with the design according to the invention the inner wall surface of the pin an even greater safety in handling is achieved.
  • the freeze-drying stopper is shown in FIGS. 1 to 4 in a magnification of approximately 5 times. It consists of rubber and contains a pin 1 intended for insertion into the container neck to be closed and a flange 2 formed therewith in one piece.
  • the pin 1 has, in addition to its special design which will be explained in the following, in principle the shape of a hollow cylinder which delimits a cavity 4 which is open to the free pin end face 3.
  • the flange 2 has an edge 2a projecting laterally beyond the pin 1, on which a lower edge extends radially outward from the pin kende plane annular boundary surface 5 is formed.
  • This boundary surface lies in a first transverse plane Q 1 penetrated perpendicularly by the longitudinal axis A of the pin, is intended for bearing against the end face of the neck of the container and limits the insertion depth of the pin in its closed position.
  • the closed central wall part 2b of the flange 2 delimits the cavity 4 axially with an inner wall surface 6 which is flat in a surface area surrounding the journal longitudinal axis A and lies in a transverse plane P which runs at a short distance from the first transverse plane Q 1.
  • the outer surface 7 of the flange 2 facing away from the peg 1 has two projections 8 each running approximately semicircularly, the diameter of which is small with respect to the outer diameter of the flange and which mark a surface area surrounding the longitudinal axis A of the pin intended for the puncture of a withdrawal cannula. From the surface area of the outer surface 7 surrounding the projections 8, further projections 9 extend radially to the longitudinal axis A of the pin and at equal angular intervals, which prevent freeze-drying stoppers lying against one another with their outer surfaces from adhering to one another or to other objects and thereby hinder their processing.
  • the pin 1 In a first section Z1 of its axial length, which is located between the first transverse plane Q1 and a perpendicular to the longitudinal axis A, the pin length in a rough approximation centrally dividing second transverse plane Q2, the pin 1 is of full-walled design, ie it has a closed outer upper peripheral surface 10a.
  • This peripheral surface is adjacent to the first transverse plane Q 1 narrow and flat annular recess 10 'and an adjoining, axially longer cylindrical surface is formed, the latter having a diameter D which is slightly larger than the inner diameter of the neck of the container and rests sealingly against the container neck when the plug is fully inserted under elastic prestress.
  • a second section Z2 of the axial length of the pin 1, which extends from the second transverse plane Q2 to the free pin end face 3, has an outer cylindrical envelope surface 10b, which has essentially the same diameter D as the upper peripheral surface 10a.
  • the passage 11 has the shape of a slot and contains two side surfaces 12a, 12b, which are substantially flat, run almost parallel to the longitudinal axis A of the pin, widen from the cavity 4 to the mouth 13 and have a mutual mean distance which is approximately the middle Corresponds to the diameter of the cavity.
  • a first inner part 12c bottom surface of the passage 11 lies in a plane parallel to the second transverse plane Q2 and in this respect offset by a small distance to the end face 3 of the pin.
  • the inner part 12c is followed by an outer part 12d of the bottom surface shaped in the form of a sector of a truncated cone, which passes into the peripheral surface 10b with an edge which forms part of the mouth 13 and is located in the second transverse plane Q2.
  • the axially outer (ie adjacent to the pin face) 15 all lie on a common third transverse plane Q3, which is perpendicular to the longitudinal axis of the pin A runs and is located approximately in the middle between the second transverse plane Q2 and the pin end face 3.
  • cams 14a-14c When the pin 1 is inserted into the container neck, these cams 14a-14c cause an inhibition by the abutment of their delimitations 15 on the end face of the container neck and define a first position of the stopper in which it is already non-positively connected by elastic deformation of the pin part adjacent to the end face of the pin is held in the neck of the container, but the inside of the container is still open to the environment via the passage 11. Vapors and gases can therefore escape from the material contained in the container during freeze drying to and around the container.
  • the cams 14a-14c are pushed back by increased application of force to the plug, the cams themselves and the material of the pin 1 surrounding them being deformed.
  • the pin can then be inserted into the container neck up to a second position (closed position), which is defined by contact of the boundary surface 5 of the flange 2 on the end face of the container neck and in which the first section Z 1 of the pin equipped with the closed upper peripheral surface 10 a a complete seal of the container neck causes.
  • the cams 14a-14c each have the shape of semi-circular elongated beads in cross-section, which extend in the circumferential direction of the pin 1, their length in this direction in each case being at least 2.5 times their axial extension.
  • a first cam 14a is arranged diametrically opposite the passage (slot) 11, such that its center lies in a first longitudinal plane L1, which contains the longitudinal axis A of the pin and passes through the middle between the side surfaces 12a, 12b of the passage 11.
  • the centers of the other two cams 14b, 14c are defined by a second longitudinal plane L2 or third longitudinal plane L3, which contain the pin longitudinal axis A containing on different sides of the first longitudinal plane L1 and with this each have the same angle ⁇ 2 or ⁇ 3 of Include approx. 110 ° (old degree).
  • a groove 16 is arranged such that its inner (i.e. adjacent to the flange 2) side wall lies in the third transverse plane Q3.
  • the groove 16 is followed by a peripheral surface 17 of the pin 1, the diameter of which is slightly larger than the diameter of the peripheral surface from which the cams 14a-14c project.
  • the peripheral surface closes via one of the easier insertion of the pin 1 into the container neck conical surface 18 on the pin end face.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Hematology (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Closures For Containers (AREA)
  • Medical Preparation Storing Or Oral Administration Devices (AREA)
  • Infusion, Injection, And Reservoir Apparatuses (AREA)
  • Prostheses (AREA)

Abstract

A lyophilization stopper made of a rubber elastic material is composed of a shank (1) and a circular disc shaped flange (2) made in one piece with the shank. The shank includes a cavity (4) which surrounds the longitudinal axis (A) of the shank and is open toward the free end face (3) of the shank, while extending toward a central closed wall portion (2b) of the flange. A first section (Z1) of the shank disposed between a first transverse plane (Q1) and a second transverse plane (Q2) has a closed outer circumferential face which has a maximum diameter (D). A subsequent second section (Z2) includes a passage which communicates with the cavity as well as a plurality of projecting blocking elements (14a-14c). The inner wall surface (19) which laterally delimits the cavity (4) and has an increasing diameter with increasing approach to the free shank end face lies completely outside a cone (K) whose axis is the longitudinal axis (A) of the shank, whose tip (K1) lies in the transverse plane (Q1) and whose tip angle ( beta ), in degrees, is larger than a value calculated according to the formula -39+75xlg (D), where "D" is the maximum diameter (D) of the first section (Z1) measured in millimeters. In this way, a particularly utilitarian stopper is obtained which does not interfere with the insertion of the hollow extraction needle.

Description

Die Erfindung betrifft einen Gefriertrocknungs-Stopfen aus gummielasti­schem Material, bestehend aus einem zur Einführung in den abzudichtenden Behälterhals bestimmten Zapfen und einem einstückig mit dem Zapfen aus­gebildeten und radial über diesen vorstehenden, im wesentlichen kreis­scheibenförmigen Flansch, dessen Längsachse mit derjenigen des Zapfens zusammenfällt, welcher Zapfen einen die Zapfen-Längsachse umgebenden Hohlraum enthält, der zur freien Zapfen-Stirnseite offen ist und sich bis zu einem zentralen geschlossenen Wandungsteil des Flansches er­streckt, wobei der Zapfen einen ersten Abschnitt seiner axialen Länge enthält, der sich zwischen einer durch die vom Zapfen radial nach außen­vorspringenden Begrenzungsfläche des Flansches gelegte erste Querebene und einer zur Zapfen-Längsachse lotrechten zweiten Querebene erstreckt und eine geschlossene äußere Umfangsfläche aufweist, deren maximaler Durchmesser geringfügig größer als der Behälterhals-Innendurchmesser ist und einen sich an den ersten Abschnitt anschließenden zweiten Abschnitt enthält, dessen äußere Hüllfläche im wesentlichen den gleichen Durchmes­ser wie der erste Abschnitt aufweist und der wenigstens einen mit dem Hohlraum kommunizierenden Durchlaß enthält, welcher sich von der Zapfen-­Stirnseite bis zu einer im zweiten abschnitt gelegenen, an die zweite Querebene angrenzende radiale Öffnung erstreckt, und wobei vom zweiten Abschnitt nach außen über Hüllfläche mehrere, durch elastische Ver­formung zurückdrängbare Hemmelemente vorstehen, deren axial äußere Be­grenzungen auf einer gemeinsamen, zur Zapfen-Längsachse lotrechten, zwischen der zweiten Querebene und der freien Zapfen-Stirnsteite gele­genen, zur Zapfen-Längsachse lotrechten dritten Querebene liegen.The invention relates to a freeze-drying stopper made of rubber-elastic material, consisting of a spigot intended for insertion into the container neck to be sealed and a flange which is formed integrally with the spigot and protrudes radially above said essentially circular disk, the longitudinal axis of which flange coincides with that of the spigot, which spigot contains a cavity surrounding the pin longitudinal axis, which is open to the free pin end face and extends to a central closed wall part of the flange, the pin containing a first portion of its axial length, which extends radially between one of the pins and the pin extends outwardly projecting boundary surface of the flange and a second transverse plane perpendicular to the pin longitudinal axis and has a closed outer circumferential surface, the maximum diameter of which is slightly larger than the inside diameter of the container neck and adjusts itself contains the second section adjoining the second section, the outer envelope surface of which has essentially the same diameter as the first section and which contains at least one passage which communicates with the cavity and which extends from the end face of the pin to one located in the second section to the second Transverse plane adjacent radial opening extends, and being from the second Section protruding outward beyond the envelope surface a plurality of restraining elements which can be pushed back by elastic deformation, the axially outer boundaries of which lie on a common third transverse plane perpendicular to the longitudinal axis of the journal, between the second transverse plane and the free front side of the journal and perpendicular to the longitudinal axis of the journal.

Bei einem bekannten derartigen Gefriertrocknungs-Stopfen ist der Zapfen über praktisch seine ganz Länge als im wesentlichen rohrförmiger Körper mit nahezu konstanter Wanddicke ausgebildet, d. h. die seitlich begren­zende Innen-Wandfläche seines zentralen Hohlraums ist angenähert eine Zylinderfläche. Bekannt sind ferner Gefriertrocknungs-Stopfen, bei denen nur der an den Flansch angrenzende erste Abschnitt der axialen Länge des Zapfens die Form eines rohrförmigen Körpers aufweist, wobei von der Stirnseite dieses Körpers eine Mehrzahl von Stiften mit gegenseitgem Ab­stand vorsteht, deren Achsen parallel zur Zapfen-Längsachse gerichtet sind, deren Durchmesser näherungsweise der Wanddicke des Körpers ent­spricht und von denen jeweils ein zurückdrängbares bzw. durch Verbiegung des Stiftes außer Eingriff bringbares Hemmelement vorsteht.In a known freeze-drying stopper of this type, the spigot is designed over practically its entire length as an essentially tubular body with an almost constant wall thickness, i. H. the laterally delimiting inner wall surface of its central cavity is approximately a cylindrical surface. Also known are freeze-drying stoppers, in which only the first section of the axial length of the journal adjacent to the flange has the shape of a tubular body, a plurality of pins projecting from one another at the end of this body, the axes of which are parallel to the journal. Longitudinal axis are directed, the diameter of which approximately corresponds to the wall thickness of the body and from each of which protrudes a retractable or disengageable by bending the pin locking element.

Gefriergut (insbesondere ein Medikament), welches in einem Gefäß enthal­ten und mit einem der vorstehend erläuterten Stopfen verschlossen ist, wird in der Regel dadurch entnommen, daß der Flansch des Stopfens mit einer Kanüle durchstochen und Flüssigkeit in das Gefäß eingebracht und die Lösung bzw. Suspension bei nach unten gehaltenem Stopfen mit der Kanüle entnommen wird. Wird die Kanüle nicht genau zentrisch in der Mit­te des Flansches angesetzt und praktisch parallel zur Zapfen-Längsachse eingestoßen, besteht die Gefahr, daß die Kanülenspitze auf die seit­liche Innen-Wandfläche auftrifft, wobei sich die Kanüle verstopfen kann oder Partikel vom Material des Zapfens ausstanzt. Nachteilig ist auch, daß von den bekannten Stopfen ein beachtliches Restvolumen von mit der Kanüle nicht entnehmbarer Lösung bzw. Suspension im Behälter verbleibt.Frozen food (in particular a medicament), which is contained in a container and is sealed with one of the plugs explained above, is usually removed by piercing the flange of the plug with a cannula and introducing liquid into the container and the solution or suspension with the stopper held down with the cannula. If the cannula is not positioned exactly in the center of the flange and practically parallel to the longitudinal axis of the plug pushed in, there is a risk that the cannula tip hits the inner side wall surface, which can clog the cannula or punch out particles from the material of the pin. It is also disadvantageous that, of the known plugs, a considerable residual volume of solution or suspension that cannot be removed with the cannula remains in the container.

Aufgabe der Erfindung ist es, einen Gefriertrocknungs-Stopfen der ein­gangs genannten Art so weiter zu bilden, daß die Möglichkeit des Auf­treffens der Kanülenspitze auf die seitliche Innenwand-Fläche stark re­duziert wird bzw. geringere Sorgfalt beim Einstich der Kanüle aufzuwen­den ist und daß auch sonstige Anforderungen an einen Gefriertrocknungs-­Stopfen erfüllt werden, insbesondere hinsichtlich geringem Restvolumen, preisgünstiger Herstellung, ausreichender Dichtigkeit und einfacher Handhabbarkeit im Zuge des Gefriertrocknungs-Vorganges. Diese Aufgabe wird erfindungsgemäß dadurch gelöst, daß die den Hohlraum seitlich be­grenzende Innen-Wandfläche vollständig außerhalb eines Kegels liegt, dessen Achse die Zapfen-Längsachse ist, dessen Spitze in der ersten Ebene liegt und dessen Spitzenwinkel in Altgrad größer ist als ein nach der Formel
-39 + 75 x lg (D)
berechneter Wert ist, wobei in der Formel "lg" den dekadischen Logarith­mus und "D" den in Millimetern gemessenen maximalen Durchmesser des ersten Abschnittes des Zapfens bedeutet.The object of the invention is to develop a freeze-drying stopper of the type mentioned in such a way that the possibility of the cannula tip hitting the lateral inner wall surface is greatly reduced or less care is required when puncturing the cannula and that other requirements are also met to a freeze-drying stopper, in particular with regard to low residual volume, inexpensive manufacture, adequate tightness and easy handling in the course of the freeze-drying process. This object is achieved in that the inner wall surface laterally delimiting the cavity lies completely outside a cone, the axis of which is the longitudinal axis of the pin, the tip of which lies in the first plane and the tip angle in degrees is greater than one according to the formula
-39 + 75 x lg (D)
is calculated value, where in the formula "lg" means the decimal logarithm and "D" the maximum diameter of the first section of the pin measured in millimeters.

Gemäß einer bevorzugten Ausgestaltung der Erfindung ist die den Hohlraum axial begrenzende Innen-Wandfläche des zentralen Wandungsteiles des Flansches in einem die Zapfen-Längsachse umgebenden Flächenbereich im wesentlichen eben ausgebildet und wobei dieser Flächenbereich in einer zur Zapfen-Längsachse lotrechten Querebene liegt, welche nahe der ersten Querebene verläuft, wobei die den Hohlraum seitlich begrenzende Innen-Wandfläche von dem die Zapfen-Längsachse umgebenden Flächenbereich ausgeht und mit zunehmender Annäherung an die freie Zapfen-Stirnseite ihren Durchmesser vergrößert.According to a preferred embodiment of the invention, the inner wall surface of the central wall part of the flange, which axially delimits the cavity, is essentially flat in a surface area surrounding the longitudinal axis of the journal, and this area lies in a transverse plane perpendicular to the longitudinal axis of the journal, which is close to the first Transverse plane runs, the inner wall surface laterally delimiting the cavity starting from the surface area surrounding the longitudinal axis of the pin and increasing in diameter as the free end face of the pin approaches.

Vorteilhaft ist der die Zapfen-Längsachse umgebende Flächenbereich der Aussenfläche des zentralen Wandungsteiles des Flansches von dem restlichen peripheren Flächenbereich durch eine kreisförmige, zur Zapfen-Längsachse konzentrische Anordnung von Vorsprüngen abge­grenzt, wodurch die Einstichstelle für die Kanüle markiert wird und in Verbindung mit der erfindungsgemäßen Ausbildung der Innen-­Wandfläche des Zapfens eine noch größere Sicherheit bei der Hand­habung erreicht wird.The area of the outer surface of the central wall part of the flange which surrounds the longitudinal axis of the plug is advantageously delimited from the remaining peripheral surface area by a circular arrangement of projections which is concentric with the longitudinal axis of the plug, thereby marking the puncture site for the cannula and in connection with the design according to the invention the inner wall surface of the pin an even greater safety in handling is achieved.

Weitere Merkmale und Vorteile der Erfindung ergeben sich aus den Ansprüchen und der nachstehenden, nicht beschränkenden Erläuterung eines Ausführungsbeispieles der Erfindung anhand der Zeichnungen. In den Zeichnungen zeigt:

  • Fig. 1 in vergrößertem Maßstab eine Draufsicht auf die Ober­seite eines Gefriertrocknungs-Stopfens;
  • Fig. 2 in vergrößertem Maßstab eine Seitenansicht des Gefrier­trocknungs-Stopfens, teilweise im Schnitt gemäß der Linie II-II in Fig. 1;
  • Fig. 3 in vergrößertem Maßstab eine andere Seitenansicht des Gefriertrocknungs-Stopfens, teilweise im Schnitt gemäß der Linie III-III in Fig. 1 und
  • Fig. 4 in vergrößertem Maßstab eine Draufsicht auf die Unter­seite des Gefriertrocknungs-Stopfens.
Further features and advantages of the invention result from the claims and the following, non-limiting explanation of an embodiment of the invention with reference to the drawings. In the drawings:
  • Figure 1 is an enlarged plan view of the top of a freeze-drying plug.
  • Figure 2 is an enlarged side view of the freeze-drying plug, partly in section along the line II-II in Fig. 1.
  • Fig. 3 in an enlarged scale another side view of the freeze-drying plug, partly in section along the line III-III in Fig. 1 and
  • Fig. 4 in an enlarged scale a top view of the underside of the freeze-drying plug.

Der Gefriertrocknungs-Stopfen ist in den Figuren 1 bis 4 in ca. 5-­facher Vergrößerung dargestellt. Er besteht aus Gummi und enthält einen für die Einführung in den zu verschließenden Behälterhals bestimmten Zapfen 1 und einen damit einstückig ausgebildeten Flansch 2. Der Zapfen 1 hat, abgesehen von seiner in der Folge noch erläuterten speziellen Ausbildung, im Prinzip die Form eines Hohlzylinders, der einen zur freien Zapfen-Stirnseite 3 offenen Hohlraum 4 umgrenzt.The freeze-drying stopper is shown in FIGS. 1 to 4 in a magnification of approximately 5 times. It consists of rubber and contains a pin 1 intended for insertion into the container neck to be closed and a flange 2 formed therewith in one piece. The pin 1 has, in addition to its special design which will be explained in the following, in principle the shape of a hollow cylinder which delimits a cavity 4 which is open to the free pin end face 3.

Der Flansch 2 weist einen seitlich über den Zapfen 1 vorstehenden Rand 2a auf, an dem eine untere, sich radial vom Zapfen nach außen erstrek­ kende plane ringförmige Begrenzungsfläche 5 ausgebildet ist. Diese Begrenzungsfläche liegt in einer von der Zapfen-Längsachse A lotrecht durchdrungenen ersten Querebene Q₁, ist zur Anlage an der Stirnfläche des Behälterhalses bestimmt und begrenzt die Einstecktiefe des Zapfens in dessen Verschlußposition. Der geschlossene zentrale Wandungsteil 2b des Flansches 2 begrenzt den Hohlraum 4 axial mit einer Innen-Wandfläche 6, die in einem die Zapfen-Längsachse A umgebenden Flächenbereich eben ist und in einer Querebene P liegt, welche in geringem Abstand zur er­sten Querebene Q₁ verläuft. Die vom Zapfen 1 abgekehrte Außenfläche 7 des Flansches 2 weist zwei jeweils angenähert halbkreisförmig verlau­fende Vorsprünge 8 auf, deren Durchmesser klein bezüglich des Außen­durchmessers des Flansches ist und die einen die Zapfen-Längsachse A umgebenden, für den Einstich einer Entnahmekanüle bestimmten Flächen­bereich markieren. Von dem die Vorsprünge 8 umgebenden Flächenbereich der Außenfläche 7 stehen radial zur Zapfen-Längsachse A und unter gleichen Winkelabständen verlaufende weitere Vorsprünge 9 vor, welche verhindern, daß mit ihren Außenflächen aneinanderliegende Gefriertrock­nungs-Stopfen aneinander oder an anderen Gegenständen haften und da­durch ihre Verarbeitung behindern.The flange 2 has an edge 2a projecting laterally beyond the pin 1, on which a lower edge extends radially outward from the pin kende plane annular boundary surface 5 is formed. This boundary surface lies in a first transverse plane Q 1 penetrated perpendicularly by the longitudinal axis A of the pin, is intended for bearing against the end face of the neck of the container and limits the insertion depth of the pin in its closed position. The closed central wall part 2b of the flange 2 delimits the cavity 4 axially with an inner wall surface 6 which is flat in a surface area surrounding the journal longitudinal axis A and lies in a transverse plane P which runs at a short distance from the first transverse plane Q 1. The outer surface 7 of the flange 2 facing away from the peg 1 has two projections 8 each running approximately semicircularly, the diameter of which is small with respect to the outer diameter of the flange and which mark a surface area surrounding the longitudinal axis A of the pin intended for the puncture of a withdrawal cannula. From the surface area of the outer surface 7 surrounding the projections 8, further projections 9 extend radially to the longitudinal axis A of the pin and at equal angular intervals, which prevent freeze-drying stoppers lying against one another with their outer surfaces from adhering to one another or to other objects and thereby hinder their processing.

In einem ersten abschnitt Z₁ seiner axialen Länge, welcher sich zwi­schen der ersten Querebene Q₁ und einer zur Zapfenlängsachse A lot­rechten, die Zapfenlänge in grober Näherung mittig teilenden zweiten Querebene Q₂ befindet, ist der Zapfen 1 vollwandig ausgebildet, d. h. er weist eine geschlossene äußere obere Umfangsfläche 10a auf. Diese Umfangsfläche ist von einer an die erste Querebene Q₁ angrenzenden schmalen und flachen ringförmigen Vertiefung 10′ und einer sich daran anschließenden, axial längeren Zylinderfläche gebildet, wobei letztere einen Durchmesser D aufweist, der etwas größer als der Innendurchmesser des Behälterhalses ist und bei vollständig eingeführtem Stopfen unter elastischer Vorspannung dichtend am Behälterhals anliegt.In a first section Z₁ of its axial length, which is located between the first transverse plane Q₁ and a perpendicular to the longitudinal axis A, the pin length in a rough approximation centrally dividing second transverse plane Q₂, the pin 1 is of full-walled design, ie it has a closed outer upper peripheral surface 10a. This peripheral surface is adjacent to the first transverse plane Q 1 narrow and flat annular recess 10 'and an adjoining, axially longer cylindrical surface is formed, the latter having a diameter D which is slightly larger than the inner diameter of the neck of the container and rests sealingly against the container neck when the plug is fully inserted under elastic prestress.

Ein zweiter Abschnitt Z₂ der axialen Länge des Zapfens 1, der von der zweiten Querebene Q₂ bis zur freien Zapfen-Stirnseite 3 reicht, weist eine äußere zylindrische Hüllfläche 10b auf, welche im wesent­lichen den gleichen Durchmesser D wie die obere Umfangsfläche 10a besitzt. Durch den zweiten Abschnitt Z₂ erstreckt sich ein Durch­laß 11 vom Hohlraum 4 zu einer in der Abwicklung im wesentlichen rechteckigen Mündung 13 an der Hüllfläche (Umfangsfläche) 10b. Der Durchlaß 11 hat die Form eines Schlitzes und enthält zwei Seiten­flächen 12a, 12b, welche im wesentlichen eben sind, zur Zapfen-­Längsachse A nahezu parallel verlaufen, sich vom Hohlraum 4 zur Mündung 13 erweitern und einen gegenseitigen mittleren Abstand ha­ben, der näherungsweise dem mittleren Durchmesser des Hohlraumes entspricht. Ein erster innerer Teil 12c Bodenfläche des Durch­lasses 11 liegt in einer zur zweiten Querebene Q₂ parallelen und diesbezüglich um eine geringe Strecke zur Zapfen-Stirnseite 3 ver­setzten Ebene. An dem inneren Teil 12c schließt sich ein in Form eines Sektors eines Kegelstumpfes geformter äußerer Teil 12d der Bodenfläche an, welcher mit einer in der zweiten Querebene Q₂ ge­legenen, einen Bestandteil der Mündung 13 bildenden Kante in die Umfangsfläche 10b übergeht.A second section Z₂ of the axial length of the pin 1, which extends from the second transverse plane Q₂ to the free pin end face 3, has an outer cylindrical envelope surface 10b, which has essentially the same diameter D as the upper peripheral surface 10a. Through the second section Z₂ extends a passage 11 from the cavity 4 to a substantially rectangular opening 13 in the development on the envelope surface (peripheral surface) 10b. The passage 11 has the shape of a slot and contains two side surfaces 12a, 12b, which are substantially flat, run almost parallel to the longitudinal axis A of the pin, widen from the cavity 4 to the mouth 13 and have a mutual mean distance which is approximately the middle Corresponds to the diameter of the cavity. A first inner part 12c bottom surface of the passage 11 lies in a plane parallel to the second transverse plane Q₂ and in this respect offset by a small distance to the end face 3 of the pin. The inner part 12c is followed by an outer part 12d of the bottom surface shaped in the form of a sector of a truncated cone, which passes into the peripheral surface 10b with an edge which forms part of the mouth 13 and is located in the second transverse plane Q₂.

Von der Umfangsfläche 10b des zweiten Abschnitts Z₂ des Zapfens springen nach außen drei einstückig angeformte Nocken 14a - 14c vor, deren axial äußere (d. h. der Zapfen-Stirnseite benachbarte) Begrenzungen 15 alle auf einer gemeinsamen dritten Querebene Q₃ liegen, welche lotrecht zur Zapfen-Längsachse A verläuft und nähe­rungsweise in der Mitte zwischen der zweiten Querebene Q₂ und der Zapfen-Stirnseite 3 gelegen ist.From the peripheral surface 10b of the second section Z₂ of the pin jump out three integrally molded cams 14a - 14c, the axially outer (ie adjacent to the pin face) 15 all lie on a common third transverse plane Q₃, which is perpendicular to the longitudinal axis of the pin A runs and is located approximately in the middle between the second transverse plane Q₂ and the pin end face 3.

Beim Einführen des Zapfens 1 in den Behälterhals bewirken diese Nocken 14a - 14c durch Anlage ihrer Begrenzungen 15 an der Stirn­fläche des Behälterhalses eine Hemmung und definieren eine erste Position des Stopfens, in welcher dieser bereits durch elastische Verformung des an die Zapfen-Stirnseite angrenzenden Zapfenteils kraftschlüssig im Behälterhals gehalten ist, wobei aber das Behäl­terinnere über den Durchlaß 11 noch zur Umgebund offen ist. Aus dem im Behälter enthaltenen Material können daher bei der Gefrier­trocknung zur Umgebund des Behälters Dämpfe und Gase austreten. Durch erhöhte Kraftanwendung auf den Stopfen werden die Nocken 14 a - 14 c zurückgedrängt, wobei die Nocken selbst und das sie um­gebende Material des Zapfens 1 verformt werden. Der Zapfen läßt sich dann in den Behälterhals bis zu einer zweiten Position (Ver­schlußposition) einführen, welche durch Anlage der Begrenzungsfläche 5 des Flansches 2 an der Stirnfläche des Behälterhalses definiert ist und in welcher der mit der geschlossenen oberen Umfangsfläche 10a aus­gestattete erste Abschnitt Z₁ des Zapfens eine vollständige Abdich­tung des Behälterhalses bewirkt.When the pin 1 is inserted into the container neck, these cams 14a-14c cause an inhibition by the abutment of their delimitations 15 on the end face of the container neck and define a first position of the stopper in which it is already non-positively connected by elastic deformation of the pin part adjacent to the end face of the pin is held in the neck of the container, but the inside of the container is still open to the environment via the passage 11. Vapors and gases can therefore escape from the material contained in the container during freeze drying to and around the container. The cams 14a-14c are pushed back by increased application of force to the plug, the cams themselves and the material of the pin 1 surrounding them being deformed. The pin can then be inserted into the container neck up to a second position (closed position), which is defined by contact of the boundary surface 5 of the flange 2 on the end face of the container neck and in which the first section Z 1 of the pin equipped with the closed upper peripheral surface 10 a a complete seal of the container neck causes.

Die Nocken 14a - 14c haben jeweils die Form von im Querschnitt angenähert halbkreisförmigen länglichen Wülsten, die sich in Umfangsrichtung des Zapfens 1 erstrecken, wobei ihre Länge in die­ser Richtung jeweils wenigstens das 2,5-fache ihrer axialen Er­streckung beträgt. Ein erster Nocken 14a ist diametral gegenüber dem Durchlaß (Schlitz) 11 angeordnet, dergestalt, daß seine Mitte in einer ersten Längsebene L₁ liegt, welche die Zapfen-Längsachse A enthält und durch die Mitte zwischen den Seitenflächen 12a, 12b des Durchlasses 11 geht. Die Mitten der beiden anderen Nocken 14b, 14c sind durch eine zweite Längsebene L₂ bzw. dritte Längsebene L₃ de­finiert, welche die Zapfen-Längsachse A enthaltend auf unterschied­lichen Seiten der ersten Längsebene L₁ angeordnet sind und mit die­ser jeweils gleich große Winkel α₂ bzw. α₃ von ca. 110° (Altgrad) einschließen.The cams 14a-14c each have the shape of semi-circular elongated beads in cross-section, which extend in the circumferential direction of the pin 1, their length in this direction in each case being at least 2.5 times their axial extension. A first cam 14a is arranged diametrically opposite the passage (slot) 11, such that its center lies in a first longitudinal plane L₁, which contains the longitudinal axis A of the pin and passes through the middle between the side surfaces 12a, 12b of the passage 11. The centers of the other two cams 14b, 14c are defined by a second longitudinal plane L₂ or third longitudinal plane L₃, which contain the pin longitudinal axis A containing on different sides of the first longitudinal plane L₁ and with this each have the same angle α₂ or α₃ of Include approx. 110 ° (old degree).

In einer zur Zapfen-Längsachse A lotrechten vierten Querebene Q₄ ist eine Nut 16 so angeordnet, daß ihre innere (d. h. dem Flansch 2 be­nachbarte) Seitenwand in der dritten Querebene Q₃ liegt.In a fourth transverse plane Q₄ perpendicular to the longitudinal axis A of the pin, a groove 16 is arranged such that its inner (i.e. adjacent to the flange 2) side wall lies in the third transverse plane Q₃.

An die Nut 16 schließt sich eine Umfangsfläche 17 des Zapfens 1 an, deren Durchmesser geringfügig größer als der Durchmesser der Umfangs­fläche ist, von der die Nocken 14a-14c vorspringen. Die Umfangsfläche schließt über eine der leichteren Einführung der Zapfens 1 in den Behälterhals dienende konische Fläche 18 an die Zapfen-Stirnseite an.The groove 16 is followed by a peripheral surface 17 of the pin 1, the diameter of which is slightly larger than the diameter of the peripheral surface from which the cams 14a-14c project. The peripheral surface closes via one of the easier insertion of the pin 1 into the container neck conical surface 18 on the pin end face.

Die den Hohlraum 4 des Zapfens 1 axial begrenzende Innen-Wandfläche 6 geht über eine gerundete Hohlkehle in eine seitlich begrenzende Innen-Wandfläche 19 über, welche die Form eines Kegelstumpfes auf­weist, dessen Achse die Zapfen-Längsachse A ist und der seinen größten Durchmesser an der Zapfen-Stirnseite 3 aufweist. Wesentlich für die Formgebund dieser Innen-Wandfläche 19 ist, daß diese an keiner Stelle innerhalb eines (gedachten) Kegels K vorsteht, dessen Achse die Zapfen-Längsachse A ist und dessen Spitze K₁ in der er­sten Querebene Q₁ liegt, wobei der in Altgrad gemessene Spitzen­winkel β dieses Kegels größer als ein nach der Formel
- 39 + 75 x lg (D)
berechneter Wert ist (D = maximaler Durchmesser in Millimetern des ersten Abschnitts Z₁).The inner wall surface 6, which axially delimits the cavity 4 of the pin 1, merges via a rounded fillet into a laterally delimiting inner wall surface 19, which has the shape of a truncated cone, the axis of which is the longitudinal axis A of the pin and its largest diameter at that Has end face 3. It is essential for the shape of this inner wall surface 19 that it does not project at any point within an (imaginary) cone K, the axis of which is the longitudinal axis A of the pin and the tip K 1 of which lies in the first transverse plane Q 1, the tip angle measured in degrees β of this cone is larger than one according to the formula
- 39 + 75 x lg (D)
calculated value is (D = maximum diameter in millimeters of the first section Z 1).

Claims (6)

1. Gefriertrocknungs-Stopfen aus gummielastischem Material, bestehend aus einem zur Einführung in den abzudichtenden Behälterhals bestimmten Zapfen und einem einstückig mit dem Zapfen ausgebildeten und radial über diesen vorstehenden, im wesentlichen kreisscheibenförmigen Flansch, dessen Längsachse mit derjenigen des Zapfens zusammenfällt, welcher Zapfen einen die Zapfen-Längsachse umgebenden Hohlraum enthält, der zur freien Zapfen-Stirnseite offen ist und sich bis zu einem zen­tralen geschlossenen Wandungsteil des Flansches erstreckt, wobei der Zapfen einen ersten Abschnitt seiner axialen Länge enthält, der sich zwischen einer durch die vom Zapfen radial nach außen vorspringenden Begrenzungsfläche des Flansches gelegte erste Querebene und einer zur Zapfen-Längsachse lotrechten zweiten Querebene erstreckt und eine ge­schlossene äußere Umfangsfläche aufweist, deren maximaler Durchmesser geringfügig größer als der Behälterhals - Innendurchmesser ist und einen sich an den ersten Abschnitt anschließenden zweiten Abschnitt enthält, dessen äußere Hüllfläche im wesentlichen den gleichen Durch­messer wie der erste Abschnitt aufweist und der wenigstens einen mit dem Hohlraum kommunizierenden Durchlaß enthält, welcher sich von der Zapfen-Stirnseite bis zu einer im zweiten Abschnitt gelegenen, an die zweite Querebene angrenzende radiale Öffnung erstreckt, und wobei vom zweiten Abschnitt nach außen über die Hüllfläche mehrere, durch elas­ tische Verformung zurückdrängbare Hemmelemente vorstehen, deren axial äußere Begrenzungen auf einer gemeinsamen, zur Zapfen-Längsachse lot­rechten, zwischen der zweiten Querebene und der freien Zapfen-Stirn­seite gelegenen, zur Zapfen-Längsachse lotrechten dritten Querebene liegen, dadurch gekennzeichnet,
daß die den Hohlraum (4) seitlich begrenzende Innen-Wandfläche (19) vollständig äußerhalb eines Kegels (K) liegt, dessen Achse die Zapfen-­Längsachse (A) ist, dessen Spitze (K₁) in der ersten Querebene (Q₁) liegt und dessen Spitzenwinkel (β) in Altgrad größer als ein nach der Formel
-39 + 75 x lg (D)
berechneter Wert ist, wobei in der Formel "lg" den dekadischen Loga­rithmus und "D" den in Millimetern gemessenen maximalen Durchmesser (D) des ersten Abschnittes (Z₁) des Zapfens (1) bedeutet.1. Freeze-drying stopper made of rubber-elastic material, consisting of a pin intended for insertion into the container neck to be sealed and a piece which is formed in one piece with the pin and projects radially above this, essentially circular disk-shaped flange, the longitudinal axis of which coincides with that of the pin, which pin is one Contains the longitudinal axis of the pin, which is open to the free face of the pin and extends to a central, closed wall part of the flange, the pin containing a first portion of its axial length, which extends between the one projecting radially outwards from the pin Boundary surface of the flange placed first transverse plane and a second transverse plane perpendicular to the longitudinal axis of the pin extends and has a closed outer circumferential surface, the maximum diameter of which is slightly larger than the inner diameter of the container neck and adjoins the first section a n includes the second section, the outer envelope surface has substantially the same diameter as the first section and contains at least one passage communicating with the cavity, which extends from the pin end face to a radial located in the second section adjacent to the second transverse plane Opening extends, and wherein from the second section to the outside over the envelope surface several, by elas table deformation projecting retractable inhibiting elements, the axially outer boundaries of which lie on a common third transverse plane perpendicular to the longitudinal axis of the journal, between the second transverse plane and the free end face of the journal, perpendicular to the longitudinal axis of the journal longitudinal axis, characterized in that
that the cavity (4) laterally delimiting inner wall surface (19) lies completely outside a cone (K), the axis of which is the longitudinal axis of the pin (A), the tip (K₁) of which lies in the first transverse plane (Q₁) and the latter Point angle (β) in degrees above one according to the formula
-39 + 75 x lg (D)
calculated value is, in the formula "lg" the decimal logarithm and "D" the maximum diameter (D) of the first section (Z 1) of the pin (1) measured in millimeters. 2. Gefriertrocknungs-Stopfen nach Anspruch 1, dadurch ge­kennzeichnet, daß die den Hohlraum (4) axial begrenzende Innen-Wandfläche (6) des zentralen Wandungsteiles ( 2b) des Flansches (2) in einem die Zapfen-Längsachse (A) umgebenden Flächenbereich im wesentlichen eben ausgebildet ist und daß dieser Flächenbereich in einer zur Zapfen-Längsachse lotrechten Querebene (P) liegt, welche nahe der ersten Querebene (Q₁) verläuft.2. Freeze-drying plug according to claim 1, characterized in that the cavity (4) axially delimiting inner wall surface (6) of the central wall part (2b) of the flange (2) in a surface area surrounding the pin longitudinal axis (A) in is essentially flat and that this surface area lies in a transverse plane (P) perpendicular to the longitudinal axis of the pin, which runs close to the first transverse plane (Q 1). 3. Gefriertrocknungs-Stopfen nach Anspruch 2, dadurch ge­kennzeichnet, daß die axial begrenzende Innenwand-Fläche (6) be­züglich der Querebene (Q₁) in Richtung zur Aussenfläche (7) des zent­ralen Wandungsteils (2b) versetzt ist.3. lyophilization stopper according to claim 2, characterized in that the axially limiting inner wall surface (6) of the transverse plane (Q₁) in the direction to the outer surface (7) of the central wall part (2b) is offset. 4. Gefriertrocknungs-Stopfen nach Anspruch 2 oder 3, dadurch gekennzeichnet, daß die den Hohlraum (4) seitlich begren­zende Innen-Wandfläche (19) von dem die Zapfen-Längsachse (A) umgebenden Flächenbereich ausgeht und mit zunehmender Annäherung an die freie Zap­fen-Stirnseite (3) ihren Durchmesser vergrößert.4. Freeze-drying stopper according to claim 2 or 3, characterized in that the cavity (4) laterally delimiting inner wall surface (19) starts from the surface area surrounding the pin longitudinal axis (A) and with increasing approach to the free pin- Front side (3) increases its diameter. 5. Gefriertrocknungs-Stofen nach Anspruch 1, dadurch ge­kennzeichnet, daß der die Zapfen-Längsachse (A) umgebende Flächenbereich der Aussenfläche (7) des zentralen Wandungsteiles (2b) des Flansches (2) von dem restlichen peripheren Flächenbereich durch eine kreisförmige, zur Zapfen-Längsachse (A) konzentrische An­ordnung von Vorsprüngen (8) abgegrenzt ist.5. Freeze-drying oven according to claim 1, characterized in that the longitudinal region of the pin (A) surrounding surface area of the outer surface (7) of the central wall part (2b) of the flange (2) from the remaining peripheral surface area by a circular to the pin -Longitudinal axis (A) concentric arrangement of projections (8) is delimited. 6. Gefriertrocknungs-Stopfen nach Anspruch 1, dadurch ge­kennzeichnet, daß der die Zapfen-Längsachse (A) umgebende Flächenbereich der Aussenfläche (7) des zentralen Wandungsteiles (2b) des Flansches (2) bezüglich des restlichen peripheren Flächenbereiches vertieft ausgebildet ist.6. Freeze-drying stopper according to claim 1, characterized in that the surface area of the outer surface (7) of the central wall part (2b) of the flange (2) surrounding the pin longitudinal axis (A) is recessed with respect to the remaining peripheral surface area.
EP88118843A 1987-12-24 1988-11-11 Bottle stopper for freeze-drying Expired - Lifetime EP0322548B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88118843T ATE91470T1 (en) 1987-12-24 1988-11-11 FREEZE DRY STOPPER.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3744174 1987-12-24
DE19873744174 DE3744174A1 (en) 1987-12-24 1987-12-24 FREEZE DRYING PLUG

Publications (2)

Publication Number Publication Date
EP0322548A1 true EP0322548A1 (en) 1989-07-05
EP0322548B1 EP0322548B1 (en) 1993-07-14

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Country Status (4)

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US (1) US4872572A (en)
EP (1) EP0322548B1 (en)
AT (1) ATE91470T1 (en)
DE (2) DE3744174A1 (en)

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US2927709A (en) * 1959-07-07 1960-03-08 Faultless Rubber Co Bottle stopple
FR1255197A (en) * 1960-04-14 1961-03-03 Pelcerf Ets Stopper for sealing vacuum flasks
US3834571A (en) * 1972-11-20 1974-09-10 Warner Lambert Co Container closure for lyophilized products
FR2416848A1 (en) * 1978-02-08 1979-09-07 Rumpler Jean Jacques MEDICINAL PRODUCT CONTAINER CAP
CA1136077A (en) * 1979-06-04 1982-11-23 Masaki Shimizu Microorganism culturing device
US4293078A (en) * 1979-11-01 1981-10-06 Becton, Dickinson And Company Vacuum indicator closure for a blood collection tube
US4286389A (en) * 1980-03-03 1981-09-01 Ims Limited Apparatus and method for lyophilizing aseptic substances

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3653528A (en) * 1970-03-03 1972-04-04 West Co Stopper for medicament flasks
FR2096680A1 (en) * 1970-05-29 1972-02-25 Barville Jean
GB2026995A (en) * 1978-08-01 1980-02-13 Coulter Electronics Closure Caps

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008129409A1 (en) * 2007-04-24 2008-10-30 Dsm Ip Assets B.V. Lyophilization cap and assembly
CN101411671B (en) * 2008-10-16 2013-08-21 应城市恒天药业包装有限公司 Novel medicinal bottle stopper for lyophilized powder formulation

Also Published As

Publication number Publication date
EP0322548B1 (en) 1993-07-14
DE3882350D1 (en) 1993-08-19
DE3744174A1 (en) 1989-07-06
ATE91470T1 (en) 1993-07-15
US4872572A (en) 1989-10-10

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