US3199216A - Apparatus for shell freezing of heat sensitive liquids - Google Patents

Apparatus for shell freezing of heat sensitive liquids Download PDF

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Publication number
US3199216A
US3199216A US130280A US13028061A US3199216A US 3199216 A US3199216 A US 3199216A US 130280 A US130280 A US 130280A US 13028061 A US13028061 A US 13028061A US 3199216 A US3199216 A US 3199216A
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container
vacuum
motor
sealing cover
heat sensitive
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US130280A
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Samuel M Broadwin
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Samuel M Broadwin
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/42Low-temperature sample treatment, e.g. cryofixation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B04CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04BCENTRIFUGES
    • B04B5/00Other centrifuges
    • B04B5/02Centrifuges consisting of a plurality of separate bowls rotating round an axis situated between the bowls
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26DRYING
    • F26BDRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
    • F26B5/06Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing

Description

1955 s. M. BROADWIN 3,199,216
APPARATUS FOR SHELL FREEZING OF HEAT SENSITIVE LIQUIDS Filed Aug. 9. 1961 INVENTOR.
5/7/7UEL IV. BRO/1D w/A United States Patent C 3 199,216 APPARATUS FUR SEliELL FREEZING OF HEAT SENSTTTVE LTQUTDS Samuel M. roadwin, 301 E. 62nd St., New York 21, N.Y. Filed Aug. 9, 1961, Ser. No. 130,28-3 6 Claims. (Ci. 34-92} This invention comprises of a new method and a novel device for evaporating or shell-freezing of heat sensitive liquids, such as organic fluids, and an inexpensive, rapid, and safe method of stoppering the fluid container without releasing the vacuum, thus preserving the dried sample from decay due to oxygen or water vapor in the air.
The rotating container is not axially rotated as in conventional centrifugal devices, but is part of a greater radius, thereby allowing increased centrifugal force with lessened speed. Further, this device permits turning in a complete circle by external means, thus allowing for vacuum connections without the necessity of a rotating vacuum seal as in conventional devices.
The stoppering device is manually operated, and consists of a rubber stopper fastened by a pin to a shaft that is separated from the evacuated area by a rubber, or other stretchable material, diaphragm. The shaft is held outwardly against atmospheric pressure by a spring. When it is desired to stopper the flask situated below the stopper, the spring is depressed until the stopper is firmly inserted in the flask, at that point the vacuum is released. The stopper is held in position by the weight of the air and the pin removed by releasing the spring.
The device of this invention is inherent in the method thereof and embodies means for eccentrically rotating a heat sensitive liquid in a container around an external center, heat producing means, vacuum retaining means, vacuum sealing means, vacuum stoppering means, vacuum releasing means, means for adjustment of speed of rotation, means for adjustment of centrifugal thrust, and a means for disassembling the device for cleaning purposes.
Various further objects and advantages of this invention will be apparent from the description contained in the specification herein. It may be pointed out that present methods for vacuum stoppering in the laboratory require heat-sealing of the glass container, which is both dangerous and restrictive in the size of glassware. Further, as this device eliminates the rotating vacuum seal found in conventional devices it enables the operator to achieve vacuum pressures to .01 micron.
The invention will be further described by reference to the accompanying drawing which is made part of this specification. The drawing is a composite sectional view of the evaporator and shell-freezer.
The invention will be further described by reference to the specific form thereof shown in the drawing, but it is pointed out that such form shown i for illustrative purposes only and is merely representative of one of the forms this invention can take. The form shown is not to be considered a limitation upon this invention whose scope i solely determined by the appended claims.
A container holding a quantity of heat sensitive liquid 8 is disposed in the holding form having rigidly aflixed at its terminal parts two spherical bearing surfaces 4 and 9. The container is so disposed that it rests on rubber gasket 7 and on rubber supports 16 and the container 3 has a capping portion 6. The spherical bearings are pivotally held in holding cups and 17. Holding cup 17 is supported by locking slide 3 which is surrounding upwardly extending portion 2. Spherical bearing 9 is disposed in holding cup 10 which is integral with adjustable rotating locking fixture and radial arm 18 which is fixed to the revolving shaft of a adjustable speed motor, here diagrammatically indicated as 19. Upwardly extending portion 2 is rigidly fixed to horizontal bed 1 which also has afiixed to it a motor 19 thus forming a support for the entire instrument. Capping portion 6 rests upon gasket 7. The capping portion 6 is provided with a vacuum port which is angularly disposed thereto and a vacuum stopcock 14 is provided for release of the vacuum. A shaft 29 is disposed through an outwardly expanding spring and centrally through a bridging structure which is integral with capping portion 6. The shaft 26 passes through a flexible diaphragm such as rubber 12 which is sealed at its outer boundary to bridging portion 21 and at its inner boundary to shaft 20. Forming part of the shaft 2% and not shown in the drawing is a short needle which penetrates rubber stopper 13 holding it in place for disposition in container 8. A heater 22 for accelerating the drying time, is disposed about the container. I
The operation of this invention will now be explained.
Container 8 is partially filled with a heat sensitive solution, and placed in holding form 5. Bearings 4 and 9 are placed in holding cups 1i) and 17 and adjustment made to fixture. 18 setting the radius of the arm. This setting is determined by previous trial and error dependent upon quantity and viscosity of the liquid. Adjustment of locking slide 3 sets proper tension on bearings. Rubber stopper 13 is afiixed to point of needle which is part of shaft 20 and vacuum stopcock 14 is closed. This portion (6 and others) is placed on gasket 7. Vacuum port 15 is connected to a vacuum pump by means of rubber hose and pumping is begun. When a sufiicient vacuum is achieved the above mentioned portion is held firmly to 5 by vacuum pressure. Motor 19 is started, rotating the liquid container around a common axis formed by the motor shaft. The rotating bearings, 4 and 9, do not rotate on their own axes, and therefore do not require, rotary vacuum seals. Further, due to the increased turning diameter, sufficient centrifugal force is developed at low speeds to produce a vortex, thus extending the evaporative surfaces and holding the liquid against the walls of the container 8, thus preventing destructive foaming. When the evaporative process is adjudged complete, shaft 20 is depressed, forcing rubber stopper 13 into container 8, vacuum release stopcock is opened and vacuum pump to port 15 is detached. The rubber stopper 13 is now held firmly due to air pressure on its outward top side and vacuum pressure on its inward bottom side. Shaft 2b is released from finger pressure and spring 11 thereupon thrusts it outward, removing the needle (shaft 20) from the rubber stopper 13. The sealed flask may now be removed. At any point in the procedure outlined above, the drying time may have been accelerated by connecting the heater 2.2 to an electrical circuit. This heater (shown on outside of holding form 5) may be inside the vacuum system.
I claim:
1. A device for shell freezing of heat sensitive liquids which includes a centrifugal device for supporting a single container, said single container having upper and lower ends supported in said device in an angular position, a motor having a vertical drive axis and driving arm extending perpendicular from said drive axis and rotated by said motor, the upper end of said container supporting device pivotally mounted at a point on the driving axis of said motor, the lower end of said container supporting device pivotally mounted on an outer extremity of said driving arm to be rotated about the motor axis to produce the necessary centrifugal force for shell freezing of the liquid in said container, said container being closed at the lower end and having an open mouth at the upper end, a vacuum sealing cover for the mouth of said container and an axially movable stopper mounted for reciprocation in the sealing cover and sealing the mouth of said container, a vacuum producing source connected to said vacuum upright elementsupporting a fixed spherical bearing at the upper end, of saidangu'larly disposedexternal axially pivotal structure and said motor driving arm vprovided with a second spherical bearing surface and in which said angularly disposed external axially pivotal 2 structure is provided with fixed 'ball b'earings that are to be mounted within the oppositely disposed'spher'ical bearinglsurfaces.
i 3. In a device according to claim 1 in which said centrifugal device for supporting a singlecontainer i maintained on a, central non-rotatable internal axis at its upper end while being rotated aboutits angularly disposed external axis.fat its lower end and providedwith means to connect saidvacuum producing means to said container at its upper end without rotation of said container or vacuum producing source. t
4. In a device according-to claim ;1 in which said vacuum sealing cover for the mouth of said container comprises a resilient manually operated valve for said stopper, supported and contained in-asealed relationship ,over saidtcontainer to permit producing a vacuum within,
I vsaid valve for said stopper provided with a needle as the a sole supporting'element for said stopper, means to force said stopper into the mouth of said container to seal said container under vacuum and withdraw said resilient manually operated valve and needle from said stopper and mean to release said vacuum above said stopper.
5. In a device according to claim 1 means to control the speed of said motor and in turn the centrifugal force produced within said container.
3 6. In a device according to claim 1 in which a heat producing means surrounds said container and is controlled to produce a definite control of the change 0 temperature during the vacuurn build up. I References Cited by the Examiner UNITED STATES PATENTS 2,304,192 12/42 Newton 34-92 X 2,324,237 7/43 Reichel.
2,388,917 11/ 45 Hormel 34-92 2,862,307 12/58 Bloomer 34 92 2,878,581 3/59 Turati 34-92 2,885,788 5/59 Leviton 345 2,897,600 8/59 1 Graham 34-5 2,907,117 10/59 Parkinson et a1. 3492 NORMAN YUDKOFF, Primary Examiner.

Claims (1)

1. A DEVICE FOR SHELL FREEZING OF HEAT SENSITIVE LIQUIDS WHICH INCLUDES A CENTRIFUGAL DEVICE FOR SUPPORTING A SINGLE CONTAINER, SAID SINGLE CONTAINER HAVING UPPER AND LOWER ENDS SUPPORTED IN SAID DEVICE IN AN ANGULAR POSITION, A MOTOR HAVING A VERTICAL DRIVE AXIS AND DRIVING ARM EXTENDING PERPENDICULAR FROM SAID DRIVE AXIS AND ROTATED BY SAID MOTOR, THE UPPER END OF SAID CONTAINER SUPPORTING DEVICE PIVOTALLY MOUNTED AT A POINT ON THE DRIVING AXIS OF SAID MOTOR, THE LOWER END OF SAID CONTAINER SUPPORTING DEVICE PIVOTALLY MOUNTED ON AN OUTER EXTREMITY OF SAID DRIVING ARM TO BE ROTATED ABOUT THE MOTOR DRIVE TO PRODUCE THE NECESSARY CENTRIFUGAL FORCE FOR SHELL FREEZING OF THE LIQUID IN SAID CONTAINER, SAID CONTAINER BEING CLOSED AT THE LOWER END AND HAVING AN OPEN MOUTH AT THE UPPER END, A VACUUM SEALING COVER FOR THE MOUTH OF SAID CONTAINER AND AN AXIALLY MOVABLE STOPPER MOUNTED FOR RECIPROCATION IN THE SEALING COVER AND SEALING THE MOUTH OF SAID CONTAINER, A VACUUM PRODUCING SOURCE CONNECTED TO SAID VACUUM SEALING COVER, AND A VACUUM RELEASE VALVE IN SAID VACUUM SEALING COVER.
US130280A 1961-08-09 1961-08-09 Apparatus for shell freezing of heat sensitive liquids Expired - Lifetime US3199216A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3241250A (en) * 1965-01-05 1966-03-22 Scientific Industries Automatic shell freezing device
US3280470A (en) * 1964-07-23 1966-10-25 Robert L Kuntz Method and apparatus for oven dehydrating compounds
US3708886A (en) * 1970-11-09 1973-01-09 Lyoflo Stopper Corp Lyoflo-stopper
US3824701A (en) * 1972-09-05 1974-07-23 B Norquist Portable centrifugal drier for small articles
US3952541A (en) * 1968-11-05 1976-04-27 Mario Rigoli Apparatus for quick freezing of aqueous solutions or suspensions to be submitted to lyophilization
US4060911A (en) * 1975-08-07 1977-12-06 Behringwerke Aktiengesellschaft Process for the preparation of a container closed under sterile conditions and containing lyophilized material

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2304192A (en) * 1940-08-16 1942-12-08 Honeywell Regulator Co Refrigeration of hygroscopic material
US2324237A (en) * 1941-03-19 1943-07-13 Reichel John Container
US2388917A (en) * 1941-10-13 1945-11-13 Hormel & Co Geo A Process for preservation of biological materials and products resulting therefrom
US2862307A (en) * 1957-08-07 1958-12-02 Univ Tennessee Res Corp Processing chamber
US2878581A (en) * 1956-11-13 1959-03-24 Turati Enrico Dryers
US2885788A (en) * 1958-05-26 1959-05-12 Leviton Abraham Process for freeze-drying of milk
US2897600A (en) * 1958-08-13 1959-08-04 Robert P Graham Process of dehydrating biological materials
US2907117A (en) * 1957-02-15 1959-10-06 Martin C Parkinson Drying device

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2304192A (en) * 1940-08-16 1942-12-08 Honeywell Regulator Co Refrigeration of hygroscopic material
US2324237A (en) * 1941-03-19 1943-07-13 Reichel John Container
US2388917A (en) * 1941-10-13 1945-11-13 Hormel & Co Geo A Process for preservation of biological materials and products resulting therefrom
US2878581A (en) * 1956-11-13 1959-03-24 Turati Enrico Dryers
US2907117A (en) * 1957-02-15 1959-10-06 Martin C Parkinson Drying device
US2862307A (en) * 1957-08-07 1958-12-02 Univ Tennessee Res Corp Processing chamber
US2885788A (en) * 1958-05-26 1959-05-12 Leviton Abraham Process for freeze-drying of milk
US2897600A (en) * 1958-08-13 1959-08-04 Robert P Graham Process of dehydrating biological materials

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3280470A (en) * 1964-07-23 1966-10-25 Robert L Kuntz Method and apparatus for oven dehydrating compounds
US3241250A (en) * 1965-01-05 1966-03-22 Scientific Industries Automatic shell freezing device
US3952541A (en) * 1968-11-05 1976-04-27 Mario Rigoli Apparatus for quick freezing of aqueous solutions or suspensions to be submitted to lyophilization
US3708886A (en) * 1970-11-09 1973-01-09 Lyoflo Stopper Corp Lyoflo-stopper
US3824701A (en) * 1972-09-05 1974-07-23 B Norquist Portable centrifugal drier for small articles
US4060911A (en) * 1975-08-07 1977-12-06 Behringwerke Aktiengesellschaft Process for the preparation of a container closed under sterile conditions and containing lyophilized material

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