[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

EP1356229A1 - Cryogenic shipping container - Google Patents

Cryogenic shipping container

Info

Publication number
EP1356229A1
EP1356229A1 EP01991461A EP01991461A EP1356229A1 EP 1356229 A1 EP1356229 A1 EP 1356229A1 EP 01991461 A EP01991461 A EP 01991461A EP 01991461 A EP01991461 A EP 01991461A EP 1356229 A1 EP1356229 A1 EP 1356229A1
Authority
EP
European Patent Office
Prior art keywords
vessel
dewar
specimen chamber
chamber
shipping container
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.)
Withdrawn
Application number
EP01991461A
Other languages
German (de)
French (fr)
Other versions
EP1356229A4 (en
Inventor
Patrick L. Mullens
Gregg Emmel
R. Kevin Giesy
Christy Thomas
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cryoport Systems LLC
Original Assignee
Cryoport Systems LLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US09/753,207 external-priority patent/US20020083717A1/en
Priority claimed from US09/753,208 external-priority patent/US20020083718A1/en
Priority claimed from US09/753,194 external-priority patent/US6467642B2/en
Application filed by Cryoport Systems LLC filed Critical Cryoport Systems LLC
Publication of EP1356229A1 publication Critical patent/EP1356229A1/en
Publication of EP1356229A4 publication Critical patent/EP1356229A4/en
Withdrawn legal-status Critical Current

Links

Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17CVESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C3/00Vessels not under pressure
    • F17C3/02Vessels not under pressure with provision for thermal insulation
    • F17C3/08Vessels not under pressure with provision for thermal insulation by vacuum spaces, e.g. Dewar flask
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N1/00Preservation of bodies of humans or animals, or parts thereof
    • A01N1/02Preservation of living parts
    • A01N1/0236Mechanical aspects
    • A01N1/0242Apparatuses, i.e. devices used in the process of preservation of living parts, such as pumps, refrigeration devices or any other devices featuring moving parts and/or temperature controlling components
    • A01N1/0252Temperature controlling refrigerating apparatus, i.e. devices used to actively control the temperature of a designated internal volume, e.g. refrigerators, freeze-drying apparatus or liquid nitrogen baths
    • A01N1/0257Stationary or portable vessels generating cryogenic temperatures
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17CVESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C13/00Details of vessels or of the filling or discharging of vessels
    • F17C13/005Details of vessels or of the filling or discharging of vessels for medium-size and small storage vessels not under pressure
    • F17C13/006Details of vessels or of the filling or discharging of vessels for medium-size and small storage vessels not under pressure for Dewar vessels or cryostats
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25DREFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
    • F25D25/00Charging, supporting, and discharging the articles to be cooled
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25DREFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
    • F25D3/00Devices using other cold materials; Devices using cold-storage bodies
    • F25D3/10Devices using other cold materials; Devices using cold-storage bodies using liquefied gases, e.g. liquid air
    • F25D3/105Movable containers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N2001/002Devices for supplying or distributing samples to an analysing apparatus
    • G01N2001/005Packages for mailing or similar transport of samples

Definitions

  • the present invention is in the field of cryogenic shipping containers.
  • Static hold time pertains to a fully charged shipper with no heat load, sitting upright, e.g., essentially not in use.
  • Functional hold time refers to the fully charged shipper in use and containing samples, e.g., in the process of being handled and transported.
  • the static hold time is often promoted as being 20 days, if the container is tilted or positioned on its side, the hold time diminishes to hours as opposed to days. This occurs because the liquid nitrogen transitions to the gaseous (vapor) phase more rapidly resulting in outgassing. The liquid nitrogen can also simply leak out of the container when it is positioned on its side.
  • the current cryogenic containers are promoted as being durable because they are of metal construction.
  • U.S. Patent No. 6,119,465 seeks to meet this need by using unique, lightweight, low-cost, durable composites and polymers in a semi-disposable vapor phase liquid nitrogen bioshipper. This is accomplished in an inherently simple, reliable, and inexpensive device that will result in reduced shipping costs, enhanced reliability and safety, and fewer service requirements.
  • the present invention builds upon the framework laid by U.S. Patent No. 6,1 19,465, the disclosure of which is specifically incorporated herein by reference. This is done by use of a cryogenic shipping container that has many significant advances over what is disclosed in our earlier patent. The end result is a much improved cryogenic shipping container that is more economical while still being reliable.
  • the present invention is generally directed to a portable, insulated shipping container.
  • the shipping container has an outer shipping container shell and a support assembly for holding a dewar vessel within the outer shipping container shell and providing impact and vibration resistance to the dewar vessel.
  • the dewar vessel has an inner vessel that holds a specimen chamber and plastic foam between its inner wall and the specimen chamber.
  • the specimen chamber allows liquid cryogen to pass through it into the plastic foam, allows liquid cryogen in a vapor phase liquid state to pass from the plastic foam into it, and acts as a filter to prevent particles or fragments of the plastic foam from entering into it.
  • the specimen chamber is an open-celled porous thermoplastic material that is cryogenically compatible, and it is especially preferred that it be an aerated polypropylene foam.
  • the plastic foam is an open cell plastic foam, and it is especially preferred that it be a phenolic foam.
  • the plastic foam can hold a normal charge of liquid cryogen in a dry vapor state regardless of the container's spatial orientation.
  • the plastic foam can be made of multiple foam segments having a maximum thickness less than a critical height with each segment being separated by a capillarity separation layer.
  • the thickness of the foam segments is preferably selected so that the head pressure of the plurality of foam segments will not cause liquid cryogen to ooze or flow out of the foam segments when their spatial orientation is changed. This thickness can be less than approximately four inches.
  • the foam can occupy substantially all of the volume between the inner wall of the inner vessel and the sample chamber.
  • Materials suitable for use as the capillarity separation layer include paper products treated to resist water and spunbonded olefin film.
  • a self-venting cap is used to restrict access to the specimen chamber when it forms a compression seal with an inner circumference of the neck of the dewar vessel.
  • the cap creates one or more tortuous paths through it when it is in the compression seal position.
  • the cap can be made of a lower component with a first plurality of apertures, an upper component having a second plurality of apertures, a seal held between the lower and upper components, and a third component secured to the upper component. It is especially desirable that the components of the cap in the vapor paths are made of a cryogenically compatible material that is non-metallic and non-conductive.
  • a first chamber can be formed between the lower and upper components while a second chamber and a vent opening can be formed between the upper and third components.
  • Vapor can travel through the cap in any of multiple tortuous vapor paths beginning with the first plurality of apertures and then proceeding through the first chamber, the second plurality of apertures, the second chamber and then out a vent opening.
  • One or more semi-permeable membranes can be used to prevent moisture (water vapor) from entering into the dewar vessel while still allowing vaporous cryogen to exit from the dewar vessel.
  • the shipping container is configured so that a reservoir will be formed within the dewar vessel when the container rests on its side so that gravity will not force vapor phase liquid cryogen in the reservoir out of the dewar vessel.
  • the reservoir can be formed by configuring the container so that there will be an angle of approximately six degrees or greater between a flat planar surface and a cross section of the specimen chamber taken from an upper end closest to its top wall and extending down through a lower end closest to its base when the side wall of the container is resting on the flat planar surface.
  • the reservoir can also be formed by a plane that is substantially parallel to the flat planar surface which intersects with the base of the specimen chamber and a first aperture of a self-venting cap that forms a compression seal with the neck of the dewar vessel.
  • the shipping container can have a funnel-shaped vessel plate affixed to the dewar vessel.
  • the shipping container can be made of a rigid thermoplastic material having a base, a side wall and a top wall.
  • the top wall can be connected to the side wall by a movable access assembly, such as a hinge and latching mechanism, and the latching mechanism can be held in a locked position by a lock.
  • the side wall can include a top side wall with a pocket for holding paperwork and a top opening for accessing a dewar opening in the dewar vessel and the top side wall can be covered by the top wall.
  • a safety strap with a locking mechanism can be affixed to the bottom of the dewar vessel and surround the dewar vessel in a closed position so that it also holds the self-venting cap in place.
  • An inner plug of a cryogenically compatible insulating plastic foam with a handle can be held in the neck portion between the self-venting cap and the specimen container.
  • the support assembly can have multiple parts or be a single piece, such as a material that is injected or poured into the shipping container's shell to fill the available space.
  • the portable shipping container can be made to comply with United States Department of Transportation/International Air Transport Association (DOT/IATA) Dangerous Goods Regulations.
  • DOT/IATA United States Department of Transportation/International Air Transport Association
  • Figure 1 is an exploded assembly drawing of a preferred embodiment of a portable, insulated shipping container according to the present invention with a containment system for dangerous materials.
  • Figure 2 is a planar cross section with a partial cutaway view of a preferred embodiment of a portable, insulated shipping container.
  • Figure 3 is an assembly drawing of a preferred embodiment of a dewar vessel assembly.
  • Figure 4 is an exploded assembly drawings of a preferred embodiment of a self-venting cap taken from reverse directions.
  • Figures 5A-5C are a planar cross section of a preferred embodiment of a portable, insulated shipping container showing connection of a preferred self- venting cap.
  • Figure 6 depicts an assembly of a preferred embodiment of a containment system.
  • the preferred embodiments of the present invention can be used as part of an overall system that utilizes several inventions.
  • an overall cryogenic shipping container system Within the shipping container, there is a dewar vessel. Within the dewar vessel, there is a specimen chamber for holding specimens. And, in certain applications, such as shipping of dangerous goods, the specimens are held within a containment system.
  • Figures 1- 6 are described in greater detail below, the following is a glossary of the elements identified in the Figures:
  • Figure 1 provides an assembly drawing that illustrates all of the components of the cryogenic shipping container, generally designated as 1 , in a disassembled state, and Figure 2 illustrates how all of these components fit together in an assembled state.
  • Figure 3 is an assembly drawing that illustrates how dewar vessel 2 is assembled.
  • the dewar vessel As shown in Figure 1 , the dewar vessel, generally designated as 2, has a specimen chamber 70 that is accessed by a dewar opening 11.
  • a sample receptacle When shipping container 1 is ready for use after it has been fully charged with a liquid cryogen, a sample receptacle is placed inside of specimen chamber 70 through dewar opening 11.
  • a containment system 80 in which a porous structural cartridge 83 is held within a bag 81 with a handle 82.
  • an inner plug 90 After containment system 80 is placed inside of specimen chamber 70, an inner plug 90, with a handle 91 , is placed inside of dewar opening 11.
  • a self- venting cap 100 is inserted into dewar opening 11 through funnel-shaped vessel plate 60 and tightened so as to create a compression seal (this is shown in Figures 5A-5C).
  • an adjustable buckle 56 of safety strap 55 can be closed and tightened (any suitable alternative connection mechanism could be substituted for a buckle, if desired).
  • Safety strap 55 can be made of a webbing material, and it is affixed to an outer bottom 57 of dewar vessel 2 by adhesive tape or some other affixation means. Safety strap 55, when properly closed and tightened, provides additional integrity to dewar vessel 2 and helps prevent loss or separation of self-venting cap 100 and containment system 80.
  • the dewar vessel assembly is held within an outer shipping container shell
  • Outer shipping container shell 40 made of a lightweight, but rigid, material that helps to provide shock and impact resistance, such as low density polyethylene.
  • Outer shipping container shell 40 has a "base” 41 , a “side wall” 42, and a “top wall” 43 that surround and enclose dewar vessel 2 during shipping.
  • base 41 is the portion of shell 40 that rests upon the flat planar surface
  • top wall 43 is the outermost portion of shell 40 distant from base 41 which is somehow movable to permit access inside of the container (e.g., the top lid of a box)
  • side wall 42 is whatever connects base 41 to top wall 43 (e.g., a square box or rectangle has four planar surfaces that form the side wall).
  • Dewar vessel 2 can be inserted into shell 40 through base 41 and then base 41 can be affixed to side wall 42 by a suitable sealing means, such as screws.
  • a suitable sealing means such as screws.
  • Mechanisms for providing evidence of tampering with shell 40, or improper orientation of container 1 during shipping, or means for tracking container 1 during shipping (e.g., by a global positioning system) can be enclosed within shell 40 at or near base 41.
  • top wall 43 is a cover that is attached to side wall 42 by a hinge mechanism 46 (comprised of two hinges) and a latch mechanism 47. During shipping, latch mechanism 47 can be held in a locked position by a lock (not shown) to provide security against tampering.
  • Top wall 43 in a closed position, covers a top side wall 42a of side wall 42.
  • Top side wall 42a includes a top opening 42b through which dewar opening 11 can be accessed when top wall 43 is in an open position, latch mechanism 47 is undone, and self-venting cap 100 is removed.
  • Top side wall 42a also includes a pocket 45 for paperwork (e.g., an inventory check list, shipping documents or operating instructions).
  • Pocket 45 is accessible when top wall 43 is not latched in place to side wall 42 and inaccessible when it is latched in place.
  • Handles 44 can be molded into side wall 42.
  • Side wall 42 can also have a certification plate assembly 48 (a certification plate 48a held in indentation 48c by rivets 48b) for affixing and displaying important information, such as a container serial number, certifications, warnings, bar codes, etc.
  • a support assembly 50 holds dewar vessel 2 within shell 40.
  • support assembly 50 is made up of several different pieces of lightweight, shock-absorbing foam material.
  • Support assembly 50 has a bottom portion 51 in contact with base 41 to protect the bottom of dewar vessel 2, side rib portions 52 in contact with side wall 42 to protect the sides of dewar vessel 2, and a top portion 53 to protect the top of dewar vessel 2.
  • Side rib portions 52 can be attached to side wall 42 by adhesive or tape.
  • Top portion 53 of support assembly 50 can be held in place by rib portions 52.
  • shipping container 1 includes a funnel-shaped vessel plate 60.
  • the funnel shape of plate 60 makes it easier to pour liquid cryogen into dewar vessel 2. It also helps to restrict access into the interior of shell 40 through top opening 42b. It also contains a position device 114 which are three nubs that are used by self-venting cap 100 to help lock it in place and form a compression seal with the outer circumference of neck portion 21 of dewar vessel 2. (Throughout this description, and in the attached claims, "circumference” or “circumferential” is used to refer to a perimeter or periphery, which may or may not be circular.
  • Vessel plate 60 is held in place by sealing it to neck portion 21 by adhesive so that there is no liquid or vapor gap between vessel plate 60 and neck portion 21. Additional stability for the seal is provided by spray foam 61 , and supports 61 help position and support plate 60 inside of shell 40.
  • Vessel plate 60 should be made of a cryogenically compatible material.
  • specimen chamber 71 When it is in its normal, upright position, i.e., when its weight is resting on base 41 , specimen chamber 71 is substantially perpendicular to base 41. This is the optimal position for container 1 because of the physical characteristics of vaporous cryogen, such as nitrogen. Vapor phase liquid nitrogen has a greater density than air, so it will behave similar to a liquid when it is confined within a container. As long as the vapor phase liquid nitrogen is retained within the dewar vessel, it helps to maintain cryogenic temperatures in the dewar vessel necessary for the cryopreservation of biologicals. This is because the temperature of vapor phase liquid nitrogen is cryogenic (100K).
  • the vapor phase liquid nitrogen will egress from the dewar vessel, much like a fluid, because vapor phase liquid nitrogen in denser than air.
  • the vapor phase liquid nitrogen will accumulate in the dewar vessel until sufficient pressure buildup forces excess vapor phase liquid nitrogen out of the dewar vessel.
  • Outer shell 40 is designed so that if container 1 ends up being stored or shipped on its side, specimen chamber 70 and dewar opening 11 will still be held at an angle thereby creating a reservoir. The reservoir will have the effect of retaining vapor phase liquid cryogen.
  • specimen chamber 70 and dewar opening 11 would be positioned in a substantially parallel position relative to the ground. Such parallel positioning would result in the vapor phase liquid nitrogen pouring out of the vessel in a similar fashion to a glass of water tipping over and spilling its contents.
  • side wall 42 is designed so that when it rests on a flat planar surface the angle formed by the intersection of the planar cross section of specimen chamber 70 with the flat planar surface is approximately six degrees or greater. This is accomplished for container 1 shown in Figure 1 by making the six planar portions of side wall 41 progressively wider as they extend away from base 41 until they reach a maximum thickness near top wall 43. The exact degree of the angle is a matter of design choice, and it will depend upon the overall configuration of the container and the desired result. However, the angle should be sufficient to produce a functional reservoir.
  • using a self-venting cap 100 that forms a compression seal about the inner circumference of neck 21 will increase the volume of the reservoir.
  • dewar vessel The basic design and functioning of a "dewar vessel” is well known and long established.
  • the term "dewar vessel” is defined in Webster's third new international dictionary of the English language, unabridged (1981 ) as "a usu. glass or metal container with at least two walls that has the space between the walls evacuated so as to prevent the transfer of heat, often has a coating (as silvering) on the inside to reduce radiation, and is used esp. for storing liquefied gases (as liquid air) or for investigations at low temperatures.”
  • Examples of various United States Patents that teach the use of dewar vessels with a liquid cryogen for use in a shipping container include 2,396,459, 3,298,185, 4,481 ,779 and 4,495,775.
  • dewar vessels disclosed in these patents, and dewar vessels used in shipping containers today share certain common characteristics. These characteristics, which will hereinafter be defined as being present in a dewar vessel, are an outer casing and an inner vessel with each having openings at their tops connected together by a neck portion forming an evacuable space between the outer casing and the inner vessel and a dewar opening into the inner vessel.
  • a preferred embodiment of dewar vessel 2 according to the present invention is constructed as follows. Neck portion 21 is sealed to specimen chamber 70 by epoxy.
  • a plastic foam 30 that holds a liquid cryogen (not shown) is formed in several segments 31 that are separated by a capillarity separation layer 32.
  • Plastic foam 30 surrounds specimen chamber 70, and then this assembly is placed inside of upper half 13a and lower half 13b which are joined together to form inner vessel 13 with an opening 14 at its top.
  • a getter pack 6 and a desiccant 7 are secured to the top outside of inner vessel 13 by epoxy and metal tape, respectively.
  • the use of a getter pack and a desiccant are well known within the industry and are not an inventive aspect of the present invention.
  • a layer of super insulation 10 is used to surround this assembly. For ease of manufacture and economy, it is especially preferred that super insulation 10 be spirally wrapped and that it be constructed of a single component (e.g., a one-sided metalized polymer film).
  • neck portion 21 is then sealed to an opening 4 in upper half 3a by epoxy which is joined together with lower half 3b to form outer casing 3 and an evacuable space 5 between outer casing 3 and inner vessel 13.
  • evacuable space 5 can only be accessed through nipple 8
  • specimen chamber 70 can only be accessed through dewar opening 11
  • cryogen cannot pass between specimen chamber 70 and plastic foam 30 (whether in a liquid or in a gaseous state) except through side wall 71 and base 72 of specimen chamber 70. Details regarding especially preferred materials useful for constructing a dewar vessel are disclosed in U.S. Patent No. 6,119,465.
  • Plastic foam 30 is preferably an open-celled plastic foam that is cryogenically compatible. It is especially preferred that plastic foam 30 be a phenolic foam (such material is inexpensive and commonly used as a water- holding base for floral arrangements). Plastic foam 30 can either be foamed in place or it can be pre-manufactured in blocks and then sectioned down into segments and inserted into the space surrounding specimen chamber 70. It is especially preferred that plastic foam 30 occupies substantially all of the volume between inner wall 15 of inner vessel 13 and specimen chamber 70.
  • plastic foam 30 retains a liquid cryogen, such as liquid nitrogen, by absorption, adsorption, and surface tension as it saturates foam 30.
  • a liquid cryogen such as liquid nitrogen
  • plastic foam 30 can absorb liquid nitrogen up to six times faster than previously used materials. This feature accelerates the process of charging dewar vessel 2 with liquid cryogen. It is especially preferred that plastic foam 30 has a free volume of between approximately 85% to approximately 95%.
  • Plastic foam 30 is preferably an "azotophilic" adsorbent capable of acquiring and retaining liquid nitrogen cryogen in place because of high surface tension that exists between the liquid nitrogen (or, if applicable, and alternative liquid cryogen) and the foam.
  • Azotophilic means nitrogen loving, i.e., having an affinity for nitrogen in any of its valence states.
  • shipping container 1 of the present invention can be shipped in any orientation, including upside down, without danger of spilling or having the liquid nitrogen directly contact a specimen vial.
  • multiple segments 31 of plastic foam 30 have a thickness or height, measured in any dimension, for a given type of foam material and cryogen, such that the liquid cryogen held within the chosen foam will not ooze or flow out of the foam when the orientation of the foam is changed.
  • at least one linear dimension of a segment will be exceeded if the segment is capable of holding liquid cryogen in one spatial orientation but oozes cryogen in any other orientation.
  • the linear dimensions of foam segments 31 be chosen to optimize the amount of liquid cryogen held within plastic foam 30 (i.e., all of foam segments 31 combined) while minimizing the number of capillarity separation layers 32 required to separate foam segments 31.
  • plastic foam is superior because it possesses a micro-porous structure that promotes capillarity, or capillary action.
  • Capillary action is the result of adhesion (adsorption) and surface tension. Adhesion of a liquid to the walls of a uniform circular vessel (or tube or pore) will cause an upward force on the liquid at the edges of the vessel. Surface tension acts to hold the surface intact, so instead of just the edges moving upward, the whole liquid surface is dragged upward. Capillary action occurs when the adhesion of the liquid to the walls is stronger than the cohesive forces between the liquid molecules. The height to which capillary action will take a liquid in a uniform circular tube is limited by surface tension.
  • the plastic foam of the present invention is made up of perfect capillary tubes (i.e., cylindrical tubes) or that the maximum height of the segments of plastic foam used in the present invention be determined by the formula stated above; instead, the important characteristic is that the plastic foam exhibits strong capillary action. Capillary action is limited by a maximum dimensional height, which will hereinafter be defined as a "critical height," that a given liquid cryogen will reach in the capillary like pores of the adsorbent plastic foam in a given spatial orientation. When the plastic foam exceeds this height, any additional plastic foam exceeding the critical height is physically incapable of retaining additional liquid cryogen in-situ as a result of capillary action.
  • the height of a given segment of plastic foam is equal to, or less than, its critical height for its intended liquid cryogen (which is usually liquid nitrogen).
  • the same principle is applicable to other dimensions if the plastic foam is being held within a container in which it could have other orientations that would cause the height of plastic foam in a given orientation to exceed the critical height.
  • Capillarity separation layers 32 do not have to be especially thick. Instead, their thickness is dependent upon a thickness that is required to perform their intended function for a given plastic foam and an intended liquid cryogen. Capillarity separation layers 32 function to seal off a plastic foam so as to limit the functional height of its capillary like pores, and thereby permit segments of plastic foam to have a height less than the critical height, and thereby prevent liquid cryogen from oozing or flowing out of the segments if their spatial orientation is changed. Capillarity separation layers 32 should be made of a cryogenically compatible material, such as treated paper, Tyvek® spunbonded olefin, or Teflon® FEP. A 3mm layer of Tyvek® has been found to perform this function well.
  • specimen chamber 70 be made of an open- celled porous thermoplastic material that is cryogenically compatible, such as an aerated polypropylene foam.
  • Specimen chamber 70 can be formed in a single piece construction with a base 72 connected to a cylindrically-shaped side wall 71 having a top opening 73. The outer circumference of side wall 71 at top opening 73 is sealed to either neck portion 21 or an inner wall of inner vessel 13.
  • Specimen chamber 70 should allow liquid cryogen to pass through it into plastic foam 30 and allow the cryogen in a vaporous state to pass into it from absorbent foam 30.
  • the thermoplastic material of specimen chamber 70 acts as a filter to prevent particles or fragments of plastic foam 30 from entering into specimen chamber 70, and it also acts as a wicking device for rapid transfer of the liquid cryogen into plastic foam 30.
  • specimen chamber 70 is lightweight and less expensive to manufacture than previous specimen chambers made of metal or a metal alloy. The combination of specimen chamber 70 and plastic foam 30 in the preferred embodiment of dewar vessel 2 results in more efficient utilization of the volume of inner vessel 13 with greatly reduced charging time.
  • plastic foam 30 occupies substantially all of the volume between inner wall 15 of inner vessel 13 and sample chamber 70, and liquid cryogen can rapidly pass from specimen chamber 70 into plastic foam 30 along the entire length of side wall 71.
  • the decreased time required to fully charge a dewar vessel with liquid cryogen is attributable to the physical properties of specimen chamber 70 and plastic foam 30. These properties can be demonstrated by pouring up to approximately fifty percent of a full charge of liquid cryogen into specimen chamber 70 of shipping container 1 and then turning container 1 upside down. By the time shipping container 1 is turned upside down, all of the liquid cryogen will be retained by plastic foam 30 and virtually no liquid cryogen will be released.
  • FIGs 4A and 4B illustrate an especially preferred self-venting cap 100 for use with a dewar vessel 2.
  • Self-venting cap 100 has four primary components-a lower component 101 with a first plurality of apertures 121 , an upper component 102 with a second plurality of apertures 122, a seal 103, and a third component 104. It is especially preferred that all of these four primary components be constructed of a cryogenically compatible material that is non-metallic and non-conductive.
  • the first, second and fourth components can be made of an injection moldable material such as Acetyl.
  • the outer circumference of lower component 101 is less than the inner circumference of neck 21 and the first plurality of apertures 121 is located inside of the outer circumference of the lower component as shown in Figures 4A and 4B.
  • seal 103 which is preferably made of silicone rubber, is attached to lower component 101 by a snap, friction fit.
  • Lower component 101 is secured to upper component 102 and third component 104 by two different means.
  • a screw 106 (threads not shown) is screwed into a female thread 108 in lower compartment 101 and held in place by plate 105.
  • a cover plate 107 (shown with a trademark of Cryoport, Inc.) covers and seals the chamber in third component 104 in which the top of plate 105 and the head of screw 106 are held.
  • Screw 106 holds all four primary components together in a cap assembly in which the individual primary parts can still move relative to each other.
  • second component 102 is held between first component 101 and third component 104
  • seal 103 is held between first component 101 and second component 102.
  • lower component 101 has a male thread 111 that screws into female thread 112 of third component 103.
  • seal 103 is held in a taut position (see Figure 5B) relative to the position it is held when male thread 111 is fully screwed into female thread 112 in a compression seal position (see Figure 5C).
  • Seal 103 changes position between Figures 5B and 5C when third component 104, which functions as a crank top, is rotated in a tightening direction that causes seal 103 to be squeezed between lower and upper components 101 and 102 so as to form a compression seal with neck 21.
  • Figure 5B shows cap 100 before it is in a compression seal position while Figure 5C shows cap 100 once it is in a compression seal position.
  • Ribs 115 of third component 104 rest against upper component 102, which serve as a stop, and thereby create a plurality of vent openings, in the compression seal position.
  • the left half of Figure 5C has been slightly rotated to show a clear vapor path instead of such a top.
  • a positioning device 113 shown as indentations in Figure 4B
  • FIG. 1 shows a second positioning device 114 (shown as nubs in Figure 1 ) to prevent cap 100 from spinning during the tightening process.
  • Vent opening 133 can be a single opening or a plurality of openings.
  • vent opening 133 is located between third component 104 and plate 60, but it could also be located between third component 104 and neck 21 if plate 60 is not used.
  • Vent opening 133 is located outside of the inner circumference of neck 21 because upper component 102 has an upper outer circumference that is located outside of the inner circumference of neck 21.
  • Self-venting cap 100 provides many advantages over traditional caps for dewar vessels.
  • self-venting cap 100 is the strength of the compression seal it forms with neck 21 of dewar vessel 2.
  • the seal can be strong enough to support the weight of dewar vessel 2 when it is not charged with a cryogen, or even stronger. This degree of strength is important when container 1 is subjected to shock or impact because cap 100 restricts access to, and effectively seals off access to, the contents of specimen chamber 70 and specimen containment systems inside of dewar vessel 2.
  • Another advantage of self-venting cap 100 is that it creates a plurality of tortuous vapor paths for venting dewar vessel 2.
  • a tortuous vapor path increases the thermal length that gas venting from the dewar vessel must travel. Increasing the thermal length increases the thermal efficiency of the dewar vessel, thereby increasing the hold time for the shipping container. Multiple venting paths increases safety because it eliminates the possibility that a single venting path might become clogged, leading to dangerous build-up of gas.
  • each of the first plurality of apertures 121 leads into first chamber 131
  • each of the second plurality of apertures 122 leads out of first chamber 131 and into second chamber 132.
  • vapor inside of dewar vessel 2 can travel in a plurality of tortuous paths when cap 100 is in the compression seal position.
  • the plurality of tortuous paths begin within neck 21 and then sequentially travel up through first plurality of apertures 121 , first chamber 131 , second plurality of apertures 132, second chamber 132 and then out vent opening 133.
  • gas need not always leave the chamber at the same point or points.
  • first and second chambers 131 and 132 provide a void space that can be accessed by a plurality of apertures, they create a number of different vapor paths, as already noted. However, they also provide a void space in which gas can accumulate and intermix. This creates an additional benefit because the chambers can have different temperature gradients, and gases entering or leaving these chambers can have different temperature gradients as a result of mixing with gas contained in these chambers.
  • Chambers 131 and 132 also act as buffer zones between gas flowing from outside of cap 100 into inner vessel 13 and gas flowing from inside of inner vessel 13 to outside of cap 100.
  • Cap 100 can also include one or more semi-permeable membranes (not shown in the Figures) to prevent moisture (water vapor) from entering from entering into the dewar vessel while still allowing vaporous cryogen to exit from the dewar vessel.
  • a membrane could be used to cover either or both of the first and second plurality of apertures 121 and 122.
  • a semi-permeable membrane could be placed at any other convenient location in the vapor path shown in Figure 5C; however, it is preferable that it be conveniently included as part of cap 100 or inner cap 90. Including a semi-permeable membrane in the cap minimizes the portion of the vapor path that is restricted by the membrane and provides the membrane with a convenient structural component for incorporation and structural integrity.
  • Figure 6 illustrates a containment system that is especially useful for dangerous materials (such as potentially biohazardous or infectious agents) that is designed and constructed to withstand the standards of UN Class 6.2 certification.
  • this containment system is used with self-venting cap 100 illustrated in Figures 4A and 4B in an especially preferred shipping container as illustrated in Figures 1 and 2, the result is an economical and superior shipping container that meets rigid shipping regulations concerning shipment of dangerous (infective) materials.
  • Containment system 80 is based upon a primary porous structural cartridge
  • bag 81 As shown in steps 1 through 4 of Figure 4, structural cartridge 83 is placed into bag 81 , bag 81 is sealed to complete containment system 80, and then containment system 80 can be lowered into specimen chamber 70 through dewar opening 11 by bag handle 82. Handle 82 can be made from a loop of the polymer film used to make bag 81.
  • Bag 81 is made of a cryogenically compatible polymer film with a sealing mechanism that assures a liquid and vapor tight seal when actuated.
  • a fluorinated ethylene propylene resin or a polyimide film have been found suitable for this purpose, and Teflon® FEP Grade 160 or Kapton® FN film are especially preferred.
  • Teflon® FEP is a fluorinated ethylene propylene resin that meets American Society for Testing and Materials ("ASTM") Standard Specification D2116-97 for FEP-Fluorocarbon Molding and Extrusion Materials.
  • Kapton® FN is a high-quality plastic film commercially available from DuPont.
  • Tyvek® spunbonded olefin and in particular DuPont® Medical grade Tyvek® types S-1059-B and S-1073B, are also suitable for use as bag 81.
  • the sealing mechanism should create a seal that prevents liquid or vapor from entering or leaving the interior of bag 81.
  • the sealing mechanism can be a mechanical closure (in which case it is especially preferred that it be constructed of two materials with dissimilar coefficients of thermal expansion), an adhesive joint, or a heat seal.
  • structural cartridge 83 contain more than one cartridge. Each cartridge has a plurality of sample apertures to hold a plurality of sample receptacles separate from one another.
  • the top cartridge of structural cartridge 83 has a base 85 and a cover 87 that mates with cartridge base 85 to enclose the plurality of sample receptacle apertures 86 and any sample receptacles 84 (vials) held within said plurality of sample receptacle apertures.
  • the bottom of cartridge base 85 is designed so that it can function as a cover 87 to mate with an additional cartridge base 88. Stacking additional cartridge bases in the same fashion increases the size of cartridge 83.
  • structural cartridge 83 i.e., cover 87, base 85 and any additional bases 88
  • cover 87, base 85 and any additional bases 88 are made of a polypropylene polymer compound.
  • Each cartridge has sufficient absorbing capacity to absorb the entire contents of all of the plurality of sample receptacles held within the plurality of sample receptacle apertures. It is especially preferred that each cartridge have sufficient absorbing capacity to absorb twice the entire contents of all of the plurality of sample receptacles held within the plurality of sample receptacle apertures.
  • Structural cartridge 83 performs two essential requirements of the
  • IATA Packing Instruction 602 which states "[mjultiple primary receptacles placed in a single secondary packaging must be wrapped individually or for infectious substances transported in liquid nitrogen, separated and supported to ensure that contact between them is prevented.”
  • Cartridge 83 clearly meets this requirement and is an advance over current practices in the art in which it is common just to wrap receptacles loosely in sheets of absorbent cloth.
  • the second requirement, found in IATA 602, states “[t]he absorbing material, for example cotton wool, must be sufficient to absorb the entire contents of all primary receptacles.” Again, cartridge 83 does this, with additional safety, and represents a significant advance in the current state of the art.

Landscapes

  • Engineering & Computer Science (AREA)
  • Thermal Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Health & Medical Sciences (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Wood Science & Technology (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Packages (AREA)

Abstract

A shipping container (1) with an outer shipping container shell (3) and a support assembly for holding a dewar vessel (2) within the outer shipping container shell and providing impact and vibration resistance to the dewar vessel (3). The dewar vessel (3) has an inner vessel (13) that holds a specimen chamber (70) and plastic foam (30) between its inner wall and the specimen chamber. The specimen chamber (70) allows liquid cryogen to pass through it into the plastic foam (30), allows liquid cryogen in a vapor phase liquid state to pass from the plastic foam (30) into it, and acts as a filter to prevent particles or fragments of the plastic foam form from entering into it.

Description

CRYOGENIC SHIPPING CONTAINER
Field of the Invention
The present invention is in the field of cryogenic shipping containers.
Background of the Invention
To ensure reproducible results in research and biotechnical processes, today's scientists and clinical practitioners have found it necessary to genetically stabilize living cells and preserve the integrity of complex molecules for storage and transport. This is accomplished by containing these materials in enclosures where cryogenic temperatures are continuously maintained at or near liquid nitrogen or vapor phase liquid nitrogen temperatures (77K and 100K, respectively).
Advances in cryopreservation technology have led to methods that allow low-temperature maintenance of a variety of cell types and molecules. Techniques are available for the cryopreservation of cultures of viruses and bacteria, isolated tissue cells in tissue culture, small multi-cellular organisms, enzymes, human and animal DNA, pharmaceuticals including vaccines, diagnostic chemical substrates, and more complex organisms such as embryos, unfertilized oocytes, and spermatozoa. These biological products must be transported or shipped in a frozen state at cryogenic temperatures to maintain viability. This requires a shipping enclosure that can maintain a cryogenic environment for up to 10 days and meet other shipping requirements such as being relatively impervious to mechanical shock and effects of directional orientation.
In addition to the already existing difficulties posed in shipping heat- sensitive biologicals, the International Air Transport Association (IATA) imposed new regulations which became effective in January 1995 pertaining to all shipments that include specimens containing infectious agents or potentially infectious agents. These regulations, endorsed by the United States Department of Transportation (DOT) and applicable to all public and private air, sea, and ground carriers, imposed greatly increased requirements upon shipping units to survive extensive physical damage (drop-testing, impalement tests, pressure containment tests, vibration tests, thermal shock, and water damage) without leakage and without fracture of the internal, primary receptacles (vials). Implementation of this regulation further complicated the shipping of frozen biologicals. Even though bioshippers are currently available using liquid nitrogen as a refrigerant, little innovation has taken place in the design of packaging for low- temperature transport. Current shippers are generally vulnerable to the physical damage and changes in orientation encountered during routine shipping procedures. Additionally, these shippers rarely comply with the IATA Dangerous Goods Regulation (effective January 1995 or as later amended). Commercial vendors have not developed or certified a cost-effective, standardized shipping unit with the necessary specimen capacity and hold time to meet user demands.
One of the main criticisms of current shippers is price, which varies from $500.00 to $1 ,000.00 or more per unit. This substantially limits their use for the transport of many biologicals. Because of the initial cost and limited production of these containers, they are designed to be reusable. However, the cost of return shipping of these heavy containers is significant, particularly in international markets. Users also complain about the absorbent filler used in the current dry shippers, which breaks down with continuous use, contaminating the interior of the container. In fact, one large user of these containers has essentially centered their entire shipping operation around cleaning the broken down absorbent material from the inside of these containers after each use. Another problem cited by users of currently available dry shippers relates to the functional hold time versus static hold time. Static hold time pertains to a fully charged shipper with no heat load, sitting upright, e.g., essentially not in use. Functional hold time refers to the fully charged shipper in use and containing samples, e.g., in the process of being handled and transported. Even though the static hold time is often promoted as being 20 days, if the container is tilted or positioned on its side, the hold time diminishes to hours as opposed to days. This occurs because the liquid nitrogen transitions to the gaseous (vapor) phase more rapidly resulting in outgassing. The liquid nitrogen can also simply leak out of the container when it is positioned on its side. The current cryogenic containers are promoted as being durable because they are of metal construction. However, rugged handling frequently results in the puncturing of the outer shell or cracking at the neck, resulting in loss of the high vacuum insulation. This renders them useless. The metal construction also adds to the weight of the container, thereby adding substantially to shipping costs. Thus, there is a need for an improved cryogenic container that can be used to ship biologicals safely, reliably, and economically.
U.S. Patent No. 6,119,465 seeks to meet this need by using unique, lightweight, low-cost, durable composites and polymers in a semi-disposable vapor phase liquid nitrogen bioshipper. This is accomplished in an inherently simple, reliable, and inexpensive device that will result in reduced shipping costs, enhanced reliability and safety, and fewer service requirements.
The present invention builds upon the framework laid by U.S. Patent No. 6,1 19,465, the disclosure of which is specifically incorporated herein by reference. This is done by use of a cryogenic shipping container that has many significant advances over what is disclosed in our earlier patent. The end result is a much improved cryogenic shipping container that is more economical while still being reliable.
Summary Of The Invention
The present invention is generally directed to a portable, insulated shipping container. The shipping container has an outer shipping container shell and a support assembly for holding a dewar vessel within the outer shipping container shell and providing impact and vibration resistance to the dewar vessel. The dewar vessel has an inner vessel that holds a specimen chamber and plastic foam between its inner wall and the specimen chamber. The specimen chamber allows liquid cryogen to pass through it into the plastic foam, allows liquid cryogen in a vapor phase liquid state to pass from the plastic foam into it, and acts as a filter to prevent particles or fragments of the plastic foam from entering into it. It is preferred that the specimen chamber is an open-celled porous thermoplastic material that is cryogenically compatible, and it is especially preferred that it be an aerated polypropylene foam. It is preferred that the plastic foam is an open cell plastic foam, and it is especially preferred that it be a phenolic foam. In a first, separate group of aspects of the present invention, the plastic foam can hold a normal charge of liquid cryogen in a dry vapor state regardless of the container's spatial orientation. The plastic foam can be made of multiple foam segments having a maximum thickness less than a critical height with each segment being separated by a capillarity separation layer. The thickness of the foam segments is preferably selected so that the head pressure of the plurality of foam segments will not cause liquid cryogen to ooze or flow out of the foam segments when their spatial orientation is changed. This thickness can be less than approximately four inches. The foam can occupy substantially all of the volume between the inner wall of the inner vessel and the sample chamber. Materials suitable for use as the capillarity separation layer include paper products treated to resist water and spunbonded olefin film.
In other, separate aspects of the present invention, a self-venting cap is used to restrict access to the specimen chamber when it forms a compression seal with an inner circumference of the neck of the dewar vessel. The cap creates one or more tortuous paths through it when it is in the compression seal position. The cap can be made of a lower component with a first plurality of apertures, an upper component having a second plurality of apertures, a seal held between the lower and upper components, and a third component secured to the upper component. It is especially desirable that the components of the cap in the vapor paths are made of a cryogenically compatible material that is non-metallic and non-conductive. A first chamber can be formed between the lower and upper components while a second chamber and a vent opening can be formed between the upper and third components. Vapor can travel through the cap in any of multiple tortuous vapor paths beginning with the first plurality of apertures and then proceeding through the first chamber, the second plurality of apertures, the second chamber and then out a vent opening. One or more semi-permeable membranes can be used to prevent moisture (water vapor) from entering into the dewar vessel while still allowing vaporous cryogen to exit from the dewar vessel. In still other, separate aspects of the present invention, the shipping container is configured so that a reservoir will be formed within the dewar vessel when the container rests on its side so that gravity will not force vapor phase liquid cryogen in the reservoir out of the dewar vessel. The reservoir can be formed by configuring the container so that there will be an angle of approximately six degrees or greater between a flat planar surface and a cross section of the specimen chamber taken from an upper end closest to its top wall and extending down through a lower end closest to its base when the side wall of the container is resting on the flat planar surface. The reservoir can also be formed by a plane that is substantially parallel to the flat planar surface which intersects with the base of the specimen chamber and a first aperture of a self-venting cap that forms a compression seal with the neck of the dewar vessel.
In yet still other, separate aspects of the present invention, the shipping container can have a funnel-shaped vessel plate affixed to the dewar vessel. The shipping container can be made of a rigid thermoplastic material having a base, a side wall and a top wall. The top wall can be connected to the side wall by a movable access assembly, such as a hinge and latching mechanism, and the latching mechanism can be held in a locked position by a lock. The side wall can include a top side wall with a pocket for holding paperwork and a top opening for accessing a dewar opening in the dewar vessel and the top side wall can be covered by the top wall. A safety strap with a locking mechanism, such as an adjustable buckle, can be affixed to the bottom of the dewar vessel and surround the dewar vessel in a closed position so that it also holds the self-venting cap in place. An inner plug of a cryogenically compatible insulating plastic foam with a handle can be held in the neck portion between the self-venting cap and the specimen container. The support assembly can have multiple parts or be a single piece, such as a material that is injected or poured into the shipping container's shell to fill the available space.
In a further, separate aspect of the present invention, the portable shipping container can be made to comply with United States Department of Transportation/International Air Transport Association (DOT/IATA) Dangerous Goods Regulations.
Accordingly, it is a primary object of the present invention to provide an improved, portable, insulated shipping container that uses a dewar vessel that can be charged with a liquid cryogen.
This and further objects and advantages will be apparent to those skilled in the art in connection with the drawings and the detailed description of the preferred embodiment set forth below. Brief Description Of The Drawings
Figure 1 is an exploded assembly drawing of a preferred embodiment of a portable, insulated shipping container according to the present invention with a containment system for dangerous materials. Figure 2 is a planar cross section with a partial cutaway view of a preferred embodiment of a portable, insulated shipping container.
Figure 3 is an assembly drawing of a preferred embodiment of a dewar vessel assembly.
Figure 4 is an exploded assembly drawings of a preferred embodiment of a self-venting cap taken from reverse directions.
Figures 5A-5C are a planar cross section of a preferred embodiment of a portable, insulated shipping container showing connection of a preferred self- venting cap.
Figure 6 depicts an assembly of a preferred embodiment of a containment system.
Detailed Description Of The Preferred Embodiments
The preferred embodiments of the present invention can be used as part of an overall system that utilizes several inventions. Broadly speaking, there is an overall cryogenic shipping container system. Within the shipping container, there is a dewar vessel. Within the dewar vessel, there is a specimen chamber for holding specimens. And, in certain applications, such as shipping of dangerous goods, the specimens are held within a containment system. Although Figures 1- 6 are described in greater detail below, the following is a glossary of the elements identified in the Figures:
1 portable, insulated shipping container 2 dewar vessel
3 outer casing of dewar vessel 2 3a upper half of outer casing 3 3b bottom half of outer casing 3
4 opening at top of outer casing 3 5 evacuable space between outer casing 3 and inner casing 13
6 getter pack
7 desiccant
8 nipple
10 layer of super insulation 11 dewar opening into inner vessel 13
13 inner vessel of dewar vessel 2 13a upper half of inner vessel 13
13b lower half of inner vessel 13
14 opening at top of inner vessel 13 15 inner wall of inner vessel 13
21 neck portion of dewar vessel 2
30 plastic foam
31 foam segment of plastic foam 30
32 capillarity separation layer of foam 30 outer shipping container shell base of outer shipping container shell 40 side wall of outer shipping container shell 40 a top side wall of side wall 42 b top opening formed in top side wall 42a top wall of outer shipping container shell 40 handle molded in outer shipping container shell 40 pocket for paperwork formed in outer shipping container shell 40 hinge mechanism latch mechanism certification plate assembly a certification plate b rivet for certification plate assembly 48 c indentation in outer shipping container shell 40 for certification plate support assembly for dewar vessel 2 bottom portion of support assembly 50 side rib portion of support assembly 50 top portion of support assembly 50 safety strap adjustable buckle of safety strap 55 outer bottom of dewar vessel 2 funnel-shaped vessel plate support for plate 60 spray foam specimen chamber side wall of specimen chamber 70 base of specimen chamber 70 top opening of specimen chamber 70 containment system bag of containment system 80 handle of containment system 80 porous structural cartridge of containment system 80 sample receptacle of containment system 80 cartridge base of containment system 80 sample receptacle apertures of containment system 80 cartridge cover of containment system 80 additional cartridge base of containment system 80 inner plug handle of inner plug 90 self-venting cap lower component of self-venting cap 100 upper component of self-venting cap 100 a lower surface of upper component 102 seal of self-venting cap 100 third component of self-venting cap 100 plate screw (threads not shown) cover plate 108 female thread in lower component 101
111 male thread
112 female thread
113 positioning device 114 second positioning device
115 rib
121 first plurality of apertures in lower component 101
122 second plurality of apertures in upper component 102 131 first chamber of self-venting cap 100 132 second chamber of self-venting cap 100
133 vent opening of self-venting cap 100
Figure 1 provides an assembly drawing that illustrates all of the components of the cryogenic shipping container, generally designated as 1 , in a disassembled state, and Figure 2 illustrates how all of these components fit together in an assembled state. Figure 3 is an assembly drawing that illustrates how dewar vessel 2 is assembled.
As shown in Figure 1 , the dewar vessel, generally designated as 2, has a specimen chamber 70 that is accessed by a dewar opening 11. When shipping container 1 is ready for use after it has been fully charged with a liquid cryogen, a sample receptacle is placed inside of specimen chamber 70 through dewar opening 11. As shown in Figure 1 , and as described in greater detail in connection with Figure 6, one form that the sample receptacle may take is a containment system 80 in which a porous structural cartridge 83 is held within a bag 81 with a handle 82. After containment system 80 is placed inside of specimen chamber 70, an inner plug 90, with a handle 91 , is placed inside of dewar opening 11. (Inner plug 90, which can be made of polyurethane foam that is cryogenically compatible, acts as both a spacer and an insulator.) Next, a self- venting cap 100 is inserted into dewar opening 11 through funnel-shaped vessel plate 60 and tightened so as to create a compression seal (this is shown in Figures 5A-5C). After the compression seal has been formed, an adjustable buckle 56 of safety strap 55 can be closed and tightened (any suitable alternative connection mechanism could be substituted for a buckle, if desired). Safety strap 55 can be made of a webbing material, and it is affixed to an outer bottom 57 of dewar vessel 2 by adhesive tape or some other affixation means. Safety strap 55, when properly closed and tightened, provides additional integrity to dewar vessel 2 and helps prevent loss or separation of self-venting cap 100 and containment system 80. The dewar vessel assembly is held within an outer shipping container shell
40 made of a lightweight, but rigid, material that helps to provide shock and impact resistance, such as low density polyethylene. Outer shipping container shell 40 has a "base" 41 , a "side wall" 42, and a "top wall" 43 that surround and enclose dewar vessel 2 during shipping. From a definitional standpoint, when container 2 is resting upon a flat planar surface (such as the ground or a floor of a transportation vehicle) in its intended and desired orientation (in other words, not on its side or upside down), base 41 is the portion of shell 40 that rests upon the flat planar surface, top wall 43 is the outermost portion of shell 40 distant from base 41 which is somehow movable to permit access inside of the container (e.g., the top lid of a box) and side wall 42 is whatever connects base 41 to top wall 43 (e.g., a square box or rectangle has four planar surfaces that form the side wall).
Dewar vessel 2 can be inserted into shell 40 through base 41 and then base 41 can be affixed to side wall 42 by a suitable sealing means, such as screws. Mechanisms for providing evidence of tampering with shell 40, or improper orientation of container 1 during shipping, or means for tracking container 1 during shipping (e.g., by a global positioning system), can be enclosed within shell 40 at or near base 41. In the preferred embodiment of shipping container 1 illustrated in Figure 1 , top wall 43 is a cover that is attached to side wall 42 by a hinge mechanism 46 (comprised of two hinges) and a latch mechanism 47. During shipping, latch mechanism 47 can be held in a locked position by a lock (not shown) to provide security against tampering. (In this context, a "lock" could include not only a traditional lock that might require a key or combination to open, but also a secured band or tamperproof device or a device that would indicate that tampering has occurred.) Top wall 43, in a closed position, covers a top side wall 42a of side wall 42. Top side wall 42a includes a top opening 42b through which dewar opening 11 can be accessed when top wall 43 is in an open position, latch mechanism 47 is undone, and self-venting cap 100 is removed. Top side wall 42a also includes a pocket 45 for paperwork (e.g., an inventory check list, shipping documents or operating instructions). Pocket 45 is accessible when top wall 43 is not latched in place to side wall 42 and inaccessible when it is latched in place. Handles 44 can be molded into side wall 42. Side wall 42 can also have a certification plate assembly 48 (a certification plate 48a held in indentation 48c by rivets 48b) for affixing and displaying important information, such as a container serial number, certifications, warnings, bar codes, etc.
A support assembly 50 holds dewar vessel 2 within shell 40. In an especially preferred embodiment, support assembly 50 is made up of several different pieces of lightweight, shock-absorbing foam material. Support assembly 50 has a bottom portion 51 in contact with base 41 to protect the bottom of dewar vessel 2, side rib portions 52 in contact with side wall 42 to protect the sides of dewar vessel 2, and a top portion 53 to protect the top of dewar vessel 2. Side rib portions 52 can be attached to side wall 42 by adhesive or tape. Top portion 53 of support assembly 50 can be held in place by rib portions 52.
As shown in Figure 1 , shipping container 1 includes a funnel-shaped vessel plate 60. The funnel shape of plate 60 makes it easier to pour liquid cryogen into dewar vessel 2. It also helps to restrict access into the interior of shell 40 through top opening 42b. It also contains a position device 114 which are three nubs that are used by self-venting cap 100 to help lock it in place and form a compression seal with the outer circumference of neck portion 21 of dewar vessel 2. (Throughout this description, and in the attached claims, "circumference" or "circumferential" is used to refer to a perimeter or periphery, which may or may not be circular. Thus, by way of example, the inner circumference of a square neck would have a square shape.) Vessel plate 60 is held in place by sealing it to neck portion 21 by adhesive so that there is no liquid or vapor gap between vessel plate 60 and neck portion 21. Additional stability for the seal is provided by spray foam 61 , and supports 61 help position and support plate 60 inside of shell 40. Vessel plate 60 should be made of a cryogenically compatible material. Once shipping container 1 is fully assembled, dewar vessel 2 should be held securely within shell 40 in a fixed position, and shell 40 and support 50 should provide impact resistance and protection to dewar vessel 2 in any spatial orientation. When it is in its normal, upright position, i.e., when its weight is resting on base 41 , specimen chamber 71 is substantially perpendicular to base 41. This is the optimal position for container 1 because of the physical characteristics of vaporous cryogen, such as nitrogen. Vapor phase liquid nitrogen has a greater density than air, so it will behave similar to a liquid when it is confined within a container. As long as the vapor phase liquid nitrogen is retained within the dewar vessel, it helps to maintain cryogenic temperatures in the dewar vessel necessary for the cryopreservation of biologicals. This is because the temperature of vapor phase liquid nitrogen is cryogenic (100K). However, if the dewar vessel is positioned upside down, the vapor phase liquid nitrogen will egress from the dewar vessel, much like a fluid, because vapor phase liquid nitrogen in denser than air. Thus, when the dewar vessel is positioned upright, the vapor phase liquid nitrogen will accumulate in the dewar vessel until sufficient pressure buildup forces excess vapor phase liquid nitrogen out of the dewar vessel.
Although it is highly desirable for shipping container 1 to be stored and shipped in its upright position when it is charged with a liquid cryogen, the realities associated with modern day shipping do not always assure such a result. The preferred embodiment of a shipping container shown in Figure 1 seeks to address this reality, and increase its efficiency, in a simple and economical fashion. Outer shell 40 is designed so that if container 1 ends up being stored or shipped on its side, specimen chamber 70 and dewar opening 11 will still be held at an angle thereby creating a reservoir. The reservoir will have the effect of retaining vapor phase liquid cryogen. By contrast, if no reservoir exists, specimen chamber 70 and dewar opening 11 would be positioned in a substantially parallel position relative to the ground. Such parallel positioning would result in the vapor phase liquid nitrogen pouring out of the vessel in a similar fashion to a glass of water tipping over and spilling its contents.
To create a reservoir, side wall 42 is designed so that when it rests on a flat planar surface the angle formed by the intersection of the planar cross section of specimen chamber 70 with the flat planar surface is approximately six degrees or greater. This is accomplished for container 1 shown in Figure 1 by making the six planar portions of side wall 41 progressively wider as they extend away from base 41 until they reach a maximum thickness near top wall 43. The exact degree of the angle is a matter of design choice, and it will depend upon the overall configuration of the container and the desired result. However, the angle should be sufficient to produce a functional reservoir. In addition, using a self-venting cap 100 that forms a compression seal about the inner circumference of neck 21 will increase the volume of the reservoir.
The basic design and functioning of a "dewar vessel" is well known and long established. In fact, the term "dewar vessel" is defined in Webster's third new international dictionary of the English language, unabridged (1981 ) as "a usu. glass or metal container with at least two walls that has the space between the walls evacuated so as to prevent the transfer of heat, often has a coating (as silvering) on the inside to reduce radiation, and is used esp. for storing liquefied gases (as liquid air) or for investigations at low temperatures." Examples of various United States Patents that teach the use of dewar vessels with a liquid cryogen for use in a shipping container include 2,396,459, 3,298,185, 4,481 ,779 and 4,495,775. The dewar vessels disclosed in these patents, and dewar vessels used in shipping containers today, share certain common characteristics. These characteristics, which will hereinafter be defined as being present in a dewar vessel, are an outer casing and an inner vessel with each having openings at their tops connected together by a neck portion forming an evacuable space between the outer casing and the inner vessel and a dewar opening into the inner vessel. A preferred embodiment of dewar vessel 2 according to the present invention is constructed as follows. Neck portion 21 is sealed to specimen chamber 70 by epoxy. A plastic foam 30 that holds a liquid cryogen (not shown) is formed in several segments 31 that are separated by a capillarity separation layer 32. Plastic foam 30 surrounds specimen chamber 70, and then this assembly is placed inside of upper half 13a and lower half 13b which are joined together to form inner vessel 13 with an opening 14 at its top. A getter pack 6 and a desiccant 7 are secured to the top outside of inner vessel 13 by epoxy and metal tape, respectively. (The use of a getter pack and a desiccant are well known within the industry and are not an inventive aspect of the present invention.) Next, a layer of super insulation 10 is used to surround this assembly. For ease of manufacture and economy, it is especially preferred that super insulation 10 be spirally wrapped and that it be constructed of a single component (e.g., a one-sided metalized polymer film). The top of neck portion 21 is then sealed to an opening 4 in upper half 3a by epoxy which is joined together with lower half 3b to form outer casing 3 and an evacuable space 5 between outer casing 3 and inner vessel 13. Once dewar vessel 2 is assembled, evacuable space 5 can only be accessed through nipple 8, specimen chamber 70 can only be accessed through dewar opening 11 , and cryogen cannot pass between specimen chamber 70 and plastic foam 30 (whether in a liquid or in a gaseous state) except through side wall 71 and base 72 of specimen chamber 70. Details regarding especially preferred materials useful for constructing a dewar vessel are disclosed in U.S. Patent No. 6,119,465.
Plastic foam 30 is preferably an open-celled plastic foam that is cryogenically compatible. It is especially preferred that plastic foam 30 be a phenolic foam (such material is inexpensive and commonly used as a water- holding base for floral arrangements). Plastic foam 30 can either be foamed in place or it can be pre-manufactured in blocks and then sectioned down into segments and inserted into the space surrounding specimen chamber 70. It is especially preferred that plastic foam 30 occupies substantially all of the volume between inner wall 15 of inner vessel 13 and specimen chamber 70.
The open cell structure of plastic foam 30 retains a liquid cryogen, such as liquid nitrogen, by absorption, adsorption, and surface tension as it saturates foam 30. The physical properties of a liquid cryogen (such as liquid nitrogen) and plastic foam 30 are such that the liquid cryogen remains in plastic foam 30 and does not migrate back into specimen chamber 70 when plastic foam 30 is properly charged and comprised of correctly dimensioned segments 31. Plastic foam 30 can absorb liquid nitrogen up to six times faster than previously used materials. This feature accelerates the process of charging dewar vessel 2 with liquid cryogen. It is especially preferred that plastic foam 30 has a free volume of between approximately 85% to approximately 95%. Plastic foam 30 is preferably an "azotophilic" adsorbent capable of acquiring and retaining liquid nitrogen cryogen in place because of high surface tension that exists between the liquid nitrogen (or, if applicable, and alternative liquid cryogen) and the foam. ("Azotophilic" means nitrogen loving, i.e., having an affinity for nitrogen in any of its valence states.) As a result, shipping container 1 of the present invention can be shipped in any orientation, including upside down, without danger of spilling or having the liquid nitrogen directly contact a specimen vial. It is especially preferred that multiple segments 31 of plastic foam 30 have a thickness or height, measured in any dimension, for a given type of foam material and cryogen, such that the liquid cryogen held within the chosen foam will not ooze or flow out of the foam when the orientation of the foam is changed. In other words, at least one linear dimension of a segment will be exceeded if the segment is capable of holding liquid cryogen in one spatial orientation but oozes cryogen in any other orientation. It is also especially preferred that the linear dimensions of foam segments 31 be chosen to optimize the amount of liquid cryogen held within plastic foam 30 (i.e., all of foam segments 31 combined) while minimizing the number of capillarity separation layers 32 required to separate foam segments 31.
It is believed that the preferred embodiment of plastic foam is superior because it possesses a micro-porous structure that promotes capillarity, or capillary action. Capillary action is the result of adhesion (adsorption) and surface tension. Adhesion of a liquid to the walls of a uniform circular vessel (or tube or pore) will cause an upward force on the liquid at the edges of the vessel. Surface tension acts to hold the surface intact, so instead of just the edges moving upward, the whole liquid surface is dragged upward. Capillary action occurs when the adhesion of the liquid to the walls is stronger than the cohesive forces between the liquid molecules. The height to which capillary action will take a liquid in a uniform circular tube is limited by surface tension. The height to which capillary action will lift a fluid depends on the weight of the fluid. At some point the force of capillary action in one direction is counteracted by the force of gravity (weight of the fluid) in an opposite direction and the suspended fluid falls because of its own weight. For a cylindrical capillary tube, this height can be determined from the formula h=2T/prg where h equals the maximum height, T equals surface tension of the liquid, p equals density of the liquid (i.e., mass/volume), r equals the radius of the capillary tube, and "g" is needed to change mass (density in grams) to force. It is not necessary that the plastic foam of the present invention is made up of perfect capillary tubes (i.e., cylindrical tubes) or that the maximum height of the segments of plastic foam used in the present invention be determined by the formula stated above; instead, the important characteristic is that the plastic foam exhibits strong capillary action. Capillary action is limited by a maximum dimensional height, which will hereinafter be defined as a "critical height," that a given liquid cryogen will reach in the capillary like pores of the adsorbent plastic foam in a given spatial orientation. When the plastic foam exceeds this height, any additional plastic foam exceeding the critical height is physically incapable of retaining additional liquid cryogen in-situ as a result of capillary action. When plastic foam is physically incapable of retaining liquid cryogen by capillary action, it fails to maximize the amount of liquid cryogen retained within the volumetric space it occupies. Thus, it is desirable that the height of a given segment of plastic foam is equal to, or less than, its critical height for its intended liquid cryogen (which is usually liquid nitrogen). The same principle is applicable to other dimensions if the plastic foam is being held within a container in which it could have other orientations that would cause the height of plastic foam in a given orientation to exceed the critical height.
Capillarity separation layers 32 do not have to be especially thick. Instead, their thickness is dependent upon a thickness that is required to perform their intended function for a given plastic foam and an intended liquid cryogen. Capillarity separation layers 32 function to seal off a plastic foam so as to limit the functional height of its capillary like pores, and thereby permit segments of plastic foam to have a height less than the critical height, and thereby prevent liquid cryogen from oozing or flowing out of the segments if their spatial orientation is changed. Capillarity separation layers 32 should be made of a cryogenically compatible material, such as treated paper, Tyvek® spunbonded olefin, or Teflon® FEP. A 3mm layer of Tyvek® has been found to perform this function well. Empirical results indicate that approximately four inches is a suitable, maximum critical height for the type of plastic foam described herein, and it is especially preferred that multiple segments 31 have a thickness of greater than approximately three inches, with a thickness of about 3.5 inches being especially preferred. It is especially preferred that specimen chamber 70 be made of an open- celled porous thermoplastic material that is cryogenically compatible, such as an aerated polypropylene foam. Specimen chamber 70 can be formed in a single piece construction with a base 72 connected to a cylindrically-shaped side wall 71 having a top opening 73. The outer circumference of side wall 71 at top opening 73 is sealed to either neck portion 21 or an inner wall of inner vessel 13. Specimen chamber 70 should allow liquid cryogen to pass through it into plastic foam 30 and allow the cryogen in a vaporous state to pass into it from absorbent foam 30. The thermoplastic material of specimen chamber 70 acts as a filter to prevent particles or fragments of plastic foam 30 from entering into specimen chamber 70, and it also acts as a wicking device for rapid transfer of the liquid cryogen into plastic foam 30. In addition to its superior physical properties, specimen chamber 70 is lightweight and less expensive to manufacture than previous specimen chambers made of metal or a metal alloy. The combination of specimen chamber 70 and plastic foam 30 in the preferred embodiment of dewar vessel 2 results in more efficient utilization of the volume of inner vessel 13 with greatly reduced charging time. Unlike many prior dewar vessels, plastic foam 30 occupies substantially all of the volume between inner wall 15 of inner vessel 13 and sample chamber 70, and liquid cryogen can rapidly pass from specimen chamber 70 into plastic foam 30 along the entire length of side wall 71. The decreased time required to fully charge a dewar vessel with liquid cryogen is attributable to the physical properties of specimen chamber 70 and plastic foam 30. These properties can be demonstrated by pouring up to approximately fifty percent of a full charge of liquid cryogen into specimen chamber 70 of shipping container 1 and then turning container 1 upside down. By the time shipping container 1 is turned upside down, all of the liquid cryogen will be retained by plastic foam 30 and virtually no liquid cryogen will be released.
Figures 4A and 4B illustrate an especially preferred self-venting cap 100 for use with a dewar vessel 2. The manner in which such a cap functions in an . especially preferred application of shipping container 1 is illustrated in Figures 5A- 5C. Self-venting cap 100 has four primary components-a lower component 101 with a first plurality of apertures 121 , an upper component 102 with a second plurality of apertures 122, a seal 103, and a third component 104. It is especially preferred that all of these four primary components be constructed of a cryogenically compatible material that is non-metallic and non-conductive. The first, second and fourth components can be made of an injection moldable material such as Acetyl. The outer circumference of lower component 101 is less than the inner circumference of neck 21 and the first plurality of apertures 121 is located inside of the outer circumference of the lower component as shown in Figures 4A and 4B.
When self-venting cap 100 is assembled, seal 103, which is preferably made of silicone rubber, is attached to lower component 101 by a snap, friction fit. Lower component 101 is secured to upper component 102 and third component 104 by two different means.
First, a screw 106 (threads not shown) is screwed into a female thread 108 in lower compartment 101 and held in place by plate 105. A cover plate 107 (shown with a trademark of Cryoport, Inc.) covers and seals the chamber in third component 104 in which the top of plate 105 and the head of screw 106 are held. Screw 106 holds all four primary components together in a cap assembly in which the individual primary parts can still move relative to each other. In this assembly, second component 102 is held between first component 101 and third component 104, and seal 103 is held between first component 101 and second component 102.
Second, lower component 101 has a male thread 111 that screws into female thread 112 of third component 103. When male thread 111 is not fully screwed into female thread 112, seal 103 is held in a taut position (see Figure 5B) relative to the position it is held when male thread 111 is fully screwed into female thread 112 in a compression seal position (see Figure 5C). Seal 103 changes position between Figures 5B and 5C when third component 104, which functions as a crank top, is rotated in a tightening direction that causes seal 103 to be squeezed between lower and upper components 101 and 102 so as to form a compression seal with neck 21. (Figure 5B shows cap 100 before it is in a compression seal position while Figure 5C shows cap 100 once it is in a compression seal position.) Ribs 115 of third component 104 rest against upper component 102, which serve as a stop, and thereby create a plurality of vent openings, in the compression seal position. (The left half of Figure 5C has been slightly rotated to show a clear vapor path instead of such a top.) A positioning device 113 (shown as indentations in Figure 4B) on lower surface 102a of upper component 102 engages with a second positioning device 114 (shown as nubs in Figure 1 ) to prevent cap 100 from spinning during the tightening process.
When self-venting cap 100 forms a compression seal with neck 21 of dewar vessel 2 (as shown in Figure 5C), vapor flow between inner vessel 13 and outside of dewar vessel 2 must flow through vent opening 133. Figure 5C illustrates one such vapor path. The path includes flow through a first chamber 131 located between lower and upper components 101 and 102, and a second chamber 132 located between second component 102 and third component 104. Vent opening 133 can be a single opening or a plurality of openings. In Figure 5C, vent opening 133 is located between third component 104 and plate 60, but it could also be located between third component 104 and neck 21 if plate 60 is not used. Vent opening 133 is located outside of the inner circumference of neck 21 because upper component 102 has an upper outer circumference that is located outside of the inner circumference of neck 21.
Self-venting cap 100 provides many advantages over traditional caps for dewar vessels.
One advantage of self-venting cap 100 is the strength of the compression seal it forms with neck 21 of dewar vessel 2. The seal can be strong enough to support the weight of dewar vessel 2 when it is not charged with a cryogen, or even stronger. This degree of strength is important when container 1 is subjected to shock or impact because cap 100 restricts access to, and effectively seals off access to, the contents of specimen chamber 70 and specimen containment systems inside of dewar vessel 2. Another advantage of self-venting cap 100 is that it creates a plurality of tortuous vapor paths for venting dewar vessel 2. A tortuous vapor path increases the thermal length that gas venting from the dewar vessel must travel. Increasing the thermal length increases the thermal efficiency of the dewar vessel, thereby increasing the hold time for the shipping container. Multiple venting paths increases safety because it eliminates the possibility that a single venting path might become clogged, leading to dangerous build-up of gas.
In the preferred embodiment of cap 100, each of the first plurality of apertures 121 leads into first chamber 131 , and each of the second plurality of apertures 122 leads out of first chamber 131 and into second chamber 132. Thus, vapor inside of dewar vessel 2 can travel in a plurality of tortuous paths when cap 100 is in the compression seal position. The plurality of tortuous paths begin within neck 21 and then sequentially travel up through first plurality of apertures 121 , first chamber 131 , second plurality of apertures 132, second chamber 132 and then out vent opening 133. In addition, because of the volume of chambers 131 and 132, gas need not always leave the chamber at the same point or points. This means there are also a plurality of shorter tortuous paths beginning within the first plurality of apertures 121 , travelling through first chamber 131 , and then up through second plurality of apertures 122. Because first and second chambers 131 and 132 provide a void space that can be accessed by a plurality of apertures, they create a number of different vapor paths, as already noted. However, they also provide a void space in which gas can accumulate and intermix. This creates an additional benefit because the chambers can have different temperature gradients, and gases entering or leaving these chambers can have different temperature gradients as a result of mixing with gas contained in these chambers. Chambers 131 and 132 also act as buffer zones between gas flowing from outside of cap 100 into inner vessel 13 and gas flowing from inside of inner vessel 13 to outside of cap 100. Cap 100 can also include one or more semi-permeable membranes (not shown in the Figures) to prevent moisture (water vapor) from entering from entering into the dewar vessel while still allowing vaporous cryogen to exit from the dewar vessel. For example, such a membrane could be used to cover either or both of the first and second plurality of apertures 121 and 122. (Alternatively, or in addition, a semi-permeable membrane could be placed at any other convenient location in the vapor path shown in Figure 5C; however, it is preferable that it be conveniently included as part of cap 100 or inner cap 90. Including a semi-permeable membrane in the cap minimizes the portion of the vapor path that is restricted by the membrane and provides the membrane with a convenient structural component for incorporation and structural integrity.)
Figure 6 illustrates a containment system that is especially useful for dangerous materials (such as potentially biohazardous or infectious agents) that is designed and constructed to withstand the standards of UN Class 6.2 certification. When this containment system is used with self-venting cap 100 illustrated in Figures 4A and 4B in an especially preferred shipping container as illustrated in Figures 1 and 2, the result is an economical and superior shipping container that meets rigid shipping regulations concerning shipment of dangerous (infective) materials. Containment system 80 is based upon a primary porous structural cartridge
83 and a bag 81. As shown in steps 1 through 4 of Figure 4, structural cartridge 83 is placed into bag 81 , bag 81 is sealed to complete containment system 80, and then containment system 80 can be lowered into specimen chamber 70 through dewar opening 11 by bag handle 82. Handle 82 can be made from a loop of the polymer film used to make bag 81.
Bag 81 is made of a cryogenically compatible polymer film with a sealing mechanism that assures a liquid and vapor tight seal when actuated. A fluorinated ethylene propylene resin or a polyimide film have been found suitable for this purpose, and Teflon® FEP Grade 160 or Kapton® FN film are especially preferred. Teflon® FEP is a fluorinated ethylene propylene resin that meets American Society for Testing and Materials ("ASTM") Standard Specification D2116-97 for FEP-Fluorocarbon Molding and Extrusion Materials. Kapton® FN is a high-quality plastic film commercially available from DuPont. It is believed that Tyvek® spunbonded olefin, and in particular DuPont® Medical grade Tyvek® types S-1059-B and S-1073B, are also suitable for use as bag 81. The sealing mechanism should create a seal that prevents liquid or vapor from entering or leaving the interior of bag 81. The sealing mechanism can be a mechanical closure (in which case it is especially preferred that it be constructed of two materials with dissimilar coefficients of thermal expansion), an adhesive joint, or a heat seal.
It is especially preferred that structural cartridge 83 contain more than one cartridge. Each cartridge has a plurality of sample apertures to hold a plurality of sample receptacles separate from one another. The top cartridge of structural cartridge 83 has a base 85 and a cover 87 that mates with cartridge base 85 to enclose the plurality of sample receptacle apertures 86 and any sample receptacles 84 (vials) held within said plurality of sample receptacle apertures. The bottom of cartridge base 85 is designed so that it can function as a cover 87 to mate with an additional cartridge base 88. Stacking additional cartridge bases in the same fashion increases the size of cartridge 83. The components of structural cartridge 83 (i.e., cover 87, base 85 and any additional bases 88) are made of a polypropylene polymer compound. Each cartridge has sufficient absorbing capacity to absorb the entire contents of all of the plurality of sample receptacles held within the plurality of sample receptacle apertures. It is especially preferred that each cartridge have sufficient absorbing capacity to absorb twice the entire contents of all of the plurality of sample receptacles held within the plurality of sample receptacle apertures. Structural cartridge 83 performs two essential requirements of the
Dangerous Goods Regulations. The first requirement, separation of the primary receptacles, is required by IATA Packing Instruction 602 which states "[mjultiple primary receptacles placed in a single secondary packaging must be wrapped individually or for infectious substances transported in liquid nitrogen, separated and supported to ensure that contact between them is prevented." Cartridge 83 clearly meets this requirement and is an advance over current practices in the art in which it is common just to wrap receptacles loosely in sheets of absorbent cloth. The second requirement, found in IATA 602, states "[t]he absorbing material, for example cotton wool, must be sufficient to absorb the entire contents of all primary receptacles." Again, cartridge 83 does this, with additional safety, and represents a significant advance in the current state of the art.
Although the foregoing detailed description is illustrative of preferred embodiments of the present invention, it is to be understood that additional embodiments thereof will be obvious to those skilled in the art. Further modifications are also possible in alternative embodiments without departing from the inventive concept.
Accordingly, it will be apparent to those skilled in the art that still further changes and modifications in the actual concepts described herein can readily be made without departing from the spirit and scope of the disclosed inventions as defined by the following claims.

Claims

Claims
1. A portable, insulated shipping container, comprising: a dewar vessel having an outer casing and an inner vessel with each having openings at their tops connected together by a neck portion forming an evacuable space between the outer casing and the inner vessel and a dewar opening into the inner vessel; a specimen chamber held within the inner vessel having a base, a side wall attached to the base, and a top opening for allowing access into the specimen chamber through the dewar opening; a plastic foam held within the inner vessel between an inner wall of the inner vessel and the specimen chamber; a self-venting cap that restricts access to the specimen chamber when it is in an engaged position; an outer shipping container shell having a base, a side wall attached to and extending upwardly from the base, and a top wall attached to the side wall opposite of the base, the top wall having a movable access assembly for gaining access from outside of the shipping container shell to the specimen chamber when the self-venting cap is not in an engaged position and the movable access assembly is in an open position but denying access to the self-venting cap in the engaged position when the movable access assembly is an a closed position; and a support assembly for holding the dewar vessel within the outer shipping container shell and providing impact and vibration resistance to the dewar vessel; wherein the specimen chamber allows a liquid cryogen to pass through the specimen chamber into the plastic foam and allows the liquid cryogen in a vapor phase liquid state to pass from the plastic foam into the specimen chamber.
2. A portable, insulated shipping container as recited in claim 1 , wherein the shipping container is configured such that when the base rests on a flat planar surface in an upright position the specimen chamber is held such that a planar cross section of the specimen chamber taken from an upper end closest to the top wall and extending down through a lower end closest to the base and continuing to the flat planar surface is substantially perpendicular relative to the flat planar surface but when the side wall rests on the flat planar surface the angle formed by the intersection of the planar cross section with the flat planar surface is approximately six degrees or greater.
3. A portable, insulated shipping container as recited in claim 1 , wherein the shipping container is configured such that when the side wall rests on the flat planar surface, a reservoir is formed within the dewar vessel underneath a plane that is substantially parallel to the flat planar surface which intersects with the first aperture and the base, and vapor phase liquid cryogen held within the reservoir will not be forced out of the dewar vessel by gravity.
4. A portable, insulated shipping container as recited in claim 1 , wherein the specimen chamber has a chamber wall comprised of an open-celled porous thermoplastic material that is cryogenically compatible and acts as a filter to prevent particles or fragments of the plastic foam from entering into the specimen chamber.
5. A portable, insulated shipping container as recited in claim 1 , wherein the plastic foam is an open cell plastic foam.
6. A portable, insulated shipping container as recited in claim 1 , wherein the plastic foam is comprised of a plurality of foam segments and each foam segment is separated from another foam segment by a capillarity separation layer, wherein each foam segment has a thickness less than a critical height when the container is resting in an upright position.
7. A portable, insulated shipping container as recited in claim 6, wherein the thickness is selected so that the head pressure of the plurality of foam segments will not cause liquid cryogen to ooze or flow out of the foam segments when their spatial orientation is changed.
8. A portable, insulated shipping container as recited in claim 1 , wherein the self-venting cap restricts access to the specimen chamber when it is in a compression seal position that forms a compression seal with an inner circumference of the neck and vapor inside the dewar vessel can travel in a plurality of tortuous paths when the cap is in the compression seal position, the plurality of tortuous paths beginning within the dewar opening and then sequentially traveling up through a first plurality of apertures, a first chamber, a second plurality of apertures, a second chamber and then out a vent opening.
9. A portable, insulated shipping container as recited in claim 8, wherein the self-venting cap creates a tortuous path through it when it is in the compression seal position, the tortuous path forces vapor inside the inner vessel to travel in a tortuous path beginning with a first aperture through the cap to a vent opening, and the first aperture is located in the cap inside an inner circumference of the neck and wherein the shipping container is configured such that when the base rests on a flat planar surface in an upright position the specimen chamber is held such that a planar cross section of the specimen chamber taken from an upper end closest to the top wall and extending down through a lower end closest to the base and continuing to the flat planar surface is substantially perpendicular.
10. A portable, insulated shipping container as recited in claim 1 , further comprising: a funnel-shaped vessel plate made of a cryogenically compatible material affixed to the dewar vessel and extending outwardly from the neck portion to create a liquid-tight and gas-tight funnel for the dewar opening.
1 1. A portable, insulated shipping container as recited in claim 1 , further comprising: a safety strap with a connection mechanism that forms a closed loop when the connection mechanism is closed and an open loop when the connection mechanism is open, the safety strap being affixed to an outer bottom of the dewar vessel and orientated such that it surrounds the dewar vessel, the vessel plate and the self-venting cap when the connection mechanism is closed, the connection mechanism being accessible through the top opening when the top wall is in open position; wherein the side wall includes a top side wall opening that is smaller than an outermost circumference of the vessel plate.
12. A portable, insulated shipping container as recited in claim 1 , wherein the plastic foam holds a normal charge of liquid cryogen so that once the normal charge has passed through the specimen chamber into the plastic foam, it will not return to the specimen chamber in a liquid state in any spatial orientation of the container.
13. A self-venting cap for a neck of a dewar vessel, comprising: a lower component with a first plurality of apertures; an upper component with a second plurality of apertures, a second chamber and a vent opening; a seal held between the lower and upper components that can form a compression seal about an inner circumference of the neck when the lower and upper components are matingly engaged in a compression seal position; and a first chamber located between the lower and upper components; wherein vapor inside the dewar vessel can travel in a plurality of tortuous paths when the cap is in the compression seal position, the plurality of tortuous paths beginning within the neck and then sequentially travelling up through the first plurality of apertures, the first chamber, the second plurality of apertures, the second chamber and then out the vent opening.
14. A self-venting cap as recited in claim 13, further comprising: a third component secured to the upper component so as to define the second chamber and vent openings between the upper and third components, wherein the upper component contains a positioning device on a lower surface capable of engaging with a second positioning device located in a fixed position relative to the neck such that once the first and second positioning devices are engaged, rotation of the third component in a tightening direction will cause the seal to be squeezed between the lower and upper components to form the compression seal.
15. A self-venting cap for a neck of a dewar vessel, comprising: a lower component having an outer circumference that is less than the inner circumference of the neck and a first plurality of apertures that is located inside of the outer circumference; an upper component having an upper outer circumference and a second plurality of apertures, the upper outer circumference being located outside of the inner circumference; a seal held between the lower and upper components that forms a compression seal with an inner circumference of the neck when the lower and upper components are matingly engaged in a compression seal position; and a third component secured to the upper component; wherein a first chamber is formed between the lower and upper components when the lower and upper components are matingly engaged in the compression seal position; wherein a second chamber and a vent opening located outside of the upper outer circumference are formed between the upper and third components when the lower and upper components are matingly engaged in the compression seal position; and wherein vapor inside the dewar vessel can travel in a plurality of tortuous paths when the cap is in the compression seal position, the plurality of tortuous paths beginning within the neck and then sequentially travelling up through the first plurality of apertures, the first chamber, the second plurality of apertures, the second chamber and then out the vent opening.
16. A self-venting cap as recited in claim 15, further comprising: a semi-permeable membrane that prevents moisture from passing through the first plurality of apertures while still allowing vaporous cryogen to pass through the first plurality of apertures.
17. A capped dewar vessel assembly, comprising: a dewar vessel having an outer casing and an inner vessel with each having openings at their tops connected together by a neck portion forming an evacuable space between the outer casing and the inner vessel and a dewar opening into the inner vessel; a specimen chamber connected to the inner vessel that extends inside the inner vessel and is accessed through the dewar opening; and a self-venting cap that restricts access to the specimen chamber when it is in a compression seal position that forms a compression seal with an inner circumference of the neck; wherein vapor inside the dewar vessel can travel in a plurality of tortuous paths when the cap is in the compression seal position, the plurality of tortuous paths beginning within the dewar opening and then sequentially travelling up through a first plurality of apertures, a first chamber, a second plurality of apertures, a second chamber and then out a vent opening.
18. A dewar vessel assembly, comprising: a dewar vessel having an outer casing and an inner vessel with each having openings at their tops connected together by a neck portion forming an evacuable space between the outer casing and the inner vessel and a dewar opening into the inner vessel; a specimen chamber held within the inner vessel that extends inside the inner vessel and is accessed through the dewar opening; and a plastic foam held within the inner vessel between an inner wall of the inner vessel and the specimen chamber; wherein the specimen chamber acts as a filter to prevent particles or fragments of the plastic foam from entering into the specimen chamber while allowing a liquid cryogen to pass through the specimen chamber into the plastic foam and allowing the liquid cryogen in a vapor phase liquid state to pass from the plastic foam into the specimen chamber.
19. A dewar vessel assembly as recited in claim 18, wherein the plastic foam is an open cell plastic foam.
20. A dewar vessel assembly as recited in claim 18, wherein the specimen chamber acts as a wicking device for rapid transfer of the liquid cryogen to the plastic foam.
21. A dewar vessel assembly as recited in claim 18, wherein the specimen chamber is comprised of an open-celled porous thermoplastic material that is cryogenically compatible.
22. A dewar vessel assembly as recited in claim 18, wherein the specimen chamber is sealed to the neck portion so that the liquid cryogen must pass through the specimen chamber to reach the plastic foam from the dewar opening and the liquid cryogen in the vapor phase liquid state must pass through the specimen chamber to reach the dewar opening from the plastic foam.
23. A containment system for samples of dangerous goods stored at cryogenic temperatures, comprising: a bag made of a cryogenically compatible polymer film with a sealing mechanism that will seal the bag when it is actuated; a porous structural cartridge for holding a plurality of sample receptacles separate from one another, comprising: a cartridge base with a plurality of sample receptacle apertures for holding the plurality of sample receptacles; and a cartridge cover that mates with the cartridge base to enclose the plurality of sample receptacle apertures and any sample receptacles held within said plurality of sample receptacle apertures; wherein the porous structural cartridge is held within the bag.
24. A containment system as recited in claim 23, wherein the polymer film is selected from the group consisting of Teflon® FEP and Kapton® polyimide film.
25. A containment system as recited in claim 23, wherein the polymer film is a fluorinated ethylene propylene resin.
26. A containment system as recited in claim 23, wherein the structural cartridge has sufficient absorbing capacity to absorb the entire contents of all of the plurality of sample receptacles held within the plurality of sample receptacle apertures.
EP01991461A 2000-12-29 2001-12-28 Cryogenic shipping container Withdrawn EP1356229A4 (en)

Applications Claiming Priority (9)

Application Number Priority Date Filing Date Title
US753207 1985-07-09
US75319500A 2000-12-29 2000-12-29
US753194 2000-12-29
US09/753,207 US20020083717A1 (en) 2000-12-29 2000-12-29 Containment system for samples of dangerous goods stored at cryogenic temperatures
US09/753,208 US20020083718A1 (en) 2000-12-29 2000-12-29 Specimen chamber for a cryogenic shipping container
US09/753,194 US6467642B2 (en) 2000-12-29 2000-12-29 Cryogenic shipping container
US753195 2000-12-29
US753208 2000-12-29
PCT/US2001/049684 WO2002053967A1 (en) 2000-12-29 2001-12-28 Cryogenic shipping container

Publications (2)

Publication Number Publication Date
EP1356229A1 true EP1356229A1 (en) 2003-10-29
EP1356229A4 EP1356229A4 (en) 2009-11-18

Family

ID=27505662

Family Applications (1)

Application Number Title Priority Date Filing Date
EP01991461A Withdrawn EP1356229A4 (en) 2000-12-29 2001-12-28 Cryogenic shipping container

Country Status (3)

Country Link
EP (1) EP1356229A4 (en)
JP (1) JP3958213B2 (en)
WO (1) WO2002053967A1 (en)

Families Citing this family (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2854681B1 (en) * 2003-05-05 2005-06-17 CRYOGENIC CONTAINER FOR THE GAS STORAGE OF PRODUCTS AND USE FOR THE STORAGE OF BIOLOGICAL PRODUCTS
JP4975554B2 (en) * 2007-08-17 2012-07-11 富士通株式会社 Portable sensor cooler using liquid nitrogen
FR2933476B1 (en) * 2008-07-02 2010-08-27 Air Liquide PORTABLE CRYOGENIC STORAGE CONTAINER AND USE
FR2975749B1 (en) 2011-05-23 2013-06-28 St Reproductive Tech Llc PORTABLE CRYOGENIC CONTAINER
DK2979044T3 (en) * 2013-03-29 2020-12-21 Tokitae Llc TEMPERATURE CONTROLLED STORAGE SYSTEMS
DK3030075T3 (en) 2013-08-08 2018-09-24 Sanofi Aventis Deutschland Cryo preservation application recovery device
EP3123143B1 (en) * 2014-03-28 2019-01-23 Board Of Trustees Of Northern Illinois University Ultra-rapid tissue cryopreservation method and apparatus
WO2017083164A1 (en) * 2015-11-10 2017-05-18 Entegris, Inc. Dry shipping container
US11596148B2 (en) 2017-11-17 2023-03-07 Savsu Technologies, Inc. Dry vapor cryogenic container with absorbent core
US10945919B2 (en) 2017-12-13 2021-03-16 Cryoport, Inc. Cryocassette
US11268655B2 (en) * 2018-01-09 2022-03-08 Cryoport, Inc. Cryosphere
US12025276B2 (en) 2018-01-09 2024-07-02 Cryoport, Inc. Cryosphere
US10859211B2 (en) 2018-07-02 2020-12-08 Cryoport, Inc. Segmented vapor plug
JP7272874B2 (en) * 2019-06-14 2023-05-12 大陽日酸株式会社 Frozen transport container, cryogenic liquefied gas absorbent case
US12013177B2 (en) * 2020-03-06 2024-06-18 Taiyo Nippon Sanso Corporation Container for cryopreservation and transportation
CN111493063A (en) * 2020-06-01 2020-08-07 中信湘雅生殖与遗传专科医院有限公司 Liquid nitrogen tank
DE102020134059A1 (en) * 2020-12-17 2022-06-23 Bernhard Sixt Thermally insulated transport container
US11691788B1 (en) 2022-01-20 2023-07-04 Cryoport, Inc. Foldable cassette bags for transporting biomaterials

Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3999653A (en) * 1975-03-11 1976-12-28 The Dow Chemical Company Packaging for hazardous liquids
DE2944464A1 (en) * 1979-11-03 1981-05-14 C. Reichert Optische Werke Ag, Wien DEVICE FOR THE CRYSTAL SUBSTITUTION OF SMALL BIOLOGICAL OBJECTS FOR MICROSCOPIC, IN PARTICULAR ELECTRON MICROSCOPIC EXAMINATIONS
US4495775A (en) * 1983-06-22 1985-01-29 Union Carbide Corporation Shipping container for storing materials at cryogenic temperatures
EP0344966A1 (en) * 1988-05-31 1989-12-06 Pro-Tech-Tube, Inc. Protective enclosure for hazardous material primary containers
US4903493A (en) * 1989-01-17 1990-02-27 Pymah Corporation Heat sink protective packaging for thermolabile goods
US4948035A (en) * 1990-01-16 1990-08-14 Container Corporation Of America Container end closure arrangement
US5024865A (en) * 1989-04-07 1991-06-18 Minnesota Mining And Manufacturing Company Sorbent, impact resistant container
US5160021A (en) * 1991-07-30 1992-11-03 Barry Sibley Leak-proof cylindrical container for the transport of diagnostic specimens or dangerous substances
US5355684A (en) * 1992-04-30 1994-10-18 Guice Walter L Cryogenic shipment or storage system for biological materials
US5779089A (en) * 1996-07-26 1998-07-14 Forma Scientific, Inc. Cryogenic storage apparatus with lid vent
US5829594A (en) * 1997-06-27 1998-11-03 Pro-Tech-Tube, Inc. Protective enclosure for shipping and storing hazardous materials
US5934099A (en) * 1997-07-28 1999-08-10 Tcp/Reliable Inc. Temperature controlled container
US6119465A (en) * 1999-02-10 2000-09-19 Mullens; Patrick L. Shipping container for storing materials at cryogenic temperatures

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3717005A (en) * 1970-10-16 1973-02-20 Martin Marietta Corp Capillary insulation
US3948409A (en) * 1974-11-12 1976-04-06 Viktor Sergeevich Ovchinnikov Cryostat
US4455842A (en) * 1981-07-15 1984-06-26 Biotech Research Laboratories, Inc. Device and method for controlled freezing of cell cultures
US4411138A (en) * 1982-08-17 1983-10-25 Union Carbide Corporation Neck tube closure assembly for cryogenic containers
US4729494A (en) * 1985-04-12 1988-03-08 Peillon Jean Pierre Container for liquid gas
DE3530168C1 (en) * 1985-08-23 1986-12-18 Messerschmitt-Bölkow-Blohm GmbH, 8012 Ottobrunn Adjustable helium II phase separator
US4790141A (en) * 1987-12-14 1988-12-13 Industrial Gas And Supply Company Apparatus and process for quick freezing of blood plasma

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3999653A (en) * 1975-03-11 1976-12-28 The Dow Chemical Company Packaging for hazardous liquids
DE2944464A1 (en) * 1979-11-03 1981-05-14 C. Reichert Optische Werke Ag, Wien DEVICE FOR THE CRYSTAL SUBSTITUTION OF SMALL BIOLOGICAL OBJECTS FOR MICROSCOPIC, IN PARTICULAR ELECTRON MICROSCOPIC EXAMINATIONS
US4495775A (en) * 1983-06-22 1985-01-29 Union Carbide Corporation Shipping container for storing materials at cryogenic temperatures
EP0344966A1 (en) * 1988-05-31 1989-12-06 Pro-Tech-Tube, Inc. Protective enclosure for hazardous material primary containers
US4903493A (en) * 1989-01-17 1990-02-27 Pymah Corporation Heat sink protective packaging for thermolabile goods
US5024865A (en) * 1989-04-07 1991-06-18 Minnesota Mining And Manufacturing Company Sorbent, impact resistant container
US4948035A (en) * 1990-01-16 1990-08-14 Container Corporation Of America Container end closure arrangement
US5160021A (en) * 1991-07-30 1992-11-03 Barry Sibley Leak-proof cylindrical container for the transport of diagnostic specimens or dangerous substances
US5355684A (en) * 1992-04-30 1994-10-18 Guice Walter L Cryogenic shipment or storage system for biological materials
US5779089A (en) * 1996-07-26 1998-07-14 Forma Scientific, Inc. Cryogenic storage apparatus with lid vent
US5829594A (en) * 1997-06-27 1998-11-03 Pro-Tech-Tube, Inc. Protective enclosure for shipping and storing hazardous materials
US5934099A (en) * 1997-07-28 1999-08-10 Tcp/Reliable Inc. Temperature controlled container
US6119465A (en) * 1999-02-10 2000-09-19 Mullens; Patrick L. Shipping container for storing materials at cryogenic temperatures

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of WO02053967A1 *

Also Published As

Publication number Publication date
JP2004517007A (en) 2004-06-10
JP3958213B2 (en) 2007-08-15
WO2002053967A1 (en) 2002-07-11
EP1356229A4 (en) 2009-11-18

Similar Documents

Publication Publication Date Title
US6467642B2 (en) Cryogenic shipping container
US20020083717A1 (en) Containment system for samples of dangerous goods stored at cryogenic temperatures
JP3958213B2 (en) Cryogenic shipping container
US6119465A (en) Shipping container for storing materials at cryogenic temperatures
EP0718212B2 (en) Insulated storage/shipping container for maintainig a constant temperature
US5934099A (en) Temperature controlled container
FI108785B (en) storage device
EP3480290B1 (en) Set for transporting culture container and unit for transporting cell or biological tissue
US4932533A (en) Thermal-stabilized container
US7422143B2 (en) Container having passive controlled temperature interior
US5160021A (en) Leak-proof cylindrical container for the transport of diagnostic specimens or dangerous substances
US20190219320A1 (en) A passive temperature control system for transport and storage containers
US8956855B2 (en) Portable cryogenic container
US6539726B2 (en) Vapor plug for cryogenic storage vessels
GB2556358A (en) A passive temperature control system for transport and storage containers
CN112368509B (en) Sectional type steam plug
US5080225A (en) Universal diagnostic sample packaging tray and pouch
WO2005054061A2 (en) Transport container for hazardous material
US20190150427A1 (en) Dry vapor cryogenic container with absorbent core
WO2017083164A1 (en) Dry shipping container
JP2006030144A (en) Sample tube heat-insulating tray and heat insulating box for multi-well plate
US20020083718A1 (en) Specimen chamber for a cryogenic shipping container
CA2515258A1 (en) Diagnostic specimen transport packaging and methods of use
WO2002041823A2 (en) Transportation of biological specimens
US12025276B2 (en) Cryosphere

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20030729

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR

AX Request for extension of the european patent

Extension state: AL LT LV MK RO SI

A4 Supplementary search report drawn up and despatched

Effective date: 20091021

17Q First examination report despatched

Effective date: 20100310

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20180703

RIC1 Information provided on ipc code assigned before grant

Ipc: F17C 7/02 20060101AFI20020715BHEP

Ipc: F17C 7/04 20060101ALI20020715BHEP