US20030118804A1 - Sample processing device with resealable process chamber - Google Patents

Sample processing device with resealable process chamber Download PDF

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Publication number
US20030118804A1
US20030118804A1 US10/324,283 US32428302A US2003118804A1 US 20030118804 A1 US20030118804 A1 US 20030118804A1 US 32428302 A US32428302 A US 32428302A US 2003118804 A1 US2003118804 A1 US 2003118804A1
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United States
Prior art keywords
film
process chamber
resealable film
resealable
sample
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.)
Abandoned
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US10/324,283
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English (en)
Inventor
William Bedingham
Gerald Deeb
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.)
3M Innovative Properties Co
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3M Innovative Properties Co
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 US09/847,467 external-priority patent/US6869666B2/en
Priority claimed from US09/894,810 external-priority patent/US6734401B2/en
Application filed by 3M Innovative Properties Co filed Critical 3M Innovative Properties Co
Priority to PCT/US2002/040970 priority Critical patent/WO2004058405A1/fr
Priority to US10/324,283 priority patent/US20030118804A1/en
Assigned to 3M INNOVATIVE PROPERTIES COMPANY reassignment 3M INNOVATIVE PROPERTIES COMPANY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BEDINGHAM, WILLIAM, DEEB, GERALD S.
Publication of US20030118804A1 publication Critical patent/US20030118804A1/en
Abandoned legal-status Critical Current

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    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5025Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures for parallel transport of multiple samples
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B01L3/50Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B01L3/5027Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • B01L3/502715Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by interfacing components, e.g. fluidic, electrical, optical or mechanical interfaces
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    • B01L3/508Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above
    • B01L3/5085Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above for multiple samples, e.g. microtitration plates
    • B01L3/50853Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above for multiple samples, e.g. microtitration plates with covers or lids
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    • B01L7/00Heating or cooling apparatus; Heat insulating devices
    • B01L7/52Heating or cooling apparatus; Heat insulating devices with provision for submitting samples to a predetermined sequence of different temperatures, e.g. for treating nucleic acid samples
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29DPRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
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    • B29D7/01Films or sheets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
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    • B32B27/00Layered products comprising a layer of synthetic resin
    • GPHYSICS
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    • G01N35/00029Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor provided with flat sample substrates, e.g. slides
    • G01N35/00069Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor provided with flat sample substrates, e.g. slides whereby the sample substrate is of the bio-disk type, i.e. having the format of an optical disk
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    • B01L2200/02Adapting objects or devices to another
    • B01L2200/026Fluid interfacing between devices or objects, e.g. connectors, inlet details
    • B01L2200/027Fluid interfacing between devices or objects, e.g. connectors, inlet details for microfluidic devices
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B01L2300/041Connecting closures to device or container
    • B01L2300/044Connecting closures to device or container pierceable, e.g. films, membranes
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    • B01L2300/0809Geometry, shape and general structure rectangular shaped
    • B01L2300/0829Multi-well plates; Microtitration plates
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B01L2300/0861Configuration of multiple channels and/or chambers in a single devices
    • B01L2300/0864Configuration of multiple channels and/or chambers in a single devices comprising only one inlet and multiple receiving wells, e.g. for separation, splitting
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    • B01L2300/0861Configuration of multiple channels and/or chambers in a single devices
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    • B01L2300/0861Configuration of multiple channels and/or chambers in a single devices
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    • B01L2400/04Moving fluids with specific forces or mechanical means
    • B01L2400/0403Moving fluids with specific forces or mechanical means specific forces
    • B01L2400/0409Moving fluids with specific forces or mechanical means specific forces centrifugal forces
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    • B01L2400/04Moving fluids with specific forces or mechanical means
    • B01L2400/0475Moving fluids with specific forces or mechanical means specific mechanical means and fluid pressure
    • B01L2400/0487Moving fluids with specific forces or mechanical means specific mechanical means and fluid pressure fluid pressure, pneumatics
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    • B01L2400/00Moving or stopping fluids
    • B01L2400/06Valves, specific forms thereof
    • B01L2400/0633Valves, specific forms thereof with moving parts
    • B01L2400/0661Valves, specific forms thereof with moving parts shape memory polymer valves
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B01L2400/0677Valves, specific forms thereof phase change valves; Meltable, freezing, dissolvable plugs; Destructible barriers
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B01L2400/0677Valves, specific forms thereof phase change valves; Meltable, freezing, dissolvable plugs; Destructible barriers
    • B01L2400/0683Valves, specific forms thereof phase change valves; Meltable, freezing, dissolvable plugs; Destructible barriers mechanically breaking a wall or membrane within a channel or chamber
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B9/00Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
    • F27B9/14Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment
    • F27B9/16Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a circular or arcuate path
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D5/00Supports, screens, or the like for the charge within the furnace
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
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    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/24Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24942Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
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    • Y10T428/249924Noninterengaged fiber-containing paper-free web or sheet which is not of specified porosity
    • Y10T428/24994Fiber embedded in or on the surface of a polymeric matrix
    • Y10T428/24995Two or more layers
    • Y10T428/249952At least one thermosetting synthetic polymeric material layer

Definitions

  • the present invention relates to devices, methods and systems for processing of sample materials, such as methods used to amplify genetic materials, etc.
  • thermal processes in the area of genetic amplification include, but are not limited to, Polymerase Chain Reaction (PCR), Sanger sequencing, etc.
  • PCR Polymerase Chain Reaction
  • Sanger sequencing etc.
  • the reactions may be enhanced or inhibited based on the temperatures of the materials involved. Although it may be possible to process samples individually and obtain accurate sample-to-sample results, individual processing can be time-consuming and expensive.
  • volume of sample material may be limited and/or the cost of the reagents to be used in connection with the sample materials may also be limited and/or expensive.
  • volume of sample material may be limited and/or the cost of the reagents to be used in connection with the sample materials may also be limited and/or expensive.
  • the present invention provides devices including resealable film used to close one or more process chambers in a sample processing device.
  • the resealable films preferably provide for controlled puncture, followed by resealing of the puncture site such that the process chamber remains substantially isolated from the surrounding environment.
  • the present invention also provides methods for delivering sample materials to a process chamber through a resealable membrane, as well as removal of materials from a process chamber through a membrane.
  • the present invention may provide an integrated solution to the need for obtaining a desired finished product from a starting sample even though multiple processes are required to obtain the finished product.
  • the process chambers are multiplexed from a loading chamber (in which the starting sample is loaded)
  • Those multiple finished samples may be the same materials where the multiplexed process chambers are designed to provide the same finished samples.
  • the multiple finished samples may be different samples that are obtained from a single starting sample.
  • film refers to a flexible article having any shape that has two major surfaces, e.g., sheet or tube.
  • the film has more than one layer.
  • the film may preferably have, e.g., a total thickness of no more than about 400 micrometers (0.016 inches), more preferably no more than about 250 micrometers (0.010 inches) depending on the materials and construction used.
  • flexural rigidity of the film refers to the product of the modulus of elasticity and moment of inertia of a film.
  • load refers to the mechanical force that is applied to a body.
  • modulus of elasticity of the film refers to the amount of force necessary to deform the film one strain unit.
  • “moment of inertia of the film” refers to the geometric stiffness of the film (i.e., the cube of the thickness divided by 12).
  • puncturability refers to the displacement to break when the load of a probe is applied to a film.
  • rescalability refers to the ability of a film to reduce the size of an opening in the film at a puncture site up to the point of completely closing the puncture site.
  • an opening that is created in the film by a puncturing object reseals such that the circumference of the opening is less than 50% of the circumference of the puncturing object. More preferably, the opening will decrease to less than 20% of the circumference of the puncturing object.
  • sealability refers to the ability of a film to form a seal around a puncturing object while it is puncturing the film.
  • “recovering stress of the film” refers to the difference between the film's tensile stress at 300% elongation as determined by ASTM standard D822 and the stress when the film is returned to its original length after stretching to 300% elongation.
  • surface friction between the film and a puncturing object refers to the linear coefficient expressing the tangential force to pull a sled covered with that film over a track consisting of the material of the puncturing object compared to the normal force (weight) of the sled.
  • the present invention provides a sample processing device including a body with at least one process chamber having a process chamber volume; resealable film attached to the body, the resealable film having an internal surface defining a portion of the process chamber volume and an external surface facing away from the process chamber volume; and friction modifying material on the external surface of the resealable film or friction modifying material incorporated into the resealable film, wherein the incorporated friction modifying material is chosen because it substantially migrates to the external surface of the resealable film.
  • the present invention provides a sample processing device including a body with at least one process chamber having a process chamber volume; resealable film attached to the body, the resealable film having an internal surface defining a portion of the process chamber volume and an external surface facing away from the process chamber volume, wherein the resealable film includes plastic material forming a first layer and elastomeric material forming a second layer attached to the first layer.
  • the present invention provides a method of manufacturing a sample processing device, the method including providing a body that includes at least one process chamber with a process chamber volume; attaching resealable film to the body, wherein the resealable film has an internal surface defining a portion of the process chamber volume and an external surface facing away from the process chamber volume; providing friction modifying material on the external surface of the resealable film to provide a targeted level of at least one of: the friction between the resealable film and a puncturing object, the flexural rigidity of the resealable film, the recovering stress of the resealable film, and the elongation at break of the resealable film.
  • the present invention provides a method of manufacturing a sample processing device by providing a body having at least one process chamber with a process chamber volume; attaching resealable film to the body, wherein the resealable film has an internal surface defining a portion of the process chamber volume and an external surface facing away from the process chamber volume; providing friction modifying material incorporated into the resealable film, wherein the incorporated friction modifying material is chosen because it substantially migrates to the external surface of the resealable film to provide a targeted level of at least one of: the friction between the resealable film and a puncturing object, the flexural rigidity of the resealable film, the recovering stress of the resealable film, and the elongation at break of the resealable film.
  • the present invention provides a method of transferring sample material by providing a sample processing device including a body with at least one process chamber having a process chamber volume; resealable film attached to the body, the resealable film having an internal surface defining a portion of the process chamber volume and an external surface facing away from the process chamber volume.
  • the method further includes puncturing the resealable film with a fluid transfer device to form an opening in the resealable film; inserting the fluid transfer device through the opening in the resealable film, wherein a portion of the fluid transfer device is located within the process chamber volume; transferring sample material into or out of the process chamber using the fluid transfer device; and removing the fluid transfer device from the process chamber, wherein the resealable film reseals the opening after removal of the fluid transfer device.
  • FIG. 1 is a top plan view of one device according to the present invention.
  • FIG. 2 is an enlarged partial cross-sectional view of a process chamber in the device of FIG. 1.
  • FIG. 3 is an enlarged partial cross-sectional view of the process chamber with a fluid transfer device inserted into the process chamber through a resealable film.
  • FIG. 4 is an enlarged partial cross-sectional view of the process chamber after removal of the fluid transfer device from the process chamber.
  • FIG. 5 depicts an apparatus used to drive a puncturing object into a film and measure the flexure at rupture or break of the film.
  • the present invention provides a device that can be used in methods that involve thermal processing, e.g., sensitive chemical processes such as PCR amplification, ligase chain reaction (LCR), self-sustaining sequence replication, enzyme kinetic studies, homogeneous ligand binding assays, and more complex biochemical or other processes that require precise thermal control and/or rapid thermal variations.
  • thermal processing e.g., sensitive chemical processes such as PCR amplification, ligase chain reaction (LCR), self-sustaining sequence replication, enzyme kinetic studies, homogeneous ligand binding assays, and more complex biochemical or other processes that require precise thermal control and/or rapid thermal variations.
  • sample processing devices may be manufactured according to the principles described in U.S. Provisional Patent Application Serial No. 60/214,508 filed on Jun. 28, 2000 and titled THERMAL PROCESSING DEVICES AND METHODS (Attorney Docket No. 55265USA19.003); U.S. Provisional Patent Application Serial No. 60/214,642 filed on Jun. 28, 2000 and titled SAMPLE PROCESSING DEVICES, SYSTEMS AND METHODS (Attorney Docket No. 55266USA99.003); U.S. Provisional Patent Application Serial No. 60/237,072 filed on Oct.
  • top and bottom may be used in connection with the present invention, it should be understood that those terms are used in their relative sense only.
  • “top” and “bottom” are used to signify opposing sides of the devices.
  • elements described as “top” or “bottom” may be found in any orientation or location and should not be considered as limiting the methods, systems, and devices to any particular orientation or location.
  • the top surface of the device may actually be located below the bottom surface of the device in use (although it would still be found on the opposite side of the device from the bottom surface).
  • FIGS. 1 and 2 One illustrative device manufactured according to the principles of the present invention is depicted in FIGS. 1 and 2.
  • the device 10 may be in the shape of a circular disc as illustrated in FIG. 1, although any other shape could be used.
  • the depicted device 10 includes a plurality of process chambers 50 , each of which defines a volume for containing a sample and any other materials that are to be processed with the sample.
  • the illustrated device 10 includes ninety-six process chambers 50 , although it will be understood that the exact number of process chambers provided in connection with a device -manufactured according to the present invention may be greater than or less than ninety-six, as desired.
  • the process chambers 50 in the illustrative device 10 are in the form of chambers, although the process chambers in devices of the present invention may be provided in the form of capillaries, passageways, channels, grooves, or any other suitably defined volume.
  • sample processing devices of the present invention may include a number of completely isolated and separate process chambers into which materials are delivered and from which materials are removed independent of the other process chambers.
  • the present invention may include conventional microtiter plates and other sample processing devices including one or more independent, isolated process chambers.
  • the device 10 of FIGS. 1 and 2 is a multi-layered composite structure including a substrate 20 , first layer 30 , and a resealable film 40 . It is preferred that the substrate 20 , first layer 30 and resealable film 40 of the device 10 be attached or bonded together with sufficient strength to resist any expansive forces that may develop within the process chambers 50 as, e.g., the constituents located therein are rapidly heated during thermal processing.
  • the robustness of the bonds between the components may be particularly important if the device 10 is to be used for thermal cycling processes, e.g., PCR amplification. The repetitive heating and cooling involved in such thermal cycling may pose more severe demands on the bond between the sides of the device 10 .
  • Another potential issue addressed by a more robust bond between the components is any difference in the coefficients of thermal expansion of the different materials used to manufacture the components.
  • the process chambers 50 in the depicted device 10 are in fluid communication with distribution channels 60 that, together with loading chamber 62 , provide a distribution system for distributing samples to the process chambers 50 .
  • Introduction of samples into the device 10 through the loading chamber 62 may be accomplished by rotating the device 10 about a central axis of rotation such that the sample materials are moved outwardly due to centrifugal forces generated during rotation.
  • the sample can be introduced into the loading chamber 62 for delivery to the process chambers 50 through distribution channels 60 .
  • the process chambers 50 and/or distribution channels 60 may include ports through which air can escape and/or other features to assist in distribution of the sample materials to the process chambers 50 .
  • sample materials could be loaded into the process chambers 50 under the assistance of vacuum or pressure.
  • the illustrated device 10 includes a loading chamber 62 with two subchambers 64 that are isolated from each other. As a result, a different sample can be introduced into each subchamber 64 for loading into the process chambers 50 that are in fluid communication with the respective subchamber 64 of the loading chamber 62 through distribution channels 60 . It will be understood that the loading chamber 62 may contain only one chamber or that any desired number of subchambers 64 , i.e., two or more subchambers 64 , could be provided in connection with the device 10 .
  • FIG. 2 is an enlarged cross-sectional view of a portion of the device 10 including one of the process chambers 50 .
  • the substrate 20 includes a first major side 22 and a second major side 24 .
  • Each of the process chambers 50 is formed, at least in part in this embodiment, by a void 26 formed through the substrate 20 .
  • the illustrated void 26 is formed through the first and second major sides 22 and 24 of the substrate 20 .
  • the substrate 20 may preferably be polymeric, but may be made of other materials such as glass, silicon, quartz, ceramics, etc. Furthermore, although the substrate 20 is depicted as a homogenous, one-piece integral body, it may alternatively be provided as a non-homogenous body of, e.g., layers of the same or different materials. For those devices 10 in which the substrate 20 will be in direct contact with the sample materials, it may be preferred that the material or materials used for the substrate 20 be non-reactive with the sample materials. Examples of some suitable polymeric materials that could be used for the substrate in many different bioanalytical applications may include, but are not limited to, polycarbonate, polypropylene (e.g., isotactic polypropylene), polyethylene, polyester, etc.
  • a first layer 30 is provided on one side of the substrate 20 in the illustrated embodiment.
  • the first layer 30 is depicted as a homogenous, one-piece integral layer, it may alternatively be provided as a non-homogenous layer of, e.g., sub-layers of the same or different materials, e.g., polymeric materials, metallic layers, etc.
  • the process chamber 50 may be formed as a depression in the substrate 20 with no first layer 30 required to define the volume of the process chamber 50 .
  • a resealable film 40 is provided on the opposite side of the substrate 20 to define the remainder of the volume of the process chamber 50 .
  • the resealable film 40 is depicted as a homogenous, one-piece integral layer, it may alternatively be provided as a non-homogenous layer of, e.g., sub-layers of the same or different materials, e.g., polymeric materials, etc.
  • the resealable film 40 includes an external surface 42 facing away from the volume of the process chamber 50 and an internal surface 44 facing the volume of the process chamber 50 .
  • At least a portion of the materials defining the volume of the process chamber 50 be transmissive to electromagnetic energy of selected wavelengths.
  • the body 20 , first layer 30 , and/or resealable film 40 may be transmissive to electromagnetic energy of selected wavelengths.
  • the selected wavelengths may be determined by a variety of factors, for example, electromagnetic energy designed to heat and/or interrogate a sample in the process chamber 50 , electromagnetic energy emitted by the sample (e.g., fluorescence), etc.
  • electromagnetic energy designed to heat and/or interrogate a sample in the process chamber 50
  • electromagnetic energy emitted by the sample e.g., fluorescence
  • a transmissive process chamber 50 By providing a transmissive process chamber 50 , a sample in the chamber can be interrogated by electromagnetic energy of selected wavelengths (if desired) and/or electromagnetic energy of the selected wavelengths emanating from the sample can be transmitted out of the process chamber 50 where it can be detected by suitable techniques and equipment. For example, electromagnetic energy may be emitted spontaneously or in response to external excitation.
  • a transmissive process chamber 50 may also be monitored using other detection techniques, such as color changes or other indicators of activity or changes within the process chambers 50 .
  • sample material 52 located within the volume of the process chamber 50 .
  • the sample material may include at least one fluid component, preferably a liquid.
  • the sample material may be a biological sample material.
  • FIG. 3 is an enlarged partial cross-sectional view of the process chamber of FIG. 2 after insertion of a fluid transfer device 70 into the volume of the process chamber 50 through the resealable film 40 .
  • the fluid transfer device 70 may be, e.g., a pipette, needle, or other device capable of taking up and/or delivering fluids.
  • the fluid transfer device 70 may preferably have sufficient structural rigidity to pierce the resealable film 40 by itself.
  • the fluid transfer device 70 may be inserted through an opening already pierced by another instrument.
  • the fluid transfer device 70 may have a sharp tip 72 as shown or the tip may be blunt depending on the properties of the resealable film 40 and the fluid transfer device itself.
  • FIG. 4 is an enlarged partial cross-sectional view of the process chamber of FIGS. 2 & 3 after removal of the fluid transfer device 70 from the volume of the process chamber 50 .
  • a portion of the sample material 52 in the process chamber 50 has been removed using the fluid transfer device 70 (although as discussed above, the fluid transfer device 70 may also deliver materials into the process chamber 50 ).
  • the opening 46 through which the fluid transfer device 70 entered and exited the process chamber includes an perforation in the resealable film 40 that reseals upon removal of the fluid transfer device 70 . While the materials used for resealable film 40 exhibit resealability of the opening 46 upon removal of a fluid transfer device as depicted in FIG. 4, the resealable film 40 may also preferably exhibit sealability when the fluid transfer device 70 is inserted through the layer 40 .
  • the resealable film 40 may be attached to the body 20 around at least the boundaries of the process chamber 50 to seal the sample materials 52 therein. Any suitable technique or combination of techniques may be used to attach the resealable film 40 to the body 20 . Examples of some suitable attachment techniques include, but are not limited to, adhesives (e.g., pressure sensitive, hot-melt, curable, etc.), thermal welding, ultrasonic welding, heat sealing, chemical welding, clamping, mechanical fasteners, etc.
  • adhesives e.g., pressure sensitive, hot-melt, curable, etc.
  • thermal welding e.g., thermal welding, ultrasonic welding, heat sealing, chemical welding, clamping, mechanical fasteners, etc.
  • the resealable film 40 may preferably be a polymeric film, preferably a polymeric film that can be controllably punctured and optionally sealed and/or resealed. Typically, these properties are determined by at least one of flexural lo rigidity of the film, the elongation at break of the film, the recovering stress of the film, and friction between the film and a puncturing object.
  • Control over puncturability in a resealable film 40 can be accomplished by modifying a surface of the film to provide desired levels of flexural rigidity of the film, the elongation at break of the film, the recovering stress of the film, and surface friction between the film and the puncturing object, e.g., a fluid transfer device 70 .
  • Modifying the surface can be accomplished by a number of methods. For example, it can include changing the modulus of the film by altering the temperature of the film prior to, and during, the penetration by a puncturing object; stretching and optionally releasing the film prior to penetration by a puncturing object; applying a modifying material to the surface of the film; or adding a modifying material to the bulk material comprising a film.
  • modifying can also include changing the thickness of one or more layers or changing the properties of the surface layer that first contacts a puncturing object.
  • a puncturing object and flexible film generally interact as follows: as the puncturing object makes contact with the film, the film deforms in the direction of the puncturing object's motion. This is accompanied by local stretching of the film in the vicinity of the puncturing object's tip.
  • the tangential stress associated with driving the puncturing object down into the film will not be great enough to overcome the normal force from the film hoop stress holding the film against the puncturing object (i.e., the product of the COF and the normal force is greater than the tangential force).
  • the puncturing object will pull the surrounding film downward with it such that the force exerted by the object will be distributed over the entire film surface in contact with the object.
  • the portion of the film not in contact with the puncturing object will also be strained as the film in contact with the object is pulled with the movement of the puncturing object. This deformation of the non-contacting film will effectively distribute the load of the puncturing object so that mechanical failure will only be caused at much larger displacements, i.e., large film deformations.
  • this ability to make contact around the puncturing object depends on the ability of the film itself to conform to the object.
  • the elastomeric core layer exerts a force generated by the tendency of the film to recover from the hoop stress to drive the film toward contact with the object.
  • the outer layer is not rigid (due to small moment of inertia, or low modulus of elasticity of the film) in comparison to the core layer then the core layer material can drive the entire film to contact the puncturing object.
  • the core layer will be less able to force the entire film to conform to the puncturing object.
  • the extent of the ability of the film to conform to the puncturing object also controls puncture resistance. If the film cannot conform to the puncturing object surface then the object will be able to concentrate its entire load immediately below its tip regardless of the COF. Conversely, if the film can conform to the puncturing object 25 surface then puncture may be impeded, if the COF is sufficiently high.
  • the puncture resistance of some film constructions can be affected by the recovery stress of the film even when the elongation at break of each of the layers of the film is substantially unchanged.
  • the films of the present invention preferably include elastomeric layers in a manner that results in a resealable film.
  • elastomeric films exert high hoop stresses, i.e., recovering forces from cylindrical deformation, (because they try to return to their original, unstressed state). It is this inward (toward the puncturing object) force that facilitates resealing.
  • the tendency of less elastic films to generate the restoring force to reseal or recover strain in response to deformation is greatly reduced in comparison to elastomeric films.
  • the opening (the area within the broken perimeter) is relatively large and the film is less able to reseal the opening depending on the size and shape of the puncturing object.
  • the resealability of openings in the films may be controlled in tandem with (though not independent of) the puncture resistance of the films.
  • Elastomeric layers also contribute to the ability of a film to seal around a puncturing object.
  • the elastic recovery of a film also allows the film to conform to the shape of the puncturing object.
  • This sealability property is advantageous when it is desirable to isolate a process chamber from a surrounding environment while a film is being punctured. For example, sealability allows a film to be punctured without allowing contaminants or other materials to pass through the puncture site.
  • the resealable is a polymeric multilayer film of two outer layers and at least one inner layer.
  • Modifying such a multilayer film can involve modifying at least one of the outer layers of the film to provide a targeted level of at least one of flexural rigidity of the film, the elongation at break of the film, the recovering stress of the film, and the friction between the film and a puncturing object.
  • the thickness and/or stiffness of an outer layer can be changed to make an overall change in the thickness or stiffness of a film.
  • modifying such a multilayer film can involve modifying an inner layer of the film to provide a targeted level of flexural rigidity of the film and elongation at break of the film.
  • films having an (AB) n A (where n is greater than 1) construction can be more flexible than films of equal thickness having an ABA construction. This occurs, for example, when the A layer is a hard stiff material and the B material is a soft, pliable material. When a film is flexed the material at one surface is compressed and the material at the opposing surface is stretched. The material in the middle of the film is not significantly compressed or stretched. If the stiff material is at or near the film's surface and the soft material is near the film's center, stretching the film requires more force than if the stiff material were near the film's center and the soft material were at the surfaces.
  • controlling the puncturability, resealability, and, optionally, sealability of a puncture site in a polymeric film can be accomplished by producing a polymeric film having at least two layers wherein a first layer includes a plastic material and a second layer includes an elastomeric material.
  • the type and amount of materials of the first layer and second layer are selected to impart specified levels of flexural rigidity of the film, the elongation at break of the film, the recovering stress of the film, and friction between the film and a puncturing object.
  • controlling the puncturability, resealability, and, optionally, sealability of a puncture site in a polymeric film can be accomplished by: selecting a polymeric material and a modifying material; combining the polymeric material and the modifying material to form a molten mixture; and forming the molten mixture into a film; wherein the type, and amount of polymeric and modifying materials 0 are selected to provide a targeted level of at least one of flexural rigidity of the film, the elongation at break of the film, the recovering stress of the film, and the friction between the film and a puncturing object.
  • the modifying material can be a variety of materials able to change at least one of flexural rigidity of the film, the elongation at break of the film, the recovering stress of the film, or the friction between the film and puncturing object, such as a lubricant, an adhesive, or other monomers, oligomers, or polymers.
  • modifying materials that can enhance puncturability include silicone oil and a wide variety of thermoplastic materials having a low COF relative to the puncturing object.
  • a high density polyethylene film would be an appropriate puncturable film if the puncturing object were a polypropylene needle.
  • modifying materials that enhance puncture resistance are elastomers resulting in relatively high COFs such as, for example, tackified elastomers or self-tacky elastomers.
  • the modifying material may be selected for its ability to slide against a specific puncturing object, thereby contributing to the resealability of the puncture site by causing a small diameter opening to be formed. The more puncturable a film is, the better it is able to reseal because the force and effect of the puncturing object is concentrated in a small area.
  • the polymeric film can include one or more layers.
  • the polymeric film can include three layers—two outer layers and a core layer.
  • the desired degree of puncture resistance and ability to seal and reseal can be affected by adjusting the properties of the film's core layers or at least one of the film's outer layers rigidity.
  • Plastic materials suitable for use in the present invention include those that are capable of being formed into a film layer, have a modulus of elasticity over 108 Pa, and cannot sustain more than 20% strain without incurring permanent set (i.e., permanent deformation) at ambient temperature.
  • suitable plastic materials include thermoplastics such as polyethylenes (high density, low density, and very low density), polypropylene, polymethylmethacrylate, polyethylene terephthalate, polyamides, and polystyrene; thermosets such as dyglycidyl esters of bisphenol A epoxy resins, lo bisphenol A dicyanate esters, orthophthalic unsaturated polyesters, bisphenol A vinyl esters.
  • Elastomeric materials suitable for use in the present invention can include any material that is capable of being formed into a thin film layer and exhibits elastomeric properties at ambient conditions. Elastomeric means that the material will substantially resume its original shape after being stretched. Further, preferably, the elastomer will sustain only small permanent set following deformation and relaxation which set is preferably less than 20% and preferably less than 10% at moderate elongation, e.g., about 400-500%. Generally any elastomer is acceptable which is capable of being stretched to a degree that causes relatively consistent permanent deformation in a plastic outer layer. This can be as low as 50% elongation.
  • the elastomer is capable of undergoing up to 300 to 1200% elongation at room temperature, and most preferably 600 to 800% elongation at room temperature.
  • the elastomer can be pure elastomer or blends with an elastomeric phase or content that will exhibit substantial elastomeric properties at room temperature.
  • Suitable elastomeric materials include natural or synthetic rubbers block copolymers that are elastomeric, such as those known to those skilled in the art as A-B or A-B-A block copolymers. Such copolymers are described for example on U.S. Pat. Nos. 3,265,765; 3,562,356; 3,700,633; 4,116,917, and 4,156,673.
  • elastomeric compositions include, for example, styrene/isoprene/styrene (SIS) block 30 copolymers, elastomeric polyurethanes, ethylene copolymers such as ethylene vinyl acetates, ethylene/propylene monomer copolymer elastomers or ethylene/propylene/diene terpolymer elastomers. Blends of these elastomers with each other or with modifying non-elastomers are also contemplated.
  • SIS styrene/isoprene/styrene
  • polymers can be added as stiffening aids such as polyvinylstyrenes such as polyalphamethyl styrene, polyesters, epoxies, 5 polyolefins, e.g., polyethylene or certain ethylene/vinyl acetates, preferably those of higher molecular weight, or coumarone-indene resin.
  • stiffening aids such as polyvinylstyrenes such as polyalphamethyl styrene, polyesters, epoxies, 5 polyolefins, e.g., polyethylene or certain ethylene/vinyl acetates, preferably those of higher molecular weight, or coumarone-indene resin.
  • the plastic layer can be an outer or inner layer (e.g., sandwiched between two elastomeric layers). In either case, it will modify the elastic properties of the multilayer film.
  • Percent recovery refers to stretched length minus the recovered length, the sum of which is divided by the original length.
  • the plastic layer will hinder the elastic force with a counteracting resisting force.
  • a plastic outer layer will not stretch with an inner elastomeric layer after the film has been stretched (provided that the second stretching is less than the first), the plastic outer layer will just unfold into a rigid sheet. This reinforces the core layer, resisting or hindering the contraction of the elastomeric core layer.
  • the friction between a puncturing object and the surface of the film should be reduced.
  • a wide variety of mechanisms can be used to reduce this friction as long as there is a concentration of stress at the point of load applied by the object.
  • This can include applying a modifying material to the film surface or selecting a different material for the outer surface of the film such that the coefficient of friction between the puncturing object and film surface is reduced.
  • a polypropylene/styrene-isoprene synthetic rubber/polypropylene multi layer film can be made more puncturable by a polypropylene tip if the film surface is sprayed with silicone oil.
  • Puncturability may be increased by stretching a film. Holding a film in a 30 stretched position can make it more puncturable because it is less able to conform to the puncturing object.
  • stretching and releasing a multilayer film comprising both elastomeric and plastic layers can decrease puncturability by decreasing the film's flexural rigidity. This can be done by stretching the multilayer film past the elastic limit of the plastic layer(s). Stretching and releasing can also lower a multilayer film's s coefficient of friction and modulus of elasticity.
  • the plastic layer can function to permit controlled release or recovery of the stretched elastomeric layer, modify the modulus of elasticity of the multilayer film and/or stabilize the shape of the multilayer film.
  • the present invention provides polymeric films, including single films with a modified surface, having varying degrees of puncturability, resealability, and, optionally varying degrees of sealability with regard to the shape of a specific type of puncturing object, e.g., a fluid transfer device.
  • the film can be punctured when the film is stretched to a given displacement by a puncturing object applied to a first major surface, but the film cannot be punctured when the film is stretched to the same displacement by the same puncturing object applied to a second opposing major surface.
  • a two-layer film having a low COF on the first major surface and a high COF on the second would be more easily punctured by a puncturing object through the first surface than through the second surface.
  • the shape of the tip of a puncturing object can also affect the puncturability of the film.
  • the single layer films of the present invention may be made by extrusion methods or any other suitable methods known in the art.
  • the multilayer films of the present invention may be formed by any convenient layer forming process such as coating, lamination, coextruding layers or stepwise extrusion of layers, but coextrusion is preferred. Coextrusion per se is know and is described, for example, in U.S. Pat. Nos. 3,557,265 and 3,479,425. The layers are typically coextruded through a specialized feedblock or a specialized die that will bring the diverse materials into contact while forming the film.
  • Coextrusion may be carried out with multilayer feedblocks or dies, for example, a three-layer feedblock (fed to a die) or a three-layer die such as those made by Cloeren 30 Co., Orange, Tex.
  • a suitable feedblock is described in U.S. Pat. No. 4,152,387.
  • streams of materials flowing out of extruders at different viscosities are separately introduced into the feedblock and converge to form a film.
  • a suitable die is described in U.S. Pat. No. 6,203,742.
  • the feedblock and die used are typically heated to facilitate polymer flow and layer adhesion.
  • the temperature of the die depends on the polymers used. Whether the film is prepared by coating, lamination, sequential extrusion, coextrusion, or a combination thereof, the film formed and its layers will preferably have substantially uniform thicknesses across the film.
  • the present invention also provides systems of puncturable, resealable films and puncturing objects (e.g., fluid transfer devices) that can be tailored to each other to obtain a desired level of puncturability. For example, if a specific fluid transfer device is to be used as a puncturing object, the properties and characteristics of a film can be made to complement the puncturing object to provide the desired level of ease of puncturability.
  • the fluid transfer device may be made of a particular material, may have a particular shape (including the shape of its tip), etc.
  • composition and structure of a film can be made to provide the appropriate flexural rigidity of the film, the elongation at break of the film, the recovering stress of the film, and friction between the film and puncturing object to provide the desired level of ease of puncturability of the film.
  • sealability and resealability of the film can be tailored in the same manner.
  • a puncturing object can be chosen based on its composition (which will affect the friction between the film and puncturing object), and its shape (including the shape of its tip), to provide the desired level of ease of puncturability, resealability, and, optionally, sealability of the film.
  • the pipette has a tip with an outside diameter of 0.84 mm and a shaft that tapered over a length of 5 mm to a substantially constant diameter of about 2 mm.
  • hole 112 in the center of clamp assembly 114 of the test apparatus had a diameter of 76 mm.
  • the puncturing object 116 was a smooth cylindrical metal probe having a hemispherical tip with a diameter of about 12 mm. The speed of the probe was 508 mm/min. The amount of deflection, i.e., displacement at peak load prior to rupture was measured in inches and converted into millimeters. Each reported value is an average of 5 test measurements.
  • the dynamic coefficient of friction of the surface of the film sample that would first contact a puncturing object was determined by using ASTM D1894-95 with the apparatus described in drawing c, FIG. 1 of the ASTM and the sled as described in Section 5.1 of the ASTM.
  • the sliding surface was a sheet of cast polypropylene film (available as7C12N from Shell Chemical Co., Beaupre, Ohio).
  • a metal filament wire was used to pull the sled and various weights were placed on the sled to achieve different forces normal to the plane of the sample being tested.
  • the normal force was calculated as the mass of the weight on the sled multiplied by the gravitational acceleration.
  • the steady-state pulling force was determined, after initial transient values, for each normal force and was plotted against the normal force.
  • the dynamic coefficient was the slope of the curve of the plotted data.
  • Example 1 illustrates the effect of the dynamic coefficient of friction of a film on the puncture resistance and resealability of a multilayer film.
  • Sample A was a three layer film with a thermoplastic elastomer core layer and high density polyethylene (HDPE) outer layers.
  • the outer layers were made of thermoplastic HDPE A (available as PETROTHENE LS3150-00, elongation percent at break of 300, Equistar Chemicals, Houston, Tex.).
  • the outer layer material was conveyed through an extruder having multiple zones with a single screw extruder (diameter of 19 mm, L/D of 32/1, available from Killion, Inc., Cedar Grove, N.J.).
  • the outer layer material extruder operated with zone temperatures increasing from 163° C. to 216° C.
  • the outer layer material was conveyed through a gear pump to the “A” and “C” channels of the three-layer Cloeren feedblock (available from Cloeren Co., Orange, Tex.) that was set at 216° C.
  • the core layer was made from a thermoplastic elastomer (available as KRATON D1107 styrene-isoprene block copolymer, recovering stress (at 300% elongation) of 2.07 MPa (300 psi), from Shell Chemical Co., Beaupre, Ohio) and conveyed through an extruder having multiple zones with a single screw extruder (diameter of 32 mm, L/D of 24/1, available from Killion, Inc.).
  • the core layer material extruder operated with zone temperatures increasing from 188° C. to 216° C.
  • the core layer material was passed to the “B” channel of the Cloeren feedblock.
  • the resulting multilayered flow stream was passed through a single orifice film die (having a width of 254 mm (10 inch) and available from EDI, Chippewa Falls, Wis.) that was set at a temperature of 216° C.
  • the resulting molten film was drop cast onto a chill roll, which was set at a temperature of 11° C., and collected.
  • the line speed was 12.2 m/min., the individual flow rates of the outer layer and core layer were such that each outer layer had a thickness of about 3.1 micrometer ( ⁇ m) and the overall film thickness was measured at about 72 ⁇ m.
  • Sample B was made as Sample A except a layer of Silicone Oil A (available as DC-200 PDMS oil from Dow Corning, Midland Mich.) was applied on one side of the three layer film.
  • Silicone Oil A available as DC-200 PDMS oil from Dow Corning, Midland Mich.
  • Sample C was made as Sample A except a layer of Silicone Oil B (available as Part No. 700-01015 PDMS oil from Rheometrics Scientific, Piscataway, N.J.) was applied on one side of the three layer film.
  • Silicone Oil B available as Part No. 700-01015 PDMS oil from Rheometrics Scientific, Piscataway, N.J.
  • Sample D was made as Sample A except a layer of pressure-sensitive adhesive (an acrylate-based pressure-sensitive adhesive (98/2 isooctyl acrylate/acrylic acid) made according to U.S. Pat. No. 5,804,610, Example 11 (except the ratio of IOA to AA was 98:2 instead of 97:3) having a thickness of approximately 125 ⁇ m was applied on one side of the three layer film by lamination.
  • a layer of pressure-sensitive adhesive an acrylate-based pressure-sensitive adhesive (98/2 isooctyl acrylate/acrylic acid) made according to U.S. Pat. No. 5,804,610, Example 11 (except the ratio of IOA to AA was 98:2 instead of 97:3) having a thickness of approximately 125 ⁇ m was applied on one side of the three layer film by lamination.
  • the effective diameters of the opening and the shaft of the puncturing object were also measured and a ratio of areas was calculated.
  • the effective area of the puncturing object calculated based on the largest diameter of the plastic pipette that entered the opening, was 2.00 mm.
  • the effective diameter of the opening for Sample A and B converting the area of the often jagged tear in the film into a circle having an equivalent area, was approximately 1.80 mm and 0.25 mm, respectively.
  • the ratio of the effective area of the puncturing object to the effective area of the resulting opening for Samples A and B were calculated to be 0.81 and 0.016, respectively.
  • Example 2 illustrates the effect of the dynamic coefficient of friction of a film on the puncture resistance of a single layer film.
  • Sample A was made by extruding very low density polyethylene (available as ENGAGE 8200 from Dow Chemical Company, Midland, Mich.) into a film having a thickness of about 75 ⁇ m. The polymer was conveyed with a single screw extruder through the core layer slot of the feedblock and single orifice film die used for Example 1.
  • very low density polyethylene available as ENGAGE 8200 from Dow Chemical Company, Midland, Mich.
  • Sample B was made as sample A except a layer of Silicone Oil A was applied one side of the single layer film.
  • Example 3 illustrates the effect of stretching and relaxing a film on the puncture resistance of the film.
  • Sample A was made in a manner similar to Sample A of Example 1 except the three layer film was further consecutively stretched in one direction to 500% of its original length in both the machine and transverse directions. Then the film was allowed to recover until it reached a steady state in approximately 10 minutes.
  • Example 4 illustrates the effect of stretching a film on the puncture resistance of the film.
  • Sample A was made by further stretching Sample A of Example 1 in one direction to 300% of its original length while held in the testing sample holder (and was punctured while it was stretched).
  • Example 5 illustrates how a film can be made less or more puncture resistance depending on which side of a film consisting of two layers of different materials first contacts the puncturing object.
  • Sample A was made by further applying different materials to each side of Sample A of Example 1. Silicone Oil A was applied to side one of the film in a manner similar to Sample B of Example 1 and adhesive was applied to side two in a manner similar to Sample D of Example 1.
  • Example 6 illustrates another way a film can be made less or more puncture resistant depending on which side of a film consisting of two layers of different materials first contacts the puncturing object.
  • Sample A was made in a manner similar to that of Sample A of Example 1 except the side-2 outer layer material was a metallocene catalyzed very low density polyethylene (VLDPE) available as ENGAGE 8200 from Dow Chemical).
  • VLDPE very low density polyethylene
  • the VLDPE was conveyed with a single screw extruder having multiple zones (Killion Model KLB075) that was operating with zone temperatures increasing from 160° C. to 216° C.
  • the material was passed to the C channel of the three-layer feedblock.
  • the line speed was 7.77 n/min. and the overall thickness was measured at 91 ⁇ m.
  • Example 7 illustrates the effect of outer layer thickness on puncture resistance.
  • Sample A-D were made as Sample A of Example 1 except gear pump settings on the outer layer extruder were adjusted to obtain a different outer layer thickness for each sample, as reported in Table 7, while the core layer extruder settings and line speed were unchanged.
  • Example 8 illustrates the effect of total film thickness on puncture resistance.
  • Sample A-C were made as Sample C of Example 7 except line speed settings were adjusted to obtain a different total film thickness for each sample, as reported in Table 8 (both extruder settings were unchanged).
  • Example 9 illustrates the effect of different outer layer materials, each having a different elongation at break, on puncture resistance of a three layer construction.
  • Sample A was made as Sample A of Example 1 except the outer layer material was HDPE B (available as DOWLEX IP60 HDPE, elongation percent at break of 225, from Dow Chemical); the extruders reached upper temperatures of 232° C., and the die was set at a temperature of 232° C. Also, the line speed and extruder flow rates were changed to result in a total film thickness of 140 ⁇ m with outer layer thicknesses of about 10 ⁇ m each.
  • HDPE B available as DOWLEX IP60 HDPE, elongation percent at break of 225, from Dow Chemical
  • the extruders reached upper temperatures of 232° C.
  • the die was set at a temperature of 232° C.
  • the line speed and extruder flow rates were changed to result in a total film thickness of 140 ⁇ m with outer layer thicknesses of about 10 ⁇ m each.
  • Sample B and Sample C were made as Sample A except the outer layer material was HDPE A (described in Example 1) and HDPE C (ALATHON M5865 HDPE from Equistar, elongation percent at break of 800), respectively.
  • Example 10 illustrates the effect of outer layer thickness on the puncture resistance and resealability of a multilayer film.
  • Sample A, B and C were the same as Sample A, B and C of Example 7 except the films were punctured with a plastic pipette having a shaft diameter of 2.0 mm instead of a metal rod having a shaft diameter of 13.7 mm.
  • Example 11 illustrates the effect of a different core material with different recovering stress on puncture resistance of an outer layer/core layer/outer layer construction.
  • Sample A was made as Sample B of Example 9 except the core material was KRATON D1112P, having a recovering stress of 1.45 MPa (210 psi), available from Shell Chemical Company.
  • Patents, patent applications, and publications disclosed herein are hereby incorporated by reference (in their entirety) as if individually incorporated. It is to be understood that the above description is intended to be illustrative, and not restrictive. Various modifications and alterations of this invention will become apparent to those skilled in the art from the foregoing description without departing from the scope of this invention, and it should be understood that this invention is not to be unduly limited to the illustrative embodiments set forth herein.

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US10/324,283 2001-05-02 2002-12-19 Sample processing device with resealable process chamber Abandoned US20030118804A1 (en)

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US09/894,810 US6734401B2 (en) 2000-06-28 2001-06-28 Enhanced sample processing devices, systems and methods
PCT/US2002/040970 WO2004058405A1 (fr) 2001-05-02 2002-12-19 Dispositif de traitement d'echantillons comportant une chambre de traitement reutilisable
US10/324,283 US20030118804A1 (en) 2001-05-02 2002-12-19 Sample processing device with resealable process chamber

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