US 4,818,488 AGrant
Process and Apparatus for Dry Sterilization of Medical Devices and Materials
Issue Date:1989-04-04
•9 Claims
•2 Drawing Sheets
Abstract
A process for dry sterilization of medical devices and materials in which these materials are subjected to an electrical discharge in a gaseous atmosphere to produce an active plasma to produce an electrically active neutral species for surface sterilization of the devices and materials.
Metadata
Inventor
- Adir Jacob
Application Information
Application Number:US 0728993
Filing Date:1987-07-14
Priority Date:1987-02-25
Art Unit:181
Classifications
IPC:
A61L 220
Field of Search:
42222;23;21
Patent Drawings (2 sheets)
Description
Description of the Drawings
In the drawing FIG. 1 is a general diagrammatic illustration of an apparatus suitable for use in the practice of this invention;
FIG. 2 is a cross-sectional view of a sterilization chamber for use in the pracice of the invention;
FIG. 3 is a cross-sectional view of another embodiment of a sterilizaton chamber for use in the practice of the invention;
FIG. 4 is a side view of the apparatus of FIG. 3; and
FIGS. 5, 6, 7, 8 and 9 are cross sectional views of alternative embodiments .
Description of Preferred Embodiments
FIG. 1 is a general diagrammatic illustration of an RF excited discharge chamber of the type used in the process of this invention. The cylindrical chamber 11 is formed, in this instance, of glass or quartz and encloses within it the material 14 to be treated. The chamber is commonly connected to a mechanical vacuum pump (not shown) that establishes sub-atmospheric pressure conditions within the chamber. An exciter coil 12 couples RF energy from RF source 13 to the gas enclosed within the gas tight chamber creating a plasma therein.
Alternatively, a microwave discharge cavity operating at 2450 MHz may replace the RF exciter coil to couple power into the gas. With a suitable selection of a reducing gas, like hydrogen, or an oxidizing gas, such as oxygen, as a typical example, a discharge may be initiated and maintained within the chamber. In the gas plasma formed by that discharge a number of excited species, both molecular and atomic, are formed. The interaction of these species with a surface of the device or material to be sterilized accomplishes the sterilization in the manner described above. The time duration of the process needed to achieve satisfactory sterilization will vary with other parameters of the discharge such as gas flow, pressure, RF power density, and load size.
In one physical embodiment the apparatus may include an inner perforated metallic cylinder mounted generally concentric with the long axis of the chamber to form within the perforated cylinder a glowless, field-free zone. In FIG. 1 a perforated cylindrical shield 15 of this type is shown in dotted lines.
When, as illustrated in FIG. 2, a microwave energy source 18 at 2540 MHz. is employed in lieu of the RF generator 13, the perforated metallic cylinder cannot be mounted concentric about the long axis of the chamber. Instead, the microwave cavity 16 is mounted at one end of chamber, 11, and a perforated metallic shield 17 may be placed just beyond it toward the opposite end of the chamber spanning the entire diameter cross section of the chamber, thus creating a field-free and glowless reactive zone immediately below it and away from the microwave cavity. These arrangements permit material 14 placed within this zone to be generally isolated from electrically charged species, while allowing the electrically neutral reactive plasma species, such as oxygen radicals, to interact with the surface of the material to be sterilized. In this manner, sterilization is commonly effected at lower process temperatures.
In the most preferred embodiments the chamber is formed of a metal outer shell with either a single internal perforated cylindrical shield, or perhaps with two such metallic shields, the RF energy being coupled, in this latter configuration between the two conducting perforated cylinders. In either case, the discharge glow is confined to the space between the inner wall of the chamber and the surface(s) of the perforated cylinder(s), leaving the work volume defined by the inner perforated cylinder field-free, void of the plasma glow, and at a relatively low operating temperature. With a microwave cavity replacing the RF energy source, a single metallic perforated shield can be used and placed just below the cavity in accordance with the operational description given for FIG. 2.
One such chamber configuration is illustrated in FIGS. 3 and 4. The cylindrical outer wall 21, typically formed of aluminum or stainless steel is maintained at ground potential and, serves as the chamber enclosure. Suitable dimensions for this chamber are a diameter of 36" and a length of 48". A metallic perforated inner cylinder 23 is mounted on insulating spacers 29 within the chamber so that it is positioned generally parallel with the long axis of the outer wall 21 of the chamber. These spacers may be formed of any suitable non-reactive and insulating type of material such as ceramic. The cylinder perforations are typically 2.5 mm diameter holes spaced in all directions from one another by approximately 0.5 cm in a triangulated manner. Longitudinal support rails 27 are fastened to the inner wall of the perforated cylinder 23 to support a wire basket 25 in which the materials and devices to be sterilized are placed. A suitable RF source 22 is coupled between the grounded outer chamber wall 21 and the perforated inner cylinder 23. Usually this RF source should be capable of producing an RF output in the range 0.0125 to 0.05 W/cm.sup.3 at frequencies in the 10-100 kilohertz or 13-27 megahertz range.
As illustrated in FIG. 4, an evacuation port 31 at the end of cylinder 21 is connected to a pump (not shown) and provides for suitable evacuation of the chamber. The gas supplied for the discharge is generally flowed through the chamber by means of perforated diffusion tubes 35. Alternately, gas may be introduced into the chamber via a gas dispersion device (not shown) mounted behind chamber door 39 from the inside.
Material to be sterilized may be placed within wire basket 25 resting on rail 27 through the entry port behind chamber door 39. Chamber door 39 may be any suitable closure that can be conveniently opened and closed and left in a sealed position during evacuation and the gas discharge operation.
FIG. 5 illustrates a second preferred embodiment of the apparatus for practicing the process of the invention. In this configuration, the outer chamber wall 21 is again formed of metal, such as aluminum or stainless steel and is electrically grounded and of similar dimensions to that illustrated in FIG. 3. Mounted within the chamber is an inner concentric cylinder 43 formed of a perforated metal and supported on insulating support struts 46. The spacing between the inner wall of the chamber and the perforated interior cylinder may range typically from 10 to 17 cm where the chamber has an I.D. of 36". A second metallic perforated cylinder 41 is concentrically mounted intermediate between the inner perforated cylinder 43 and the inner wall of the chamber. This second perforated cylinder is supported on insulating struts 47 and is spaced typically 4 to 7 cm away from the inner perforated cylinder 43. The insulator struts may again be formed of a ceramic material. Mounted on the interior of the inner concentric cylinder 43 are support rails 27 for carrying a wire basket which would contain the materials to be sterilized. Both the outer chamber wall 21 and the inner perforated cylinder 43 are electrically connected to point of potential reference (ground). Electrical connections would most usually be made through ceramic seal feedthroughs 48 and 49. The intermediate cylinder 41 is electrically connected to one side of the RF power supply 22, the other side of which is connected to the point of potential reference.
While a variety of conventional RF sources may be used, the most typical value for the RF frequency is 13.56 MHz or, alternatively, 10-100 KHz. As in the embodiment of FIG. 4 longitudinally extending gas diffusion tubes 35 may be employed to provide the gas to the interior of the chamber. Typically each tube would have holes of diameter between 0.5 and 1.5 mm, spaced approximately 1" apart along its length. The hole diameters closer to the gas source would be of the smaller diameter. Alternatively, gas inlets may be provided behind door 39. As indicated in embodiments of FIGS. 3, 4 and 5 the perforated inner cylinders may be open-ended at both ends or, may be closed with the same perforated stock as is used to form the cylinder(s). The sterilization chambers described in FIGS. 3, 4 and 5 may be connected to a microwave discharge source, typically operating at 2540 MHz, in lieu of an RF energy source. In this case, the concentric perforated metallic cylinder(s) may be replaced by a single perforated shield in accordance with the operational description given for FIG. 2.
FIG. 6 illustrates a third preferred embodiment of the apparatus for practicing the process of the invention. In this diagrammatic description the outer chamber wall 21 is again formed of metal, such as aluminum or stainless steel, and is of similar dimensions to that illustrated in FIG. 3. Mounted within the chamber are two planar, metallic, electrodes 50 and 51, preferably constructed of aluminum which may be coated with insulating aluminum oxide. The gap 52 between the electrodes, 50 and 51, is adjustable by virtue of the movable bottom electrode 50. Terminals A and B are connected to the electrodes via an insulating feedthrough 48. The outer end of these terminals may be connected to an RF source (not shown) in such a way that when terminal B is connected to a ground potential, terminal A must be connected to the RF source, or vice versa, providing for an electrical symmetrical configuration. The work load to be sterilized is placed on bottom electrode 50.
It is important to maintain the distance between the electrodes always smaller than the distance of the RF-powered electrode's edge to the grounded chamber's wall. This enables a well defined and intense plasma glow to be confined to space 52 between the electrodes and prevents deleterious sparking. The electrode material may also be made of the perforated stock previously mentioned. However, it is desirable to have the RF-powered electrode made of solid stock to enable water-cooling of that electrode. The bottom electrode may also be made of solid stock to enable a cool surface upon which the work load to be sterilized will be placed. This chamber will commonly be evacuated to 10 microns Hg before gas introduction via the perforated gas diffusion tubes 35. Practical device sterilization can be obtained with process parameters for gas flow rates in the range 20 to 1000 scc/m, corresponding to a total sterilization reaction pressure of 10-1000 microns Hg, at a range of RF power densities of 0.0125 to 0.05 W/cm.sup.3.
FIG. 7 illustrates in diagrammatic form yet another preferred embodiment for practicing the process of the invention. The outer wall of chamber 21 is again formed of metal, such as aluminum or stainless steel maintained at ground potential, and is of similar dimensions to that illustrated in FIG. 3. Mounted within the chamber is a single planar, metallic, electrode 50, preferably constructed of aluminum which may be coated with insulating aluminum oxide to reduce RF sputtering. This electrode is commonly connected to an RF source in the MHz range and carries the work load to be sterilized. This electrode has commonly a total surface area which is at least four times smaller than the total internal surface area of the chamber.
This electrical configuration is usually referred to as asymmetric and is conducive to generating an extremely uniform plasma glow filling the entire volume of the process chamber. It is also responsible for the development of a characteristic accelerating potential at the surface of electrode 50, associated with a thin "dark space" through which positive plasma ions will accelerate and impinge on the electrode and the work loadiit normally carries.
The main advantage of this configuration is its ability to render efficient sterilization at relatively low power densities in the range of 0.0125-0.025 W/cm.sup.3. This configuration is also easily scalable as a function of work load size and its configuration.
This process chamber commonly operates with at least an order of magnitude lower pressure than the pressure for chambers described in FIGS. 1 through 6, while the gas dispersion tubes 35 are similar in construction to those previously mentioned. To prevent RF sputtering of electrode 50 due to positive ion bombardment, it may either be hard-anodized or alternatively aluminum oxide spray-coated.
One particular sub-configuration to that described in FIG. 7 is illustrated in FIG. 8. In this configuration a metallic perforated enclosure 51 totally surrounding and containing electrode 50 may be used, and connected to a separate RF source 22a. This perforated enclosure may be equipped with an open/close hinging mechanism (not shown) to enable access for material to be sterilized to be placed on electrode 50 contained within enclosure 51. This yields the beneficial effect of being able to separately control the abundance of sterilizing active species and their impinging energy. RF power applied to electrode 50, which may or may not include a negative DC potential from a separate DC supply, (not shown), will control energy of ion impingement, while RF power applied to the auxiliary perforated enclosure will control active species abundance.
With this configuration, RF power sources operating at 100 KHz and 13.56 MHz may be used in the various posssible permutations. Interesting results are obtained by mixing both frequencies while being applied to a single element. Commonly, one frequency has to be applied at a higher power fraction, usually around 90% of the total applied power to the same element. Such interesting process results were obtained when the two different frequencies were mixed and applied to electrode 50 in the absence of any auxiliary perforated enclosure. The mixed frequency concept also lends itself to low power density sterilization in the range 0.0125 to 0.025 W/cm.sup.3, with the advantage of maintaining the overall temperature relatively low (below 50.degree. C.), particularly when electrode 50 is water-cooled.
It is worth noting that the auxiliary perforated enclosure ought to be of high mesh transparency to allow the plasma glow to extend past it and contact electrode 50. Best operating conditions will be obtained for the smallest surface area of this perforated metallic enclosure.
FIG. 9 illustrates diagrammatically a preferred embodiment for practicing the process of the invention under atmospheric pressure conditions in ambient air. In this configuration no vacuum capability is required. Material to be sterilized s placed on grounded conveyor belt 62 which sweeps the load across the discharge gap created between conveyor belt 62 and RF-powered electrode 61. The powered electrode produces of a large plurality of needle-like discharges, which create individual discharge sparks toward the counter grounded electrode 62. The larger the gap between the electrodes, the higher the power needed to initiate the discharge in air.
Sterilization is effected due to ozone formation following the discharge of oxygen in the ambient air. power density requirements in the range 5 to 15 W/cm.sup.2 are not uncommon. Maintaining a controlled relative humidity of 50 to 60% in the discharge gap will facilitate initiation of the discharge and promote atomic oxygen generation. The latter serves as a precursor to ozone formation, the final desired sterilant in this configuration.
Ozone toxicity inhibits wide acceptance of such a corona discharge in air for the purpose of medical device sterilization. Alternatively, therefore, the RF-powered electrode 61 may assume a configuration comprised of multiple open nozzles 65, capable of dispersing oxidizing gases immediately adjacent to conveyor belt 62. In this configuration the discharge would still be created in ambient air, however the dispersion through the open nozzles 65 of a judiciously selected feed gas will increase the local concentration of its active species 63 relative to that of ozone. In this manner, sterilization would be attributable to active species derived from any feed gas introduced into the hollow RF-powered electrode 61 and not to the deleterious ozone gas.
The dispersing nozzles 65 may assume different configurations. For example, separate nozzle tubes may be inserted into a hollow section of electrode block 61, which may or may not be of different material than electrode block 61. These tubes may also be screwed into electrode block for easy replacement. A typical hole size for each individual nozzle is in the range 0.015-0.040".
The advantages of this discharge configuration are mainly in terms of system simplicity and in the context of continuous operation, coupled with the ability to easily change the residence time of a work load within the discharge gap.
Disadvantages are commonly associated with erosion and degradation of both electrode block 61 and conveyor belt 62. Electrode 61 should be constructed from oxidation-resistant materials (e.g., tungsten, molybdenum or alloys thereof). Conveyor belt 62 ought to be resistant to electrical punch-through and be constructed from fluorinated, or fluorinated/chlorinated hydrocarbons (e.g., DuPont products). High melting polyimides or Kalrez-like synthetics may serve as alternate construction materials for the conveyor belt. Kalrez is a polymide manufactured by DuPont.
Set forth below are specific examples of suitable operating parameters for effective sterilization employing an apparatus as illustrated in FIG. 1 where the outer chamber wall is formed of quartz glass. These results were achieved with a chamber 8" ID. by 8" long. In some examples operation included the metallic perforated cylinders as indicated in the embodiments of FIG. 3 and 4 to provide device sterilization in a field-free and glowless operation. In others the configuration was without such shielding internal cylinders.
For each of the examples the general technique involved was one in which the material to be sterilized was placed within a Tyvek bag which itself was sealed and placed in a wire basket within the chamber.
The materials used for verification of sterilization effectiveness were "Attest" vials obtained from 3M Company, each vial contained a bacterial strip having an original spore population of not less than 1.times.10.sup.6 Bacillus Subtilis var Niger per strip. The strips contained in the permeable plastic vials were not brought into contact with the culture solution contained in any of the vials prior to sterilization. The vials were placed within the Tyvek bags during the plasma sterilization.
For each example the chamber was first evacuated to an initial low pressure level after the materials (in the bag or pouches) were placed within the wire basket in the chamber. The chamber was thereafter filled with the appropriate gas prior to striking the discharge, and the gas continued to flow through the chamber at a controlled rate to establish a steady state sterilization pressure. The discharge was initiated by the application of RF power as indicated. The discharge was maintained for a controlled time period at the end of which the chamber was first evacuated, then backfilled with air and later opened and the samples removed. The temperature within the chamber during the process was maintained at less than 60.degree. C.
Subsequent to the tests the spore strips were submitted to an independent testing laboratory which performed a total plate count on the sample strips using a procedure in which 100 milliliters of sterile deionized water were added to each strip in a sterile whirl-pak bag. The bag was then placed in a lab blender for 10 minutes. One 10 milliliter aliquot of sample, a duplicate one milliliter sample, and two consecutive 10.sup.-1 dilutions were plated using Tryptic Soy Agar. The plates were then incubated at 30.degree.-35.degree. for 72 hours. After incubation, the plates were read and recorded, and the results calculated on a Colony Forming Unit (CFU) basis.
Example 1
Example 2
Example 3
Example 4
Example 5
Example 6
Example 7
Example 8
Example 9
For the following examples, the initial spore population was 2.2.times.10.sup.6 spores/strip.
Example 10
Field-Free Operation (With metallic perforated shield)
Example 11
Example 12
Field-Free Operation (With metallic perforated shield)
Gas: Helium/Argon (50%/50%, v/v)
Flowrate (total): 78 scc/min
Pressure: 0.38 torr
Power Density: 0.015 W/cm.sup.3
Exposure Time: 60 min
Resultant Microbial Count: 4.3.times.10.sup.2 CFUs
Percent Kill 99.9800%
Example 13
Field-Free Operation (With metallic perforated shield)
Example 14
Field of Operation (With metallic perforated shield)
Example 15
Field-Free Operation (With metallic perforated shield)
Gas: Laboratory Air (22.degree. C.,RH:52%)
Flowrate: 42 scc/min
Pressure: 0.40 torr
Power Density: 0.015 W/cm.sup.3
Exposure Time: 30 min
Resultant Microbial Count: 70 CFUs
Percent Kill: 99.9970%
Claims
Having described the specific process and apparatus of the invention as defined by the below appended claims.
1. A method for sterilization of medical devices and material comprising the steps of, placing said devices and materials within a metallic perforated electrode, generally cylindrical in shape, said electrode being positioned within, and generally concentric with, a gas-tight confining chamber, said chamber being generally cylindrical, formed from metal and connected to a point of potential reference, evacuating said chamber to a substantially low pressure and introducing a gas consisting of argon, or helium, or a mixture thereof, into said chamber, initiating an electrical discharge in said gas within said chamber by application of RF voltage between said internal perforated electrode and the metal chamber wall, creating a gas plasma, having a substantially field free and glowless volume within the perforated electrode containing said devices and materials, whereby said devices and materials are contacted by substantially electrically neutral active species at a temperature below that which would be detrimental to said devices and materials, maintaining said gas plasma for a controlled period of time, maintaining a flow of said gas through said chamber during said electrical discharge; and evacuating the gas plasma residual gases from said chamber prior to withdrawing said devices and material from it.
2. A method for sterilization of medical devices and materials enclosed within sealed pouches formed of gas permeable materials comprising the steps of: placing said pouches containing said material or devices to be sterilized within a metallic perforated electrode generally cylindrical in shape, said electrode positioned within, and generally concentric with a gas-tight confining chamber, said chamber being generally cylindrical, formed from metal and connected to a point of potential reference, evacuating said chamber to a substantially low pressure and introducing a gas consisting of argon, or helium, or a mixture thereof, into said chamber, initiating an electrical discharge in said gas within said chamber by application of RF voltage between said internal perforated electrode and the metal chamber wall creating a gas plasma, and having a substantially field free and glowless volume within the perforated electrode containing said pouches, said pouches containing said material devices and materials, whereby said devices and materials are contacted by substantially electrically neutral active species at a temperature below that which would be detrimental to said devices and materials, and maintaining said gas plasma for a controlled period of time, maintaining a flow of said gas through said chamber during said electrical discharge; and evacuating the gas plasma residual gases from said chamber prior to withdrawing said sealed pouches from it.
3. A method for sterilizing medical devices and materials enclosed within pouches formed of gas permeable materials comprising the steps of, placing said pouches containing said devices and materials within a first metallic perforated electrode generally cylindrical in shape, said electrode being positioned within and generally concentric with a gas-tight confining chamber, said gas-tight chamber being metallic and generally cylindrical, said gas-tight chamber and said first perforated electrode being connected to a point of potential reference, said chamber enclosing a second perforated metallic electrode positioned between and generally concentric with said gas-tight chamber and said first perforated electrode, evacuating said chamber to a substantially low pressure and introducing a gas consisting of argon, or helium, or a mixture thereof, into said chamber, initiating an electrical discharge in said gas within said chamber by application of RF voltage between said second perforated electrode and said point of potential reference creating a gas plasma having a substantially field free and glowless volume within said first perforated electrode containing said devices and materials, whereby said devices and materials are contacted by substantially electrically neutral active species at a temperature below that which would be detrimental to said devices and materials, maintaining said gas plasma for a controlled period of time, maintaining a flow of said gas through said chamber during said electrical discharge; and evacuating the gas plasma residual gases from said chamber prior to withdrawing said pouches from it.
4. A method for sterilization of medical devices and materials comprising the steps of, placing said devices and materials on a metallic electrode, said electrode being positioned within a gas-tight confining chamber being made of metal and connected to a point of potential reference, the internal surface area of said chamber being substantially larger than the surface area of said electrode, evacuating said chamber to a substantially low pressure and introducing a gas consisting of argon, or helium, or a mixture thereof, into said chamber, initiating an electrical discharge in said gas within said chamber by application of RF voltage between said metallic electrode and the metal chamber wall creating a gas plasma, further including a perforated metallic enclosure within said chamber, and electrically insulated from it, said enclosure also being insulated from, and surrounding and containing said metallic electrode and said devices and materials positioned thereon, whereby said devices and materials are contacted by substantially electrically neutral active species at a temperature below that which would be detrimental to said devices and materials, applying an RF voltage of one frequency to said perforated enclosure and a different frequency to said metallic electrode, maintaining said gas plasma for a controlled period of time, maintaining a flow of said gas through said chamber during said electrical discharge; and evacuating the gas plasma residual gases from said chamber prior to withdrawing said devices and materials from it.
5. A method for sterilization of medical devices and materials comprising the steps of, placing said devices and materials on a metallic electrode, said electrode being position within a gas-tight confining chamber, said chamber being made of metal and connected to a point of potential reference, the internal surface area of said chamber being substantially larger than the surface area of said electrode, evacuating said chamber to a substantially low pressure and a gas consisting of argon, or helium, or a mixture thereof, into said chamber, initiating an electrical discharge in said gas within said chamber by application of RF voltage between said metallic electrode and the metal chamber wall creating a gas plasma, further including a perforated metallic enclosure within said chamber, said enclosure being insulated from, but surrounding and containing said metallic electrode and said devices and materials positioned thereon, said enclosure being connected to said point of potential reference, whereby said devices and materials are contacted by substantially electrically neutral active species at a temperature below that which would be detrimental to said devices and materials, maintaining said gas plasma for controlled period of time, maintaining a flow of said gas through said chamber during said electrical discharge; and evacuating the gas plasma residual gases from said chamber prior to withdrawing said devices and materials from it.
6. A method in accordance with either one of the claim 4 or 5, wherein said medical devices and materials are enclosed within pouches of gas permable material when said devices and materials are placed within said chamber and remain so until said devices and materials are withdrawn from said chamber.
7. A method in accordance with any one of claim 1, 2, 3, 4, or 5 wherein said gas is substantially pure argon.
8. A method in accordance with any one of claim 1, 2, 3, 4, or 5 wherein said gas is substantially pure helium.
9. A method in accordance with any one of claim 1, 2, 3, 4, or 5 wherein said gas is a gaseous mixture of 50% helium and 50% argon.
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