U.S. patent number 3,606,996 [Application Number 04/821,276] was granted by the patent office on 1971-09-21 for method for sterilization.
This patent grant is currently assigned to Chemotronics, Inc.. Invention is credited to James M. Wolf.
United States Patent |
3,606,996 |
Wolf |
September 21, 1971 |
METHOD FOR STERILIZATION
Abstract
A method for the sterilization utilizing essentially
instantaneous and transient thermal pulses generated in a gaseous
medium in contact with the surfaces. The thermal pulses kill the
micro-organisms and have a duration of less than about 1 second so
that the surface is not damaged. The surface to be treated is
substantially free of liquid material so that the thermal pulse
acts directly upon the micro-organisms. The sterilization is
particularly useful for medical and industrial purposes.
Inventors: |
Wolf; James M. (Ann Arbor,
MI) |
Assignee: |
Chemotronics, Inc. (Ann Arbor,
MI)
|
Family
ID: |
25232985 |
Appl.
No.: |
04/821,276 |
Filed: |
May 2, 1969 |
Current U.S.
Class: |
422/4 |
Current CPC
Class: |
A61L
2/20 (20130101); A61L 2/04 (20130101); A61L
2202/26 (20130101) |
Current International
Class: |
A61L
2/04 (20060101); A61L 2/20 (20060101); A61l
001/00 () |
Field of
Search: |
;21/1,2,60,82-83,85,91,92,93 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Wolk; Morris O.
Assistant Examiner: Zatarga; Joseph T.
Claims
I claim:
1. The method for the treatment of surfaces requiring sterilization
in order to destroy micro-organisms on the surface which
comprises:
a. providing a surface to be sterilized inside a bag in a sealed
and confined space defined by a rigid chamber confining the bag to
prevent rupture;
b. contacting the surfaces to be sterilized inside the bag with a
gaseous medium, the surfaces in contact with the gaseous medium
being substantially free of liquid material which masks the
surfaces from sterilization;
c. transiently exposing the surfaces to a thermal pulse produced by
the ignition of a combustible mixture of gaseous oxidizer and
oxidizable materials said pulse being generated in the gaseous
medium in the bag which is confined by the rigid chamber and having
peak temperatures substantially above the minimum temperatures
required to destroy the micro-organisms without damage to the
surfaces; and
d. removing the bag from the rigid chamber such that it is sealed
so as to at least prevent pathogenic micro-organism contamination
of the surface before subsequent use.
2. The method of claim 1 wherein the surfaces are in the form of a
fabric which is sterilized in the sealed and confined space.
3. The method of claim 1 wherein the surfaces are in the form of an
instrument which is sterilized in the sealed and confined
space.
4. The method of claim 1 wherein oxidizing conditions are
maintained in the gaseous medium during generation of the thermal
pulse.
5. The method of claim 1 wherein the surface to be treated is dried
to remove liquid material before being contacted with the gaseous
medium and wherein the gaseous medium is substantially dry.
6. The method of claim 1 wherein the surface is aseptically handled
prior to use to prevent micro-organism contamination.
7. The method of claim 1 wherein the gaseous medium consists of the
mixture of gaseous oxidizer and oxidizable materials
8. The method of claim 7 wherein the combustible gaseous material
is a mixture of hydrogen and air.
9. The method of claim 7 wherein the combustible gaseous material
is a mixture of hydrogen and oxygen.
10. The method of claim 7 wherein the combustible gaseous material
is a mixture of methane and air.
11. The method of claim 7 wherein the combustible material is a
mixture of methane and oxygen.
Description
BACKGROUND OF THE INVENTION
The present invention is concerned with methods for sterilization
wherein heat in the form of transient thermal pulses generated in a
gaseous medium in contact with the surface to be sterilized is
utilized. More particularly the present invention utilizes thermal
pulses generated in the gaseous medium for less than about 1 second
which are produced by the ignition of a combustible composition as
the gaseous medium or by the adiabatic compression and
decompression of the gaseous medium.
The prior art methods of sterilization having a direct relation to
the present invention particularly rely upon heating in some form
for relatively long periods of time to kill micro-organisms. See
for instance Kirk-Othmer, VOL. 13, (1968) beginning at pg, 457
wherein various commercial sterilization methods are discussed. In
general temperatures in the range of 100.degree. to 200.degree. C.
are used for periods of time ranging from several minutes to hours.
Also known is direct flame heating of the surface to be sterilized
wherein the bulk of the article is heated as well to temperatures
approaching the flame temperature (about 2,600.degree. C. maximum);
however, this technique can produce damage to the bulk of the
article and cannot be used with flammable materials. Also the use
of a direct flame produces nonuniform heating of the article.
The generation of thermal pulses in a gaseous medium is known to
the prior art as particularly shown by U.S. Pat. No. 3,175,025 and
3,329,759; however, it was not recognized that articles could be
sterilized as a result of treatment and thus they were not handled
so as to prevent micro-organism contamination, particularly
contamination by pathogenic micro-organisms.
SUMMARY
It is therefore an object of the present invention to provide a
method whereby sterilization can be achieved utilizing transient
thermal pulses which uniformly heat the surfaces of the article. It
is further an object of the present invention to provide a method
wherein the article is undamaged by the thermal pulse because of
the transient nature of the heating. These and other objects will
become increasingly apparent from the following description.
The objects of the present invention are provided by the method for
the treatment of surfaces requiring sterilization in order to kill
micro-organisms on the surfaces which comprises: (a) contacting the
surfaces to be sterilized with a gaseous medium, the surfaces in
contact with the gaseous medium being substantially free of liquid
material; (b) transiently exposing the surfaces to a thermal pulse
generated in the gaseous medium having peak temperatures
substantially above the minimum temperatures required to kill the
micro-organisms without damage to the surface; and (c) handling the
surfaces so as to at least prevent pathogenic micro-organism
contamination before subsequent use. The use of combustible gaseous
material as the gaseous medium which is ignited to produce the
thermal pulse is particularly preferred.
DESCRIPTION OF DRAWING
FIGS. 1 to 3 schematically illustrate various forms of equipment
which can be used in the process of the present invention. FIGS. 1
and 3 illustrate preferred forms wherein a combustible material is
provided in a confined space and ignited to generate the thermal
pulse. FIG. 2 illustrates a piston and cylinder arrangement for
adiabatically compressing and decompressing a gaseous medium to
generate the thermal pulse.
FIG. 4 schematically illustrates the steps of the method of the
present invention including provision of the gaseous medium,
generation of the thermal pulse and one form of handling to prevent
micro-organism contamination using a sealed bag.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The equipment which can be utilized in the process of the present
invention is generally known to the prior art as shown by the above
cited U.S. Pat. Nos. 3,175,025 and 3,329,759. The gaseous medium is
provided in contact with the surface to be treated in a confined
space or chamber along with a means for generating the thermal
pulse in the gaseous medium, such as by the use of a combustible
gaseous material and ignition or by the use of substantially
adiabatic compression and decompression of the gaseous medium. The
following is a brief description of preferred specific forms of
such equipment.
Referring to the drawing and FIG. 1, a confined space 13 is defined
by chamber 10 and cover 11 secured for instance by bolts 14. Within
the confined space 13 mounted on projections 10a is provided the
article 12 to be sterilized. An ignition device 15 is provided
within the confined space 13 which is actuated by a spark generator
means 16. A conduit and valve 18 leads into the confined space 13
which is connected to vacuum means 19 with valve 18 and provided to
evacuate the confined space 13 of air. Gaseous fuel supply means 21
is provided with valve 20 to supply fuel to the confined space 13
after evacuation for ignition by the ignition means 15 and
preferably and optionally a blanket gas supply means 23 with valve
22 to provide a gaseous material in the confined space 13 after
ignition of the gaseous fuel to aid in the prevention of
contamination after sterilization when the cover 11 is removed.
Referring to FIG. 2, a cylinder 24 is provided with a recess 25 for
holding the article 27 to be sterilized and is mounted on
projections 24a. A piston 26 is fitted to the cylinder 24 and a
gaseous medium is provided within the defined confined space 28.
The gas is compressed substantially adiabatically by applying a
force F to the piston 26, thus heating the gaseous medium and the
surface 27a of the article 27 for sterilization and then
immediately decompressed to prevent overheating of the article.
Referring to FIG. 3, an article 30 to be sterilized is provided
within a flexible bag 29, such as polyethylene bag, which is fitted
with or sealed to an ignition tube 31 at the open end of the bag 29
such as by a band 32. The end of the tube 31 outside of the bag 29
is fitted with an ignition device 34. At least the bag 29 with the
article 30 can be provided in a clean chamber 33 or preferably the
chamber 33 fits the confines of the bag 29 such that it is not
ruptured by the ignition of the combustible gaseous material. A
cover 42 with bolts 43 provides closure of the chamber 33. The
ignition device 34 is provided with the spark actuator means 16 and
conduit and valve 17 is attached to the exposed end of the tube 31
with the vacuum means 19 and valve 18 and gaseous fuel supply means
21 and valve 20 and operated as is the device of FIG. 1. The
blanket of gaseous material after sterilization is unnecessary,
since the clean chamber 33 or bag 29 is utilized and this is also
possible with the devices of FIGS. 1 and 2.
Regardless of the equipment used, the method of the present
invention involves three basic steps as illustrated in FIG. 4 in
Steps 1, 2 and 3. In Step 1, the article 35 is provided in the
confined space 37 with the gaseous medium 36 in contact with the
surfaces 35a of the article 35 to be sterilized. The surfaces 35a
must be substantially free from liquid material whether from the
gaseous medium 36 or originally present on the article 35. If
necessary the article 35 is dried to remove liquid material. The
gaseous medium 36 is preferably dry. In Step 2, the gaseous medium
is either compressed and decompressed or ignited to create a
thermal pulse 38 having peak temperatures substantially above the
minimum temperatures required to kill the micro-organisms and
without damage to the article 35. In Step 3, the surfaces 35a of
the article 35 are handled so as to at least prevent contamination
by pathogenic micro-organisms before subsequent use. Preferably the
article 35 is aseptically handled to prevent any micro-organism
contamination. Thus the article 35 can be transferred from the
confined space 37 and placed in a bag 39, such as a polyethylene
bag, sealed such as by a clip 40 at the open end and containing a
sterile atmosphere 39. Where the device shown in FIG. 3 is utilized
such that the chamber 3 prevents rupture of the bag 29 during
ignition of the combustible gaseous material by confining the bag
29, this has been found to be a simple and inexpensive means of
preventing contamination before use and is preferred. The ignition
products of the combustible gaseous material are sterile and thus
do not need to be replaced with a blanket gaseous material although
it is preferred to use the blanket gaseous material in instances
where the ignition products could be damaging to the article in
order to prevent chemical contamination of or reaction with the
article treated.
The article to be sterilized must be bathed by the thermal pulse on
all surfaces to be sterilized. This is accomplished by mounting the
article on support means in the confined space which allow the
gaseous medium to contact the surfaces to be treated, such as the
optional projections 10a, 24a and 33a shown in FIGS. 1 to 3 which
provide minimum contact with the surfaces to be sterilized.
Alternatively the article can be repetitively treated with
repositioning of the surfaces of the article to insure treatment
with the thermal pulse.
The gaseous medium utilized will depend upon the equipment used and
the composition of the article being sterilized. Where adiabatic
compression equipment is used it is preferred to use a gaseous
medium which is compatible with the article being treated. Thus
rare gases or hydrogen or nitrogen have been used with good result.
Where the composition of the article is resistant to destructive
oxidation, such as stainless steel, oxygen can be used which
further augments the treatment with the thermal pulse because of
oxidative destruction of the micro-organisms.
Where ignition of a combustible gaseous material is used, it is
preferred to use a mixture of an oxidizable gaseous material and an
oxidizer gaseous material which is compatible with the material
being treated such that the byproducts of combustion do not
contaminate or react with the article or otherwise adversely affect
the article. For this reason methane (or other lower alkanes,
alkenes and alkynes containing 1 to 4 carbon atoms) and hydrogen
are the preferred oxidizable materials and air or oxygen are the
preferred oxidizer materials since water and/or carbon dioxide is
generated by the reaction. Oxidizing conditions, as discussed
above, can be produced by providing a stoichiometric excess of the
oxidizer, oxygen. Other oxidizable materials which can be used are
for instance ammonia, hydrazine, hydrogen sulfide, carbon monoxide
and various hydrocarbons such as acetylene, ethylene oxide and
cyanogen. Suitable oxidizer materials are pure oxygen which is
preferred, oxygen with gaseous diluents such as air, air alone,
halogens such as fluorine and chlorine, ozone and various nitrogen
oxides. Mixtures of single or multiple oxidizer materials with
single or multiple oxidizable materials can be used, but these are
not preferred because of the possible effect on the article of the
byproducts of the reaction. The energy produced by the combustible
gaseous material can be increased or decreased by regulating the
charge pressure prior to ignition. Various compounds which rapidly
decompose with accompanying transient release of thermal energy
upon suitable initiation can also be used singly or multiply to
produce the transient elevated gaseous temperatures such as
acetylene and nitrogen dioxide.
In each instance the thermal pulse generated is transient, and
usually this step is complete in less than l second. The treatment
does not damage or destroy the article because the surfaces in
contact with the gaseous medium are only briefly in contact with
the thermal pulse while the bulk of the article is only heated to a
limited degree. Also, the total energy of the thermal pulse is
maintained at less then the energy which would damage or destroy
the article. For this reason articles composed of metals, ceramics,
plastics and naturally occuring materials can be sterilized. Woven
and nonwoven fabrics, such as blankets and bandages and the like,
stainless steel medical instruments and other articles with
surfaces requiring sterilization have been successfully
treated.
Having generally described the method of the present invention, the
following are specific examples.
EXAMPLE 1
Utilizing the equipment illustrated in FIG. 1, a roll of square
woven fabric (cotton and polyester fiber) 6 inches long and 4
inches in diameter was provided in the chamber 10 measuring 41/2 in
diameter by 61/4 inches high. The chamber 10 was closed with the
cover 11 and bolted with bolts 14. The chamber was evacuated to 10
of Hg and then a combustible mixture of 60 percent hydrogen and 40
percent oxygen by volume (molar excess of oxygen) at three
atmospheres absolute was provided in the confined space and
ignited. A blanket of nitrogen was then provided in the confined
space and then the cover was removed and the article transferred to
a sterile bag for subsequent use. It was found upon culture testing
of a portion of the article that it was sterile and that the
article was undamaged by the treatment.
EXAMPLE 2
The treatment of example 1 was repeated with the same size roll of
cotton muslin using a mixture of 662/3 percent hydrogen and 331/3
percent oxygen by volume (stoichiometric mixture) at two
atmospheres absolute. The results were the same as those of example
1.
EXAMPLE 3
The treatment of example 1 was repeated with a polypropylene
perforated tube measuring 6 inches long by 13/8 inches in diameter
used as a support for microfiltration using a mixture of 75 percent
hydrogen and 25 percent oxygen by volume at 4 atmospheres absolute.
The results were the same as those of example 1.
EXAMPLE 4
The procedure of example 1 was repeated using a 2 diameter by 21/2
inches high chamber with a stainless steel (300 series) surgical
pin measuring 2 inches long by 1/2 inch in diameter using a mixture
of 52 percent hydrogen and 48 percent oxygen (stoichiometric excess
of oxygen) by volume at 500 p.s.i.g. The results were equivalent to
those of example 1
EXAMPLE 5
The procedure of example 4 was repeated with a gold alloy dental
crown using a mixture of 75 percent hydrogen and 25 percent oxygen
by volume (stoichiometric excess of hydrogen) at 500 p.s.i.g. The
results were equivalent to those of example 1.
EXAMPLE 6
The procedure of example 1 was repeated with a nonwoven fabric of 3
denier polypropylene fiber measuring 6 inches long by 4 inches in
diameter using a mixture of 662/3 percent hydrogen and 331/3
percent oxygen by volume (stoichiometric) at two atmospheres
absolute. The results were equivalent to those of example 1.
EXAMPLE 7
Using the equipment illustrated in FIG. 2, wherein the confined
space 28 measured l8 inches long and 2 inches in diameter, portions
of the articles of examples 1 to 6 were provided in the recess 25
in an atmosphere of nitrogen as a neutral atmosphere, hydrogen as a
reducing atmosphere or in certain instances oxygen as an oxidizing
atmosphere and the gas rapidly compressed and decompressed along
the l8 inch length of the chamber by the piston 26 such that there
was a gas compression ratio of about 40 to 1. The results were
similar to those of examples 1 to 6.
EXAMPLE 8
Using the equipment of FIG. 3, a large steel enclosure was provided
measuring 3 feet in diameter by 6 feet long. A large roll of cotton
gauze was provided in a polyethylene bag 29 and the enclosure 33
filled with the bag and roll. The treatment of example 2 was
repeated with equivalent results.
EXAMPLE 9
To test the effectiveness of sterilization a polyethylene film
surface was smeared with the pathogenic bacteria Escherichia Coli
and subjected to the treatment of example 2. It was found the E.
Coli was killed.
EXAMPLE 10
To test the effectiveness of sterilization, the bacteria Bacillus
Stearothermophilus was smeared on a steel surface and subjected to
the treatment of example 4. This bacteria is utilized by those
skilled in the sterilization art to determine the efficacy of
sterilization and normally requires steam at 250.degree. F. for 15
minutes to kill it. Culturing at above about 55.degree. C. is
required for growth. It was found that the bacteria was killed.
In the manner of examples 1 to 10, micro-organisms including virus,
bacteria, mold and yeast were treated by the method of the present
invention and killed. It was found that the thermal pulse
preferentially heated the micro-organisms on the surfaces to the
destruction point because of their very small size and thin cross
section so long as there was no masking effect by liquids or solids
on the surfaces to be sterilized.
In the handling of the article after sterilization, any one of
various known techniques can be utilized. The article can be kept
in the sterilizing unit before use or be placed in a sterile
container. In any event, care must be taken to prevent
contamination by at least pathogenic micro-organisms before use and
possibly even during use for some applications.
It is intended that the foregoing description be only illustrative
of the present invention and it is intended that the present
invention be limited only by the hereinafter appended claims.
* * * * *