AU2007202095B2 - Method and Apparatus for Formulating and Controlling Chemical Concentrations in a Gas Mixture - Google Patents

Method and Apparatus for Formulating and Controlling Chemical Concentrations in a Gas Mixture Download PDF

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AU2007202095B2
AU2007202095B2 AU2007202095A AU2007202095A AU2007202095B2 AU 2007202095 B2 AU2007202095 B2 AU 2007202095B2 AU 2007202095 A AU2007202095 A AU 2007202095A AU 2007202095 A AU2007202095 A AU 2007202095A AU 2007202095 B2 AU2007202095 B2 AU 2007202095B2
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chemical
concentration
capacitor
gas mixture
capacitance
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Michael A. Centanni
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Steris Corp
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Description

14/O0J 2007 FRI 15:35 FAX Smoorenburg Attorneys IF AUSTRALIA II0/2 R005/024 METHOD AND APPARATUS FOR FORMULATING AND CONTROLLING CHEMICAL CONCENTRATIONS IN A GAS MIXTURE Field of the Invention The present invention relates to a method and apparatus for formulating and controlling chemical concentrations in a gas mixture, and more particularly to a method and apparatus for formulating and controlling concentrations of deactivating chemicals in Cl a gas mixture inside a chamber. PCT Application PCTIUS2004/O 15400 as filed and as Cl amended is hereby fully incorporated by references.
Background of the Invention The degree of polarity of a molecule is expressed in terms of a "dipole moment".
Molecules, such as water, that exhibit a separation of charge within the molecule, have non-zero dipole moments. If the separated charges are equal in magnitude but opposite in sign, the magnitude of the dipole moment is equal to the product of the value of one of the separated charges and the distance of separation between the charges. The dipole moment is a vector that points from the negatively charged side of the molecule to the positively charged side of the molecule. The dipole moment depends on three factors, namely, (1) polarity of the molecule, the magnitude of the separated charge, and the geometry of the molecule. It is known that different molecules will have different dipole moments.
For instance, molecules of deactivating chemicals, such as ozone and hydrogen peroxide (14202), have different dipole moments than molecules of water The present invention uses differences in the dipole moments of different molecules as a means for formulating and controlling the concentration of a chemical component in a gas mixture.
Summary of the Invention According to a first aspect of the present invention there is provided a chemical concentration detecting system for determining a concentration of a chemical component in a gas mixture, including: sensing means responsive to changes in the concentration of the chemical component in the gas mixture, said sensing means including a capacitor having first and second conducting elements exposed to the gas mixture, wherein said gas mixture comprises a dielectric therebetween, said capacitor having an electrical property that varies according to the concentration of the chemical component in the gas mixture; COMS ID No: ARCS-161058 Received by P1 Australia: Time 15:44 Date 2007-09-14 14/09 2007 FRI 15:36 FAX Smoorenburg Attorneys IP AUSTRALIA Q006/024 o 2
O
a memory for storing a set of data including property values associated with the Selectrical property and concentration values corresponding with said property values that are indicative of the concentration of the chemical component in the gas mixture; and processing means receiving data from the sensing means and determining the concentration of the chemical component in the gas mixture by accessing the set of data stored in the memory.
0 0 0 COMS ID No: ARCS-161058 Received by IP Australia: Time 15:44 Date 2007-09-14 14/09 2007 FRI 15:36 FAX Smoorenburg Attorneys IP AUSTRALIA Q007/024 o 3 0 According to a second aspect of the present invention there is provided a method C) for determining a concentration of a chemical component in a gas mixture, comprising: exposing a capacitor, having first and second conducting elements, to the gas mixture, wherein said gas mixture comprises a dielectric therebetween, said capacitor having an electrical property that varies according to the concentration of the chemical component in the gas mixture; C pre-storing data including electrical property values associated with said electrical C property of said capacitor and concentration values corresponding with said electrical Sproperty values that are indicative of the concentration of the chemical component in said C'i gas mixture determining an electrical property value associated with the capacitor; and accessing said memory using said electrical property value to determine the concentration of the chemical component in the gas mixture.
COMS ID No: ARCS-161058 Received by IP Australia: Time 15:44 Date 2007-09-14 14/09 2007 FRI 15:36 FAX Smoorenburg Attorneys IP AUSTRALIA Q008/024 o 3a c Other aspects and preferred aspects are disclosed in the specification and/or CD defined in the appended claims, forming a part of the description of the invention.
An advantage of the present invention is the provision of a method and apparatus for formulating and controlling chemical concentrations that senses concentration using electrical properties of a capacitor.
Another advantage of the present invention is the provision of a method and Capparatus for formulating and controlling chemical concentrations in a gas mixture 0< comprised of multiple chemical components.
COMS ID No: ARCS-161058 Received by IP Australia: Time 15:44 Date 2007-09-14 10/05 2007 THU 15:32 FAX Smoorenburg Attorneys IP AUSTRALIA Q007/044 0 o 4 10011] Still another advantage of the present invention is the provision of a method and apparatus for formulating and controlling chemical concentrations that is o simple and inexpensive to implement [00121 These and other advantages will become apparent from the following description of a preferred embodiment taken together with the accompanying 0drawings and the appended claims.
0 0 (N Brief Description of the Drawings S[0013] The invention may take physical fonrm in certain parts and arrangement o of parts, a preferred embodiment of which will be described in detail in the specification and illustrated in the accompanying drawings which form a part hereof, and wherein: 10014] PIG. 1 is a block diagram of a chemical concentration formulating and controlling system, according to a preferred embodiment of the present invention; [0015 PFIG. 2 is a schematic diagram illustrating a sensor circuit; [00161 FIG. 3 is a schematic diagram illustrating a first alternative sensor circuit; 100171 PIG. 4 is a schematic diagram illustrating a second alternative sensor circuit; and [0018] FIG. 5 is a flow diagram illustrating a method for formulating and controlling chemical concentration in a chamber.
Detailed Description of a Preferred Embodiment [0019] It should be understood that the term "gas," as used herein, includes (a) chemical components that are gases at room temperature, and chemical components that are in a vapor phase due to vaporization of a liquid. Moreover, while a preferred embodiment of the present invention is described herein with particular reference to deactivation of biocontamrination, it is contemplated that the invention may also be used in deactivation of other types of contamination, including but not limited to, biowarfare agents and chemical warfare agents organosulfur agents, such as mustard gas HD, HS); G-series nerve agents organophosphate nerve agents), such as tabun sain soman and cyclosarin V-series COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:32 FAX Smoorenburg Attorneys IP AUSTRALIA A008/044 0 0 nerve agents, such as VX, VE, VG, VM and V-gas; vegetative and endospore forming bacteria anthrax); fungi; and virus).
o [0020J Referring now to the drawings wherein the showings are for the purposes of illustrating a preferred embodiment of the invention only and not for purposes of limiting same, FIG. I shows a contamination deactivating system 0according to a preferred embodiment of the present invention. System 10 includes C chemical sources 70A-70C, valves 72A-72C, flowmeters 74A-74C, conduits C 75C, a treatment chamber 100, and a chemical concentration formulating and o controlling system Chemical sources 70A-70C respectively provide a source of o chemicals A, B and C. Conduits 75A-75C respectively provide a travel path for chemicals A, B and C to enter chamber 100. Valves 72A-72C are movable between open and closed positions to respectively control the flow of chemicals A, B and C Sinto conduits 75A-75C. Where the chemicals A, B, or C are generated in a vaporization process vaporized hydrogen peroxide), the respective valve 72A- 72C may be omitted from system 10. Flowmeters 74A-74C are preferably conventional flowmeters comprised of a primary device, a transducer and a transmitter. The transducer senses the fluid that passes through the primary device.
The transmitter produces a usable flow signal from the raw transducer signal. The flow of gas through conduits 75A-75C is precisely regulated using flowmeters 74A- 74C.
(0021] It should be understood that chemicals A, B and C may include "deactivating chemicals" (including, but not limited to antimicrobial chemicals), as well as "base chemicals" and "pre-treatment chemicals." Base chemicals act as a diluent for a deactivating chemical, or as a vehicle or a carrier for a deactivating chemical. The base chemical may itself be a deactivating chemical or have deactivating properties. Pre-treatment chemicals include chemicals that make a contamination more susceptible to deactivation by a deactivating chemical. In the case of prions, pre-treatment chemicals may operate to change a conformational state of the prions, making the prions more susceptible to deactivation. Furthermore, while a preferred embodiment of the present invention is described with reference to a system 10 using three chemicals A, B and C, the number of chemicals used for contamination deactivation may be greater or less than three.
COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:33 FAX Smoorenburg Attorneys IP AUSTRALIA I009/044 c6 100221 In a preferred embodiment, chamber 100 provides a region wherein articles, devices, apparatus, and other objects are exposed to a plurality of deactivating O chemicals to effect deactivation of biocontamination decontamination or sterilization). In the illustrated embodiment, chamber 100 is a "flow-through" chamber having input ports 1 A-i IC in communication with conduits 75A-75C, and an output port 120. The volume of chamber 100 may range from less than I cubic 'I foot to over 1 million cubic feet. A blower or fan (not shown) may be provided to c,1 facilitate the flow of chemicals A, B and C through chamber 100. A filter a Obacteria-retentive filter) may be located at output port 120 to prevent entry of 0 contaminants into chamber 100 through output port 120.
[0023j Chemical concentration formulating and controlling system is generally comprised of a sensor circuit 20, a processing unit 50, an output unit 62, and an input unit 64. Sensor circuit 20 includes a capacitor C, to sense concentration of chemical components in a gas mixture inside chamber 100, as will be described in detail below.
It should be appreciated that the chemical concentration formulating and controlling system may include a plurality of sensor circuits 20 in order to sense concentration of chemical components in more than one region of chamber 100.
10024) A gas mixture in chamber 100 may include (but is not limited to) chemical components that are deactivating chemicals for biocontamination deactivation, such as antimicrobial chemicals decontaminants and sterilants), "base" chemicals, and air. It is contemplated by the inventor that the gas mixture may include chemical components not specifically identified herein, as well as chemical components unrelated to a biocontamination deactivation process, including chemicals having different dipole moments.
100251 In a preferred embodiment processing unit 50 operates with sensor circuit 20, receives data flow signals from flowmeters 74A-74C, and outputs control signals to valves 72A-72C. In addition, processing unit 50 may also output other control signals for the operation of other system elements, such as control means (not shown) for controlling the production of a gas a vaporization system) at sources 70A-70C. Processing unit 50 may also output signals to an output unit 62 to provide operator information in an audible and/or visual form. Accordingly, output unit 62 may take the form of an audio speaker and/or visual display unit. Input unit 64 provides a means for entering information into processing unit 50. In this regard, COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:33 FAX Smoorenburg Attorneys AUSTRALIA II1/4 [a 010/044 input unit 64 may take the form a keyboard, keypad, switches, and the like. In a preferred embodiment, processing unit 50 takes the faorm of a microcomputer or o microcontroller, including a memory 52 for data storage.
[00261 Referring now to FIG. 2, there is shown a detailed schematic of an exemplary sensing circuit 20. Sensor circuit 20 takes the form of a "bridge circuit." As is well known to those skilled in the art, bridge circuits arc used to determine the c-i value of an unknown impedance in termis of other impedances of known value.
0 Highly accurate measurements are possible because a null condition is used to o determine the unknown impedance. The bridge circuit is used to determine a 0 capacitance value indicative of the concentrations of chemical components in chamber 100. In the embodiment shown in FIG. 2, sensing circuit 20 is generally comprised of a voltage source 22, a null detector 30, an electronic potentiometer 40, a capacitor C 1 Of known capacitance, and a capacitor C, Capacitor O, is a conventional capacitor located outside chamber 100, or is insulated from the gas mixture inside chamber 100.
j00271 Capacitor C, is directly exposed to a gas mixture inside chamber 100, wherein the gas mixture fills the gap between the conducting plates of capacitor C,, thereby acting as an insulator or "dielectric" of capacitor Sensor circuit provides data indicative of a capacitance corresponding to a chemical concentration. In this regard, capacitance will vary in accordance with changes in the concentration of chemical components inside chamber 100.
400283 It should be appreciated that the gas mixture may not be the sole dielectric in the gap between the conducting plates of capacitor CX. In this regard, it is contemplated that one or more solid dielectric materials may also be preset in the gap, including, but not limited to, organic or inorganic materials. Furthermore, it should be understood that the plates of capacitor C, may be heated to minimize condensation thereon.
f0029] In a preferred embodiment, capacitor C. is a parallel plate capacitor.
However, it should be appreciated that capacitor C, could be constructed in a different formn. For example, could be a cylindrical or spherical capacitor. If a spherical capacitor is used as capacitor holes must be placed in the outer shell of the capacitor such that the gas mixture can enter and exit the capacitor.
100301 Electronic potentiometer 40 finctions in the same manner as a mechanical potentiometer. In this regard, electronic potentiometer 40 is a three COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:34 FAX Smoorenburg Attorneys IP AUSTRALIA R011/044 0 0 8 c terminal device. Between two of the terminals is a resistive element. The third terminal known as the "wiper" is connected to various points along the resistive o element The wiper is digitally controlled by processing unit 50 (see FIG. The wiper divides the resistive element into two resistors RBc and RAC. Electronic potentiometer 40 may take the form of a digitally programmable potentiometer available from Catalyst Semiconductor, Inc. of Sunnyvale, California.
[0031J In a preferred embodiment, voltage source 22 provides an AC voltage Ci signal, such as a sinusoidal or pulse waveform. Null detector 30 is a device for o detecting a null condition a short circuit), such as a galvanometer, a voltmneter, a C- frequency-selective amplifier, and the like.
[00321 Operation of sensor circuit 20 will now be described in detail. The elements of the bridge circuit are connected between junctions AC, BC, AD, and BD.
Electronic potentiometer 40 is operated by processing unit 50 to vary the resistances RBc and RAC until the potential difference between junctions A and B (VAs) is zero.
When this situation exists, the bridge is said to be balanced or is "nulled." The following relationships then hold for voltages in the main branches: VAC VBc, and VAD Ve,, where VAc is the voltage between junctions A and C, Vac is the voltage between junctions B and C, VAD is the voltage between junctions A and D, and VBD is the voltage between junctions B and D. Accordingly, VAWVAC V n/VaC VAD VRDWAVC yIVc) [0033! The capacitance of capacitor C, is connected between junctions A and D with a known capacitance of capacitor C between junctions B and D. Electronic potentiometer 40, connected from junction A to junction C to junction B, is adjusted by processing unit 50 to vary the voltages Vc and Vac.
100341 When a null is detected by null detector 30, current flows from junction C to junction A to junction D, and a current I flows from junction C to COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:34 FAX Smoorenburg Attorneys IP AUSTRALIA 9012/044 0 0 9 Sjunction B to junction D. The voltage VAC across junctions A to C, and the voltage Vic across junctions B to C are: 0 vc Rc and V hR to') 100351 The voltage across a capacitor with capacitance C, current I, and Sfrequency f is: 2rfC 0 Therefore, the voltages VAo and V 80 may be expressed as:
VAD
V 2 V 2 2zfC, 100361 As discussed above, VAD Vs(V,o>Vc), Vc =lIR.,c. and Vc Rc. Therefore, C, C, R c RAC I [0037] In view of the forgoing relationship, when a null condition is detected, the resistance values for RBc and RAC, along with the known capacitance value of capacitor Cl, can be used to determine unknown value of capacitance for capacitor Cx.
100381 Differences in dipole moments of different molecules are used to determine the concentration of a chemical component in a gas mixture. In this regard, the dielectric constant of a capacitor is dependent on electronic "polarizability." Polarization is the ability of molecules to form a dipole under an electric field or the ability of the electric field to line up or rotate an inherent dipole, such as water molecules. In the event there is only one chemical component in the gas mixture that has a measurable dipole moment, the concentration of the chemical component is determined.
10039] As discussed above, the gas mixture fills the gap between the conducting plates of capacitor C, thereby acting as a dielectric of capacitor CA. By configuring capacitor C as an element of a bridge circuit, a measure of resistance COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:35 FAX Smoorenburg Attorneys IP AUSTRALIA R013/044 values RAc and RBc, when the bridge is balanced or nulled, can be used to determine the capacitance of capacitor The capacitance of capacitor CX is indicative of o concentrations of chemical components in chamber 100, since the permittivity of the respective dielectric is affected by the concentrations of the chemical components in the gas mixture.
ON 10040j It is well known that for a parallel plate capacitor C (icse)(A/d) (EXAd), where C is capacitance, c is the dielectric constant, &D is the permittivity of free space (8.85 x 10-12 a is the permittivity (Farads/ieter) of the capacitor dielectric, A is the area of the capacitor plates (m 2 and d is the separation in meters c'i between the capacitor plates. As E increases, the capacitance C will increase. Where the capacitor is a parallel plate capacitor with circular plates of diameter D, C (xI Fs)/(4d).
10041] It will be appreciated that the dielectric constant K of the capacitor can be determined according to the following expression: 4dC 1c= rTD2 ro' where the value of capacitance, C, is determined as discussed above. The dielectric constant (Kc) of the capacitor can also be determined by determining the capacitance with the dielectric in place between the conducting plates and then determine the capacitance without the dielectric in place The ratio of the two capacitances equals the dielectric constant, Cd
CO
[00421 The response of a capacitor is influenced by the characteristics frequency) of the AC waveform applied thereto. In this regard, capacitive reactance is a function of frequency. Capacitive reactance is the opposition offered to the flow of alternating current by pure capacitance, and is expressed in ohms (X Accordingly, frequency of the waveform generated by voltage source 22 influences the response of capacitors. Thus, the flequency selected for voltage source 22 should preferably be a frequency that will provide a generally linear response for capacitance as the concentration of a chemical component inside chamber 100 is varied. This will facilitate the use of interpolation and extrapolation of capacitance COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:35 FAX Smoorenburg Attorneys IP AUSTRALIA Q014/044 0 values, as will be discussed further below. If a suitable linear response is not obtained, then an expanded set of data points may be stored in memory 52.
10043] It should be appreciated that while one embodiment of the present invention includes a sensor circuit 20 in the form of a bridge circuit, other types of circuits and techniques (including other types of bridge circuits, and capacitance meters) known to those skilled in the art, are suitably used to measure capacitance.
o For example, FIG. 3 illustrates an alternative sensor circuit 20A. Sensor circuit 20A is ci oan LC resonant circuit, having a variable capacitor CA located outside chamber 100 (or ci otherwise isolated from the gas mixture inside chamber 100), and a capacitor C.
odirectly exposed to the gas mixture. In this regard, capacitor C, is located in chamber 100, wherein the gas mixture fills the gap between the conducting plates of capacitor Cx, thereby acting as an insulator or "dielectric" of capacitor CX, Since the resonance frequency wo [L(CA 2 the unknown capacitance of capacitor C, can be determined.
10044] FIG. 4 illustrates yet another alternative sensor circuit 20B suitable for use in connection with the present invention. Sensor circuit 20B is a "charge transfer" sensor circuit. Charge transfer sensor circuits are recognized to provide resolutions of fractions of a femtoFarad. In a charge transfer sensor circuit the unknown capacitance of a sense electrode is determined by charging the sense electrode to a fixed potential, and then transferring that charge to a charge detector comprising a capacitor of known capacitance. In sensor circuit 20B, capacitor C of unknown capacitance is located in chamber 100, wherein the gas mixture fills the gap between the conducting plates of capacitor C, thereby acting as an insulator or "dielectric" of capacitor Capacitor C is first connected to a DC reference voltage via a switch Si. Switch Si is reopened after C is satisfactorily charged to the potential of V, Then, after as brief as possible a delay so as to minimize leakage effects caused by conductance, switch S2 is closed and the charge present on C. is transfMed to capacitor Cs the charge detector). Once the charge Q is satisfactorily transferred to capacitor C, switch S2 is reopened. By reading voltage the capacitance of capacitor C can be determined.
Vs may be input to an amplifier to provide the scaling necessary to present an analogto-digital converter (ADC) with a useful range of voltage for digital processing.
Switch S3 acts as a reset means to reset the charge between charge ransfer cycles, so that each charge transfer cycle has a consistent initial condition. Switches Si, S2 and COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:36 FAX Smoorenburg Attorneys IP AUSTRALIA [a015/044 0 o 12 S3 may be electromechanical switches or transistors. Preferably, digital control logic is used to control switches S 1 S2 and S 3 In a preferred embodiment, C. is selected to be o significantly larger that C.
100451 The equations governing sensor circuit 20B are as follows:
V
8 Vr therefore CIq C. V-CS[VrVJ.
o [0046 It is recognized that in some cases, the capacitance of the capacitor oexposed to the gas mixture located in chamber 100 may be in the range of subfemtoFarad capacitance to low picoFarad capacitance 0.1 fF to 100 pF), and that changes in concentration of chemical components in the gas mixture may only result in a change of capacitance in the range of low picoFarad capacitance or even ferntoFarad capacitances. Accordingly, the sensor circuit used to measure capacitance may need to have high sensitivity to allow for measurement of small values of capacitance. One high sensitivity sensor circuit is the charge transfer sensor circuit described above. Other high sensitivity circuitry is provided by such devices as the PTL 110 capacitance transducer from Process Tomography Limited of Cheshire, United Kingdom. The PTL 110 mesures small values of capacitance (up to picoFarads) with a resolution of i ferntoFarad. A 1616 Precision Capacitance Bridge from ]ET Labs, Inc. of Westbury, New York, allows for measurement of capacitances in the range from 10-7 pF to ItOF. Tektronix produces the Tektronix 130 LC Meter that measures capacitance from 0.3 pF to 3 pF. It has also been acknowledged in the prior art literature that capacitance sensor circuits using modern operational amplifiers and analog-to-digital converters (ADCs) can easily obtain resolutions-to 0.01 pF.
[0047 It should be appreciated that while a preferred embodiment of the present invention uses a measure of a capacitor's capacitance to determine concentrations, it is also contemplated that a measure of other electrical properties of a capacitor may be used to determine concentrations, including, but not limited to, voltage, current, resistance, reactance, charge, permittivity, dielectric constant, or a change in any other electrical property.
10048 With reference to FIGS. I and 5, operation of a prefeured embodiment of the chemical concentration formulating and controlling system, will now be COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:36 FAX Smoorenburg Attorneys IP AUSTRALIA [a016/044 0 o 13 described in detail. FIG. 5 provides a flow diagram 200 describing the formulation and control processes. As described above with reference to FIG. 1, chamber 100 is a "flow through" chamber. Accordingly, deactivating chemicals input to chamber 100 are continuously maintained, and flushed through chamber 100 by exiting through output port 120.
[00491 While operation of a prefered embodiment of the present invention is odescribed herein with reference to "deactivating chemicals" for deactivation of ci o "biocontamination" it is not intended to limit the scope of the present invention. As ci indicated above, chemicals A, B, and C may be selected from chemicals, including, obut not limited to, deactivating chemicals, base chemicals, and pre-treatment chemicals. Moreover, as also noted above, the contamination to be deactivated includes, but is not limited to, biocontamination, chemical warfare agents or biological warfare agents.
[00501 As an initial step, a data set table of data representative of a graph of capacitance versus concentration), relating capacitance of capacitor C to concentration, is detenined for each deactivating chemical of interest (step 210), and stored in memory 52 (step 220). In this regard, atmospheres of individual deactivating chemicals are created inside chamber 100), and the capacitance of capacitor C, is measured as a function of concentration. For instance, capacitor Cx is exposed to verified concentrations of a first deactivating chemical ozone) to determine a -data set associated with the first deactivating chemical. After chamber 100 is evacuated, capacitor C, is exposed to verified concentrations of a second deactivating chemical ethylene oxide) to determine a data set associated with the second deactivating chemical. The forgoing steps are repeated to obtain additional data sets for other deactivating chemicals chlorine dioxide and vaporized hydrogen peroxide).
100511 It should be appreciated that the concentrations of the deactivating chemicals may be verified using well known analytical tools. The analytic tool is preferably selected in accordance with concentration ranges, size of region, desired response time, and duration of measurement. Examples of well known analytic tools for measuring concentrations of chemical components include, but are not limited to, Fourier Transform Infrared (FTIR) spectroscopy, and high quality near-infrared (NIR) spectroscopy.
COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:37 FAX Smoorenburg Attorneys IP AUSTRALIA [017/044 14 [0052] After the data sets are stored in memory 52 for each deactivating chemical of interest, processing unit 50 can commence "formulation" operations.
O With reference to step 230 (FIG. a user selects one or more biocontaminations to be treated using input unit 64 spores, fungi, viruses, bacteria, prions, and other t biocontaminants). Processing unit 50 then determines a proper formulation of deactivating chemicals for deactivation of the one or more selected contaminants (step C' 240). In this regard, processing unit 50 is pre-programmed with data for determining C' appropriate concentrations of a blend of deactivating chemicals to effect proper 0 deactivation of the selected biocontamination(s). For example, if spores are selected
O
C' as the biocontamination, a blend of deactivating chemicals most effective at deactivating spores is determined X ppm of vaporized hydrogen peroxide and Y ppm of ozone). Typically, the range of concentration for treatment with vaporized hydrogen peroxide is 70 ppm to 9000 ppm. However, detecting concentrations of vaporized hydrogen peroxide below 70 ppm may be important to ensure evacuation of vaporized hydrogen peroxide from the chamber. It is contemplated that processing unit 50 is programmed to recognize a hierarchy of contaminants, wherein some contaminants are more difficult to deactivate than others prions). Accordingly, processing unit 50 may determine a deactivation chemistry for deactivating a more difficult to deactivate contamination, that would likewise be effective to deactivate less difficult to deactivate contaminants. For example, a deactivation chemistry effective to deactivate prions might also be effective to deactivate spores and bacteria.
Therefore, processing unit 50 is programmed to determine an optimum deactivation chemistry for deactivating a plurality of selected contaminants.
[0053] After processing unit 50 has determined the concentrations of each chemical component in the blend of deactivating chemicals, each chemical component is sequentially added to chamber 100 in their respective concentrations to form a gas mixture of combined deactivating chemicals (step 250). For example, if the determined blend of deactivating chemicals is comprised of X ppm of chemical A ozone) and Y ppm of chemical B chlorine dioxide), processing unit will maintain valves 72B and 72C in a closed position, and open valve 72A to release chemical A into chamber 100. As indicated above, flow of gas through conduits is precisely regulated using flowmeters 74A-74C. The concentration of chemical A is determined using sensor circuit 20 and the pre-stored data sets. If the capacitance COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 TLHIU 15:37 FAX Smoorenburg Attorneys 4-3. IF AUSTRALIA j1/4 R018/044 0 of capacitor C. is not found in the pre-stored data, the stored data may be interpolated or extrapolated to obtain a concentration corresponding to the measure capacitance of o ~capacitor C,.
100541 When the desired concentration level of X ppm of chemical A is sensed by sensor circuit 20, the flow of chemical A is regulated to maintain that desired concentration level. Next, processing unit 50 opens valve 728 to release cbemical B ci into chamber 100. The concentration of chemical B is increased inside chamber 100 0 until Sensor circuit 20 indicates a capacitance value equal to the sum of: the o capacitance value corresponding to X ppm of chemical A and the capacitance o value of Y ppm of chemical B, where the capacitance values of and have been Pre-stored in memory 52, as discussed above in connection with step 220.
10051 It is believed that the capacitance values corresponding to various concentrations of different chemicals are additive on the basis of the following analysis. It is known that for a gas at room temperature or above, having a permanent dipole moment of p, the dielectric constant may be approximated by.
K=1I+ 4xnp 2 /3kT where n is the number of molecules per unit volume, k is Boltzmann's constant (k= 1.38 x 10" ergfK) and T is the temperature in kelvins. It should be noted that for a given temperature, the dielectric constant (ic) increases linearly with n, the number of molecules of gas per unit volume. The permittivity can then be calculated as follows: Thus, as a result of this formula, it is believed that the capacitance (for a parallel plate capacitor: C as measured as a function of the concentration of a particular polar gas, will increase linearly with concentration. For better sensitivity, two or more capacitors may also be connected in parallel in sensor circuit 20. it is also believed that each data set representative of a curve of capacitance versus concentration for gases of differet dipole moments, will have different slopes. In actuality, for gases that have permanent dipole moments, the dielectric constants -calculated from this COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:38 FAX Smoorenburg Attorneys IP AUSTRALIA [a019/044 0 o 16 equation tend to be somewhat less than the experimental values as the molecules acquire an extra induced dipole moment when placed in an electric field.
o 10056 For single polar gases and mixtures of polar gases, there exists a dipoledipole interaction between the gases. In the case of a single polar gas, it is believed that this dipole-dipole interaction is inherent in the data taken, in the capacitance versus concentration data. In the case of a mixture of different polar gases, the dipole- 0 dipole interaction is not inherent in the data, unless the capacitance versus 0 concentration were measured for the mixture. It is believed, however, that in a mixture of gases, the dipole-dipole interaction may be neglected for the following o reasons. Namely, the force of the dipole-dipole interaction depends on a constant 3) times the product of each dipole moment divided by the distance separating the different dipole moments to the fourth power times an orientational quantity composed of the product of cosines and sines of various angles. Simply stated: F a pjp2(orientational factor)/r.
100571 Since the dipole-dipole force drops off as r 4 the different dipoles need to get very close together to affect one another. Given this relationship, the fact that the gas molecules are moving rapidly and that the gas molecules are somewhat dilute, it is believed that the effect of the dipole-dipole interactions on the capacitance versus concentration curves may be neglected. However, it is understood that this interaction does exist so that when two or more different polar gas molecules are mixed together to form a deactivating atmosphere, the treatment of the gases as separate, noninteracting gases is an approximation. However, as indicated hereinabove, it is believed that the effect that the dipole-dipole interaction between different polar gases of a mixture has on the capacitance versus concentration curves can be neglected without deviating from the spirit of the present invention.
(00581 Referring now to step 260, processing unit 50 continues to monitor the capacitance value sensed by sensor circuit 20, in order to maintain the concentration level in chamber 100 at the desired level, for an appropriate time period. In this regard, processing unit 50 is programmed with the proper exposure time periods to properly deactivate biocontamination associated with the articles or devices inside chamber 100.
COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:38 FAX Smoorenburg Attorneys IP AUSTRALIA Q020/04 4 o 17 10059j It should be understood that preferably one chemnical component should not be added to chamber 100 that would react with, and thus diminish, another o chemical component's (or its own) concentration and effectiveness in deactivating the biocontaniination. However, in the event that some mixed chemical comlponenits rect, if the flow rate into chamber 100 is faster than the reaction rate, the gas mixture in chamber 100 may still be operative to deactivate the biocontamnination. It Should also 0 be understood that the temperature at which the data sets are determined at step 210 0 should generally be the same temperature used during deactivation processing steps 250 and 260.
o 100601 It will be appreciated that for those deactivating chemicals that are 'vaporized, a carier gas will be needed to carry the vaporized deactivating chemical into chamber 100. Examples of such a carrier gas include, but are not limited to, nitrogen, helium, argon and oxygen.
[00611 Processing unit 50 may also be programmed to output other signals, such as control signals for controlIling the production of a gas a vaporization proces). Processing unit 50 may also output signals to output unit 62 to provide an audible and/or visual indicator when the desired concentrations are not within an acceptable range, and when a deactivation process is complete, The visual indicator may assist an operator by including a display of concentration levels.
100621 It is recognized that the deactivating chemicals may be hazardous.
Therefore, it should be understood that well known conventional means may be used to destroy any deacivating chemicals exhausted from chamber 100 through output port 120. The conventional means, include but are not limited to, heating, scrubbing, and catalytic conversion.
[00631 As indicated above, the response of a capacitor is influenced by the characteristics frequency) of' the AC waveform. applied thereto. Therefore, frequency of the AC waveform. applied to capacitor C, should be the same throughout steps 210-260.
[10064] Furthermore, capacitance values corresponding to various concentrations of different chemicals are believed to be additive, as discussed above.
However, it should be appreciated that the capacitance values associated with the concentration of two or more chemical components combined in a gas mixture may also be determined by measuring the capacitance of capacitor C. as the concentrations COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:39 FAX Smoorenburg Attorneys IP AUSTRALIA tj2/4 R021/044 0 18 of the chemical components are varied. In this regard, capacitor Q is exposed to a gas mixture comprised of two or more chemical components. The capacitance of o capacitor CQ is determined as a function of the concentration of the chemical components, as the concentration of each of the chemical components is varied. In this manner, a large set of data is collected and pro-stored in memory 52 that relates capacitance of capacitor C, to several different combinations of concentrations of the ci two or more chemical components. When the concentrations of the chemical c-i components are being formulated, processing unit 50 accesses the pre-stored data to o deternine the concentrations of the two or more chemical components in the gas 0 mixture.
100651 Many deactivating chemicals decay over time due to chemical activity and environmental conditions thermal and photo degradation). For example, Ozone is known to rapidly degrade as the ozone molecule (03) decomposes into molecular oxygen and vaporized hydrogen peroxide is known is decompose into water vapor and molecular oxygen. Consequently, it has been observed in deactivation systems that the concentration of chemical components used in the system Wil decrease over the course of a deactivation processing cycle as a result of decay. In accordance with the present invention, as data sets table of data representative of a time decay graph of capacitance versus concentration), relating capacitance of capacitor Qx to concentration, are determined for each deactivating chemical of interest (step 210), additional data sets are acquired that relate capacitance of capacitor C 1 as a function of time dine decay data sets), for each deactivating chemical of interest. In this respect, data is acquired that is indicative of changes in the concentration of the deactivating chemical due to decay.
[00661 While the process for monitoring the decay of deactivating chemicals is described herein with reference to sensing a change a decrease or an increas) in capacitance, it should be appreciated that the process for monitoring the decay of dcactivating chemicals may alternatively be carried out by sensing a change in voltage, current resistance reactance, charge, pernittivity, dielectric constant or a change in any other electrical property of the capacitor(s).
100671 In the case of a plurality of deactivating chemicals, the capacitance values for each time decay data set can be summed to determine a data set COMS ID No: SBMI-07327252 Received by IP Australia: Time (I-tm) 15:49 Date 2007-05-10 10/05 2007 THU 15:39 FAX Smoorenburg Attorneys 4- IP AUSTRALIA 2/4 Q022/044 0 19 representative of a time decay graph or curve of total capacitance the sumn of the Ct capacitance contributed by all of the deactivating chemicals) as a function of time.
100681 As a deactivation process proceeds, the loss in concentration of each 0 deactivating chemical can be determined with reference to the time decay data sets.
For example, if there are two deactivating chemicals A and B in chamber 100 dining a deactivation proess, when an operating time period elapses, decay of each o deactivating chemical will contribute to a decrease in the total capacitance measured by sensor circuit 20. It should be understood that the present invention may also be used to monitor decay where only one deactivating chemical is used.
[(#0691 The operating time period may be estaished by selecting a C1 Predetermined time interval, sensing a decrease in total capacitance as established by the decay of deactivating chemicals A and B below a threshold value, or sensing a Predetermined percetage dec-reas in total capacitance. It should be appreciated that the timne decay data sets, ibe., of each deactivating chemical, also provide an indication of the rate at which each deactivating chemical decays. This decay rate data can be used for various purposes, including, but not limited to, selecting an appropriate predetermined time interval, threshold value, or percentage decrease.
10070] To replenish both deactivating chemnicals A and B to full concentration levels, reference is made to the time decay data sets relating capacitance as a function of time for each deactivating chemical. These time decay data sets provide a means for determining bow much of the decreas in total capacitance is attributable to the decay Of each of the deactivating chemicals A and B, during the operating time period.
Accordingly, the concentration of each of the deactivating chemicals A and B can the be increased an appropriate amount, thus returning each of the deactivating chemicals A and B to their original concentrations. The capacitance values of the time decay data sets can be related to a specific concentration value using the capacitance versus concentration data sets discussed above. Each deactivating chemical is thus.
replenished until the loss in capacitance for a given time interval, as determined by referencing the individual capacitance versus time curves for each of the deactivating chemicals, is regained.
(00711 It should be understood that in cases where the concentration of a first deactivating chemical decreases more rapidly than a second deactivating chemnical, just the first deactivating chemical may need to be replenished when a first Operating COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:40 FAX Smoorenburg Attorneys IP AUSTRALIA Ij2/4 R023/044 02 time interval has elapsed. When a second operating time interval has elapsed it may then he necessary to replenish both the first and second deactivating chemical.
o100721 If there are no time decay data sets stored for one or more of the specific concentrations of deactivating chemicals used in an actual deactivation Process, but data are stored for other concentrations of the same deactivating chemicals, the available stored data can be interpolated to generate suitable time decay 0data sets for each concentation of the deactivating chemicals actually used.
0 Furthermore, data obtainted during a deactivation process may also be added to the stored data so that future deactivation processes using the same chemistries can be more accurately controlled.
100731 It should be understood that historical data may be used to develop equations wherein an electrical property of a capacitor is expressed as a function of time capacitance Likewise, equations may be developed wherein change in an electrical property of a capacitor is expressed as a function of a change in time Acapacitance For example, one can measure a portion of the time decay curve of an electrical property of a capacitor for a specific deactivating chemical. Once this portion of data has been taken, conventional curve fitting methods can be used to develop an equation that relates the change in an electrical property of the capacitor as a function of time. Since each value of the electrical property of the capacitor corresponds to a unique concentration of the deactivating chemical, the stored equation would provide values of the electrical properties of the capacitor that correspond to a range of concentrations of the deactivating chemical extending from concentrations of 00/ to 100%. Thus, the entire time decay data set is contained in one equation. Typical curve filling or regression analyses may used. For example, the method of least squares may be used to provide an equation that corresponds to the portion of data taken. The method of least squares assumes that the best-fit curve of a given type is the curve that has the minimum sum of the deviations squared (least square error) from a given set of data. If, for instance, during an actual deactivation processing cycle the initial concentration of a deactivating chemical corresponds to a measured electrical property of the capacitor equal to X and if a time interval of T has passed since the inception of the run, the system would use the stored equation to determine the value of the electrical property after time interval T has Passed. The deactivating chemical would be replenished until the original electrical COMS ID No: SBMI-07327252 Received by IP Australia: lime 15:49 Date 2007-05-10 10/05 2007 THU 15:40 FAX Smoorenburg Attorneys IP AUSTRALIA I024/044 o21 cxl property X of the capacitor was restored. In addition, as mentioned above, the time derivative of this equation could be taken thus providing an equation that relates a O change in an electrical property of the capacitor to a change in time.
[00741 As indicated above, there may be more than one sensor circuit 20, each sensor circuit 20 having one or more capacitors for sensing concentration. A capacitor for sensing concentration changes due to decay is preferably located in a region of ochamber 100, wherein the gas molecules have a high residence time, such as a slow cxl oflow rate region of chamber 100, or a "dead zone" region formed in chamber 100, wherein the flow rate is at or near zero.
[0075] While the operation of a preferred embodiment of the present invention has been described with reference to chemical components chemicals A, B, and C) that are deactivating chemicals, it should be understood that chemical components introduced into chamber 100 may include, but-are not limited to, deactivating chemicals antimicrobials), base chemicals diluents for a deactivating chemical, or vehicles or carriers for a deactivating chemical), pre-treatment chemicals, and combinations thereof. For example, chemical A may be a pre-treatment chemical and chemicals B and C may be deactivating chemicals.
10076] The deactivating chemicals include, but. are not limited to, chemicals selected from the group consisting of: hypochlorites, iodophors, quaternary ammonium chlorides (Quats), acid sanitizers, aldehydes (formaldehyde and glutaraldehyde), alcohols, pheuolics, peracetic acid (PAA), chlorine dioxide. Specific examples of deactivating chemicals include, but are not limited to, vaporized hydrogen peroxide, vaporized bleach, vaporized peracid, vaporized peracetic acid, ozone, ethylene oxide, chlorine dioxide, halogen containing compounds, ammonia gas, other gaseous oxidahts, and mixtures thereof The halogens of the halogen containing compounds include, but are not limited to, chlorine, fluorine and bromine.
100771 Examples of base chemicals include, but are not limited to, de-ionized water vapor, distilled water vapor, a vaporized alcohol a tertiary alcohol), and mixtures thereof. As indicated above, the base chemical may itself be a deactivating chemical. Therefbre, the base chemical may also be any one of the deactivating chemicals listed above.
100781 Some examples of atmospheres that may be created inside chamber 100, include, but are not limited to: ozone; vaporized hydrogen peroxide and water COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10 10/05 2007 THU 15:41 FAX Smoorenburg Attorneys IP AUSTRALIA Q025/044 S22 0 Cvapor; ethylene oxide; vaporized hydrogen peroxide, water vapor and ozone; vaporized hydrogen peroxide, water vapor and ethylene oxide; ozone and ethylene oxide; and vaporized hydrogen peroxide, water vapor, ozone and ethylene oxide.
0 Other modifications and alterations will occur to others upon their reading and understanding of the specification. It is intended that all such modifications and Salterations be included insofar as they come within the scope of the invention as claimed O or the equivalents thereof.
N "Comprises/comprising" when used in this specification is taken to specify the presence of stated features, integers, steps or components but does not preclude the O 10 presence or addition of one or more other features, integers, steps, components or groups C thereof.
COMS ID No: SBMI-07327252 Received by IP Australia: Time 15:49 Date 2007-05-10

Claims (11)

  1. 2. A chemical concentration detecting system according to claim 1, wherein said capacitor is selected from the group consisting of: a parallel plate capacitor, a cylindrical capacitor, and a spherical capacitor.
  2. 3. A chemical concentration detecting system according to claim 1 or 2, wherein said processing means determines a concentration of the chemical component in the gas mixture using said property values to locate corresponding concentration values stored in said memory.
  3. 4. A chemical concentration detecting system according to claim 1, 2 or 3, wherein said processing means interpolates or extrapolates said set of data to determine the concentration of the chemical component in the gas mixture. A chemical concentration detecting system according to any one of claims 1 to 4, wherein said chemical component is an antimicrobial chemical. COMS ID No: ARCS-161058 Received by IP Australia: Time 15:44 Date 2007-09-14 14/09 2007 FRI 15:37 FAX Smoorenburg Attorneys -4-44 IP AUSTRALIA Ij1/2 Q010/024 o 24 Cl6. A chemical concentration detecting system according to claim 5, wherein said antimicrobial chemical is a gaseous oxidant.
  4. 7. A chemical concentration detecting system according to claim 5 or 6, wherein said antimicrobial chemical is selected from a group consisting of: vaporized hydrogen peroxide, vaporized peracid, vaporized peracetic acid, vaporized bleach, ozone, ethylene 0 oxide, ammonia gas, a halogen containing compound, and mixtures thereof o8. A chemical concentration detecting system according to any one of claims I to 7, O wherein said electrical property that varies according to the concentration of the chemical component is selected from the group consisting of the following: resistance, voltage, current, reactance, charge, permittivity, and dielectric constant.
  5. 9. A method for determining a concentration of a chemical component in a gas mixture, including: exposing a capacitor, having first and second conducting elements, to the gas mixture, wherein said gas mixture comprises a dielectric therebetween, said capacitor having an electrical property that varies according to the concentration of the chemical component in the gas mixture; pre-storing data including electrical property values associated with said electrical property of said capacitor and concentration values corresponding with said electrical property values that are indicative of the concentration of the chemical component in said gas mixture determining an electrical property value associated with the capacitor; and accessing said memory using said electrical property value to determine the concentration of the chemical component in the gas mixture. A method according to claim 9, wherein said step of accessing said memory to determine the relative concentration of the chemical component in said gas mixture includes: -using said electrical property values to locate corresponding concentration values. COMS ID No: ARC5-161058 Received by IP Australia: Time 15:44 Date 2007-09-14 14/09 2007 FRI 15:37 FAX Smoorenburg Attorneys AUSTRALIA01/2 [a 011/024 o
  6. 11. A method according to claim 9 or 10, wherein said method further includes: interpolating or extrapolating the pre-stored data to determine the concentration of the CO chemical component in said gas mixture.
  7. 12. A method according to claim 9, 10 or 11, wherein said chemical component is an a> antimicrobial chemical.
  8. 013. A method according to claim 12, wherein said antimicrobial chemical is a gaseous o oxidant.
  9. 14. A method according to claim 12 or 13, wherein said antimicrobial chemical is selected from a group consisting of: vaporized hydrogen peroxide, vaporized peracid, vaporized peracetic acid, vaporized bleach, ozone, ethylene oxide, ammonia gas, a halogen containing compound, and mixtures thereof. A method according to any one of claims 9 to 14, wherein said electrical property that varies according to the concentration of the chemical component is selected from the group consisting of the following: resistance, voltage, current, reactance, charge, permittivity, and dielectric constant.
  10. 16. A method for determining a concentration of a chemical component in a gas mixture as claimed in claim 9, substantially as herein described with reference to the accompanying drawings.
  11. 17. A chemical concentration detecting system as claimed in claim 1, substantially as herein described with reference to the accompanying drawings. COMS ID No: ARCS-161058 Received by IP Australia: Time 15:44 Date 2007-09-14
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US20040178804A1 (en) * 2003-03-14 2004-09-16 Steris Inc. Method and apparatus for detection of contaminants in a fluid

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