Calibration cartridge for use in calibrating ancillary sensors on a permeation analyzer

Abstract

A calibration cartridge and method of calibrating at least one ancillary sensor of a target-analyte permeation analyzer using the calibration cartridge. The calibration cartridge includes a manifold block and a previously calibrated calibration ancillary sensor. The manifold block defines a chamber configured and arranged to interface with the target-analyte permeation analyzer for fluid communication with each of a test gas having a known concentration of a target-analyte and an inert target-analyte-free carrier gas used by the target-analyte permeation analyzer to measure permeation across a solid test sample. The previously calibrated calibration ancillary sensor is in sensing communication with the chamber for sensing and measuring the same ancillary parameter as one of the instrument's ancillary sensors.

Description

CALIBRATION CARTRIDGE FOR USE IN CALIBRATING ANCILLARY SENSORS ON A PERMEATION ANALYZER BACKGROUND

[0001] Permeation analyzers are widely used to measure the transmission rate of various analytes, typically O2, CO2 or water vapor, through films and containers. A leading source of permeation analyzers is AMETEK-MOCON, who offer permeation analyzers under the brands OX-TRAN for measuring the transmission rate of O2, PERMATRAN for measuring the transmission rate of CO2 and AQUATRAN for measuring the transmission rate of water vapor.

[0002] These permeation analyzers employ cartridges which interact with a test film or container to create chambers sealed off from one-another and separated by the test film or container, with a drive cell in fluid communication with a source of gas having a known nonzero concentration of the target-analyte (e.g., O2, CO2 or water vapor) and the test cell in fluid communication with a source of inert carrier gas e.g., N2) for transporting any target- analyte that permeates through the film or container from the drive cell into the test cell to a primary sensor capable of detecting and measuring target- analyte in the inert carrier gas.

[0003] Numerous variables can meaningfully impact test results, including flow rate Q of test and carrier gases through the drive and test cells respectively, relative humidity RH of the test and carrier gases flowing into the drive and test cells respectively, temperature T of the test and carrier gases within the drive and test cells respectively, and pressure P of the test and carrier gases within the drive and test cells respectively. Hence, permeation analyzers typically include ancillary sensors for monitoring each of these variables and signaling when the variable is outside an acceptable range for allowing remedial action.

[0004] The ancillary sensors need to be periodically calibrated, as they are susceptible to drift and occasionally experience impact damage. Calibration of these ancillary sensors on permeation analyzers typically requires either an onsite visit by a trained and qualified service representative, or transport of the permeation analyzer to a repair and servicing facility. Both are expensive and involve substantial down time.

[0005] Hence, a substantial need exists for an option allowing on-site customer calibration of ancillary sensors on permeation analyzers that does not require the presence of a trained and qualified service representative.SUMM RY OF THE INVENTION

[0006] A first aspect of the invention is a calibration cartridge for calibrating at least one instrument ancillary sensor of a target-analyte permeation analyzer, wherein the targetanalyte permeation analyzer measures permeation across a solid test sample using a test gas having a known concentration of a target-analyte and an inert target- analyte-free carrier gas, and each instrument ancillary sensor measures a different ancillary parameter.

[0007] A first embodiment of the first aspect of the invention is a calibration cartridge that includes a manifold block and a previously calibrated calibration ancillary sensor. The manifold block is configured and arranged to interface with the target-analyte permeation analyzer for placing a chamber within the manifold block into discrete fluid communication with each of the test gas and the carrier gas. The previously calibrated calibration ancillary sensor is in sensing communication with the chamber for sensing and measuring the same ancillary parameter as one of the instrument ancillary sensors.

[0008] A second embodiment of the first aspect of the invention is a calibration cartridge that includes a manifold block and a plurality of previously calibrated calibration ancillary sensor. The manifold block is configured and arranged to interface with the targetanalyte permeation analyzer for placing a chamber within the manifold block into discrete fluid communication with each of the test gas and the carrier gas. The previously calibrated calibration ancillary sensors are each in sensing communication with the chamber for sensing and measuring one of the ancillary parameters sensed and measured by one of the instrument ancillary sensors.

[0009] Third and fourth embodiments of the first aspect of the invention are calibration cartridges that interface with target- analyte permeation analyzers that operate by interfacing with a removable test-sample retention cartridge so as to place a solid test sample secured within the test-sample retention cartridge into fluid communication with a test gas having a known concentration of a target-analyte and an inert target- analyte-free carrier gas whereby the solid test sample maintains physical separation of the test and carrier gases from which permeation of target- analyte through the solid test sample from the test gas into the carrier gas can be sensed and quantified by a target-analyte sensor.

[0010] The third embodiment of the first aspect of the invention is a calibration cartridge that includes a manifold block and a previously calibrated calibration ancillary sensor. The manifold block is configured and arranged for removable interfacing with thetarget- analyte permeation analyzer as a surrogate test-sample retention cartridge, for placing a chamber within the manifold block into separated fluid communication with the test gas and the carrier gas. The previously calibrated calibration ancillary sensor is in sensing communication with the chamber for sensing and measuring the same ancillary parameter as one of the instrument ancillary sensors.

[0011] The fourth embodiment of the first aspect of the invention is a calibration cartridge that includes a manifold block and a plurality of previously calibrated calibration ancillary sensor. The manifold block is configured and arranged for removable interfacing with the target-analyte permeation analyzer as a surrogate test-sample retention cartridge, for placing a chamber within the manifold block into separated fluid communication with the test gas and the carrier gas. The previously calibrated calibration ancillary sensors are each in sensing communication with the chamber for sensing and measuring one of the ancillary parameters sensed and measured by one of the instrument ancillary sensors.

[0012] A second aspect of the invention is a method of calibrating at least one instrument ancillary sensor of a target-analyte permeation analyzer, wherein the targetanalyte permeation analyzer measures permeation across a solid test sample using a test gas having a known concentration of a target-analyte and an inert target- analyte-free carrier gas, and each instrument ancillary sensor measures a different ancillary parameter.

[0013] A first embodiment of the second aspect of the invention includes the steps of:(A) obtaining a calibration cartridge having a previously calibrated calibration ancillary sensor that measures the same ancillary parameter as one of the instrument ancillary sensors,(B) interfacing the calibration cartridge and the target-analyte permeation analyzer to form an interfaced unit, (C) effecting flow of the test gas into or through the interfaced unit and into contemporaneous sensing communication with each of the instrument ancillary sensor and the calibration ancillary sensor that measure the same ancillary parameter, (D) contemporaneously sensing and measuring the ancillary parameter of the test gas flowing into or through the interfaced unit with the instrument ancillary sensor to obtain an instrument ancillary parameter value and the calibration ancillary sensor to obtain a calibration ancillary parameter value, (E) comparing the instrument ancillary parameter value and the calibration ancillary parameter value to obtain a variation value A therebetween, and (F) calibrating the instrument ancillary sensor based upon the variation value A.

[0014] A second embodiment of the second aspect of the invention includes the steps of: (A) obtaining a calibration cartridge having a plurality of previously calibrated calibration ancillary sensors, each operable for sensing and measuring one of the ancillary parameters sensed and measured by one of the instrument ancillary sensors, (B) interfacing the calibration cartridge and the target-analyte permeation analyzer to form an interfaced unit, (C) effecting flow of the test gas into or through the interfaced unit and into contemporaneous sensing communication with each of the plurality of instrument ancillary sensors and each of the calibration ancillary sensors, (D) contemporaneously sensing and measuring ancillary parameters of the test gas flowing into or through the interfaced unit with each of the plurality of instrument ancillary sensors to obtain an instrument ancillary parameter value for each ancillary parameter and each of the plurality of calibration ancillary sensors to obtain a calibration ancillary parameter value for each ancillary parameter, (E) comparing the instrument ancillary parameter value and the calibration ancillary parameter value for each ancillary parameter value to obtain a variation value A therebetween, and (F) calibrating each of the instrument ancillary sensors based upon the variation value A for the ancillary parameter measured by the instrument ancillary sensor.

[0015] A third embodiment of the second aspect of the invention includes the steps of: (A) obtaining a calibration cartridge having a previously calibrated calibration ancillary sensor that measures the ancillary parameter measured by one of the instrument ancillary sensors, (B) interfacing the calibration cartridge and the target- analyte permeation analyzer to form an interfaced unit, (C) effecting flow of a designated gas selected from the carrier gas and the test gas into or through the interfaced unit and into contemporaneous sensing communication with each of the instrument ancillary sensor and the calibration ancillary sensor, (D) contemporaneously sensing and measuring the ancillary parameter of the designated gas flowing into or through the interfaced unit with the instrument ancillary sensor to obtain an instrument ancillary parameter value and the calibration ancillary sensor to obtain a calibration ancillary parameter value, (E) comparing the instrument ancillary parameter value and the calibration ancillary parameter value to obtain a variation value A therebetween, and (F) calibrating the instrument ancillary sensor based upon the variation value A.

[0016] A fourth embodiment of the second aspect of the invention includes the steps of: (A) obtaining a calibration cartridge having a plurality of previously calibrated calibration ancillary sensors, each operable for sensing and measuring one of the ancillary parameterssensed and measured by one of the instrument ancillary sensors, (B) interfacing the calibration cartridge and the target-analyte permeation analyzer to form an interfaced unit, (C) effecting flow of a designated gas selected from the carrier gas and the test gas into or through the interfaced unit and into contemporaneous sensing communication with each of the plurality of instrument ancillary sensors and each of the calibration ancillary sensors, (D) contemporaneously sensing and measuring ancillary parameters of the designated gas flowing into or through the interfaced unit with each of the plurality of instrument ancillary sensors to obtain an instrument ancillary parameter value for each ancillary parameter and each of the plurality of calibration ancillary sensors to obtain a calibration ancillary parameter value for each ancillary parameter, (E) comparing the instrument ancillary parameter value and the calibration ancillary parameter value for each ancillary parameter value to obtain a variation value A therebetween, and (F) calibrating each of the instrument ancillary sensors based upon the variation value A for the ancillary parameter measured by the instrument ancillary sensor.BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 A is a schematic view of a prior art target- analyte permeation analyzer for measuring target-analyte permeation of films and membranes, with the analyzer equipped with ancillary sensors for measuring ancillary parameters.

[0018] Figure IB is a schematic view of the target- analyte permeation analyzer depicted in Figure 1 A operably connected to a calibration cartridge in accordance with the invention for calibrating the ancillary sensors of the target- analyte permeation analyzer.

[0019] Figure 2A is a schematic view of a prior art target-analyte permeation analyzer for measuring target-analyte permeation of containers, with the analyzer equipped with ancillary sensors for measuring ancillary parameters.

[0020] Figure 2B is a schematic view of the target- analyte permeation analyzer depicted in Figure 2A operably connected to a calibration cartridge in accordance with the invention for calibrating the ancillary sensors of the target- analyte permeation analyzer.DETAILED DESCRIPTION OF A PREFERRED EMBODIMENTDefinitions

[0021] As utilized herein, including the claims, the phrase “ancillary parameter” means a variable capable of impacting a permeation measurement other than a sensor detecting and / or quantifying target-analyte. Exemplary ancillary parameters are flow rate, relative humidity except when water vapor is the target-analyte, temperature and pressure.

[0022] As utilized herein, including the claims, the phrase “ancillary sensor” means a sensor detecting a parameter capable of impacting a permeation measurement other than a sensor detecting and / or quantifying target-analyte. Exemplary ancillary sensors are flow sensors, relative humidity sensors except when water vapor is the target-analyte, temperature sensors and pressure sensors.

[0023] As utilized herein, including the claims, the phrase “separate or separated fluid communication” when used in reference to test and carrier gases means the gases are physically separated (<?.g. , separate sub-chambers or cells) or temporally separated (<?.g., separately timed flows through a common chamber).

[0024] As utilized herein, including the claims, the phrase “target-analyte” means the analyte whose permeability through a test sample is being measured. Exemplary targetanalytes are O2, CO2 and water vapor.

[0025] As utilized herein, including the claims, the phrase “test sample” means an article whose permeability is being measured. Exemplary test samples include packaging films, whole finished packages and containers.Nomenclature TableConstruction

[0026] Referring generally to Figures 1 A, IB, 2A and 2B, the invention is directed to calibration cartridge 300 for calibrating an instrument ancillary sensor 160n of a targetanalyte permeation analyzer 100.

[0027] Referring generally to Figures 1A and 2 A, the target-analyte permeation analyzer 100 includes at least a test sample cartridge 10, a target- analyte sensor 130, a controller 140, a user interface 150 and one or more instrument ancillary sensors 160n.Target-Analyte Permeation Analyzer - Films and Membranes

[0028] Referring to Figure 1 A, target- analyte permeation analyzers 100 for measuring permeation of a film or membrane TSF include a test sample cartridge 10 that defines a testing chamber 19 operable for engaging a test film TSF such that the testing chamber 19 is sealingly separated by the test film TSF into a first cell 19i and a second cell 192.Specifically, the test sample cartridge 10 can include at least (i) a first plate 11 defining the first cell 19i, (ii) a second plate 12 defining the second cell 192, (iii) a clamping mechanism (not shown) for releasable clamping of the first and second plates 11 and 12 for changing test films TSF. The target-analyte sensor 130 is in fluid communication with the second cell 192 for sensing target analyte which has permeated through the test film TSF from the first cell 19i into the second cell 192.

[0029] An exemplary embodiment of a system capable of measuring the transmission rate of a target- analyte through a test film TSF utilizing a target-analyte permeation analyzer instrument 100 is depicted in Figure 1 A. The test sample cartridge 10 defines a testing chamber 19 sealingly divided by a film TSF to be tested into a first cell 19i and a second cell 192.

[0030] A source of test gas TG containing a known concentration of a target analyte, communicates with the first cell 19i via test gas cartridge inlet fluid flow line HOmTG for continuously providing the first cell 19i with test gas to ensure that the concentration of target-analyte within the first cell 19i remains constant throughout a test period. Test gas within the first cell 19i exits via test gas cartridge outlet fluid flow line IIOIITG.

[0031] A source of an inert carrier gas CG communicates with the second cell 192 via carrier gas cartridge inlet fluid flow line HOmcG for flushing the second cell 192 prior to testing and then during testing carrying target- analyte which has permeated through the test film TSF from the first cell 19i into the second cell 192 to the target-analyte sensor 130. Inert carrier gas within the second cell 192 exits via carrier gas cartridge outlet fluid flow line HOncG, which splits for selectively and alternatively venting the inert carrier gas directly to atmosphere during flushing of the second cell 192 prior to testing, or directing the inert carrier gas into target-analyte sensor 130 for measurement of target-analyte during testing. Suitableinert carrier gases include specifically, but not exclusively, nitrogen, argon, helium, krypton, a blend of nitrogen and hydrogen, etc.

[0032] Channels (not shown) in the test sample cartridge 10 and a flow control system 140 direct and control the flow of test gas into and out from the first cell 19i and inert carrier gas into and out from the second cell 192.

[0033] A shutoff valve 120TG can be provided in test gas cartridge inlet fluid flow line llOmTG for controlling the flow of test gas through the first cell 19i. Similarly, a shutoff valve 120CGI can be provided in carrier gas cartridge inlet fluid flow line HOmcG for controlling the flow of inert carrier gas through the second cell 192. A separate three-way valve 129CG2 can be placed in carrier gas cartridge outlet fluid flow line HOncG for selectively and alternatively directing flow of inert carrier gas exiting the second cell 192 directly to atmosphere during flushing of the second cell 192 prior to testing or into targetanalyte sensor 130 for measurement of target- analyte in the carrier gas during testing.

[0034] The target- analyte sensor 130 for sensing target- analyte is placed in fluid communication with the second cell 192 for sensing the presence of target-analyte within the second cell 192. Typical target-analytes of interest include oxygen, carbon dioxide and water vapor. The target- analyte sensor 130 may be selected from any of the wide variety of commercially available sensors capable of detecting the target-analyte of interest, with electrochemical sensors generally preferred based upon the high sensitivity and low cost of such sensors and the fact that such sensors, when employed in the present invention, follow Faraday’s Law - eliminating the need to calibrate the sensor.

[0035] The target- analyte sensor 130 communicates via electrical leads (unnumbered) with a suitable central processing unit 140 equipped with electronic memory (not shown) for storing, and a user interface 150 having a keyboard, mouse, display, touchscreen, and / or printer for reporting target- analyte concentrations detected by the target- analyte sensor 130.

[0036] The test sample cartridge 10, formed from the first 11 and second 12 plates, has a lateral width extending from a right side to a left side, a longitudinal thickness extending from a top major surface to a bottom major surface, and a transverse z length extending from a front edge to a back edge.

[0037] The first plate 11 has an interior major surface which faces the second plate 12 when the plates 11 and 12 are clamped together to form the test sample cartridge 10, and anexterior major surface which is the bottom major surface of the test sample cartridge 10 when the plates 11 and 12 are clamped together to form the test sample cartridge 10.

[0038] Inlet and outlet ports in the first plate 11 are configured and arranged for fluid connection to test gas cartridge inlet fluid flow line IIOHITG and test gas cartridge outlet fluid flow line I IOIITG respectively, for directing test gas into and out from the first cell 19i.

[0039] In similar fashion the second plate 12 has an interior major surface which faces the first plate 11 when the plates 11 and 12 are clamped together to form the test sample cartridge 10, and an exterior major surface which is the top major surface of the test sample cartridge 10 when the plates 11 and 12 are clamped together to form the test sample cartridge 10.

[0040] Inlet and outlet ports in the second plate 12 are configured and arranged for fluid connection to carrier gas cartridge inlet fluid flow line HOmcG and carrier gas cartridge outlet fluid flow line HOncG respectively, for directing inert carrier gas into and out from the second cell 192.

[0041] The first and second plates 11 and 12 each preferably comprise a unitary metal piece to eliminate cracks, seams, joints and fissures through the plates 11 and 12 and into fluid communication with the respective cells 19i and 192.

[0042] A set of alignment pins (not shown) can extend longitudinally out from the interior major surface of the first plate 11 with corresponding alignment holes (not shown) provided in the interior major surface of the second plate 12 for accepting insertion of the alignment pins, so as to ensure a proper and consistent alignment and rotational orientation of the plates 11 and 12 relative to one another. Alternatively, placement of the alignment pins and alignment holes on the first and second plates 11 and 12, can be reversed.

[0043] An edge leakage minimizing feature can be provided, such as a longitudinally aligned pair of upper and lower O-rings (unnumbered) positioned within the interface between the first and second plates 11 and 12, for engaging and compressing a periphery of the test sample TS film TSF around the testing chamber 19 when the plates 11 and 12 are clamped together. Compression of the sample TS test film TSF around the testing chamber 19 forms a peripheral edge seal around the testing chamber 19 so as to control leakage of target analyte into the second cell 192 and thereby ensure that target analyte found within the second cell 192 permeated across the test film TSF from the first cell 19i into the second cell

[0044] Any of the well known and readily available compressing and clamping devices may be used as the clamping mechanism (not shown) to clamp the plates 11 and 12 together, including specifically but not exclusively manually-operated lever and rotary mechanical actuators such as a plurality of bolts and threaded bolt holes or pass through bolt holes in or through the plates 11 and 12 respectively, circumscribing the first and second cells 19i and 192 respectively, or electromechanical actuators such as a servomotor, pneumatic actuators, or hydraulic actuators.

[0045] A compression sensor (not shown) can be employed to sense and report the clamping pressure and / or force exerted upon and / or experience by the plates 11 and 12, and reporting the value to the controller 140 for maintaining a consistent compression pressure and / or force for each sample TS test film TSF.

[0046] A variety of ancillary parameters can impact permeation measurement, including specifically but not exclusively flow rate, relative humidity, temperature and pressure of each of the test and carrier gases residing in or flowing through each of the first and second cells 19i and 192. Quality target- analyte permeation analyzers 100 include instrument ancillary sensors 160n(i.e., instrument ancillary sensors for measuring various carrier gas ancillary parameters (n) 160cGn and instrument ancillary sensors for measuring various test gas ancillary parameters (n) 160TGII) and corresponding modules for maintaining a consistent value of the ancillary parameter (n) based upon the sensed value of the ancillary parameter (n).

[0047] As with the target-analyte sensor 130, instrument ancillary sensors 160n communicate via electrical leads (unnumbered) with the central processing unit 140 for reporting ancillary parameters (n) 160cGn and 160TGH detected by the instrument ancillary sensors 160n.Calibration Cartridge for Tarset-Anal te Permeation Analyzer - Films and Membranes

[0048] The calibration cartridge 300 is configured and arranged to interface with a target- analyte permeation analyzer 100 as a surrogate test sample cartridge 10. The calibration cartridge 300 includes a manifold block 310 defining a chamber 319 for physically or temporally separated selective fluid communication of the manifold chamber 319 with each of the carrier gas and test gas delivered to the target-analyte permeation analyzer 100. The calibration cartridge 300 includes one or more calibrated calibrationancillary sensors 360n (i.e., calibration ancillary sensors for measuring various carrier gas ancillary parameters (n) 360cGn and calibration ancillary sensors for measuring various test gas ancillary parameters (n) 360TGH), each of which sense and measure the same ancillary parameter as one of the instrument ancillary sensors 160n of the target-analyte permeation analyzer 100.

[0049] As with the instrument ancillary sensors 160n, the calibrated calibration ancillary sensors 360n communicate via suitable means such as electrical leads (unnumbered) or a wireless communication module 400 such as bluetooth, with the central processing unit 140 for reporting ancillary parameters (n) 360cGn and 360TGII detected by the calibrated calibration ancillary sensors 360n.

[0050] The calibration ancillary sensors 360n are pre-calibrated whereby any deviation A between the parameter value measured by the instrument ancillary sensor 160n for parameter n and the parameter value measured by the calibration ancillary sensor 360n for the same parameter can be used to calibrate the instrument ancillary sensor 160n.Tarset-Analyte Permeation Analyzer - Containers

[0051] Referring to Figure 2A, target- analyte permeation analyzers for measuring permeation through a package or container TSp can include a test sample cartridge 10 for use in conjunction with a target-analyte permeation testing instrument 100 for measuring transmission rate of a target analyte through an empty package or container TSp.

[0052] One embodiment of the test sample cartridge 10 has a footplate (not separately numbered) and a vessel atop the footplate (not separately numbered) defining a testing chamber (unnumbered) operable for releasably engaging an overlay (not shown) constructed from a gas impermeable material such that the testing chamber is separated by the overlay into a first side volume (predominately within the footplate) and a second side volume (predominantly within the vessel) throughout a testing period, with (i) at least one orifice (not shown) through the overlay within a defined zone on the overlay operable for providing fluid communication between the first and second side volumes throughout a testing period, (ii) a first set of inlet and outlet ports (not shown) for providing flow of a target-analyte free inert carrier gas from a source of carrier gas CG through carrier gas fluid flow line IIOCG into and out from the first side volume throughout a testing period, and (iii) a second set of inlet and outlet ports (not shown) for providing flow of a test gas containing a known concentration of target analyte from a source of test gas TG through test gas fluid flow line IIOTG into and outfrom the second side volume, other than through the at least one orifice through the overlay, throughout a testing period, whereby sealed mounting of the open end of the empty package or container TSp onto the overlay, such as by a sealant (not shown), over the defined zone of the overlay with the package or container TSp retained within the second side volume divides the second side volume into an container volume 319i enclosed by the empty package or container TSp in exclusive fluid communication with the first side volume and the targetanalyte free inert carrier gas, and a headspace volume 3192 surrounding the empty package or container TSp and enclosed by the cartridge 10 in exclusive fluid communication with the target- analyte containing test gas.

[0053] The vessel can be made from any material capable of sealingly separating the headspace volume 3192 from the surrounding atmosphere including metal, plastic and glass. The vessel is preferably transparent for allowing visual observation of the empty package or container TSp within the headspace volume 3192.

[0054] Test gas fluid flow line IIOTG delivers test gas to the headspace volume 3192 of the vessel to achieve a steady known concentration of target analyte within the headspace void volume 3192 during testing. A test gas outlet (unnumbered) can be configured and arranged on the cartridge 10 to simply vent test gas from the headspace volume 3192 during testing as sensing of the test gas is not performed and typical target analytes tested, e.g., oxygen, carbon dioxide and water vapor, are harmless analytes found in abundance in Earth’s atmosphere.

[0055] Carrier gas fluid flow line IIOCG delivers carrier gas from a source of targetanalyte free carrier gas CG to the container volume 319i enclosed by the empty package or container TSp of the vessel and then from the container volume 319i to either atmosphere during flushing of the container volume 3191 prior to commencement of the testing period or to the target-analyte sensor 130 of the target-analyte permeation testing instrument 100 during testing periods.

[0056] The test sample cartridge 10 for measuring transmission rate of a target analyte through an empty package or container TSp is used in conjunction with a targetanalyte permeation testing instrument 100 for measuring transmission rate of a target analyte through an empty package or container TSp. In general terms, the target-analyte permeation testing instrument 100 includes a carrier gas fluid flow line IIOCG in fluid communicationwith a source of target- analyte free carrier gas CG and a test gas fluid flow line IIOTG in fluid communication with a source of target-analyte containing test gas TG.

[0057] Upon opening of a fluid flow valve 120TG in the test gas fluid flow line IIOTG, target- analyte containing test gas flows from the source of target- analyte containing test gas TG into the headspace volume 3192 and then out of the headspace volume 3192 through the test gas outlet port or vent to atmosphere.

[0058] Upon opening of a primary valve 120CGI in the carrier gas fluid flow line IIOCG, target- analyte free carrier gas flows from the source of the gas CG through the container volume 3191 enclosed by the empty package or container TSP mounted onto the overlay via orifices in the overlay, and then selectively via three way venting valve 120CG2 to atmosphere or target- analyte sensor 130. The instrument 100 includes a controller 140 and a user interface 150 for setting and controlling flow of target-analyte free carrier gas, setting and controlling sensing parameters for sensing of target- analyte carried by the carrier gas from the container volume 319i to the target-analyte sensor 130, and recording and reporting sensed target-analyte and calculated target- analyte transmission rate values.

[0059] As with target-analyte permeation analyzers 100 for measuring permeation of a film or membrane TSF, target- analyte permeation analyzers 100 for measuring permeation through a package or container TSP, a variety of ancillary parameters can impact permeation measurement, including specifically but not exclusively flow rate, relative humidity, temperature and pressure of each of the test and carrier gases residing in or flowing through each of the container volume and headspace volume 319i and 3192. Quality target-analyte permeation analyzers 100 include instrument ancillary sensors 160n (i.e., instrument ancillary sensors for measuring various carrier gas ancillary parameters (n) 160cGn and instrument ancillary sensors for measuring various test gas ancillary parameters (n) 160TGII) and corresponding modules for maintaining a consistent value of the ancillary parameter (n) based upon the sensed value of the ancillary parameter (n).

[0060] As with the target-analyte sensor 130, instrument ancillary sensors 160n communicate via electrical leads (unnumbered) with the central processing unit 140 for reporting ancillary parameters (n) 160cGn and 160TGH detected by the instrument ancillary sensors 160n.Calibration Cartridge for Target-Analyte Permeation Analyzer - Containers

[0061] The calibration cartridge 300 described for use in calibrating the instrument ancillary sensors 160n of a target- analyte permeation analyzer 100 for measuring permeation of a film or membrane TSF, are suitable mutandis mutatis for use in calibrating the instrument ancillary sensors 160nof a target-analyte permeation analyzer 100 for measuring permeation of a test package or container TSP, adjusted as appropriate to interface with the fluid flow lines IIOCG and IIOTG of the target-analyte permeation analyzer 100 for measuring permeation of a test package or container TSp.

Claims

We claim:

1. A calibration cartridge for calibrating an instrument ancillary sensor of a targetanalyte permeation analyzer, wherein the instrument ancillary sensor measures an ancillary parameter, and the target- analyte permeation analyzer is configured and arranged to measure permeation across a solid test sample using a test gas having a known concentration of a target-analyte and an inert target-analyte-free carrier gas, the calibration cartridge comprising:(a) a manifold block configured and arranged to interface with the target- analyte permeation analyzer for placing a chamber within the manifold block into discrete fluid communication with each of the test gas and the carrier gas, and(b) a previously calibrated calibration ancillary sensor in sensing communication with the chamber for sensing and measuring the same ancillary parameter as the instrument ancillary sensor.

2. A calibration cartridge for calibrating a plurality of instrument ancillary sensors of a target- analyte permeation analyzer, wherein each instrument ancillary sensor measures a different ancillary parameter, and the target- analyte permeation analyzer is configured and arranged to measure permeation across a solid test sample using a test gas having a known concentration of a target-analyte and an inert target-analyte-free carrier gas, the calibration cartridge comprising:(a) a manifold block configured and arranged to interface with the target- analyte permeation analyzer for placing a chamber defined by the manifold block into discrete fluid communication with each of the test gas and the carrier gas, and(b) a plurality of previously calibrated calibration ancillary sensors in sensing communication with the chamber, each operable for sensing and measuring one of the ancillary parameters sensed and measured by one of the instrument ancillary sensors.

3. The calibration cartridge of claim 1 wherein the ancillary parameter sensed and measured by the instrument ancillary sensor is selected from the group consisting of a test gas flow sensor, a carrier gas flow sensor, a test gas relative humidity sensor, a carrier gas relative humidity sensor, a test gas temperature sensor, a carrier gas temperature sensor, a test gas pressure sensor and a carrier gas pressure sensor.

4. The calibration cartridge of claim 2 wherein the ancillary parameters sensed and measured by the plurality of instrument ancillary sensors are selected from the group consisting of a test gas flow sensor, a carrier gas flow sensor, a test gas relative humidity sensor, a carrier gas relative humidity sensor, a test gas temperature sensor, a carrier gas temperature sensor, a test gas pressure sensor and a carrier gas pressure sensor.

5. The calibration cartridge in accordance with claim 1 or 2 wherein the target- analyte permeation analyzer is operable for measuring permeation of oxygen across the solid test sample.

6. The calibration cartridge in accordance with claim 1 or 2 wherein the target- analyte permeation analyzer is operable for measuring permeation of water vapor across the solid test sample.

7. The calibration cartridge in accordance with claim 1 or 2 wherein the target-analyte permeation analyzer is operable for measuring permeation of carbon dioxide across the solid test sample.

8. The calibration cartridge in accordance with claim 1 or 2 wherein the target- analyte permeation analyzer is operable for measuring permeation across a solid test sample film.

9. The calibration cartridge of in accordance with claim 1 or 2 wherein the target- analyte permeation analyzer is operable for measuring permeation from an interior enclosed space of a solid test sample container to surrounding atmosphere.

10. A calibration cartridge for calibrating an instrument ancillary sensor of a targetanalyte permeation analyzer, wherein the instrument ancillary sensor measures an ancillary parameter, and the target- analyte permeation analyzer is configured and arranged to interface with a removable test-sample retention cartridge so as to place a solid test sample secured within the test-sample retention cartridge into fluid communication with a test gas having a known concentration of a target-analyte and an inert target-analyte-free carrier gas whereby the solid test sample maintains physical separation of the test and carrier gases from which permeation of targetanalyte through the solid test sample from the test gas into the carrier gas can be sensed and quantified by a target-analyte sensor, the calibration cartridge comprising:(a) a manifold block configured and arranged for removable interfacing with the target-analyte permeation analyzer as a surrogate test-sample retention cartridge, for placing a chamber within the manifold block into separated fluid communication with the test gas and the carrier gas, and(b) a previously calibrated calibration ancillary sensor in sensing communication with the chamber for sensing and measuring the same ancillary parameter as the instrument ancillary sensor.

11. A calibration cartridge for calibrating a plurality of instrument ancillary sensors of a target- analyte permeation analyzer, wherein each instrument ancillary sensor measures a different ancillary parameter, and the target- analyte permeation analyzer is configured and arranged to interface with a removable test-sample retention cartridge so as to place a solid test sample secured within the test-sample retention cartridge into fluid communication with a test gas having a known concentration of a targetanalyte and an inert target- analyte-free carrier gas whereby the solid test sample maintains physical separation of the test and carrier gases from which permeation of target-analyte through the solid test sample from the test gas into the carrier gas can be sensed and quantified by a target-analyte sensor, the calibration cartridge comprising:(a) a manifold block configured and arranged for removable interfacing with the target-analyte permeation analyzer as a surrogate test-sample retention cartridge, for placing a chamber within the manifold block into separated fluid communication with the test gas and carrier gas, and(b) a plurality of previously calibrated calibration ancillary sensors in sensing communication with the chamber, each operable for sensing and measuring one of the ancillary parameters sensed and measured by one of the instrument ancillary sensors.

12. The calibration cartridge of claim 10 wherein the ancillary parameter sensed and measured by the instrument ancillary sensor is selected from the group consisting of a test gas flow sensor, a carrier gas flow sensor, a test gas relative humidity sensor, a carrier gas relative humidity sensor, a test gas temperature sensor, a carrier gas temperature sensor, a test gas pressure sensor and a carrier gas pressure sensor.

13. The calibration cartridge of claim 11 wherein the ancillary parameters sensed and measured by the plurality of instrument ancillary sensors are selected from the groupconsisting of a test gas flow sensor, a carrier gas flow sensor, a test gas relative humidity sensor, a carrier gas relative humidity sensor, a test gas temperature sensor, a carrier gas temperature sensor, a test gas pressure sensor and a carrier gas pressure sensor.

14. The calibration cartridge in accordance with claim 10 or 1 1 wherein the target- analyte sensor is an oxygen sensor.

15. The calibration cartridge in accordance with claim 10 or 11 wherein the target-analyte sensor is a water vapor sensor.

16. The calibration cartridge in accordance with claim 10 or 11 wherein the target-analyte sensor is a carbon dioxide sensor.

17. The calibration cartridge in accordance with claim 10 or 11 wherein the target-analyte permeation analyzer is operable for measuring permeation across a solid test sample film.

18. The calibration cartridge in accordance with claim 10 or 11 wherein the target- analyte permeation analyzer is operable for measuring permeation from an interior enclosed space of a solid test sample container to surrounding atmosphere.

19. A method of calibrating an instrument ancillary sensor of a target- analyte permeation analyzer, wherein the instrument ancillary sensor measures an ancillary parameter, and the target- analyte permeation analyzer is configured and arranged to measure permeation across a solid test sample using a test gas having a known concentration of a target- analyte and an inert target-analyte-free carrier gas, the method including the steps of:(a) obtaining a calibration cartridge having a previously calibrated calibration ancillary sensor that measures the ancillary parameter measured by the instrument ancillary sensor,(b) interfacing the calibration cartridge and the target-analyte permeation analyzer to form an interfaced unit,(c) effecting flow of the test gas into or through the interfaced unit and into contemporaneous sensing communication with each of the instrument ancillary sensor and the calibration ancillary sensor,(d) contemporaneously sensing and measuring the ancillary parameter of the test gas flowing into or through the interfaced unit with the instrument ancillarysensor to obtain an instrument ancillary parameter value and the calibration ancillary sensor to obtain a calibration ancillary parameter value,(e) comparing the instrument ancillary parameter value and the calibration ancillary parameter value to obtain a variation value A therebetween, and(f) calibrating the instrument ancillary sensor based upon the variation value A.

20. A method of calibrating a plurality of instrument ancillary sensors of a target-analyte permeation analyzer, wherein each instrument ancillary sensor measures a different ancillary parameter, and the target- analyte permeation analyzer is configured and arranged to measure permeation across a solid test sample using a test gas having a known concentration of a target- analyte and an inert target-analyte-free carrier gas, the method including the steps of:(a) obtaining a calibration cartridge having a plurality of previously calibrated calibration ancillary sensors, each operable for sensing and measuring one of the ancillary parameters sensed and measured by one of the instrument ancillary sensors,(b) interfacing the calibration cartridge and the target-analyte permeation analyzer to form an interfaced unit,(c) effecting flow of the test gas into or through the interfaced unit and into contemporaneous sensing communication with each of the plurality of instrument ancillary sensors and each of the calibration ancillary sensors,(d) contemporaneously sensing and measuring ancillary parameters of the test gas flowing into or through the interfaced unit with each of the plurality of instrument ancillary sensors to obtain an instrument ancillary parameter value for each ancillary parameter and each of the plurality of calibration ancillary sensors to obtain a calibration ancillary parameter value for each ancillary parameter,(e) comparing the instrument ancillary parameter value and the calibration ancillary parameter value for each ancillary parameter value to obtain a variation value A therebetween, and(f) calibrating each of the instrument ancillary sensors based upon the variation value A for the ancillary parameter measured by the instrument ancillary sensor.

21. The method of claim 19 wherein the ancillary parameter sensed and measured by the instrument ancillary sensor is selected from the group consisting of a test gas flow sensor, a test gas relative humidity sensor, a test gas temperature sensor, and a test gas pressure sensor.

22. The method of claim 20 wherein the ancillary parameters sensed and measured by the plurality of instrument ancillary sensors are selected from the group consisting of a test gas flow sensor, a test gas relative humidity sensor, a test gas temperature sensor, and a test gas pressure sensor.

23. The method in accordance with claim 19 or 20 wherein the target-analyte permeation analyzer is operable for measuring permeation of oxygen across the solid test sample.

24. The method in accordance with claim 19 or 20 wherein the target-analyte permeation analyzer is operable for measuring permeation of water vapor across the solid test sample.

25. The method in accordance with claim 19 or 20 wherein the target-analyte permeation analyzer is operable for measuring permeation of carbon dioxide across the solid test sample.

26. The method in accordance with claim 19 or 20 wherein the target- analyte permeation analyzer is operable for measuring permeation across a solid test sample film.

27. The method in accordance with claim 19 or 20 wherein the target- analyte permeation analyzer is operable for measuring permeation from an interior enclosed space of a solid test sample container to surrounding atmosphere.

28. A method of calibrating an instrument ancillary sensor of a target- analyte permeation analyzer, wherein the instrument ancillary sensor measures an ancillary parameter, and the target- analyte permeation analyzer is configured and arranged to measure permeation across a solid test sample using a test gas having a known concentration of a target- analyte and an inert target-analyte-free carrier gas, the method including the steps of:(a) obtaining a calibration cartridge having a previously calibrated calibration ancillary sensor that measures the ancillary parameter measured by the instrument ancillary sensor,(b) interfacing the calibration cartridge and the target-analyte permeation analyzer to form an interfaced unit,(c) effecting flow of a designated gas selected from the carrier gas and the test gas into or through the interfaced unit and into contemporaneous sensing communication with each of the instrument ancillary sensor and the calibration ancillary sensor,(d) contemporaneously sensing and measuring the ancillary parameter of the designated gas flowing into or through the interfaced unit with the instrument ancillary sensor to obtain an instrument ancillary parameter value and the calibration ancillary sensor to obtain a calibration ancillary parameter value,(e) comparing the instrument ancillary parameter value and the calibration ancillary parameter value to obtain a variation value A therebetween, and(f) calibrating the instrument ancillary sensor based upon the variation value A.

29. A method of calibrating a plurality of instrument ancillary sensors of a target-analyte permeation analyzer, wherein each instrument ancillary sensor measures a different ancillary parameter, and the target-analyte permeation analyzer is configured and arranged to measure permeation across a solid test sample using a test gas having a known concentration of a target-analyte and an inert target-analyte-free carrier gas, the method including the steps of:(a) obtaining a calibration cartridge having a plurality of previously calibrated calibration ancillary sensors, each operable for sensing and measuring one of the ancillary parameters sensed and measured by one of the instrument ancillary sensors,(b) interfacing the calibration cartridge and the target-analyte permeation analyzer to form an interfaced unit,(c) effecting flow of a designated gas selected from the carrier gas and the test gas into or through the interfaced unit and into contemporaneous sensing communication with each of the plurality of instrument ancillary sensors and each of the calibration ancillary sensors,(d) contemporaneously sensing and measuring ancillary parameters of the designated gas flowing into or through the interfaced unit with each of the plurality of instrument ancillary sensors to obtain an instrument ancillary parameter value for each ancillary parameter and each of the plurality of calibration ancillary sensors to obtain a calibration ancillary parameter value for each ancillary parameter,(e) comparing the instrument ancillary parameter value and the calibration ancillary parameter value for each ancillary parameter value to obtain a variation value A therebetween, and(f) calibrating each of the instrument ancillary sensors based upon the variation value A for the ancillary parameter measured by the instrument ancillary sensor.

30. The method of claim 28 wherein the ancillary parameter sensed and measured by the instrument ancillary sensor is selected from the group consisting of a carrier gas flow sensor, a carrier gas relative humidity sensor, a carrier gas temperature sensor, and a carrier gas pressure sensor.

31. The method of claim 29 wherein the ancillary parameters sensed and measured by the plurality of instrument ancillary sensors are selected from the group consisting of a carrier gas flow sensor, a carrier gas relative humidity sensor, a carrier gas temperature sensor, and a carrier gas pressure sensor.

32. The method in accordance with claim 28 or 29 wherein the target-analyte permeation analyzer is operable for measuring permeation of oxygen across the solid test sample.

33. The method in accordance with claim 28 or 29 wherein the target-analyte permeation analyzer is operable for measuring permeation of water vapor across the solid test sample.

34. The method in accordance with claim 28 or 29 wherein the target-analyte permeation analyzer is operable for measuring permeation of carbon dioxide across the solid test sample.

35. The method in accordance with claim 28 or 29 wherein the target-analyte permeation analyzer is operable for measuring permeation across a solid test sample film.

36. The method in accordance with claim 28 or 29 wherein the target-analyte permeation analyzer is operable for measuring permeation from an interior enclosed space of a solid test sample container to surrounding atmosphere.

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