OxySense OxyPerm 5250i User manual

OxyPerm®
Permeation
Chamber
Users Guide
© Industrial Physics Product Integrity
OxySense
An Industrial Physics Product Integrity Brand
68 Branum Road, Devens, MA 01434. USA
Phone: [phone]
Website: www.oxysense.com
Email: [email protected]
Technical Support email: [email protected]
Document Revised: July, 2020
Information in this document is subject to change without notice. Any reference to a company or
data used as examples herein is ctitious unless otherwise noted. No part of this document may
be reproduced or transmitted in any form or by any means for any purpose without express
written permission.
All other company and product names are the trademarks or registered trademarks
of their respective companies.
All Rights Reserved

Document update: July 2020
Copyright ©Industrial Physics Product Integrity
All Rights Reserved
Information in this document is subject to change without notice. All company and product names used
herein are the trademark or registered trademarks of their respective owners. Referencing a company or
data found herein, for any purpose without express written permission, is prohibited.
Alway follow all local and national safety guidelines and any additional safety guidelines specic to your
organization. Consult with your organization’s safety ocer prior to performing work.
Electronic equipment should be protected for unexpected electrical events such as power dips and surges.
Consult your organization’s electrical engineering ocer prior to installation and operating electrical
equipment.
Any description of standards, protocols, practices, or procedures are given as guidance and may not fully
align with the standards, protocols, practices, or procedures of your organization’s quality assurance pro-
gram. Consult your organization’s quality assurance ocer prior to beginning work.

Table of Contents
1.0 Introduction ................................................................................. 1
2.0 How it works ................................................................................. 2
2.1 Instrumentation........................................................................... 2
2.2 Dynamic Accumulation................................................................ 2
2.3 Film Permeation Tests.................................................................. 2
2.3.1 Test Parameters .................................................................. 3
2.4 Visulation DA .............................................................................. 3
3.0 Equipment, Material and Supplies ..................................................... 4
3.1 Equipment ................................................................................. 4
3.2 Materials ................................................................................. 4
3.3 Supplies ................................................................................. 4
4.0 Permeation Chamber Overview .......................................................... 5
5.0 Gas Cylinders and Flow Meters .......................................................... 7
6.0 OTR Determination -Test Setup......................................................... 8
6.1 Placing Film in the Chamber........................................................... 8
6.2 Purging the Sensing Well ................................................................ 10
6.3 Purging the Sensing Well (optional)................................................. 12
7.0 Data Acquisition ............................................................................ 14
7.1 Overview of the Film Permeation Module......................................... 15
7.2 Creating a Permeation Test File ...................................................... 20
7.3 Configuring Test Parameters........................................................... 22
7.4 Acquiring Data ............................................................................... 25
7.4.1 Time Intervals ..................................................................... 26
7.4.2 Frequently Asked Questions aout Time Intervals ................. 27
7.4.3 Using the Timer Feature..................................................... 28
8.0 Data Analysis ................................................................................. 30
8.1 Data Quality Indicators .................................................................. 30
8.1.1 The OTR Graph................................................................... 30
8.1.2 The Oxygen Graph .............................................................. 31
8.1.3 The R2Value....................................................................... 31
OxySense Gen III - Operations Manual

9.0 Data Interpretation ............................................................................ 32
9.1 The Conditioning Phase .................................................................. 32
9.2 Rejecting Data ................................................................................ 33
9.2.1 Gen III Software .................................................................. 33
10.0 Trouble Shooting ........................................................................... 35
11.00 Technical Support ............................................................................ 36
Appendix A: .. O2XYDot®Calibration.......................................................... A-1
Appendix B:.. Basic Principles of Film OTR by Dynamic Accumulation ... B-1
List of Figures
Figure 2-1: DA Visualization................................................................. 3
Figure 4-1: Permeation Chamber Disgram (Exterior) ............................. 5
Figure 4-2: Permeation Chamber Diagram (Interior).............................. 6
Figure 5-1: Flow Meter Attachment Diagram ........................................ 7
Figure 5-2: OxySense Flow Meter.......................................................... 7
Figure 8-1: The OTR Graph .................................................................. 30
Figure 8-2: The Oxygen Graph ............................................................. 31
Figure 8-3: The R2Value ...................................................................... 31
Figure 9-1: Conditioning and Permeation Phases.................................. 32

Permeation Chamber User’s Manual
Page 1
Copyright © Industrial Physics Product Integrity 2020
1.0 Introduction
The OxyPerm Permeation Chamber is manufactured exclusively by Industrial
Physics Product Intergrity, Devens, MA, U.S.A.and is designed for the purpose of
determining oxygen transmission rates(OTR) of flat, polymer films when used in conjunction
with an OxySense® 5000 series oxygen analyzer. The Permeation chamber is part of
OxySense’s OxyPerm line oxygen analysis accessories.
OxySense 5000 series instruments are equipped with OxySense’s Gen III software which
includes the modules required for capturing oxygen permeation data and calculating the
OTR of films reported in either milliliters (cubic centimeters) per square-meter per day
(ml/m2/day) or milliliters per 100 square-inches per day (ml/100in2/day).
The remainder of this document discusses how to perform the following tasks:
•Setup the permeation chamber for OTR determination
•Calibrate the permeation chamber’s O2xyDot® oxygen sensor
•Use the Gen III software to capture data for OTR Determination
•Generate OTR reports

Permeation Chamber User’s Manual
Page 2
2.0 How it Works
The information contained in the following subsections is provided to “demystify” OTR
analysis. Your understanding of the method and the instrumentation will greatly increase
the ease of producing a valid OTR result.
2.1 Instrumentation
Using an OxySense® instrument, one is able to obtain non-invasive (i.e. in-situ) oxygen
concentration measurements by way of fluorescence quenching analysis, where, an
optical, oxygen-selective sensor (e.g. an OxyDot®) resides within a sealed container,
affixed to a transparent surface. The instrument is capable of capturing the optical signal
from the sensor and transducing the signal in to an oxygen concentration.
The OxyPerm® Permeation Chamber is equipped with an OxyDot® that resides within the
chamber, opposite a transparent reading window. An OxySense® 5000 series instrument is
used to capture an oxygen concentration reading from the sensor without disturbing the
integrity of the chamber. The space where the OxyDot® resides is isolated from the
oxygen-containing atmosphere by the material being analyzed.
2.2 Dynamic Accumulation
OxySense employs the principle of dynamic accumulation (DA) for OTR determination,
where oxygen gas that permeates through the material gradually accumulates within a
container. OxySense® instrumentation, which is ideal for the in-situ measurement of
oxygen accumulation, is used to record the increasing oxygen concentration within that
container over time. The OTR is then calculated from the oxygen accumulation data.
2.3 Film Permeation Tests
When determining OTR by DA using the OxyPerm® permeation chamber, the portion of the
chamber where the OxyDot® resides, called the sensing well, is first purged with an inert
gas (i.e. nitrogen) rendering the volume surrounding the sensor free of oxygen. The portion
of the well opposite the sensing well is called the driving well, the volume of which is filled
by an oxygen-containing gas (e.g. pure oxygen or air).
As gas crosses from the driving well through the film and in to sensing well, the oxygen
concentration rises. Data is captured periodically over time. The recorded oxygen
concentration and time data is then used to calculate the OTR as the oxygen and time
data are both directly correlated to the permeability of the film.
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Permeation Chamber User’s Manual
Page 3
2.3.1 Test Parameters
The key parameters that must be known prior the test are 1) the oxygen concentration in
the driving well, 2) the surface area of the film exposed to the sensing well, and 3) the
volume of the sensing well.
2.4 Visualizing DA
The following diagram illustrates what is happening in the permeation chamber throughout
the test. It is provided to visualize what occurs throughout the course of the test. Please
note that this is a simplified visualization provided only as a visual aid.
Figure 2-1: DA Visualization
N2
N2
N2
N2N2
N2N2
N2N2
O2
O2O2
O2
O2O2
O2O2
O2O2
O2
N2
N2
N2
N2N2
N2
N2
N2N2
O2
O2O2
O2
O2O2
O2O2
O2O2
O2
O2
N2
N2
N2N2
N2O2
N2N2
N2
O2O2
O2
O2O2
O2O2
N2O2
O2
N2
O2O2
N2
O2N2
O2O2
N2O2
O2
O2
N2
N2
ON2
N2O2
O2N2
At Time 0 (beginning of the test) the sensing well is
filled with pure nitrogen and the driving well
contains oxygen.
As time progresses, gas exchange occurs
between the driving and sensing wells. The
amount of oxygen in the sensing well increases.
At Time 1, the oxygen concentration in the sensing
well has increased. Gas exchange continues At Time n, the oxygen concentration in the sensing
well has further increased. Time and oxygen data
are used to calculate OTR.
Copyright © Industrial Physics Product Integrity 2020Copyright © Industrial Physics Product Integrity 2020

Permeation Chamber User’s Manual
Page 4
3.0 Equipment, Materials and Supplies
The following list gives the equipment, materials and supplies needed to perform OTR
determination using the OxySense® Permeation Chamber. All items are required for a test
except for those that are optional as noted.
3.1 Equipment
•OxySense® 5000 series oxygen analyzer
•OxySense® Permeation Chamber
•Gas flow meter, 0.05 L/min (0.1 SCFH)
3.2 Materials
•Gas tubing, ¼” (6mm) O.D., nylon or similar
•Gas-tight fittings and connectors
3.3 Supplies
•Nitrogen cylinder, 99.99+% pure, < 1ppm oxygen by volume
•High vacuum grease, Dow-Corning or similar
•Non-abrasive tissue, Kimwipe® or similar
•Oxygen cylinder, 99.99+% pure (optional)
•Air cylinder, certified 21% oxygen (optional)
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Permeation Chamber User’s Manual
Page 5
4.0 Permeation Chamber Overview
The permeation chamber is assembled and tested at the OxySense manufacturing facility.
The following diagram depicts the permeation chamber and its assembled components.
Serial Number
Reading Pen
Insertion
Locking Bolts
Sensing Well
Outlet
Sensing Well
Inlet
Driving Well
Outlet
Driving Well
Inlet
Figure 4-1: Permeation Chamber Diagram (Exterior)
G
F
E
D
C
B
A
PermeationChambe
r
A0000-100001
Top
EG
C
D F
B
A
(top view)
(side view)
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Permeation Chamber User’s Manual
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Sensing Well
Driving Well
O2xyDot®
Sensing Well
Outlet
Sensing Well
Inlet
Driving Well
Outlet
Driving Well
Inlet
Figure 4-2: Permeation Chamber Diagram (Interior)
G
F
E
D
J
I
H
(interior view)
H
I
J
D
F
E
G
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Permeation Chamber User’s Manual
Page 7
5.0 Gas Cylinders and Flow Meters
The sensing well must be purged with an inert
gas (nitrogen) prior to beginning a test. In
order to do this without causing damage to
the film, you must use a flow meter (e.g.
rotameter) capable of maintaining a flow
rate of 0.05 liters per minute (L/min) (0.1
standard cubic-feet per hour (SCFH)). A flow
meter may be procured from OxySense or a
gas supply retailer. The following figure
depicts the connections between a nitrogen
cylinder (99.99+% pure), a flow meter, and a
permeation chamber.
You must use a two-stage regulator on the
gas cylinder. It is recommended that you set
the outlet pressure on the tank regulator to
70 kiloPascals (kPa) (10 pounds per square-
inch (psi)). You may set the outlet pressure
higher as long as you do not exceed the
maximum pressure allowed by the flow
meter and the flow meter is able to maintain
a constant flow of 0.05 L/min.
IMPORTANT: The flow rate of
gas through the permeation
chamber should be set to
0.05 L/min (0.1 SCFH) and
must not exceed 0.1 L/min (0.2 SCFH).
Flow rates greater than 0.1 L/min will
pressurize the sensing well or the driving
well, causing the film inside the chamber
to distort, bulge, and possibly rupture. To
ensure this does not happen, you must
acquire and use a flow meter to
regulate the flow of gas.
Gas
C
y
linder
Flow
Mete
r
Permeation
Chamber
Figure 5-1: Flow Meter Attachment Diagram
Gas Out
Gas In
Rotamete
r
Adjustment
Knob
Check
Valve
Figure 5-2: OxySense® Flow Meter
!
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Permeation Chamber User’s Manual
Page 8
6.0 OTR Determination – Test Setup
Film OTR is determined by placing a film sample in the permeation chamber, purging the
sensing well with nitrogen (99.99+% pure), having a known concentration of oxygen in the
driving well (either ambient or 100%), and collecting data over time. In this section you will
learn how to perform the following tasks:
•Place film in the chamber
•Purge the sensing well
•Purge the driving well (optional)
IMPORTANT: Ensure that the OxyDot® has been calibrated according to the
directions provided in Appendix A. You must calibrate the OxyDot® prior to
OTR Analysis.
6.1 Placing Film in the Chamber
The first step in setting up a test is placing film in the chamber. To ensure that an gas-tight
seal in maintained around the film, the chamber is equipped with a Viton o-ring which
seals the film to the top-side of the chamber. Additional, vacuum grease is applied around
the outer edge of the sensing will to adhere to the film to the top-side of the chamber and
create and aid in sealing the film.
Film Placement Steps:
Step 1: Open all four valves on the chamber. Step 2: Loosen and remove the locking bolts.
!
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Permeation Chamber User’s Manual
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Step 3: Place the chamber on your working
surface so that the interior of the chamber is
facing up.
Step 4: Obtain a tube of vacuum grease. Using your fingers or a dull, non-abrasive utensil (e.g.
a swab), create a thin ring of grease around the outer perimeter of the sensing well. The ring does
not need to be more than 1 cm wide (3/8”)
Cut a sample of the film to be tested. The film
sample should be cut in to a square
approximately 6.5 x 6.5 cm (2.5 x 2.5”) in
dimension.
NOTE: You should only handle the film by its
edges. Try not to touch the portion of the film
that will be exposed to the sensing well.
Residual oil transferred to the film from your
finger tips can alter the efficiency of the test.
NOTE: The dimensions of the film do not need to
be exact. However, the film must be of
sufficient length and width to ensure that there
are no gaps between the chamber’s o-ring
and the edges of the film.
6.5cm
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Permeation Chamber User’s Manual
Page 10
Step 5: Center and place the film sample
over the sensing well. Be sure that the film is
positioned such that there will be no gaps
between the o-ring of the bottom-side of the
chamber and the edges of the film.
Step 6: If necessary, smooth out the film using
your index finger. Begin by placing your index
finger near the outer edge of the sensing well
and gently glide your finger toward the out
edge of the film. Work your way around the
entire perimeter of the sensing well until all
visible wrinkled have bee smoothed out.
NOTE: Do not to touch the portion of the film
that is directly over the sensing well. Residual oil
transferred to the film from your finger tips can
alter the efficiency of the test.
Step 7: Close the chamber and insert the
locking bolts. Tighten the locking bolts by
turning clockwise.
IMPORTANT: Do not use a tool such
as pliers or channel locks when
tightening the locking bolts. Only
Hand-tighten the bolts. Over-
tightening the locking bolts can damage the o-
ring or the threading on the locking bolt inserts.
6.2 Purging the Sensing Well
In this section you will learn how to purge the sensing well with an inert gas. The sensing
well must be purged with an inert gas so that the initial oxygen concentration in the sensing
well is 0%. In the proceeding steps, you will use high-purity nitrogen (99.99+% pure) to purge
the sensing well.
!
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Permeation Chamber User’s Manual
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IMPORTANT: If you have not yet calibrated the O2xyDot®, proceed to Appendix
A O2xyDot® Calibration. After calibrating the O2xyDot® you may proceed to
Section 5.3 Purging the Driving Well
Sensing Well Purging Steps:
Step 1: Be sure that there is film in the chamber. If you have not placed film in the chamber,
please go to Section 6.1 Placing Film in the Chamber
Step 2: Connect the regulator of a nitrogen cylinder (99.99+% purity) to the inlet of the flow
meter using a length of ¼” gas tubing and tubing connectors with ferrules. Connect a length of
¼” gas tubing and tubing connectors with ferrules to the outlet of the flow meter.
Step 3: Open the tank valve of the certified
gas cylinder and any check valves that may
be installed on your regulator or flow meter.
The flow of gas will begin. Set the flow meter
to a rate of 0.05 L/min (0.1 SCFH). Allow the
gas to flow for 30 seconds to flush the
connected tubing.
IMPORTANT: Flow rate must not
exceed 0.1 L/min (0.2 SCFH). Flow
rates greater then 0.1 L/min can
cause damage to the film.
Step 4: Ensure that both of the valves at the
top of the chamber are fully open.
1.0
.8
.6
.4
.2
.1
0.1 SCFH
!
!
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Permeation Chamber User’s Manual
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Step 5: Connect the outlet of the flow meter to the inlet valve of the top half of the permeation
chamber using a length of ¼” gas tubing and tubing connectors with ferrules. Allow the gas to
flow through the top of the chamber for 60 seconds.
Step 6: Close the valves to the sensing well
in the following sequence: Close the inlet
valve first and then quickly close the outlet
valve.
IMPORTANT: You must close the
inlet valve and then the outlet
valve in that order. If you close the
outlet valve before the inlet valve,
the sensing well will pressurize causing the film
in the chamber to distort, bulge and possible
rupture.
Step 7: Close the tank valve on the nitrogen cylinder and any check valves between the
cylinder’s regulator and the flow meter.
Disconnect the tubing from the permeation chamber’s inlet.
Step 8: Proceed to one of the following sections:
If you plan to use ambient oxygen in the driving well, proceed to section 7.0
If you plan to purge the driving well with 100% oxygen, proceed to Section 6.3
6.3 Purging the Driving Well (optional)
In this section you will learn how to purge the driving well with concentrated oxygen
(99.99+% purity). This is recommended for high barrier films, that is, films with OTRs of 50
cc/m2/day or less (3 cc/100in2/day or less). Alternatively, the driving well may simply be left
opened to the atmosphere. Purging the driving well with concentrated oxygen will simply
accelerate the film permeation test. When leaving the chamber open to the atmosphere,
the film permeation test will take approximately five-times longer than when the driving
well is purged with concentrated oxygen.
1
2
!
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Permeation Chamber User’s Manual
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IMPORTANT: Be sure to consult your organization’s Health and Safety director
before acquiring and using concentrated oxygen in your facility. Be sure to
comply with all local or state safety regulations.
If you plan to use atmospheric oxygen (i.e. air) in the driving well, you may skip this section
and proceed to Section 7.0.
Driving Well Purging Steps:
Step 1: Be sure that there is film in the chamber and that the O2xyDot® is calibrated and that
the sensing well has been purged with an inert gas (nitrogen).
If you have not placed film in the chamber, please go to Section 5.1 Placing Film in the Chamber.
If you have not purged the sensing well, go to Section 5.3 Purging the Sensing Well.
If you have not calibrated the O2xyDot®, go to Appendix A O2xyDot® Calibration.
Step 2: Connect the regulator of a concentrated oxygen cylinder (99.99+% purity) to the inlet of
the flow meter using a length of ¼” gas tubing and tubing connectors with ferrules.
Step 3: Open the tank valve of gas cylinder
and any check valves that may be installed
on your regulator or flow meter.
The flow of gas will
begin. Set the flow rate
to 0.05 L/min (0.1 SCFH).
Allow the gas to flow for
30 seconds to flush all
connected tubing.
IMPORTANT:
Flow rate
must not
exceed 0.1
L/min (0.2 SCFH). Flow
rates greater then
0.1 L/mincan cause
damage to the film.
Step 4: Ensure that both of the valves at the
bottom of the chamber are fully open.
1.0
.8
.6
.4
.2
.1
0.1 SCFH
!
!
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Permeation Chamber User’s Manual
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Step 5: Connect the outlet of the flow meter to the inlet valve of the top half of the permeation
chamber using a length of ¼” gas tubing and tubing connectors with ferrules.
Purge the driving well for at least 4 minutes at 0.05 L/min (0.1 SCFH)
Step 6: Close the valves to the driving well
in the following sequence: Close the inlet
valve and then quickly close the outlet valve.
IMPORTANT: You must close the inlet
valve and then the outlet valve in
that order. If you close the outlet
valve before the inlet valve, the
sensing well will pressurize causing the film in
the chamber to distort, bulge and possibly
rupture.
Step 7: Close the tank valve on the oxygen cylinder and any check valves between the
cylinder’s regulator and the flow meter.
Step 8: Disconnect the tubing from the permeation chamber’s inlet.
Step 9: Proceed to Section 7.0 Data Acquisition.
6.4 Temperature
The room(s) where the permeation chamber is stored and analyzed must be maintained
within the range of 23±2°C while the test is in progress. This is necessary to ensure that
results from your tests are comparable to results obtained by others.
1
2
!
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Permeation Chamber User’s Manual
Page 15
7.0 Data Acquisition
After setting up the permeation chamber for use in the film permeation test, you may
proceed to acquire data using the OxySense® 5000 Series instrument and the Gen III
Software.
As stated in Section 2.0 How It Works, the film permeation test is carried out by monitoring
and recording the incremental increase in oxygen concentration in the sensing well over
time. The rate at which oxygen permeates in to the sensing well is calculated by the
software and is used to determine the OTR of the film in either mL/m2/day or
mL/100in2/day.
Data points are acquired by capturing readings from the permeation chamber’s O2xyDot®
which is visible through the reading window located on the top portion of the permeation
chamber, situated above the sensing well. The data is recorded in % (v/v) oxygen
concentration or partial pressure of oxygen (PO2) in millibar (mbar).
This section will guide you through the film permeation test setup in the Gen III software.
The following items are included in this section:
•Overview of film permeation software features
•Creating a test file in the Gen III Software
•Configuring test parameters
•Acquiring data
In section 8.0 Data Interpretation you will learn how to monitor the progress of a film
permeation test, how to work with data, and how to determine when a test is complete.
7.1 Overview of the Film Permeation Module
This section discusses the features of the Film Permeation module. The Film Permeation
module is the portion of the Gen III software which is used for film permeation test and is
located in the Film Permeation tab in the software. There are two screens you will see when
using the Film Permeation module:
•The Oxygen Permeation Tests screen
•The OTR screen
The following figures depict the two screens listed above. An explanation of the features in
each screen is given below each figure.
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Permeation Chamber User’s Manual
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Open Button
Browse Active Button
Browse All Button
View Log File Button
View Graph Button
Capture Button
Setup Button
Timer Button
Print Report Button
End Test Button
Chamber Serial
Number Box
Test Name Box
Open
Opens the current test for the permeation chamber with the serial number
specified in the Chamber Serial Number box. If there is no active test for the
specified chamber, the software will prompt you to create a new test. If it is
the first time that you have used a permeation chamber with your
instrument, the software will prompt you to add the permeation chamber
to the system.
Browse Active
Opens the Browse Active window which contains a list of active tests for all
permeation chambers currently in use with the instrument. You may also
perform such tasks as Change Test Description and Export to CSV in the
Browse Active window.
Browse All
Opens the Browse All window which contains a list of active and closed
tests for all permeation chambers that have been used with the instrument.
You may also perform such tasks as Change Test Description and Export to
CSV in the Browse All window.
View Log File Opens the OTR screen and displays a table of the recorded oxygen values
for the active test associated with the specified permeation chamber.
B
A
10
9
8
7
6
5
4
3
2
1
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