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.
Copyright © Industrial Physics Product Integrity 2020

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)
Copyright © Industrial Physics Product Integrity 2020

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)
Copyright © Industrial Physics Product Integrity 2020

Permeation Chamber User’s Manual
Page 6
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
Copyright © Industrial Physics Product Integrity 2020