By Joel Fischer, MOCON Purpose of Barrier Packaging What is - PowerPoint PPT Presentation

ASTM Flexible Barrier Packaging Meeting Belfast, Northern Ireland Latest Techniques for Whole Package Permeation Measurements By Joel Fischer, MOCON

Purpose of Barrier Packaging

What is Permeation?

Permeation Basics Solution-diffusion mechanism Sample Wall Test Gas Detector Source • The gas absorbs at the entering face and dissolves in the material at the high- pressure side of the material • Diffuses through the polymer • Desorbs or outgases at the low-pressure side

Permeation – What does it look like? Equilibrium 600 PERMEATION RATE (g-mil/m 2 -day-mm Hg) 500 400 300 Normal barrier sample 200 100 0 0 50 100 150 200 250 TIME (hours) • There is no universal time to reach equilibrium. • Each material has its own nature. Usually, the better the barrier, the longer the test duration.

Permeant / Polymer Relationship Polymer Oxygen* PET 2.3 Nitrogen* Carbon Dioxide* HDPE 73 17 580 * 23C/25C (cm3 x mil)/(100in2 x day x atm) L. Massey, Permeability Properties of Plastics and Elastomers, 2 nd Edition

WVTR with Added “Total” Pressure = =

20.9% (Room Air) versus 100% O 2 OTR 0.0012 cc/day 0.0052 cc/day Eq. Time 4 days 4 days

Effect of Temperature on Transmission Rate of Organic Compounds in LDPE *K. Cooksey, IMPORTANT FACTORS FOR SELECTING FOOD PACKAGING MATERIALS BASED ON PERMEABILITY

Relative Humidity Effects OTR *K. Cooksey, IMPORTANT FACTORS FOR SELECTING FOOD PACKAGING MATERIALS BASED ON PERMEABILITY

ASTM WVTR Methods - Co mparison Testing Methods E 96 E 398 F 1249 D 6701 Gravimetric RH Probe Modulated IR RH Probe Sheet and Film Sheet and Film Sheet and Film Sheet and Film Material Material Material Material for very high transmitters D 3079 D 7709 (‘11) Gravimetric Pouches, Pharma Blisters/ Packages

ASTM OTR Methods - Co mparison Methods Comparison D-1434 D-3985 , F-1307 F-2622 F-2714 Manometric And F-1927 (Various sensor ) Fluorescent Decay of Method Headspace O2 (Coulometric (Isostatic Method) sensor ) - (Isostatic Method) -Testing film only -Absolute sensor -Sensor calibration Oxygen content of required package headspace -Sample stressed -Testing both film and Packages -Testing both film Package Permeability and PKG Studies and Leak Detection

Package WVTR – Same Apparatus as F-1249

Typical Sample Types

Sample # Conditions WVTR g/(p x d) Average WVTR 1 0.00009 23C / 100%RH 0.00007 2 0.00005 3 0.00007

Sample # Conditions WVTR g/(p x d) Average WVTR 1 0.0024 23C / 100%RH 0.0019 2 0.0015 3 0.0017

Optimizing Packaging Carbon Dioxide – Testing on One Bottle Bottle w/ Closure: 1.05 cc/day Bottle w/ Epoxy over closure: 0.62 cc/day Bottle w/ Epoxy over closure and finish 0.57 cc/day

OTR Optical Film Analysis

Measuring OTR for Perforated Films 0.25 4.00E+06 *Accumulate to 0.21% oxygen 3.50E+06 0.2 3.00E+06 Oxygen % *Report Units in cc/day for cc/day 2.50E+06 0.15 perforated films 2.00E+06 0.1 1.50E+06 1.00E+06 0.05 5.00E+05 0 0.00E+00 0 30 60 90 120 150 180 210 240 270 Time (seconds)

Perforated Film OTR Data # of OTR OTR vs Perforations Perfs (cc/day) OTR (cc/day) 1 42 400 300 2 115 200 100 3 138 0 10 241 1 2 3 4 5 Perforations 18 375

Containers with “Leaky” Seals…

Testing Loosely Sealed Packages OpTech ™ -O 2 Light Pulse Instrument Window With Sensor Loose Fitting Container Lid Purge lines Accumulate to 0.21% O2 Valve

OTR Analysis for a Loosely Sealed Package OTR Data for Loose Sealed Bottle 1,400 0.25 cc/(package*day) 1,200 0.2 Oxygen % 1,000 OTR 0.15 800 600 0.1 400 0.05 200 0 0 1 5 6 13 14 15 16 18 20 21 22 Time (minutes)

Analyzing Leaky Packages (Capsules)

Testing Capsule As Film Epoxy Capsule Over Hole Add Volume To Cell

Analyze Leaky Capsule As Film Volume Extension

Secure The Film in Cell

Data Comparison Sample OTR (half) OTR (full) MVTR (half) MVTR (full) cc/day cc/day g/day g/day 1 0.028 3.04 0.021 0.039 2 0.0076 5.32 0.013 0.027 23C / Room air (10%RH) 23C / 75% RH

Solubility Solubility represents the dissolution of permeant into polymer and relates the concentrations within the film to the partial pressure of the permeant.

Oxygen Solubility within Polymers 0.48ml of O 2 0.0006 Outgassing rate (cc/min) 0.0005 0.0004 Bottle A Bottle B 0.0003 Half Bottle A 0.0002 Empty 0.0001 0 0 500 1000 1500 2000 2500 3000 Time (minutes) ASTM D-3985 coulometric sensor

Evaluate changed from glass to polymer components and between rubber plungers Possible new test method?

ASTM Flexible Barrier Packaging Meeting Belfast, Northern Ireland Thank You!