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

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Dec 27, 2022 164 likes •501 views

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

SLIDE 1

By Joel Fischer, MOCON

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

SLIDE 2

Purpose of Barrier Packaging

SLIDE 3

What is Permeation?

SLIDE 4

Permeation Basics

Solution-diffusion mechanism

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

Test Gas Source Detector

Sample Wall

SLIDE 5

Equilibrium

There is no universal time to reach equilibrium.
Each material has its own nature. Usually,

the better the barrier, the longer the test duration.

100 200 300 400 500 600 50 100 150 200 250 TIME (hours) PERMEATION RATE (g-mil/m2-day-mm Hg) Normal barrier sample

Permeation – What does it look like?

SLIDE 6

Permeant / Polymer Relationship

Polymer Oxygen* PET 2.3 HDPE 73

* 23C/25C (cm3 x mil)/(100in2 x day x atm) L. Massey, Permeability Properties of Plastics and Elastomers, 2nd Edition

Nitrogen* Carbon Dioxide* 17 580

SLIDE 7

WVTR with Added “Total” Pressure

=

SLIDE 8

Eq. Time 4 days

4 days OTR 0.0012 cc/day 0.0052 cc/day

20.9% (Room Air) versus 100% O2

SLIDE 9

Effect of Temperature on Transmission Rate of Organic Compounds in LDPE

*K. Cooksey, IMPORTANT FACTORS FOR SELECTING FOOD PACKAGING MATERIALS BASED ON PERMEABILITY

SLIDE 10

Relative Humidity Effects OTR

*K. Cooksey, IMPORTANT FACTORS FOR SELECTING FOOD PACKAGING MATERIALS BASED ON PERMEABILITY

SLIDE 11

ASTM WVTR Methods - Comparison

Testing Methods E 96 E 398 F 1249 D 6701

Gravimetric Sheet and Film Material D 3079 D 7709 (‘11) Gravimetric Pouches, Pharma Blisters/ Packages RH Probe Sheet and Film Material Modulated IR Sheet and Film Material RH Probe Sheet and Film Material for very high transmitters

SLIDE 12

ASTM OTR Methods - Comparison

Methods Comparison

D-1434 Manometric Method D-3985, F-1307 And F-1927 (Coulometric sensor ) (Isostatic Method) F-2622 (Various sensor ) (Isostatic Method) F-2714 Fluorescent Decay of Headspace O2

Testing film only
Sample stressed
Absolute sensor
Testing both film

and Packages

Sensor calibration

required

Testing both film

and PKG Oxygen content of package headspace Package Permeability Studies and Leak Detection

SLIDE 13

Package WVTR – Same Apparatus as F-1249

SLIDE 14

Typical Sample Types

SLIDE 15

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

SLIDE 16

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

SLIDE 17

SLIDE 18

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

SLIDE 19

OTR Optical Film Analysis

SLIDE 20

Measuring OTR for Perforated Films

*Accumulate to 0.21% oxygen *Report Units in cc/day for perforated films

0.05 0.1 0.15 0.2 0.25 30 60 90 120 150 180 210 240 270

Time (seconds)

Oxygen %

0.00E+00 5.00E+05 1.00E+06 1.50E+06 2.00E+06 2.50E+06 3.00E+06 3.50E+06 4.00E+06

cc/day

SLIDE 21

Perforated Film OTR Data

# of Perfs OTR (cc/day)

1 42 2 115 3 138 10 241 18 375

OTR vs Perforations

100 200 300 400 1 2 3 4 5

Perforations

OTR (cc/day)

SLIDE 22

Containers with “Leaky” Seals…

SLIDE 23

Testing Loosely Sealed Packages

Loose Fitting Container Lid Window With Sensor Light Pulse OpTech™-O2 Instrument

Purge lines Accumulate to 0.21% O2 Valve

SLIDE 24

OTR Analysis for a Loosely Sealed Package

OTR Data for Loose Sealed Bottle

200 400 600 800 1,000 1,200 1,400 1 5 6 13 14 15 16 18 20 21 22

Time (minutes)

OTR cc/(package*day)

0.05 0.1 0.15 0.2 0.25

Oxygen %

SLIDE 25

Analyzing Leaky Packages (Capsules)

SLIDE 26

Testing Capsule As Film

Epoxy Capsule Over Hole Add Volume To Cell

SLIDE 27

Analyze Leaky Capsule As Film Volume Extension

SLIDE 28

Secure The Film in Cell

SLIDE 29

Data Comparison

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

SLIDE 30

Solubility

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

SLIDE 31

Oxygen Solubility within Polymers

0.48ml of O2

0.0001 0.0002 0.0003 0.0004 0.0005 0.0006 500 1000 1500 2000 2500 3000 Time (minutes) Outgassing rate (cc/min) Bottle A Bottle B Half Bottle A Empty

ASTM D-3985 coulometric sensor

SLIDE 32

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

SLIDE 33