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O N T H E Q U A L I T Y L I N E
PERMEABILITY TESTING:
THE CHALLENGES AND SOLUTIONS
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Agenda of Presentation
• Permeability Theory
– Mechanism of Permeation
– Factors Affecting Permeation Rates
– Challenges of Permeability Measurement
• Water Vapour Permeation
– Traditional measurement method
– Automatic measurement method
• Oxygen Permeation
– A new automatic measurement method
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Model of Permeability Phenomenon
Phase 2Phase 1 Package Wall
F F
p2
p1
c2c1
Sorption Desorption
Diffusion (Fick’s Law)
Gas or vapour transfer through a package wall
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Variables Affecting Permeation & Diffusion
1. Compositional Variables:a) Chemical composition of polymer and penetrant
b) Morphology of the polymer
c) Concentration of the penetrant
d) Presence of copermeant
2. Environmental and Geometric Factorsa) Temperature
b) Relative humidity
c) Packaging geometry
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Typical Permeation & Time Lag Curve
LTime, t
Q (
ml
at
ST
P)
Steady
State
Unsteady State
A
B
Q: amount of penetrant permeated as a function of time t
L: time lag
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Challenges of Permeability Measurement
• Precise control of key parameters essential
– Testing temperature
– Permeant driving force
– Relative humidity
• Measurement can be time-consuming
– Conditioning time (before testing begins)
– Repeated tests (to ensure steady state)
– High barrier materials take even longer to measure
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Challenges of Perm. Measurement (2)
• ”True” Permeabilities not easily verified
– No published values for laminates, composites,
coatings
– Variations can exist within a single polymer
– Temperature relation is material-dependent
• Interpretation of Results
– Permeability, permeance, transmission rate
– Influence of ambient conditions (atm. pressure)
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Water Vapour Permeability Testing
• Some typical Applications:
– Food packaging: uniform and optimised shelf life
ensures high-quality product
– Pharmaceutical packaging: product protection (e.g.
Shelf life), maintenance of dry or aqueous conditions
– Electronics: protection of components
– Construction: weather-proofing, optimising interior
atmosphere
– Textiles & Hygiene: maximum personal comfort and
optimal product function
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Gravimetric Permeability Measurement Methods
Cup method Desorption („Wet Cup“)
High RH (climate chamber)
Cup method Absorption („Dry Cup“)
Absorbent material
Water or salt solution
Low RH (climate chamber)
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Challenges of Gravimetric Method
• Correct sealing of cup is essential
• Climatised chamber required
• Labour-intensive preparation of samples
• Time-consuming, especially for high barrier
materials (up to 4 weeks or more for 1 test)
• Reproducibility is sometimes poor
• Salt solutions messy and corrosive
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Automated WVTR Testing:
Dynamic Relative Humidity Measurement
Measuring Principle : Compare time required for incremental RH
increase in Upper Chamber (i.e. 9.5 --> 10.5 % RH)
Lower
Chamber:
saturated
atmosphere
Upper
Chamberdry
Sensor and
Electronics
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Measuring Cycle of Automatic WVTR Tester
10%
10.1%
9.9%
Upper limit
Lower limit
Underdry
Measuring
interval
Relative
humidity
Underdry cycles
Humidity compensation
cycles
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Advantages of Automatic WVTR Tester
• Humidity sensor directly in test chamber
• Measuring time: inverse relation to WVTR
• Fast results even for high barrier materials
• Measurement of both low and high WVTR
• Sample preparation and changing easy
• Self-contained instrument: no PC needed
• Very little maintenance required
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Oxygen Permeability Testing
• Some typical Applications:
– Food packaging: uniform and optimised shelf
life, prevention of product degradation (e.g.
microbial growth, oxidative rancidity)
– Pharmaceutical packaging: product protection
and shelf life (prevention of oxidation reactions)
– Electronics: protection of components
– Medical products: permeable membranes (e.g.
Gas-permeable contact lenses)
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Gas Permeability Testing: Differential Pressure Method
Key to Components:
1: Transmission Cell
2: Film Sample
3: Filter Paper
4: Cell volume-control
device
5: Pressure Sensor
6: Gas Feeder
7: Vacuum Pump
8: Gas Supply
9: Stop Valves
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Limitations of Differential Pressure Method
• Poor sensitivity at very low OTR rates
• Pressure gauges ”blind” to gas type being
measured
• Generally limited to dry gas: measurements
with humidified gases required complicated
calculation procedure
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Oxygen Permeability Measurement:
Equal Pressure Method
O2
N2
F
F
H
HS
OM
F: Flow regulation
H: Humidifier
S: Sensor
OM: Gas outlet manifold
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Zirconium Oxide Sensor
Gas sampleinput
Gas sampleoutput
Thermo
Heatingelement
Sensor EMF+ -
Insulation
Measures Oxygen Partial Pressure
Measuring principle follows Nernst Equation
Reference: Atmospheric Air (20.9% O2)
Measuring range: 0.01 ppm - 100% O2
Reproducibility: Better than 10 ppb O2
Sensor lifetime: 5 years or more
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Zirconium Oxide Sensor (2)
• Sensor signal proportional to Logarithmic O2 partial pressure
• Logarithmic signal yields high sensitivity at low O2 partial pressures
• Sensor Millivolt output → O2 concentration
Zirconium Sensor Response
0,00001
0,0001
0,001
0,01
0,1
1
10
100
0 50 100 150 200 250 300
Sensor Signal (mV)
Oxyg
en
Co
nte
nt
(%)
0 mV = 20,9% O2
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OTR Tester Measuring Principle
• Reference measurement (bypassing the chamber)
• Sample measurement (through the chamber)
• O2 conc. difference is proportional to permeability
OM
O2
N2
F
F
H
H S
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Advantages of New Automatic OTR Tester
• Broad range of OTR values (high & low)
• Precise control of test and carrier gas
relative humidity
• Long sensor lifetime (5 years or more)
• Easy to operate
• Self-contained instrument: no PC needed
• Very little maintenance required
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Summary
• Permeability Testing important to development of high-tech packaging solutions and assurance of product uniformity
• Permeation theory can be complex, and measurement is sometimes time-consuming, labour-intensive and challenging to verify results
• Automated permeability testers provide faster, easier and reliable testing:– WVTR: Dynamic Relative Humidity Measurement
– OTR: Equal Pressure Method with Zirconium Oxide Sensor
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O N T H E Q U A L I T Y L I N E
Thank you for your Attention!
For more information, please visit our
website:
www.pbi-dansensor.com
O N T H E Q U A L I T Y L I N E
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