Transcript MOCON INSTRUMENT MAINTENANCE

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CASE STUDY – Permeation
Testing of Flavor/ Aroma
Compounds
MOCON 2007 Internet Seminar Series
August 12, 2007
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Can One Predict or Rank the
Transmission Rate of a
Permeant through an array of
Materials, based on the
Transmission Rate of a
different Permeant?
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Background Information
• A company needs to contain the odor
generated from a waste process.
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Background Information
• The company has oxygen transmission
rate equipment “in house”.
• They want to know if this equipment can
be used to screen potential barrier
materials for their odor barrier properties.
• The company requested a comparative
study between different polymer film types.
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Background Information
The Goal:
Compare odor barrier with
oxygen barrier to determine if
oxygen barrier property can be
used for odor barrier prediction.
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What Is Smelly?
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What Is Smelly?
• Chemical and Chemical Reactions are
responsible for odors.
• Which chemicals does one choose to represent
a particular odor?
• Sensory Testing – can help choose a consensus
of the odor (i.e. good vs. bad) and descriptors.
• GC testing can quantify the chemicals
comprising the odor.
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What Is Smelly?
• A MOCON lab in Texas
performed an odor
characterization study of
the “smelly” material.
• They utilized a Multidimensional Gas
Chromatograph with FID
/ PID / Olfactory / MS
Detectors
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What Is Smelly?
The Results:
Over 100 different aroma chemicals
were identified from the samples.
– d- limonene (terpene / essential oil
family) was a prominent chemical in all
of the tested samples.
– Toluene (aromatic hydrocarbon) was
also found in the aroma profile.
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Material Selection
Which Materials to Analyze?
– Should be practical for processing
– Should be economical, due to large
volumes of material needed
– Other issues?
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Material Selection
Barrier Name
Polymer Family
OPP
PVDC Copolymer
OPP with barrier
coating
Nylon-6
PET
Poly(olefins)
Poly(vinyls)
Multi-layered
Structure
Poly(amides)
Poly(esters)
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Odor Barrier Study
• Analysis Temp: 23C
• Using the saturated vapor pressure of
limonene and toluene at 23C
– Toluene: (25.59mmHg), Limonene: (1.84 mmHg)
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Odor Barrier Study
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Odor Barrier Study
Example of Organic Transmission Rate Data
0.0140
ug/(m2 day)
0.0120
0.0100
0.0080
0.0060
0.0040
0.0020
0.0000
0
10
20
30
40
50
60
70
80
Days
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Odor Barrier Results - (d- Limonene)
Material
Name
OPP
PVDC
Copolymer
OPP with
barrier coating
Nylon-6
PET
Limonene-TR
Thickness
Normalized
Ranking
(g*mil)/(m2-day)
(1 = best, 5 = worst)
5.84
5
0.038
3
1.67
4
8.2 x 10-5
1.4 x 10-4
1
2
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Odor Barrier Results - (Toluene)
Material
Name
OPP
PVDC
Copolymer
OPP with
barrier coating
Nylon-6
PET
Toluene -TR
Thickness
Ranking
Normalized
(g*mil)/(m2-day)
(1 = best, 5 = worst)
750
5
162
4*
21
3*
3.8 x 10-4
3.6 x 10-4
2
1
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Oxygen Barrier Study
• Analysis Temp:
– 23C
• Test Gas:
– 100% O2 (dry)
• Carrier Gas:
– 98%N2
– 2%H2 (dry)
• Instrument:
– MOCON Oxtran® 2/21
• Methodology:
– ASTM D-3985
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Oxygen Barrier Study
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Oxygen Barrier Study
Example of Oxygen Transmission Rate Data
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Oxygen Barrier Results
Material
Name
OPP
PVDC
Copolymer
OPP with
barrier coating
Nylon-6
PET
Oxygen Transmission
Thickness
Ranking
Normalized
(cc*mil)/(m2-day)
(1 = best, 5 = worst)
1200
5
28
2
2.0
1
42
56
3
4
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Odor Barrier / Oxygen Barrier
Comparison
So, how do they compare?
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Odor Barrier / Oxygen Barrier
Comparison
Barrier Comparison
10000
1000
1000
10
1
100
0.1
0.01
10
0.001
Oxygen Permeation
cc/(m2*day)
Organic Permeation
g*mil/(m2-day)
100
0.0001
1
0.00001
OPP
PVDC
PET
Sample Name
Nylon-6
PVDC/OPP
Toluene-TR
Limonene-TR
OTR
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Odor Barrier / Oxygen Barrier Comparison
Material Name
OPP
PVDC
Copolymer
OPP with
barrier coating
Nylon-6
PET
Transmission Rate
(Normalized)
d – Limonene
Toluene
Oxygen
(gm*mil)/(m2-day)
(gm*mil)/(m2-day)
(cc*mil)/(m2-day)
5.84
750
1200
0.038
162
28
1.67
21
2.0
8.2 x 10-5
1.4 x 10-4
3.8 x 10-4
3.6 x 10-4
42
56
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Odor Barrier / Oxygen Barrier Comparison
Material Name
Transmission Rate
(Normalized)
d – Limonene
Toluene
Oxygen
(gm*mil)/(m2-day)
(gm*mil)/(m2-day)
(cc*mil)/(m2-day)
OPP
5.84
750
1200
PVDC Copolymer
0.038
162
28
OPP with barrier
coating
1.67
21
2.0
Nylon-6
8.2 x 10-5
3.8 x 10-4
42
PET
1.4 x 10-4
3.6 x 10-4
56
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Odor Barrier / Oxygen Barrier Comparison
Material Ranking
Material Name
OPP
PVDC
Copolymer
OPP with
barrier coating
Nylon-6
PET
(1 = best, 5 = worst)
d - Limonene
Toluene
Oxygen
5
5
5
3
4
2
4
3
1
1
2
2
1
3
4
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Conclusions
Oxygen transmission rate testing of different polymer
families could not accurately predict or rank the organic
barrier properties of the same films.
Material Name
Transmission Rate
(Normalized)
d – Limonene
Toluene
Oxygen
(gm*mil)/(m2-day)
(gm*mil)/(m2-day)
(cc*mil)/(m2-day)
PVDC Copolymer
0.038
162
28
OPP with barrier
coating
1.67
21
2.0
Nylon-6
8.2 x 10-5
3.8 x 10-4
42
PET
1.4 x 10-4
3.6 x 10-4
56
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Conclusions
There is no “universal” conversion factor from
oxygen results to organic results
Organic to Oxygen Ratio
Material Name
d – Limonene TR
Oxygen TR
Toluene TR
Oxygen TR
OPP
0.0048
0.63
PVDC Copolymer
0.0014
5.79
OPP w/ coating
0.84
10.5
Nylon-6
1.95 x 10-6
9.05 x 10-6
PET
2.50 x 10-6
6.4 x 10-6
Average Ratio
0.17
3.4
Standard Deviation
0.37
4.7
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Conclusions
For the same polymer material, different
organics can yield different and
unpredictable results. This is largely due to
polymer / permeant interactions.
Material Name
d – Limonene
Toluene
(gm*mil)/(m2-day)
(gm*mil)/(m2-day)
PVDC Copolymer
0.038
162
OPP with barrier
coating
1.67
21
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Conclusions
• In most cases, the best way to determine
whether a material is a good organic
(aroma or odor) barrier, is to:
– First : Determine which organics are the key
players.
– Second: Test the material with the proper
permeant.
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Recommendation for a Future
Study
Even though oxygen transmission testing
was a poor tool for ranking the overall
organic barrier for differing materials, it
may prove meaningful to use an oxygen /
aroma correlation when comparing
barrier properties of like polymers of
different thickness, grades or added
coatings.
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Thank you
For additional questions or a copy of
today’s seminar, please send an email
to
[email protected]
or go to
www.mocon.com
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Please join us for next month’s
seminar entitled:
Measuring Solubility and
Diffusivity in Materials
Wednesday, September 12, 2007
10:00 am Central
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