Real World Challenges in Challenges in Plastic Analysis Analysis
Real World Challenges in Challenges in Plastic Analysis Analysis
Real World Challenges in Challenges in Plastic Analysis Analysis
Challenges in
Plastic
Analysis
Presented By:
D J
Dr. Jack
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AccuStandard
St d d
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Why Is There a Need for a
Industrial Additive Standards?
Good Science
• Analytical work relies on a comparison
that is made with well-characterized
well characterized
standards
• Whether a laboratory prepares their
standards in-house, or buys them from
y the
an outside source, there is always
need to know that they are prepared and
identified correctly
AccuStandard
125 Market Street • New Haven, CT 06513
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Why Is There a Need for a Industrial
Additi Standards?
Additive St d d ? (cont.)
( t)
• Regulatory requirements
– ASTM – Method D6042-96
Determination of Phenolic Antioxidants & Erucamide Slip
Additives in Polyproylene Homopolymer Formulations
Using Liquid Chromatography
– ASTM – Proposed Method D7065-06
P-tert-Octylphenol, Nonylphenol Monoethoxylate &
Nonophenol Diethoxylate and Tech Nonylphenol, Mono-
and Di
Di-ethoxylate
ethoxylate
– FDA
– EU Directives
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Categories of Polymer Additives
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Chemical Additive Standards are
different…
• Typically we think of a Chemical
Reference Standard as a single pure
analyte
• Typically a Reference Standard has a
traceability link to a NIST SRM or other
Primary Standard
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Chemical Additive Standards are
different… (cont.)
• Chemical Additives are often technical
mixes of several different chemicals
• Purity may be less than 90%
• Characterization in a real world sample
can be
b challenging
h ll i
• Traceability can be dubious
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Extraction Methods
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Polymer Sample in GC Inlet
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Polymer Sample in GC Inlet with
Aluminum Foil Plug
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Analysis
• LC/MS
– Higher molecular weight capability
– No thermal degradation
– Poor resolution
• GC/MS
– Better resolution
– Possible thermal degradation
– Lower molecular weight capability
AccuStandard
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You can ID a compound by the
Representative Fragments
Ethanox 310
– Penterythritol tetrakis (3-(3,5-di-t-butyl-4-
hydroxyphenyl)propionate
OH
MW = 1177.65
C73H108O12
O
O C
4
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Ethanox 310 GC and Mass
Spectrum of the Major Fragment
2e+07 3500000
1.8e+07
3000000
1.6e+07
2500000
1.4e+07
1.2e+07
2000000
1e+07
1500000 292
8000000 147
57
4000000
203
500000 161
91 128
2000000 115 185
77
103 173 235 249 261
45
0
Time-->5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00 45.00 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280
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Insulators containing PBDEs
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Abundance TIC: PBB.D
1600000
1400000
1200000
1000000
800000
600000
400000
200000
Time--> 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 24.00 26.00 28.00
Abundance Scan 3049 (26.553 min): PBB.D
110000 406
100000
90000 564
74
80000
70000
60000
50000
40000
30000 137
223 297
20000
10000 325
110 170 251 484
45 377 455 522 609 655
0
m/z--> 50 100 150 200 250 300 350 400 450 500 550 600 650
Pharmaceutical Delivery Systems
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Gelled Product
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Conclusion
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Questions
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Phone No: (203) 786-5290 • Fax No: (203) 786-5287
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