An Integrated Analytical Approach to Solving Complex ... Event/201… · 21 An Integrated...
Transcript of An Integrated Analytical Approach to Solving Complex ... Event/201… · 21 An Integrated...
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An Integrated
Analytical Approach
to Solving Complex
Polymer Problems
Scott D. Hanton and Chanell Brown
Intertek Allentown
October 2015
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Acknowledgments
Intertek colleagues
• Sherri Bassner
• Todd McEvoy
• Devon Shankweiler - GPC
• Scott Voth – DSC + TGA
• Ann Kotz - NMR
• Sharon Gardner – FTIR & TGA/IR
• Ellen Link – Failure Analysis
• Menas Vratsanos – DMA
• Jackie Sturgeon – SEM/EDS
• Ed Sydlik – ICP
• Cindy Mengel-Smith – XRF
• Steve Deppen – GC/MS
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Outline
• Intertek introduction
• Polymer analysis
• High performance SEC
• Integrated analytical approach
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Extensive Global NetworkE
More than
1,000 laboratories and offices
•FTSE 100 company in the
Support Services sector
•Revenues of $3.5 billion in 2014.
More than
120 countries
Approximately
38,000 people
Introduction to Intertek
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Intertek Allentown
Your Problem-Solving Partner
Problem-Solving Teams
Inorganic Analysis
Microscopy, metallurgy, surface science, diffraction,
failure analysis, , particle size
Residue ID, ceramics, polymer
structure, electronic and nano-materials
Titrations, trace metals
System stability, impurity analysis, gases/chemicals
Material Properties
Rheology, thermal analysis/hazards,
sorption
Polymer systems, catalysis, reaction
studies, gas separation
Organic Analysis
Chromatography, MS, NMR,
spectroscopy
Chemical structure identification, degradation
analysis, impurity analysis
Mechanical/
environ.
Testing
(Pittsfield)
Extractables
and
Leachables
(Whitehouse)
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Introduction
• Polymer chemistry continues to be vital
• New products
• New uses
• New research
• Significant challenges presented in polymer analysis
• Multiple monomers
• Solubility
• Complex structures
• Complex formulations
• Require multiple and powerful tools to analyze polymers
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Polymer Detective
• What is it?
• What are its properties?
• How does it behave?
• What else is in it?
• Where is it?
• How big is it?
• How much of it is there?
• What is its chemical structure?
• How is it connected?
• What’s on the end?
What?
Where?
How?
Who?
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Polymer Analysis Decision Tree
Identity
FTIR
Raman
CHNOS
SEC
Material Properties
Density
Rheology
DSC
TMA
Sorption
Morphology
SEM
AFM
Components
TGA
XRF
GC
LC
Chemical Structure
NMR
MS
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GPC Offerings
• Traditional GPC
• Organic solvents: THF, DMF, NMP, CHCl3, …
• Aqueous
• Amine separation methods
• High temperature GPC
• Solvent = TCB
• Triple detection
• GPC fraction collection
• High performance SEC
• Waters APC
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GPC Fraction Collection
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GPC Fraction Collection of Polyolefin
Blank
Sample 1 injection 1
Sample 1 injection 2
Sample 1 injection 3
• GPC fractions for FTIR analysis for end group analysis
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GPC Fraction Collection of Polyolefin
• FTIR clearly identifies Anhydride end group
EsAc
EsAnhFraction #1
EsAcEs
AnhFraction #2
Anh
Fraction #3
Anh
Fraction #4
Anh
Fraction #5
AnhFraction #6
Anh
Fraction #7
Anh
Fraction #8
-0.04
-0.03
-0.02
-0.01
0.00
0.01
0.02
0.03
Ab
sor
ba
nc
e
1000 1500 2000 2500 3000 3500 4000
W avenumbers (cm-1)
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GPC Fraction Collection of Polyolefin
• Anhydride end group concentration inverse to MW
Bulk
Sample
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Benefit of Higher Performance SEC
• Fast new solvent equilibration time (2 – 4 hours)
• Many different solvents
• Columns operate under high back pressure
• Improved resolution
• Sub 3µm hybrid particle column technology
• Low dispersion
• Fast analysis time (10 – 15 minutes)
• Waters’ Advanced Polymer Chromatography
(APC)
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APC Analysis: Polyurethane Prepolymer
Total Run Time 15
min @ 0.6ml/min flow
rate
Mn 2000
Mw 7000
RSD ≤1%
• Clearly characterize MWD
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APC Analysis of Polyurethane Prepolymer
• Obtain MWD and slice table for PMN
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APC Analysis of Polyesters
Sample 1 Mn 1,200 Mw 5,900 PD 4.9
Sample 2 Mn 1,300 Mw 6,900 PD 5.3
• Show differences between competitive products
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APC Analysis of Polyisobutylene
• Show MWD variation across a family of products
Mn range from
5k – 34k D Mw range from
16k – 135k D
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APC Analysis of Lubricants
• Distinguish a series of different lubricating oils
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Integrated Analytical
1. Polypropylene plastic bowls
2. Styrene-butadiene copolymer
3. Polycarbonate failure analysis
4. Plasticized PVC
5. Black specks in polycarbonate
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An Integrated Analytical Approach
• Use multiple analytical techniques to solve the technical questions
• GPC to determine molecular weight distribution
• TGA to determine concentration of filler
• TGA-IR to determine volatiles released during heating
• DSC to determine melting behavior and crystallinity
• FTIR, NMR, and GC/MS to determine chemical composition
• Microscopy to examine fractography
• SEM-EDS, ICP-OES, and XRF to determine elemental composition
• DMA to determine rheological properties
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1. Characterization of Polypropylene Plastic Bowls
• HT-GPC shows competitor has higher MWD
Mw = 364kD
Mw = 224kD
Log MW
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Sample 1
Sample 2
1. Characterization of Polypropylene Plastic Bowls
• TGA shows competitor has higher inorganic filler (1.7% vs 1.1%)
500 C 800 C
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DSC Plot – Second Heating
1. Characterization of Polypropylene Plastic Bowls
• DSC shows competitor has additional melts
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2. Characterization of Styrene-Butadiene Copolymer
• GPC shows heat aging leads to higher MWD of polymer
Copolymer
region
Low mass
additives
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2. Characterization of Styrene-Butadiene Copolymer
• FTIR shows little chemical difference from heat aging
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2. Characterization of Styrene-Butadiene Copolymer
• 1H and 13C NMR shows differences additive concentrations
13C NMR spectra of carbonyl region
P P P P P E
E
E
E E
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3. Polycarbonate Failure Analysis
• Cracking away from bolt holes
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3. Polycarbonate Failure Analysis
• FTIR confirmed PC and found no significant chemical changes
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3. Polycarbonate Failure Analysis
• GPC, TGA-IR, and DSC found no significant differences
Identical
MWD
by GPC
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3. Polycarbonate Failure Analysis
White debris and cracking Mud cracking was noted on the
exposed surface of the hole.
The fracture exhibited limited
microductiliy
• Optical and SEM cracking from chemical attack
SEM
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3. Polycarbonate Failure Analysis
• SEM-EDS show variety of elements in white deposits
Ice melt may
be responsible
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4. Compare Two Different Polymer Materials
• FTIR and NMR show the polymers to be plasticized PVC
FTIR spectra
are essentially
the same for
both materials
FTIR spectra shows the plasticizer to be phthalate esters
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4. Compare Two Different Polymer Materials
• FTIR and NMR show the polymers to be plasticized PVC
NMR spectra
are essentially
the same for
both materials
NMR spectra shows the plasticizer to be 45% of the materials
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4. Compare Two Different Polymer Materials
• GC/MS – didecyl phthalate and other small differences
BHT
1-dodecanol
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4. Compare Two Different Polymer Materials
• GPC shows differences between the polymers
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4. Compare Two Different Polymer Materials
• XRF shows small differences between the polymers
Element (wt. %) Sample 2 Sample 1
Si 0.062 0.10
Zn 0.011 0.005
Ca 0.007 0.021
P 0.006 0.012
S 0.006 0.005
Fe 0.004 0.012
Al 0.003 0.040
Ti <0.002 0.005
K <0.002 0.004
Organics
(balance) 99.90 99.80
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4. Compare Two Different Polymer Materials
• ICP-OES
• Sample 1 – 60 ppm Tin
• Sample 2 – 99 ppm Tin
• Use Tin concentration to calculate the concentration
of stabilizer
• Sample 1 – 0.028% stabilizer
• Sample 2 – 0.046% stabilizer
• ICP quantifies stabilizer differences between the polymers
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4. Compare Two Different Polymer Materials
Sample 2B
Sample 2A
Sample 1
DMA Frequency Sweep Data at 25oC
E’
Tan (δ)
• DMA shows modulus differences between the polymers
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5. “Good vs “Bad” Polycarbonate
• GPC shows low mass species in “Bad” sample
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5. “Good vs “Bad” Polycarbonate
• FTIR shows no difference between samples
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5. “Good vs “Bad” Polycarbonate
• FTIR shows phenolic resin in black specks in “Bad” sample
Subtraction Result:*106420.04 / D2601216, bad CH# 311257 / dark material from inclusion a, sec'n a / Continuum microscope miuns clear
0.0
0.2
0.4
0.6
0.8
Ab
s
Subtraction Result:*106420.04 / D2601216, bad CH# 311257 / dark material from inclusion a, sec'n b / Continuum microscope miuns clear
0.0
0.2
0.4
Ab
s
Subtraction Result:*106420.04 / D2601216, bad CH# 311257 / dark material from inclusion b, sec'n a / Continuum microscope minus clear
0.00
0.05
0.10
0.15
Ab
s
Subtraction Result:*106420.04 / D2601216, bad CH# 311257 / dark material from inclusion b, sec'n b / Continuum microscope minus clear
0.00
0.10
0.20
0.30
Ab
s
1000 1500 2000 2500 3000 3500 4000
Wavenumbers (cm-1)
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Summary
• SEC/APC
• Solving wide range of polymer science problems
• Benefit from high performance APC
• Developed GPC fraction collection methods
• Integrated analytical
• Combine many different analytical methods
• Solve complex problems
• Unknown materials
• Failure analysis
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Questions?
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Valued Quality. Delivered.