Breaking it Down: Polymer Deformulation

Breaking it Down
Polymer Deformulation Studies using
FT-IR Coupled to TGA
Polymers Supply Chain
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Molecular Spectroscopy in the Polymer Manufacturing Process
Process NIR
• Material Characterization
 Control & Monitoring
• Material Verification
 Incoming, In-process & Finished
• Deformulation
 Root Cause Analysis & Reverse Engineering
NIR
Production
Shipping
Receiving
QC
R&D
Routine FT-IR
Advanced FT-IR
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FT-IR Microscopy
Raman Microscopy
Overview
• Deformulation
• What is it?
• Why do it?
• Common materials
• FT-IR as a deformulation tool
• TGA coupled with FT-IR
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Deformulation
• Failure Analysis
• Known material gone wrong
• Reverse Engineering
• Unknown material composition
• Polymers
• Plastics
• Fillers, formulation
• Biopolymers
• Rubber
• Carbon Black: O-Rings, Tires
• Epoxies, Resins, Adhesives
• Entrained solvents, breakdown products
• Fabrics, Paper products
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The Nicolet iS50 FT-IR
iS50 ABX Three
Beamsplitter Exchanger
Built-in iS50 ATR
Sample Compartment
TGA Module
Triple Detectors
Touch Point
Operation
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TGA-IR: The Basics
Temperature Ramp
Weight Loss Curve
Derivative Weight Loss Curve
IR
Balance
Pan
Vapor
Heated Transfer
Line
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Infrared Series File
Desired Information
• Quantitative: How much material is coming off?
• T “G” A – Gravimetric Analysis = quant
• Qualitative: What came off?
• FT-IR – Vibrational information = qual
• Process: Similar yet different, why?
• Profiles of materials versus time (temperature)
• It takes all three to get formulation
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TGA-FTIR: Experiment
1.0
1.0
Infrared Spectrometer
0.90
0.9
0.85
0.9
0.80
0.8
0.75
0.8
0.7
0.50
0.5
0.45
0.6
Absorbance
Absorbance
Absorbance
0.70
0.7
0.65
0.60
0.6
0.55
Infrared Spectrum
0.5
0.4
0.40
0.4
0.35
0.3
0.30
0.3
0.25
0.2
0.20
0.2
IR Beam
IR Beam
0.15
0.1
0.1
0.10
0.05
0.0
IR Window
H2O
CH
H2O 4
4000
4000
3500
3500
3500
3000
3000
3000
2500
2000
Wavenumbers (cm-1)
2500
2500
20002000
Wavenumbers
(cm-1)
Wavenumbers
(cm-1)
1500
1500 1500
1000
1000 1000
500
500
CH4
CH
H2O4
H2O
Mirror
Heated Transfer Line
Exhaust
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Furnace
CH4
CH4
CH4
Transfer
Gas In
Sample
Simple Situation – Calcium Oxalate
• Three weight-loss peaks
• H2O ; CO + CO2 ; CO2
• H2O
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Classic Root Cause Analysis
Gaskets analysis
Good
Good
Bad
Subtraction
Bad
Search result
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TGA Current State
Series Window
Right Click -Copy
Search
Slow and Time-Consuming
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Complete Analysis: Mercury TGA
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Mercury TGA
Fast Answers with Search Results, Component
Profile Information and Match information all in one
window!
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How Many Components?
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Full Deformulation: 7 Components
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Structural Foam
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TGA-IR Analysis of Museum Materials
• Museum needs to display artifacts
• Must balance preservation with aesthetics
• What if display material slowly outgases?
• Low level concentrations
• Encased material – concentrates gases
• Long term exposure possible
Mummy Case of Paankhenamun
Cartonnage (gum, linen, and papyrus) with
gold leaf, Third Intermediate Period, Dynasty
22, c. 945-715 B.C.; h. 170.2 cm;
William M. Willner Fund, 1910.238.
Art Institute of Chicago
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TGA-IR Data of Display Materials: Velvet
Ammonia and acetic acid detected
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Mercury TGA Also Works for Kinetics!
• Reaction of urethane
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Conclusions - Deformulation using FT-IR & TGA
• TGA coupled to FT-IR advances capabilities to break materials down
• Mercury TGA software simplifies the analysis of complex mixtures
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Please Contact Us for More Information
View our website:
www.thermoscientific.com/polymers
or
Please feel free to email me:
[email protected]
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