Basic Theory and Instrument Design of FT-IR 1 The world leader in serving science Thermal Analysis and Rheology Short Course Concord, NH April 10, 2018 Hyphenated Spectroscopy Techniques 2 Analytical Instruments Overview Industry-leading technologies to solve a broad range of complex challenges Chromatography & Mass Spectrometry Chemical Analysis Instruments Materials & Structural Analysis • Life sciences mass spectrometry • Liquid, ion, gas chromatography • Inorganic/trace elemental analysis • Laboratory informatics • Electron microscopy • Molecular and elemental spectroscopy • 2D/3D imaging software • Portable analytical instruments • Air-quality monitoring • Radiation safety and security • Process instruments Corp. Fin. to update to LTM Revenue ending in Q1 2017
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Basic Theory and Instrument Design of FT-IR
1
The world leader in serving science
Thermal Analysis and Rheology Short CourseConcord, NHApril 10, 2018
Hyphenated Spectroscopy Techniques
2
Analytical Instruments Overview
Industry-leading technologies to solve a broad range of complex challenges
Chromatography & Mass Spectrometry
Chemical AnalysisInstruments
Materials & Structural Analysis
• Life sciences mass spectrometry
• Liquid, ion, gas chromatography
• Inorganic/trace elemental analysis
• Laboratory informatics
• Electron microscopy
• Molecular and elemental spectroscopy
• 2D/3D imaging software
• Portable analytical instruments
• Air-quality monitoring
• Radiation safety and security
• Process instruments
Corp. Fin. to update to LTM
Revenue ending in Q1 2017
Basic Theory and Instrument Design of FT-IR
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3
The widest range of analytical methods to drive deeper materials insights
EDS
Elemental imaging at high spatial resolution
Raman
Chemical compound
identification
Identification of both
organic and inorganicmaterials
FTIR
Chemical compound
identification
Identification of organic
materials in bulk state
XRF
Bulk state elemental
composition
XRD
Structural crystallinity
and composition
XPS
Surface analysis
quantitative chemical
state
We deliver a full spectrum of analytical tools that enable customers to advance their research, product development, and quality control capabilities
UV-Vis
Quantitative measurement of reflection
or transmission properties of
a material
Electron Microscopy
Multiscaleimaging & analysis of
various materials
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Wavenumbers(cm-1)
Wavelength (µµµµm)
The Electromagnetic Spectrum
107 106 105 104 103 102
x-rays
ultraviolet
visible
near-IR
mid - IR
far-IR
XRF UV-Vis Infrared
10-3 0.01 0.1 1 10 100
radio
Technique
Range
Basic Theory and Instrument Design of FT-IR
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• Work fast…
• Little or no sample prep, rapid screening
• …on a range of samples…
• Organics, inorganics, films, coatings, paper, fibers, more
• …and answer fundamental questions
• What is this stuff? How much is in there? In what form?
• Analyze samples from ‘cradle to grave’
• R & D, process control, QA/QC, failure analysis, waste
The Power of Molecular Spectroscopy
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Core Molecular Spectroscopy Techniques
FTIR• Chemical fingerprint • Fast analysis
picoSpin NMR• Benchtop NMR• No cryogens
Raman Spectroscopy• Chemical fingerprint • Fast analysis• Greater sampling options –microscopy options
Basic Theory and Instrument Design of FT-IR
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• Energy varies along the x-axis
• Wavelength in nanometers or microns, Wavenumber (cm-1)
• Response is along the y-axis
• Absorbance, transmittance, reflectance
• Different molecules absorb light differently (“Peaks”)
• This is what enables spectroscopy to tell us something!
General ‘Rules’ for Molecular Spectroscopy
Energy
Re
sp
on
se
“Peaks”
The world leader in serving science
Polymer Deformulation Studies using FT-IR Coupled to TGA
Breaking it Down
Basic Theory and Instrument Design of FT-IR
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Overview
• Deformulation
• What is it?
• Why do it?
• Common materials
• FT-IR as a deformulation tool
• Classical technique
• TGA coupled with FT-IR
• Physical property correlation with chemical data
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Deformulation
• Reverse Engineering
• Unknown material composition
• Failure Analysis
• Known material gone wrong
• Polymers
• Plastics
• Fillers
• Formulation
• Rubber
• Carbon Black: O-Rings, Tires
• Epoxies, Resins, Adhesives
• Entrained solvents, Breakdown products
• Fabrics, Paper products
Basic Theory and Instrument Design of FT-IR
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TGA-IR: The Basics
Vapor
IRBalance
Pan
Heated TransferLine
Temperature Ramp
Weight Loss Curve
Derivative Weight Loss Curve
Infrared Series File
Quantitative: How much is coming off?T “G” A – Gravimetric Analysis
Qualitative: What is coming off?FT-IR – Chemical information
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TG
A F
urn
ac
e
TransferGas In
Sample
Heated Transfer Line
IR BeamIR Beam
FT-IR Spectrometer
Exhaust
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
Absorb
ance
500 1000 1500 2000 2500 3000 3500 4000
Wavenumbers (cm-1)
Infrared Spectrum
H2O
H2OH2O
H2O 0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
Ab
so
rba
nce
1000 1500 2000 2500 3000 3500
Wavenumbers (cm-1)
CH4CH4
CH4
CH4 0.05
0.10
0.15
0.20
0.25
0.30
0.35
0.40
0.45
0.50
0.55
0.60
0.65
0.70
0.75
0.80
0.85
0.90
Ab
so
rba
nce
500 1000 1500 2000 2500 3000 3500 4000
Wavenumbers (cm-1)
CH4
CH4
TGA-FTIR: Experiment
TGA Gas Cell
TGA Gas Cell
Basic Theory and Instrument Design of FT-IR
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Experimental Set-up
Low Volume
IR Gas CellTGA Conditions
• Sample size: 10 – 15mg
• TGA program: N2 Purge Isothermal
• Temperature : Ambient up to 650 C
FT-IR Conditions• Transfer line temp: 300 C
• TGA-IR Module temp: 300 C
• Data Collection: 8 cm-1, 5 scans/spectrum
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Simple Situation – Calcium Oxalate
• Three weight-loss peaks
• H2O ; CO + CO2 ; CO2
• H2O
Basic Theory and Instrument Design of FT-IR
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• Polymers
• Textiles
• Coatings
• Residual solvent
• Product stability
• Additive analysis
Example Applications
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Good
Bad
Subtraction
Good
Bad
Search result
Gasket analysis
Classic Root Cause AnalysisClassic Root Cause Analysis
Basic Theory and Instrument Design of FT-IR
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• These nanoparticles are stabilized by ligands
• Heating breaks down the complexes, releasing ligand
Deformulating Nanoparticles
TOPO
ODPA
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• A critical electronic component, in a sealed chamber, was degrading
• Concern was for outgassing of other materials in the chamber
• The insulation of a wire was found to be the cause
GS shows total IR response as function of time-Peaks in GS correlate to sample weight loss and significant off-gassing detectedFor NYCO, 1 major thermal event was observed at ~26min- Next slide will show IR spectra in that time region
Basic Theory and Instrument Design of FT-IR
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NYCO Evolved Gas Spectra
Linked spectrum at 26.122 min.Linked spectrum at 25.782 min.
Linked spectrum at 26.377 min.Linked spectrum at 26.632 min.