HANDHELD FTIR – BEST ON-SITE CHEMISTRY
ANALYSIS SOLUTION
Presented by: Dr. Yanqia Wang
Outline
 Background of FTIR Spectrometry and Agilent Handheld
FTIR - TopScan 4300
 Versatile sampling interfaces (Diamond/Ge ATR, Specular
Reflection, Grazing Angle Reflection and Diffuse
Reflection) to satisfy different applications.
 Powerful and user-friendly software to assist easy data
collection and analysis qualitatively and quantitatively.
 Excellent outcome from real applications.
 Potential Applications
Infrared Light
Heat
Motion of atoms and molecules
IR radiation/absorption
Principles of IR Spectroscopy
• Most organic molecules absorb light in the infrared
region to yield IR absorption spectra
• Absorption at certain frequencies or wavenumbers
corresponds specifically to certain vibrations of
functional groups
• Absorbance of the spectral features is associated with
the concentration of the certain components
• Qualitative and Quantitative Characterization
FTIR Spectrometer
Key components of an FTIR spectrometer.
Reference
IR Source
Laser
Moving
Mirror
Laser
Detector
Fixed Mirror
Sample
Cell
IR Detector
Smaller is Better
Computer Evolution
FTIR Evolution
Mobile FTIR (Thanks to Smaller Interferometer)
1998 – Mini
2002 – Midget
Size:10 ¼” x 12” x 4 ½”
Size:4 ¼” x 2 ½” x 5 ¾”
Weight: 10 lbs.
Weight: 3.6 lbs
2007 – Micro
Size:2 ½” x 2 ¾” x 4 ¼”
Weight: 1.9 lbs
2013
Nano
Comparison Research vs Field FTIR Spectrometer
~4x scale
Source:
Laser:
Beam Splitter:
Alignment:
Detector:
8
Multiple
vs
Gas Phase
vs
Interchangeable vs
Multi-adjustments vs
Multiple
vs
Single
Solid State
Fixed
Pin in place
Single
Trading Rules
Number of Adjustments versus Alignment Tolerance
•Optimum adjustments
•Stable Performance
•“Field” system
Performance
Performance
•Maximum Adjustments
•Optimum Performance
•“Research” system
0
Alignment
0
Alignment
Agilent portable systems are designed to have stable performance. Small
changes in alignment have a minimal effect on performance.
9
Common Specifications
Multiple Instruments from the same engine
Frequency range
– 5100 – 650 cm-1 (ZnSe)
– 7000 – 350 cm-1 (KBr)
Maximum Resolution
– 2 cm-1
Non-hygroscopic optics
– ZnSe beam splitter
Power
– AC or Onboard Lithium Ion Battery
Operating temperature
– 0⁰ to 50⁰ C
Humidity
– 95% non-condensing
RELIABLE: “From White Coats to Work Boots”
Where to find a Handheld FTIR?
• Parking lots, Mine pits, Workshops, Warehouses, wild field …
Anywhere and even a regular lab
Agilent Confidential
Moving Measurements From the Lab to the Field
Analysis on Location
Too big for lab / object can not be moved
Faster Time to Answer
Lab is too far / samples need to be sent away
Deployment of Routine Analysis Program
Non technical user can used field systems
Increase QBD (quality by design) effort
Cost savings
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March 17, 2016
Requirements for Field and Routine Use
Effective Performance
• Achieve required measurement limits
• Analytical performance still matters
Form Factor – Compact, Rugged, Portable, Versatile
• System needs to go where the sample is
• Frequent travel/inexperienced users - subjects it to shock and
vibration
Correct Sampling Interfaces
• Little or no sample prep
• Versatility: Multiple uses and matrices
Ease of Use and Provide Answers
• Easy to understand, meaningful results
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Handheld Opto-Chemical Instrumentation
Smart Phone
UV-Vis
NIR
FTIR
QCL-MIR
Light-absorption Based
Raman
XRF
LIBS
Light-interaction (e.g. Scattering ,Emission) Based
Sci-Fi do-it-all
Advantages of Handheld FTIR over other Handheld
Systems
• FTIR can be used for both chemical qualification and quantitation
•
Non-destructive
•
Works for a wide variety of samples with versatile sampling
interfaces
•
Abundant spectral database and method support.
•
Less sample restriction (e.g. fluorescence interference for Raman)
•
Safety (Laser, X-Ray)
Advantages of TopScan 4300 over Other Handheld
FTIR
•
Really “Handheld”
•
Truly Rugged
– Same optics that are used in our bench systems – not a
WATERED DOWN VERSION
– Can be used in any direction
– Permanently aligned optics (No “dynamic alignment” is
necessary)
•
High Flexibility
•
Optics/Sealed Desiccated Compartments
–No need to worry about KBr beam-splitters and desiccant
–No need to purge your system
Competitive
14 lbs
8.6” x 11.8”
Evolution of Handheld FTIR 4300
18
Confidentiality Label
March 17, 2016
Award Winning Design (TopScan 4300)
Multi Functional
RFID Embedded Accessory
Ergonomic Design
2KG, balanced
Mobile and PC
Control
Robust and Graceful
Battery or AC
http://www.brettcapron.com/agilent-4300-ftir/
Agilent Confidential
4300 Handheld FTIR Overview
The most powerful handheld FTIR ever developed
OVERVIEW
• Ergonomics
– ~4.5 lbs, balanced
• Engine + electronics ~60 in3
MARKETS
•Expand existing markets
•Materials
•Energy
•Food
• Performance Optimized
WHY WE WILL BE
SUCCESSFUL
 Proven applications
 Better ergonomics
 Increased usability
 Defend current market
position
• Great scan speed (5.6
scans/second@ 4 cm-1)
• Fast software response
Agilent Confidential
Handheld Models
Features
Lightweight
Measurement Speed
Software Response
4300MCT
4300DTGS
2 kg
5.6 scans/sec
ExoScan 4100
3.2 kg
2.3 scans/sec
2.3 scans/second
Every 0.3 sec
Every 1 sec
Smart Sampling
RFID
None
Sample Interface
Docking Station
Interchangeable
Yes
Interchangeable
Yes
Battery Life
SNR
Resolution
Frequency Range
Interferometer
Detector
Battery
2+ hours
>4000:1
>3000:1
4 cm-1
5500 – 1100 cm-1 5100 – 650 cm-1
Nano
MCT
DTGS
Pair, Hot-swap
3 hours
>3500:1
4 cm-1
5000 – 650 cm-1
Micro
DTGS
Single
Agilent Confidential
TopScan 4300 Advantages
for Field Measurement
Lighter weight, Balanced, Ergonomic
– 2 kg
Compact size
– Access to difficult sample locations
High performance
– Meets the needs of challenging applications
Integrated Computer
– Fast response for real time answers
Ease of use
– Straightforward application-specific software
– Microlab
Agilent Confidential
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March 17, 2016
IR Sampling Techniques
Path length
Io
Specular
Reflectance
I1
Sample
Diffuse
Reflectance
Sample
ATR Crystal
Sample
Transmittance
•
•
•
Liquid cell
Gas cell
KBr pellet
technique
Reflectance
(External)
Reflectance
(Internal)
Other Types of
Accessories
•
•
•
•
•
Bulk
Diffuse reflectance
accessory
Specular reflectance
accessory
Grazing angle
reflectance accessory
Surface
ATR
accessory
•
Surface
Fiber optics
probe
Photo-acoustic
spectroscopy
(PAS)
Attenuated Total Reflectance (ATR)
Diamond/Ge ATR
•
•
•
•
Surface contact required
Solids or liquids
Consistent path length
Little or No sample Prep
Infrared Energy Path
Evanescent Wave
~ 2 um
Sample
Reflectance
Diffuse Reflectance
Specular Reflectance
Handheld FTIR with Multiple Sample Interfaces
Spherical ATR
• ID of Solids or liquids
• Gross surface contamination
• Thick coating identification - paints
External Reflectance (45⁰)
• Metal and composite surfaces
• Surface oxidation, coating thickness and chemistry
• ID of thin coatings
Grazing Angle (~82⁰)
•
•
•
•
Used for smooth metal surfaces
Cleaning validation
Trace contaminant identification
Bonding applications
Diffuse Reflectance
• Rough samples
• Geology applications
• Heat damage applications
4300 Handheld FTIR - Sampling Flexibility
RFID:
• Easily change I/F’s in the
field
• RFID Identifier
• Auto-sets Gain in the
Field when changed
• Allows user to lock
methods according to
sampling interface
Sampling interfaces available:
• Diffuse reflectance
• External Reflectance
• Diamond ATR
• Ge ATR
• Grazing Angle Reflectance
4300 Handheld FTIR - Instrument Stand
Upward Looking Position
Stages for External Ref, Grazing
Angle, D-ATR and Ge-ATR
sample interfaces
Downward Looking Position
Diffuse Reflectance for Powders,
soils, and other complex sample
media
How do I choose the right system for me?
Laboratory
or field
deployable
system?
Cary 630
• Interchangeable
sampling interfaces
• Auto Recognition
• No alignment
• KBr or ZnSe Optics
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Choice A:
Lab based system
Flexibility
Dedicated
analysis
or
flexibility?
Dedicated
5500 Series FTIR
• Dedicated sampling interfaces
• Optimized for performance
• No alignment
• ZnSe Optics Only
March 17, 2016
How do I choose the right system for me?
Laboratory
or field
deployable
system?
Choice B:
Combined Use
System
NDT
4300 TopScan FTIR
• Interchangeable sampling interfaces
• ZnSe Optics
• Battery Operated
• Docking Station for Laboratory
Development work
30
Sample
type:
NDT or
Liquids/
Powders
4500 Series FTIR
• Dedicated sampling interfaces
• Optimized for performance
• Battery or Mains line
• ZnSe Optics for portability
March 17, 2016
How do I choose the right system for me?
Laboratory
or field
deployable
system?
4100 Exoscan
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Choice C:
Field Use system
How often
is it in the
field?
4300 - DTGS
4300 - MCT
Microlab PC – Method Driven Software
• Visually instruct users through collection
• User Levels
Administrator, Certification, Operator
• Methods
Data collection
Library search
Quantitative
• Results
Green, yellow, red display based on limits
• PC and Mobile
Full collection/ prediction on mobile
Sync. Between mobile and PC
Microlab PC - Fast Data Collection
Microlab PC – Quant Module
• The latest Microlab PC has
embedded a Quant module,
a Simple, guided methods
development package for
quantitative applications.
• Different Quant Algorithms
allows single/multiplecomponent quantitations
– Simple Beer’s Law
– Classical Least Squares
– Inverse Least Squares
(Also known as Inverse
Beer’s Law, or Multiple
Linear Regression)
Microlab PC – Easy Report Generation
• MicrolabPC component
formatting
• Microsoft Word Add-on
enables easy report
formatting
• Multiple template
function
• PDF generation
Infield Applications for Handheld 4300
•
Materials
– Coatings
•
•
•
Coating Identification
Surface cleanliness and preparation
Coating wear and weathering
– Composites
•
•
Heat and UV Damage on Composites
Composite Cure
– Polymers
•
•
•
UV resistance and weathering
Polymer ID.
Energy
•
•
Wind
– Heat damage, coating wear and composite
cure of wind blades
Solar
– Coating performance, UV damage, Material ID
• Geology
•
•
•
•
Ground Truth-ing
Mineralogy
Soil Science
Food
•
Incoming ID, Product Quality
Agilent Confidential
Handheld Application – Heat Damage
Composites Serve as Primary
Structural Material
Oxidation of Carbon Composite
787-8
Aircraft and other structures will
increasingly be constructed from
composite material
Other
Steel 5%
10% CFRP
Carbon laminate
Carbon sandwich
Other composites
Titanium
15%
Aluminum
43%
Misc.
9%
Composites
50%
Titanium
Aluminum
20%
Composites are susceptible to heat and
oxidative damage
Heat or UV Damage
In service or mfg damage
Infrared provides an effective nondestructive testing to detect heat
damage
0.12
0.1
High damage
Absorbance
Chemical damage of the epoxy resin
Prior to delamination
0.14
0.08
0.06
0.04
0.02
No damage
0
2000
5990-7792EN_AppNote
1900
1800
1700
1600
1500
Wavenumber
1400
1300
1200
Hand Held FTIR Surface Contamination
Diffuse Reflectance and Grazing Angle
FTIR well suited to surface
contamination
Hydrocarbon and Silicone are strong
absorbers
Unique signal = positive ID of
contaminant
Different Sample Interfaces for
Aluminum and Carbon Fiber
Aluminum highly reflective
-> Grazing angle interface
Carbon fiber low reflectivity
-> Diffuse Reflectance
38
Soil Analysis by Handheld FTIR
- Soil Mid-IR signal can be correlated to key
parameters (pH/Hydrogen, Electrical
Conductivity, Extractable Al, Ca, Mg and Total
Carbon and Nitrogen)
- Massive amount samples: time consuming
and expensive
- Comparison between benchtop and mobile
FTIR (PLS-Cross Validation predictions and
comparisons)
39
Hand Held FTIR in Art Conservation
Measurement of oxalates on paint
FTIR has been used for years in art
conservation
Typically microscopy
Small samples removed from
paintings for analysis
Beigan’s Chao-Tian Temple in Taiwan
Vibrant red painted doors
Stained black
Soot? Algae growth?
Diffuse Reflection (Non-destructive)
Black covering most of door
Red spots where black wore off
Oxalates found on black areas
Oxalates formed as a by-product of biological
growth
Oxalate formation and removal is a growing
area of art conservation
40
Potential Application: Ground-Zero Chemical ID
In 2015, a series of massive explosions
rocked Tian Jin, a harbor city in China.
Hundreds tons of different hazardous
chemicals on ground zero need to be
identified ASAP. Handheld FTIR is
believed to be the best solution
NaNO3
KNO3
NH4NO3
NaCN
41
Potential Application: Melamine/Urea Formaldehyde
Dinnerware ID
Plastic shatter-proof dinnerware has become
very popular in people’s life. Melamine
Formaldehyde dinnerware is widely used due
to its strength and heat-resistance.
While someone thinks cheaper Urea
Formaldehyde can do the “same” thing.
Fine for hot soup
Melamine Formaldehyde
Nothing hot
42
Summary
• Agilent Handheld FTIR provided a valid way to bring
spectrometers to the samples, enable fast and accurate
on-site or in-field FTIR analysis.
• Wide selection of sampling interfaces can meet the
challenges of different applications.
• Easy-using software ensure customer’s need for fast
data collection and qualification/quantitation
characterization
• The value of the handheld FTIR has been approved by
many successful applications.
4300 Handheld FTIR Demonstration
https://www.youtube.com/watch?v=OVKg3s4GswU
44
Confidentiality Label
March 17, 2016