Innovations in FTIR and UV-Vis: New molecular spectroscopy solutions for your elemental analysis lab
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Transcript of Innovations in FTIR and UV-Vis: New molecular spectroscopy solutions for your elemental analysis lab
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Innovations in FTIR and UV-Vis:
New molecular spectroscopy solutions
for your elemental analysis lab
Agilent Technology and Science Symposium, Houston, June 27th 2013
Michelle Tomba Product SpecialistMolecular Spectroscopy
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Outline
• Innovation in FTIR – true innovation!• Cary 630 FTIR – maximum flexibility with innovative
sampling • FTIR and portability – a reality!• Applications
• The new UV-Vis way – be faster and more efficient!
• Cary 60 with fiber optic probes
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FTIR Innovation Combines with Efficiency, Ease of Use and True Portability
Hand Held
Portable
Analyzers
Agilent Confidential
Routine
Research
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WHY FTIR?
70 u
m
70 um
Chemical Image
Image @ 3295 cm-1 - Nylon 3500 3000 2500 2000 1500 1000
0.2
0.1
0.0
Wavenumber
Abs
orba
nce
Image @ 1285 cm-1, poly phthalate, ~4 microns
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Why most chemists are avoiding FTIRIssues related to instrumentation
• Not stable (vibration, conditioning, humidity…)• Alignment of optics• Requirement for purge gas• Bulky• Long acquisition time (minutes)
Issues related to sample preparation• KBr pellets, NaCl plates -> long, costly, non-
reproducible, humidity• Liquid cells -> tedious, tricky handling• Difficult to run unstable samples
Issues related to software• For spectroscopists– requirement for data
manipulation
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Why most chemists used to avoid FTIRIssues related to instrumentation
• Not stable (vibration, conditioning, humidity…)• Alignment of optics• Requirement for purge gas• Bulky• Long acquisition time (minutes)
Issues related to sample preparation• KBr pellets, NaCl plates -> long, costly, non-
reproducible, humidity• Liquid cells -> tedious, tricky handling• Difficult to run unstable samples
Issues related to software• For spectroscopists– requirement for data
manipulation
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Cary 630 FTIR – Innovation on all aspectsSolving problems through innovation…
630 EngineDialPath TumblIR
Di, Ge, ZnSe ATRDiff/Spec Reflectance Transmission
Agilent Confidential
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Cary 630 FTIR – Anywhere and with ease of useSize, reliability, consistency and robustness
• Toxic API (ex: anticancer drugs)
• Air sensitive compounds• Explosive/Hazard risks
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Cary 630 with DialPath Sampling TechnologyAs easy for liquid measurement as using ATR, and with the added benefit of variable and extended pathlength
Oil/lubricants
Environmental
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DialPath Changes How Liquids are Analyzed by FTIR• Qualitative (raw material ID) and
quantitative (impurity levels determination) analysis on a SINGLE accessory – no need for disassembling of traditional liquid transmission cell to change pathlengths
• Viscous liquids analyzed without blockage and leakage issues typically associated with traditional variable transmission cells
• Handles viscous liquids and volatile solvents equally well
• As easy to use as ATR, but more sensitive with 30-1000 micron pathlengths available 250mL Fill Volume
3mL Fill Volume
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Lab Interfaces on Portable FTIRs
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Why portable instruments (ex: FTIR)?Need an answer now and/or can’t bring the sample
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Agilent Confidential
Handheld, Portable and Dedicated FTIRs
HandheldPortableDedicated
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Oils, Lubricants and Biodiesel in Diesel Fuel5500t with TumblIRsampling technology
• Biodiesel fuel contamination– Biodiesel is deleterious to stored diesel fuel used for back up generator for nuclear fuel
rods• Biodiesel blending • Turbine Oil - Mineral Oil Based
– Turbine Condition Monitoring– GST Turbine Oil Condition Monitoring
• Hydraulic Fluid - Mineral Oil Based– DTE Hydraulic Oil
• Hydraulic Fluid - Polyol ester– Quintolube
• Hydraulic Fluid - Phosphate Ester– EHC Condition Monitoring
• Gear Oil - Mineral Oil Based– Gear Oil condition monitoring
• Oil Health– Level of antioxidant in turbine oil
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Handheld FTIR ApplicationsCoatings for Anodized and Coated Aluminium
Highly polished, anodized then subsequently coated (with a variety of coatings) aluminium high reflectivity reflectors. Samples ran with the 45° Spectral Reflectance interface for a 4100 ExoScan FTIR.
Spectra on next slide
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The spectra are distinct, and also vary directly with the thickness of the coating under examination.
Silicone based coating
Acryl-cyanate based coating
2° alcohol plus alkyl based coating
Different levels of Al-oxide formation
Handheld FTIR ApplicationsCoatings for Anodized and Coated Aluminium
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Intuitive: Routine FTIR must have flexible, simple to use (intuitive) software
Software guides the user through
the selected method. Also recognizes the
correct sampling interface to guide proper sampling techniques and
cleaning.
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8453 Key Features…• Photodiode array detector for complete spectrum capture• Fast full spectrum kinetics• Multi-component analysis• Small footprint – open sample compartment
Cary 60 Key Features…• Fiber optics for improved workflow• Analysis of small volumes• Xenon flash lamp for low ongoing costs of ownership• Photometric range (4.0 Abs with cuvette)
for turbid solutions
UV-Vis Spectroscopy in the Laboratory
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Cary 60 with Fiber optic Flexibility for increased throughput
Fiber Optics
QA/QC on raw materials and finished product in manufacturing
Chemical identification or study of chemical processes
Wavelength Scans – What is it?
Kinetics – what processes are occurring?
Wavelength Scans – What is it?
Concentration – How much?
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Cary 60 - Fiber Optic Probes
Replaceable Tips Various selection of pathlengths Cleanable and reusable.MicroprobesDiameter: < 4 mm10mm (2-5mm option) pathlength
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Cary 60 UV-Vis – Nano/Microvolumes Accurate spectro measurementsSmall volume measurements -
Traycell- Save precious sample – measure 0.5 to 10 µL- Accurate and reproducible results - Excellent linear dynamic range- Flexibility – no additional dedicated system
required
mg/mL
1
Abs
Abs
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April 22, 2023Confidentiality Label
• Remote (<1.5m from instrument) diffuse reflection measurements! • Fiber optic accessory with movable detector• 1.5 mm light patch – inbuilt CCD allows visualization of position• Needs fiber optic coupler (G6865A – for Cary 60)• Understand the sample surface porosity ie small beam
Requested by the Art Restoration Community
Cary 60 – Surface measurementsNon-destructive testing
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Innovation for Advanced Surface Measurements
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Questions?