real-time in situ ftir reaction analysis evolution of ... · internal usage only 1989 - reactir...
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Real-time In Situ FTIR Reaction Analysis Evolution of TechnologyCurrent State-of-the-Art
July 23, 2009CPAC Summer InstituteSeattle, WA
Internal usage only
Evolution of Reaction Analysis Technologies
Optical modules- Interferometer- Detector- Sampling technology interface
Software- Real-time data collection and analysis- Chemometric algorithms to facilitate conversion of data to information
Sampling Technology- Probes- Gas cells- Liquid flow cells
Internal usage only
1989 - ReactIR 2000 1993 - ReactIR 1000 2000 - ReactIR 4000
Weight 250 lbs
in lab
Weight 90 lbs
on bench top
Weight 40 lbs
in fume hood
Reaction Analysis System Evolution
Internal usage only
ReactIR™ 45mChemical Engineering
MonARC™Classified Area
ReactIR™ Product Family 2009
ReactIR™ iC10Organic chemistry
Internal usage only
Reaction Analysis Core Technologies
■ Optical module– Interferometer– Detector– Sampling technology interface
■ Software– Real-time data collection and analysis– Chemometric algorithms to facilitate conversion of data to information
■ Sampling Technology– Probes– Gas cells– Liquid flow cells
Internal usage only
Evolution of Software
1995 - ReactIR 2.0 2000 - ReactIR 3.0
Internal usage only
Revolution of Software – iC IR
2005 - iC IR 1.0
2006 - iC IR 2.0
2007 - iC IR 3.0
2008 - iC IR 4.0
Internal usage only
iC IR – Linked Views
Internal usage only
Reaction Analysis Core Technologies
Optical module- Interferometer- Detector- Sampling technology interface
Software- Real-time data collection and analysis- Chemometric algorithms to facilitate conversion of data to information
Sampling Technology- Probes- Gas cells- Liquid flow cells
Internal usage only
1982 - Circle Cell
1985 - Circle reactor
1986 - HATR 1988 - HATR Reactor
1994 - Comp Probes1996 - Comp Pressure Vessel
Evolution of FTIR Sampling Technology
2000 - TIARA Vessel
2002 – Chalcogenide Optical Fiber Conduit and 6mm diameter probe
Internal usage only
Heated Gas Cell
External TemperatureController
K1 MirrorTo ReactIR
Heated Gas Cell
Gas Inlet/Outlet
Internal usage only
Comp™ Probe Technology Range
6.3mm (1/4”) and 9.5mm (3/8”) diameter AgX FiberConduit probes- -80°C to 180°C- Vacuum to 69bar (1,000 psi)
Standard 16mm (5/8”) & 25.4mm (1”) Sentinel™ probes- -80°C to 200°C- Vacuum to 6.9 bar (100 psi)
High-pressure 16mm & Sentinel™ \ probes- Up to 100 bar (1500 psi)
Post-design Sentinel™- Up to 300°C- Up to 345bar (5000 psi)
ATR in diamond or silicon
16mm probes Sentinel™
Silver Halide (AgX) FiberConduit™
Internal usage only
Dip Tubes
Custom specifications- Flange- Dip tube length8AgX fiber dependent
- Materials of construction
Internal usage only
Production – Dip Tubes
Dip tube in production vessel
AgX FiberConduitto Dip tube
Internal usage only
Flow Cells in Production - Streamline™
■ Streamline™ flow cell– Standard product– Custom as required– Heating option– Air cooled– Ultrasonic option
Internal usage only
Flow Cells in Production
■ Custom Flow cell- Flange- Flowpath diameter- Material of contruction
■ Uses standard Sentinel™ probe
■ Ultrasonic optional
Internal usage only
DS Series AgX Design Introduced 2009
Input/ Output Fibers
RTD connector
Modular design:•Independent construction•Easily repairable
Color Coding:•Top (seal type)
•Gold = gold•White = Teflon
•Bottom (sensor seal)•Blue = diamond•Silver = silicon
Internal usage only
MultiplexIR for the ReactIR™ 45m
Expanded applications- Simultaneous measurement of
headspace and liquid phase- More reaction information from a single
instrument
Improved efficiency- Multiplex experiments – complete 2
experiments at the same time- Improve reaction understanding -
integrated ReactIR™ and ALR, complemented by iC IR™/ iControl™
Internal usage only
Evolution of the flowcell
Adapted from AgX FiberConduit™ technologyIntegrated DiComp™ or SiComp™ ATR technology
- Covers broad range of chemistry applications
Conforms to standard HPLC and liquid handling technologyDirect interface to ReactIR™ technology – allows maximum sensitivity – low concentration reaction component monitoring
Internal usage only
DS Series Flow Cell
Plug-n-play technology with ReactIR™ - no alignment requiredSpecifically design for lab process R&D with direct scalability to productionEasy to clean system – quickly advance to next projectAmbient to 75C temperature control – flexibility to conform to chemistry requirementsPressure up to 50bar – doesn’t limit use with standard flow chemistry systems
Internal usage only
MultiplexIR & DS Series Flow Cells
Multiplexing- Monitor multi-step chemistry- Monitor up to 2 different flow systems
Built-in modularity allows enhanced usability for process development
- Plug-n-play technology permits use of probe based ReactIR™ reaction monitoring technology with the same system
Internal usage only
DS Series Flow Cell Schematic
21
Internal usage only
Reaction Analysis Resources
22
mt.com/reaction-analysis– Introduction to real-time in situ FTIR– Flash piece on method of measurement
mt.com/reactir– ReactIR™ product family page
YouTube.com/user/mtautochem– Sampling technology options– Comparing instrument capabilities– Coming Soon! Software training tutorials