Real-time In Situ FTIR Reaction Analysis Evolution of Technology Current State-of-the-Art. July 23, 2009 CPAC Summer Institute Seattle, WA
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1 Real-time In Situ FTIR Reaction Analysis Evolution of Technology Current State-of-the-Art July 23, 2009 CPAC Summer Institute Seattle, WA
2 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
3 Reaction Analysis System Evolution ReactIR ReactIR ReactIR 4000 Weight 250 lbs in lab Weight 90 lbs on bench top Weight 40 lbs in fume hood
4 ReactIR Product Family 2009 ReactIR ic10 Organic chemistry ReactIR 45m Chemical Engineering MonARC Classified Area
5 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
6 Evolution of Software ReactIR ReactIR 3.0
7 Revolution of Software ic IR ic IR ic IR ic IR ic IR 4.0
8 ic IR Linked Views
9 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
10 Evolution of FTIR Sampling Technology Circle Cell Comp Probes Comp Pressure Vessel TIARA Vessel Circle reactor HATR HATR Reactor 2002 Chalcogenide Optical Fiber Conduit and 6mm diameter probe
11 Heated Gas Cell Heated Gas Cell Gas Inlet/Outlet External Temperature Controller K1 Mirror To ReactIR
12 Comp Probe Technology Range 16mm probes Sentinel 6.3mm (1/4 ) and 9.5mm (3/8 ) diameter AgX FiberConduit probes C to 180 C - Vacuum to 69bar (1,000 psi) Standard 16mm (5/8 ) & 25.4mm (1 ) Sentinel probes 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 Silver Halide (AgX) FiberConduit
13 Dip Tubes Custom specifications - Flange - Dip tube length 8AgX fiber dependent - Materials of construction
14 Production Dip Tubes Dip tube in production vessel AgX FiberConduit to Dip tube
15 Flow Cells in Production - Streamline Streamline flow cell Standard product Custom as required Heating option Air cooled Ultrasonic option
16 Flow Cells in Production Custom Flow cell - Flange - Flowpath diameter - Material of contruction Uses standard Sentinel probe Ultrasonic optional
17 DS Series AgX Design Introduced 2009 Input/ Output Fibers Color Coding: Top (seal type) Gold = gold White = Teflon RTD connector Bottom (sensor seal) Blue = diamond Silver = silicon Modular design: Independent construction Easily repairable
18 MultiplexIR for the ReactIR 45m Improved efficiency - Multiplex experiments complete 2 experiments at the same time - Improve reaction understanding - integrated ReactIR and ALR, complemented by ic IR / icontrol Expanded applications - Simultaneous measurement of headspace and liquid phase - More reaction information from a single instrument
19 Evolution of the flowcell Adapted from AgX FiberConduit technology Integrated DiComp or SiComp ATR technology - Covers broad range of chemistry applications Conforms to standard HPLC and liquid handling technology Direct interface to ReactIR technology allows maximum sensitivity low concentration reaction component monitoring
20 DS Series Flow Cell Plug-n-play technology with ReactIR - no alignment required Specifically design for lab process R&D with direct scalability to production Easy to clean system quickly advance to next project Ambient to 75C temperature control flexibility to conform to chemistry requirements Pressure up to 50bar doesn t limit use with standard flow chemistry systems
21 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
22 DS Series Flow Cell Schematic 21
23 Reaction Analysis Resources 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 22
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