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