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Combining Analytical Sensors and Ne. SSI to Improve Process Understanding Brian Marquardt and Dave Combining Analytical Sensors and Ne. SSI to Improve Process Understanding Brian Marquardt and Dave Veltkamp Applied Physics Laboratory / Center for Process Analytical Chemistry University of Washington Seattle, WA 98105

Project Goals and Objectives Establish research platforms integrating microreactors, Ne. SSI, and analytical monitoring Project Goals and Objectives Establish research platforms integrating microreactors, Ne. SSI, and analytical monitoring for the multidisciplinary investigation of bio-processing and bio-fuels related processes. These systems will be used to support other CPAC and University projects investigating bioprocessing, provide opportunities for student education, and allow development of additional instrumentation and techniques for monitoring bio-processes.

Project Research Plan Task 1: integrate the microreactors with the Ne. SSI™ fluidics system Project Research Plan Task 1: integrate the microreactors with the Ne. SSI™ fluidics system and the analytical monitoring instruments. Task 2: characterize the systems so their properties (i. e. , flow, mixing, heat transfer, residence time, etc. ) are well understood. Task 3: development of the on-line analytical to monitor the key operational parameters and reaction progress. Task 4: development of strategies and implementations for automation and control of the system. n Software and hardware for data and control communication interfaces (hopefully utilizing a Gen II Ne. SSI™-bus network) will need to be developed and tested.

Ne. SSI with an Array of Micro. Analytical Techniques will Impact Many Industries Process Ne. SSI with an Array of Micro. Analytical Techniques will Impact Many Industries Process Control Process Optimization Product Development

Sensing Technologies Gas Chromatography n Thermal Desorption (? ) Dielectric (√) Spectroscopies n n Sensing Technologies Gas Chromatography n Thermal Desorption (? ) Dielectric (√) Spectroscopies n n IR (+), NIR (+) UV- Vis (+) Raman (√) Fluorescence (+) Impedance (+) Conductivity (√) Refractive Index (√) Vapochromic Sensors (+) GLRS (+) Particle Sizing n Light scattering (? ) Turbidity (+) p. H (√) RGA (+) Mass Spectrometry (√) LC, SEC, IC (+) Terrahertz (? )

Corning Microreactor + Ne. SSI Corning Microreactor + Ne. SSI

Interfacing Ne. SSI™ to ASI micro. Fast GC™ GC sipper port EP-IR gas cell Interfacing Ne. SSI™ to ASI micro. Fast GC™ GC sipper port EP-IR gas cell Vapochromic sensor optical cell Complete gas/vapor sensing test platform on the bench top n n Gas delivery, vapor generation, and blending in Ne. SSI™ Real time verification of composition using GC and EP-IR Easily extended to include other analytical and sample treatments

Ne. SSI Ballprobe - Raman/NIR/UV Ne. SSI Ballprobe - Raman/NIR/UV

Agilent Ne. SSI Dielectric Sensor Cable to Agilent Network Analyzer Dielectric Probe Close up Agilent Ne. SSI Dielectric Sensor Cable to Agilent Network Analyzer Dielectric Probe Close up of Coaxial Probe Tip Inner Body O-ring (inside) Swagelok 2 -Port Valve Base Outer Body Exploded View

Liquid Chromatography for Ne. SSI™ Scott Gilbert, CPAC Visiting Scholar Crystal Vision Microsystems LLC Liquid Chromatography for Ne. SSI™ Scott Gilbert, CPAC Visiting Scholar Crystal Vision Microsystems LLC Atofluidic Technologies, LLC Split flow approach to sampling Liters per minute sample in diluent in microliters per minute micromixer nanoliters per minute m-fluidic LC Chip for On-line Sample Pretreatment Pulsed electrochemical detection (on-chip) column mobile phase in

Ne. SSI Gas Generation System Mass Flow Controllers Mixed Gases O 2 N 2 Ne. SSI Gas Generation System Mass Flow Controllers Mixed Gases O 2 N 2 Automated Circor Ne. SSI Gas/Vapor System Features of Circor Ne. SSI System : 1. 4 State dilution, able to produce and maintain gas concentrations in ppb range 2. Fully automated system, set and forget capability

Vapochromic Ne. SSI Sensor Design simple design reversible response low power inexpensive Ne. SSI Vapochromic Ne. SSI Sensor Design simple design reversible response low power inexpensive Ne. SSI compatible fast response times high quantum efficiency long term sensor stability sensitive to a variety of analytes large number of available vapochromic compounds (selectivity)

Vapochromic Ne. SSI Sensor Design Fiber optic cable to Ocean Optics Spectrometer Fiberoptic Probe(405 Vapochromic Ne. SSI Sensor Design Fiber optic cable to Ocean Optics Spectrometer Fiberoptic Probe(405 nm LED) Inner Body O-ring (inside) Swagelok 2 -Port Valve Base Close up of Outer Body Tip Outer Body Vapochromic Tip Exploded View

Development of a Micro-NMR System M. Mc. Carthy, UC Davis NMR spectrum of a Development of a Micro-NMR System M. Mc. Carthy, UC Davis NMR spectrum of a 3 micro liter water sample using a RF micro-coil

Other potential commercial analyzers for Ne. SSI/microreactor project Other potential commercial analyzers for Ne. SSI/microreactor project

C 2 V fast micro-GC http: //www. c 2 v. nl/ C 2 V fast micro-GC http: //www. c 2 v. nl/

At-Line GC’s with Ne. SSI Compat. Agilent 3000 Micro GC ABB Natural GC Siemens At-Line GC’s with Ne. SSI Compat. Agilent 3000 Micro GC ABB Natural GC Siemens micro. SAM

Applied Analytics Inc. Diode Array OMA-300 A Fiber-optics-diodearray process analyzer For on-line concentration monitoring Applied Analytics Inc. Diode Array OMA-300 A Fiber-optics-diodearray process analyzer For on-line concentration monitoring

Applied Analytics Microspec IR FEATURES Ideal for monitoring PPM level WATER in various solvents Applied Analytics Microspec IR FEATURES Ideal for monitoring PPM level WATER in various solvents In stream quantitative measurements Contains no moving parts and Extremely robust allowing for installations in process stream environments Replaces analyzers such as process spectrometers in the process plant.

Ne. SSI™ IR Gas Cell Ne. SSI™ IR Gas Cell

Ne. SSI Compatible Spectroscopic Cell Axiom Analytical, Inc. Currently Available FFV Series Transmission Cells Ne. SSI Compatible Spectroscopic Cell Axiom Analytical, Inc. Currently Available FFV Series Transmission Cells (Near-IR, UV-Visible) n FNL-120 UV-Visible ATR Cell In Development n Raman Cells (Single- and Multi-pass) Possible Development n Diffuse Reflectance Cells (For turbid liquids) n Mid-IR ATR Cells n Courtesy of Mike Doyle Axiom Analytical, Inc.

Ne. SSI Project Deliverables Integrate Ne. SSI, microreactors and analytics Develop and publish the Ne. SSI Project Deliverables Integrate Ne. SSI, microreactors and analytics Develop and publish the Ne. SSI Gen III specification Continue development of interfaces for analytical instrumentation n liquid sample vaporizer using nanoliter volume inkjettype injectors and heated carrier stream Direct liquid injection to GC Direct liquid injection to Mass spec n Likely will need to generalize Scott Gilbert’s dilution stream device On-board dilutant (solvent) storage reservoirs Pneumatic pumping (piston/syringe pump)

Analytical-on-Ne. SSI Gen III Spec. Work with Sponsors, Vendors, End-users n n Draft at Analytical-on-Ne. SSI Gen III Spec. Work with Sponsors, Vendors, End-users n n Draft at Fall 2008 CPAC Meeting Final at Spring 2009 CPAC Meeting Goal is to provide analytical developers with a clear idea of what they must design to and what they can expect from Ne. SSI n n Compendium of parameters Example reference systems Generally useful to extend application base of Ne. SSI

Typical info for the Gen lll Spec Application operational setting ranges Available sample conditioning Typical info for the Gen lll Spec Application operational setting ranges Available sample conditioning options Power budget limits and example calculation Communication protocols, messages, and rates n Much of this work will be performed with the help of Bruce Finlayson's senior project students and from our work at CPAC

Acknowledgments Center for Process Analytical Chemistry CPAC Post-doc – Tom Dearing Students – Charles Acknowledgments Center for Process Analytical Chemistry CPAC Post-doc – Tom Dearing Students – Charles Branham and Wes Thompson, UW Vendors who provided slides Professor Kent Mann, Univ. of Minnesota Scott Gilbert – UW Visiting scholar Swagelok, Parker and Circor ABB, Agilent, Aspectrics, Honeywell, Exxon. Mobil