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Combining Analytical Sensors and NeSSI to Improve Process Understanding

This project aims to integrate microreactors, NeSSI, and analytical monitoring for bio-processing research, providing a platform for education and innovation. Tasks include system integration, characterization, online monitoring, and automation strategies. Impact in industries like process control, optimization, and product development.

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Combining Analytical Sensors and NeSSI to Improve Process Understanding

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

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

  3. Project Research Plan • Task 1: integrate the microreactors with the NeSSI™ 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. • Software and hardware for data and control communication interfaces (hopefully utilizing a Gen II NeSSI™-bus network) will need to be developed and tested.

  4. NeSSI with an Array of Micro-Analytical Techniques will Impact Many Industries • Process Control • Process Optimization • Product Development

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

  6. Corning Microreactor + NeSSI

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

  8. NeSSI Ballprobe - Raman/NIR/UV

  9. Agilent NeSSI 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

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

  11. NeSSI Gas Generation System Mass Flow Controllers Mixed Gases O2 N2 Automated Circor NeSSI Gas/Vapor System Features of Circor NeSSI System : 4 State dilution, able to produce and maintain gas concentrations in ppb range Fully automated system, set and forget capability

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

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

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

  15. Other potential commercial analyzers for NeSSI/microreactor project

  16. C2V fast micro-GC http://www.c2v.nl/

  17. At-Line GC’s with NeSSI Compat. ABB Natural GC Agilent 3000 Micro GC Siemens microSAM

  18. Applied Analytics Inc. Diode Array • OMA-300 • A  Fiber-optics-diode-array process analyzer • For on-line concentration monitoring

  19. 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.

  20. NeSSI™ IR Gas Cell

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

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

  23. Analytical-on-NeSSI Gen III Spec. • Work with Sponsors, Vendors, End-users • 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 NeSSI • Compendium of parameters • Example reference systems • Generally useful to extend application base of NeSSI

  24. 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 • Much of this work will be performed with the help of Bruce Finlayson's senior project students and from our work at CPAC

  25. 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, ExxonMobil

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