Utilizing NeSSI™ for Analytical Applications Brian Marquardt Dave Veltkamp Center for Process Analytical Chemistry (CPAC) University of Washington, Seattle, WA

Project Overview Goal is to support NeSSI™ related development within CPAC Developing infrastructure and platforms Developing sensors and applications Promote and support wider NeSSI™ adoption and use Web based support Interaction with NeSSI community

What does NeSSI™ Provide Simple “Lego®-like ” assembly (√) Easy to re-configure No special tools or skills required Overall lower cost of build – reduce time to configure/install by 75% Improved reliability Lower cost of ownership – reduce total cost by 40% Standardized flow components (√) “Mix-and-match” compatibility between vendors Growing list of components Standardized electrical and communication (+) “Plug-and-play” integration of multiple devices Simplified interface for programmatic I/O and control Advanced analytics (+) Micro-analyzers Integrated analysis or “smart” systems √ now + soon

The NeSSI™ “rail” Concept *Sensor/Actuator Manager Standard Mechanical Interface “Rail” Standard Electrical (Digital) Interface “Rail” Anyone’s Sensor Anyone’s Actuator SAM* Standard “Applets” P V “connectivity” ISA/ANSI SP76 NeSSI™ Bus Enabler for Micro Analytical Opportunities exist to exploit NeSSI™ standards in other laboratory applications It is really about creating a set of standard interfaces, so current and new analytical devices and sample system components can be quickly and easily integrated into the process environment. A standard electrical interface that will provide power, a standard communication format, and standard protocol between these devices. A standard software package that will allow for inter device communication, control, and diagnostics at the installation level. And a standardized portal and protocol for communication with the plant DCS or Enterprise Management System. A standard mechanical interface. A standardized footprint for interfacing these devices and components with the process sample.

NeSSI™ Sensing Technologies Chromatography Thermal Desorption (?) GC (+) LC (chip based) (+) SEC, IC (?) Dielectric (√) Spectroscopies IR (+), NIR (+) UV- Vis (+) Raman (√) Fluorescence (+) Refractive Index (√) Vapochromic Sensors (+) GLRS (+) Particle Sizing Light scattering (?) Conductivity (√) Turbidity (+) pH (√) SPR (+) Mass Spectrometry (√) Impedance (+) Terrahertz (?), NMR (?) √ now + soon ? maybe

Where Does NeSSI™ Fit in the Lab Instrument/Sensor Interfaces Design standards make development simpler Simplified design, construction, and reconfiguration Reduced sample variability to account for Calibration/validation built-in Consistent physical environment for measurement Stream switching and/or mixing allow generation of standards to match analytical requirements Bridge to micro analytical developments Reaction monitoring Microreactors and continuous flow reactors Batch reactors (with fast loop) Sample Preparation Gas handling (mixing, generation, delivery) Liquid handling (mixing, dilution, conditioning, etc.)

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

Vapochromic Sensor Interface Optical sensor based on vapochromatic compounds Responds to different analytes by intensity and wavelength shifts in fluorescence signal Optical detection using simple spectrometer LED excitation light source Simple reflectance 2 fiber optical measurement Use of BallProbe™ to provide single-sided optical interface Vapochrome coated on ball surface Inserted into standard NeSSI™ tube fitting block NeSSI™ system provides controlled delivery and mixing of gas streams to sensor

NeSSI™ Gas Mixing System Using a customized Ballprobe™ reflectance probe for vapochromic detection Ocean optics USB VIS spectrometer Ballprobe™ coated with vapochrome Swagelok NeSSI™ system Brooks MFC’s and controller

Vapochromic O2 Sensor Response

New Gas Sensor Testing System More capability to generate analytical vapors, gas blending, and on-line dilution of vapor streams for method development work Vapor generation initially off-system – research opportunity for integrating onto NeSSI™ platform Serial dilution possibilities allows wide concentration range to be investigated

NeSSI Raman Sampling Block Parker Intraflow NeSSI substrate Sample conditioning to induce backpressure to reduce bubble formation and the heated substrate allows analysis at reactor conditions

NeSSI™ Microreactor Delivery /Calibration System Reactor Feed 1 Pump 1 Product Stream Reactor Feed 2 Real-time Calibration waste prod Pump 2 Raman Probe

Parker Intraflow™ System

IMM Microreactors and MicroMixers Liquid Microreactor Micro Mixer Heat Exchanger Mixer-Heat Exchanger  Caterpillar Mixer Backbone Block NeSSI™ Adapter

Fuel Cell Research Goal: to study the water uptake properties of Nafion 112 by varying the relative humidity of the input gas streams to better understand membrane hydration and its effects on fuel cell performance. NeSSI™ System for gas flow and humidity sensing 3 Voltmeters,1 Ammeter Thermocouple and Humidity sensor Thermocouple and Humidity sensors H2 in PEM Fuel Cell Air in Both Streams Purge to outside environment Fan/Blower Or Pump Tank (might run system without a tank)

Where Are We Now? Development continues on control system Data I/O, comm., and control hardware Software for DAQ, automation and control NeSSI microreactor system becoming reality Parker Intraflow™ fluidic system designed and being built IMM, Microglass, CPC mixers and reactor components here or coming soon LC, Raman, dielectric, RI detection demonstrated or close to Headspace and media sampling systems RGA analyzer, Thermo MS systems running Filter system from CIRCOR functionally tested Vapochromatic sensor test and development platform operational and providing good results Large improvement over traditional lab gas handling systems NeSSI™ flexibility allows for evolutionary improvements

What’s Ahead Continue gas sensing work with focus on application development Vapochromatic BTEX sensor (array) Vapochromatic humidity sensor for fuel cells Fermentation headspace/off-gas monitoring Continue development of control and acquisition software Begin characterizing flows and dispersion in the NeSSI™ systems Important for analytical and mixing applications Continue developing analytical interfaces to bring more instrumentation to NeSSI™ Working with Vendors of new technology In-house fiber optic flow cell for NeSSI™

Acknowledgements Swagelok, CIRCOR, and Parker (NeSSI™ systems and components) Brooks Instruments and Flowmatrix (MFCs) Thermo and Merk/Horiba (Mass Spec.) Agilent (Dielectric) IMM, Microglass, and CPC (microreactors) UOP (server for NeSSI™ web sites) ExxonMobil, Kraft, others (applications) NeSSI™ Steering Team CPAC