Utilizing NeSSI for Analytical Applications Brian Marquardt Dave Veltkamp

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

Courtesy of Dow Chemical, Fort Saskatchewan, Canada Objective 1 Facilitate the acceptance / implementation of modular, miniature & smart sample system technology based on ANSI/ISA SP76 standard substrate Objective 2 Provide a technology bridge to the process for...“sensor/lab-on-a-chip” micro-analytical devices NeSSI™ Objectives

Courtesy of Dow Chemical, Freeport, Texas Objective 3 Promote the concept of... field-mounted (By-Line) smart analytical systems Objective 4 Lay the groundwork for Pipe to Pixel™ open connectivity architecture for intrinsically safe transducer communications and industry standard communication protocols OPC Gateway T Sample System Gas Analyzer SAM IS bus NeSSI™ Objectives (cont.)

CIRCOR µMS 3 System

Swagelok ® MPC System

Parker Intraflow™ System

Metering Valve Adapter Regulator Manual & Air Op 2-way Diaphragm Inline & By pass Filters - Sintered & Borosilicate Toggle Relief Check Needle Non-Spill Quick Disconnect Surface Mount Flow Components Many different physical controls and conditioning components available

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

NeSSI™: Enabler for MicroAnalytical (the “rail” concept) Standard Mechanical Interface “Rail” Standard Electrical (Digital) Interface “Rail” Anyone’s Sensor Anyone’s Actuator SAM* Standard “hockey-puckPC” P V *Sensor/Actuator Manager Standard “connectivity ”

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

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

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

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 Sampling /Calibration System Reactor Feed 1 Reactor Feed 2 Product Stream Real-time Calibration waste prod Raman Probe Pump 1 Pump 2

Example NeSSI Sensor Interface Sensor is a vapochromatic compound Responds to different compounds by intensity and wavelength shifts in fluorescence signal Responds to different compounds by intensity and wavelength shifts in fluorescence signal Optical detection using simple VIS spectrometer Optical detection using simple VIS spectrometer LED excitation light source LED excitation light source Simple reflectance 2 fiber optical measurement Simple reflectance 2 fiber optical measurement Use of BallProbe to provide single-sided optical interface Vapochrome coated on ball surface Vapochrome coated on ball surface NeSSI™ system to control delivery and mixing of gas stream

NeSSI Gas Mixing System Using a customized ballprobe reflectance probe for vapochromic detection - Ocean optics spectrometer - ballprobe coated with vapochrome - NeSSI substrate with 2 MFC’s

Vapochromic O 2 Sensor Response

Where are we now? Development continues on control system Data I/O, comm., and control hardware Data I/O, comm., and control hardware Software for DAQ, automation and control Software for DAQ, automation and control NeSSI microreactor system becoming reality Parker Intraflow™ fluidic system designed Parker Intraflow™ fluidic system designed IMM, Microglass, CPC mixers and reactor components here or coming soon IMM, Microglass, CPC mixers and reactor components here or coming soon LC, Raman, dielectric, RI detection LC, Raman, dielectric, RI detection Headspace and media sampling systems RGA analyzer, Thermo MS systems running RGA analyzer, Thermo MS systems running Filter system from CIRCOR functionally tested Filter system from CIRCOR functionally tested