Combining Analytical Sensors and Ne SSI to Improve

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

What is Ne. SSI™? Industry-driven effort to define and promote a new standardized alternative to sample conditioning systems for analyzers and sensors n n n Standard fluidic interface for modular surface-mount components Standard wiring and communications interfaces Standard platform for micro analytics

Ne. SSI™ - objectives Facilitate the acceptance / implementation of modular, miniature & smart sample system technology based on ANSI/ISA SP 76 standard Provide a technology bridge to the process for. . . “sensor/lab-on-a-chip” micro-analytical devices Promote the concept of field-mounted (By-Line) smart analytical systems Lay the groundwork for Pipe to Pixel™ open connectivity architecture for intrinsically safe transducer communications and industry standard communication protocols

What does Ne. SSI™ Provide Simple “Lego-like” assembly n n Easy to re-configure No special tools or skills required Standardized flow components n n “Mix-and-match” compatibility between vendors Growing list of components Standardized electrical and communication (Gen II) n n “Plug-and-play” integration of multiple devices Simplified interface for programmatic I/O and control Advanced analytics (Gen III) n n Micro-analyzers Integrated analysis or “smart” systems

Benefits of Being Ne. SSI™ Your condition space is constrained n Volumes, flow rates, pressures, and viscosities inherently bounded by architecture Your interfaces are defined n n Electrical power, communication, and sample are all available in a standard way Power budget could be main driver to miniaturize Your sample conditioning can be defined and controlled n Specify up-stream and down-stream Ne. SSI components (and verify) All this means your analytical can be more directed and focused

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

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 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 (? )

Ne. SSI™: Enabler for Micro. Analytical Standard “connectivity (the “rail” concept) ” Standard Electrical (Digital) Interface “Rail” Anyone’s Sensor P Anyone’s Actuator V SAM* Standard “hockey-puck. PC” Standard Mechanical Interface “Rail” *Sensor/Actuator Manager What technologies are available Suitability for modular sampling systems

Phased Micro Gas Analyzer

PHASED micro. GC Network D/A A/D Mod Valve Press/ Temp Substrate On/Off and Modulating valves Other Analytical: Ion, Nox. O 2, p. H Conductivity, NOx, Turbidity, Density, Opacity Refractive Index, Others Chemometric Sensors for Complex Analytical Measurements. Substrate Flow Sensor w/ Temp, Pressure w/ Temp PHASED * Micro GC Moisture in Dry Gases *PHASED: Courtesy of Honeywell

MICRO-GC GCM 5000 < 20 W Power 3 x 2 x 0. 6 inches 100 gm / 3 oz. www. slsmt. com SLS

ABB Natural Gas Chromatograph Dimensions: 6. 75“ dia. × 16'' long × 9. 00'' tall Weight: Approximately 28 lb. (12. 7 Kg) Analysis section contains stream selection solenoids, pressure regulation, 32 bit digital detector electronics and a dual-train chromatograph in a single, replaceable module (coffee-cup sized)

Siemens micro. SAM GC Valveless live injection with software-adjustable injection volume Maintenance-free column switching and electronic pressure control Accurate measuring results by multiple parallel microdetectors Can be mounted directly at the sample extraction point because only a single auxiliary gas and very little electrical power is required Simple remote control with Windows-based software and Ethernet communication

Agilent 3000 Micro GC Custom configurations with 1 to 4 replaceable chromatographic channels. Choose from various micromachined injectors, columns, sample conditioners, and application-specific reports. The modular GC design maximizes uptime, with repair as simple as exchanging one module for another. Increase sensitivity, maintain high precision, remove unwanted contaminants from your sample, or speed up analysis with variable, fixed or backflush injection options. Digital pneumatics control carrier gas flow electronically, enhancing reliability and precision while further simplifying operation. Dimensions: 5. 9” x 9. 8” x 16. 1” Wt: 18 – 37 lbs (portable)

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 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 Ballprobe - Raman/NIR/UV

Sentelligence Current NIR Sensors Removable Tip Version - NIR Sensors

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™ IR Gas Cell

IR Microsystems Microarray 64 Board Dimensions: 66 x 53 2 mm Wilks Enterprise Infra. Spec Variable Filter Array

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 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

Aspectrics EP-IR with Gas Cell 15” 7” Spectrometer 5. 2” Gas cell Glow source

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 System for Gas/Vapor Generation and Sensor Calib.

CPAC Ne. SSI Developments

New Gas Calibration System

Gas Sensor Calibration System

Fringing Field Dielectric Ne. SSI Sensor Alex Mamishev EE and Brian Marquardt CPAC, UW

Ne. SSI Raman Sampling Block • Reactor Ne. SSI substrate • Sample conditioning to induce backpressure to reduce bubble formation and the heated substrate allows analysis at reactor conditions

Pt. O 2 Ne. SSI Sensor 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

Calibrated Gas Generation

Application of Permeation Apparatus

Acknowledgments Center for Process Analytical Chemistry 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