Combining Analytical Sensors and NeSSI to Improve PAT

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 PAT

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

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

4. Where Does NeSSI™ Fit in the Lab • Instrument/Sensor Interfaces • Design standards make development simpler • Reduced toolset to be mastered • 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 • 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.)

5. The NeSSI Could Become the Base for a Micro-Analytical Lab‘A DEVELOPMENT PLATFORM’

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

7. 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 (√)

8. P V NeSSI™:Enabler for MicroAnalytical Standard “connectivity” • (the “rail” concept) Standard Electrical (Digital) Interface “Rail” SAM* Standard “hockey-puckPC” Anyone’s Actuator Anyone’s Sensor Standard Mechanical Interface “Rail” *Sensor/Actuator Manager • What technologies are available • Suitability for modular sampling systems

9. Phased Micro Gas Analyzer

10. PHASED microGC Other Analytical: Ion, Nox. O2, pH Conductivity, NOx, Turbidity, Density, Opacity Refractive Index, Others Chemometric Sensors for Complex Analytical Measurements. Network Network D/A A/D Mod Valve Press/ Temp Substrate Substrate Substrate On/Off and Modulating valves Flow Sensor w/ Temp, Pressure w/ Temp PHASED *Micro GC Moisture in Dry Gases *PHASED: Courtesy of Honeywell

11. MICRO-GC SLS • GCM 5000 • < 20 W Power • 3 x 2 x 0.6 inches • 100 gm / 3 oz. • www.slsmt.com

12. 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)

13. Siemens microSAM GC • Valveless live injection with software-adjustable injection volume • Maintenance-free column switching and electronic pressure control • Accurate measuring results by multiple parallel micro-detectors • 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

14. Agilent 3000 Micro GC Dimensions: 5.9” x 9.8” x 16.1” Wt: 18 – 37 lbs (portable) • Custom configurations with 1 to 4 replaceable chromatographic channels. Choose from various micro-machined 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.

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

16. 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.

17. NeSSI IR Gas Cell

18. Sentelligence Current NIR Sensors Removable Tip Version - NIR Sensors

19. IR Microsystems Microarray 64 Wilks Enterprise InfraSpec Variable Filter Array

20. 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

21. 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

22. Aspectrics EP-IR with Gas Cell 15” 7” Spectrometer 5.2” Gas cell Glow source

23. 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

24. NeSSI System for Gas/Vapor Generation and Sensor Calib.

25. CPAC Funded Technology Developments

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

27. Spreeta SPR sensing components • SPIRIT system performs SPR detection using Texas Instruments’ Spreeta SPR chips • Chips are mass-produced by TI, cost ~$4 in large quantities • Each chip can perform three simultaneous measurements • Systems contain 8 chips, for 24 total sensing channels Each Spreeta chip contains all of the optical components needed for sensitive SPR measurement of biomolecular interactions Clem Furlong, et al, UW

28. Fringing Field Dielectric NeSSI Sensor Alex Mamishev EE and Marquardt CPAC, UW

29. Raman/NIR/UV-Vis Sensor Module

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

31. PtO2 NeSSI Sensor 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

32. Calibrated Gas Generation

33. Application of Permeation Apparatus

34. Acknowledgments • Center for Process Analytical Chemistry • Students – Charles Branham and Wes Thompson, UW • Professor Kent Mann, Univ. of Minnesota • Clem Furlong – UW Medical Genetics • Mike McCarthy and group – UC Davis • Scott Gilbert – UW Visiting scholar • Swagelok, Parker and Circor • ABB, Agilent, Aspectrics, Honeywell, ExxonMobil