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

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

9. Phased Micro Gas Analyzer

10. PHASED microGC D/A A/D Mod Valve Press/ Temp 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.

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
i.e. MicroSAM uses a thermal conductivity detector array integrated on silicon to measure all column and vent flows as well as the injection peak itself

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
                                                                                                      Board Dimensions: 66 x 53 mm 2
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. Liquid Chromatography for NeSSI™
Scott Gilbert, CPAC Visiting Scholar Crystal Vision Microsystems LLC Atofluidic Technologies, LLC
Split flow approach to sampling
m-fluidic LC Chip for On-line Sample Pretreatment
Pulsed electrochemical
detection (on-chip)
Liters per minute
micromixer
diluent in
column
mobile phase in
sample in
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
Vapochromic sensor optical 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

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
In the SPIRIT system, SPR is detected using mass-produced Spreeta sensing components manufactured by Texas Instruments. Each chip contains a complete optical system, including LED light sources, a molded plastic prism, a gold-coated sensor chip, and a diode array detector. Each chip provides three sensing channels( 200 μ-wide gold stripes); the SPIRIT system contains eight chips, for a total of 24 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