Brian Marquardt and Dave Veltkamp

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 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 LabA 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 (v)
• RGA ()
• Mass Spectrometry (v)
• LC, SEC, IC ()
• Terrahertz (?)

• Gas Chromatography
• Thermal Desorption (?)
• Dielectric (v)
• Spectroscopies
• IR (), NIR ()
• UV- Vis ()
• Raman (v)
• Fluorescence ()
• Impedance ()
• Conductivity (v)
• Refractive Index (v)

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NeSSI Enabler for MicroAnalytical
Standard connectivity

• (the rail concept)

Standard Electrical (Digital) Interface Rail
SAM
Standard hockey-puckPC
Anyones Actuator
Anyones Sensor
Standard Mechanical Interface Rail
Sensor/Actuator Manager

• What technologies are available
• Suitability for modular sampling systems

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Phased Micro Gas Analyzer
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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
Moisture in Dry Gases
PHASED Micro GC
PHASED Courtesy of Honeywell
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MICRO-GC SLS

• GCM 5000
• lt 20 W Power
• 3 x 2 x 0.6 inches
• 100 gm / 3 oz.
• www.slsmt.com

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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

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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

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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.

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NeSSI IR Gas Cell
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Sentelligence Current NIR Sensors
Removable Tip Version
- NIR Sensors
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IR Microsystems Microarray 64
Wilks Enterprise InfraSpec Variable Filter Array
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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
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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
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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

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NeSSI System for Gas/Vapor Generation and Sensor
Calib.
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CPAC Funded Technology Developments
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Development of a Micro-NMR System
NMR spectrum of a 3 micro liter water sample
using a RF micro-coil
M. McCarthy, UC Davis
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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
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Fringing Field Dielectric NeSSI Sensor
Alex Mamishev EE and Marquardt CPAC, UW
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Raman/NIR/UV-Vis Sensor Module
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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

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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
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Calibrated Gas Generation
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Application of Permeation Apparatus
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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