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Brian Marquardt , Charles BranhamKent Mann – University of MinnesotaDave Veltkamp – C8 Medisys
Applied Physics Laboratory /Center for Process Analytical ChemistryUniversity of WashingtonSeattle, WA 98105
Combining Analytical Sensors and NeSSI to Improve Process Understanding
Analytical Sampling for Online Applications
Why Use Microreactors?
High Throughput Experimentation For..
Discovery and screeningProcess optimizationProcess developmentProcess controlProduction?
Challenges To Using Microreactors
Analytical characterizationSampling and screeningData handlingProcess modeling and feed back control (particularly if they are used for production)Reaction optimization – move toward feed forward control????
CPAC/FDA/Corning MicroReactor
Collaborative project between 3 entities to improve reaction development and optimization through the use of continuous microreactors, NeSSI and analyticsFunded by the FDA to demonstrate the benefits of improved reactor design, effective sampling and online analytics to increase process understandingProject begins November 2008
Corning Microreactor + NeSSI
NeSSI Ballprobe - Raman/NIR/UV
Spectroscopic Analysis of ReactorPossible problems with performing online spectroscopic measurements
Bubble formation in sample linesdue to pressure dropsample degassing
Phase change between reactor and analyzerdue to temperature or pressure change
Most PAT problems are due to sampling not measurement deviceNeed better systems to sample processes
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
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 interfacesStandard platform formicro analytics
What does NeSSI ProvideSimple “Lego-like” assembly
Easy to re-configureNo special tools or skills required
Standardized flow components“Mix-and-match” compatibility between vendorsGrowing list of components
Standardized electrical and comm. (Gen II)“Plug-and-play” integration of multiple devicesSimplified interface for programmatic I/O and control
Advanced analytics (Gen III)Micro-analyzersIntegrated analysis or “smart” systems
Benefits of Being NeSSIYour condition space is constrained□ Volumes, flow rates, pressures, and viscosities inherently
bounded by architectureYour interfaces are defined□ Electrical power, communication, and sample are all available
in a standard way□ Power budget could be main driver to miniaturizeYour sample conditioning can be defined and controlled□ Specify up-stream and down-stream NeSSI components (and
verify)All this means your analytical can be more directed and focused
Where Does NeSSI Fit in the LabInstrument/Sensor Interfaces
Design standards make development simplerReduced toolset to be masteredReduced sample variability to account for
Calibration/validation built-inConsistent physical environment for measurementStream switching and/or mixing allow generation of standards to match analytical requirements
Reaction monitoringMicroreactors and continuous flow reactorsBatch reactors (with fast loop)
Sample PreparationGas handling (mixing, generation, delivery)Liquid handling (mixing, dilution, conditioning, etc.)
NeSSI with an Array of Micro-Analytical Techniques will Impact Many Industries
• Process Control• Process Optimization• Product Development
NeSSI Sensing TechnologiesGas Chromatography
Thermal DesorptionDielectricSpectroscopies
IR NIR UV- Vis Raman Fluorescence
Impedance Conductivity Refractive Index
Particle SizingLight scattering (?)
Turbidity pHRGAMass SpectrometryLC, SEC, ICTerahertz (?)
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”
PV
*Sensor/Actuator Manager
Standard“connectivity
”
What technologies are availableSuitability for modular sampling systems
C2V Fast Micro-GC
http://www.c2v.nl/
At-Line GC’s with NeSSI CompatibilityABB Natural GC
Siem
ens microS
AM
Agilent 3000 M
icro GC
Applied Analytics Inc. Diode Array OMA-300 A Fiber-optics-diode-array process analyzerFor on-line concentration monitoring
Applied Analytics Microspec IR
FEATURESIdeal for monitoring PPM level WATER in various solventsIn stream quantitative measurementsContains no moving parts andExtremely robust allowing for installations in process stream environmentsReplaces analyzers such as process spectrometers in the process plant.
Small Diameter ATR-IR-Fiber ProbesFiber Photonics Inc.
www.fibrephotonics.comDiamond ATR-IR-Fiber Probe of 2.7mm diameter in NeSSI
Agilent NeSSI Dielectric SensorCable 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™ IR Gas Cell
NeSSI Compatible Optical Cells Axiom Analytical, Inc.
Courtesy of Mike DoyleAxiom Analytical, Inc.
Currently Available
FFV Series Transmission Cells (Near-IR, UV-Visible)FNL-120 UV-Visible ATR Cell
In DevelopmentRaman Cells (Single- and Multi-pass)
Possible DevelopmentDiffuse Reflectance CellsMid-IR ATR Cells
Chevron NeSSI/Analytical UnitSpecifications
ASI Microfast GCParker NeSSI gas handling/sampling systemCarrier gasMobility
NeSSI based Analytical Developments at CPAC
NeSSI Gas/ Vapor System
NeSSI Gas/Vapor System
Permeation Tower
Aspectrics EPIR w/ glass cell
N2 Waste
NeSSI Flow Cell
ASI microFAST GC
NeSSI Calibration Gas Generation System
Features of NeSSI System :• 4 Stage dilution, able to produce and maintain gas concentrations in ppb
range• Fully automated system, set and forget capability
Automated NeSSI Gas/Vapor System
N2
O2
Mixed Gases
Mass FlowControllers
Gas Mixing System LabView Control Program
Design of Small Fiber Optic SensorsOxygenMoistureAmmoniaHydrogenCommon Solvents
AlcoholsEstersAmines
Chlorinated OrganicsOrganic Hydrocarbons
(BTEX)Carbon Dioxide
(in development)Hydrogen Sulfide
(in development)
• vapochromic chemistry• optical response to analyte
• simple design• reversible response• low power• inexpensive• fast response times• high quantum efficiency• long term sensor stability• sensitive to a variety of analytes• wireless communication• battery powered
Modular NeSSI Oxygen Gas Sensor
Exploded View
1/16 in bifurcated fiber optic fiber
1/16 to 1/8 in Swagelok union
Agilent NeSSI Mount
Sensor Body
Close up of Outer Body Tip
Vapochromic Tip
Fiber optic ferrule with plastic housing
Sensor response to O2
Pre
dict
ed O
2%
Calculated O2 %
R2 = 0.990, 3 PCRMSEC = 1.0744
20 replicates at each concentrationConcentration range: 0 -100% Oxygen
Inte
nsity
(cou
nts)
Wavelength (nm)
100 %
0%
120
100
80
60
40
20
01009080706050403020100
Future Miniature Oxygen Sensor
Oxygen Sensor and probe Oxygen Sensing Tip
Liquid Chromatography for NeSSI™ Scott Gilbert, CPAC Visiting Scholar
Crystal Vision Microsystems LLCAtofluidic Technologies, LLC
• Split flow approach to sampling
• μ-fluidic LC Chip for On-line Sample Pretreatment
• Pulsed electrochemical detection (on-chip)
micromixer
diluent in
column
mobile phase in
sample in
Liters per minute
microliters per minute
nanoliters per minute
Development of a Micro-NMR System
M. McCarthy, UC Davis
AcknowledgmentsCenter for Process Analytical ChemistryStudents – Charles Branham and Wes Thompson, UWVendors who provided slidesProfessor Kent Mann’s Group, Univ. of MinnesotaScott Gilbert – UW Visiting scholarSwagelok, Parker and Circor ABB, Agilent, Aspectrics, Honeywell, ExxonMobil