Utilizing NeSSI™ for Utilizing NeSSI™ for Analytical ApplicationsAnalytical Applications

Brian MarquardtBrian MarquardtDave VeltkampDave Veltkamp

Center for Process Analytical Chemistry (CPAC)Center for Process Analytical Chemistry (CPAC)University of Washington, Seattle, WAUniversity of Washington, Seattle, WA

Project OverviewProject Overview

Goal is to support NeSSI™ related Goal is to support NeSSI™ related development within CPACdevelopment within CPAC

Developing infrastructure and platformsDeveloping infrastructure and platformsDeveloping sensors and applicationsDeveloping sensors and applications

Promote and support wider NeSSI™ Promote and support wider NeSSI™ adoption and useadoption and use

Web based supportWeb based supportInteraction with NeSSI communityInteraction with NeSSI community

What does NeSSI™ ProvideWhat does NeSSI™ ProvideSimple “LegoSimple “Lego®®--like ” assembly (like ” assembly (√√))

Easy to reEasy to re--configureconfigureNo special tools or skills requiredNo special tools or skills requiredOverall lower cost of build Overall lower cost of build –– reduce time to configure/install by 75%reduce time to configure/install by 75%Improved reliabilityImproved reliabilityLower cost of ownership Lower cost of ownership –– reduce total cost by 40%reduce total cost by 40%

Standardized flow components (Standardized flow components (√√))“Mix“Mix--andand--match” compatibility between vendorsmatch” compatibility between vendorsGrowing list of componentsGrowing list of components

Standardized electrical and communication (Standardized electrical and communication (++))“Plug“Plug--andand--play” integration of multiple devicesplay” integration of multiple devicesSimplified interface for programmatic I/O and controlSimplified interface for programmatic I/O and control

Advanced analytics (Advanced analytics (++))MicroMicro--analyzersanalyzersIntegrated analysis or “smart” systemsIntegrated analysis or “smart” systems √√ nownow ++ soonsoon

The NeSSI™ “rail” ConceptThe NeSSI™ “rail” ConceptEnabler for Micro AnalyticalEnabler for Micro Analytical

Opportunities exist to exploit NeSSI™ Opportunities exist to exploit NeSSI™ standards in other laboratory applicationsstandards in other laboratory applications

The NeSSI™ “rail” ConceptThe NeSSI™ “rail” ConceptThe NeSSI™ “rail” ConceptThe NeSSI™ “rail” Concept

*Sensor/Actuator Manager

Standard Mechanical Interface “Rail”

Standard Electrical (Digital) Interface “Rail”

Anyone’s Sensor Anyone’s Actuator

SAM*

Standard“Applets”

PV

Standard“connectivity”

ISA/ANSI SP76

NeSSI™ Bus

NeSSI™ Sensing TechnologiesNeSSI™ Sensing TechnologiesChromatographyChromatography

Thermal Thermal DesorptionDesorption ((??))GC (GC (++) ) LC (chip based) (LC (chip based) (++))SEC, IC (SEC, IC (??))

Dielectric (Dielectric (√√))SpectroscopiesSpectroscopies

IR (IR (++), NIR (), NIR (++))UVUV-- VisVis ((++))Raman (Raman (√√))Fluorescence (Fluorescence (++))

Refractive Index (Refractive Index (√√)

Vapochromic Sensors (Vapochromic Sensors (++))GLRS (GLRS (++))Particle SizingParticle Sizing

Light scattering (Light scattering (??))

Conductivity (Conductivity (√√))Turbidity (Turbidity (++))pH (pH (√√))SPR (SPR (++))Mass Spectrometry (Mass Spectrometry (√√))Impedance (Impedance (++))TerrahertzTerrahertz ((??), NMR (), NMR (??)) )

√√ nownow ++ soon soon ?? maybemaybe

Where Does NeSSI™ Fit in the LabWhere Does NeSSI™ Fit in the LabInstrument/Sensor InterfacesInstrument/Sensor Interfaces

Design standards make development simplerDesign standards make development simplerSimplified design, construction, and reconfigurationSimplified design, construction, and reconfigurationReduced sample variability to account forReduced sample variability to account for

Calibration/validation builtCalibration/validation built--ininConsistent physical environment for measurementConsistent physical environment for measurementStream switching and/or mixing allow generation of standards to Stream switching and/or mixing allow generation of standards to match analytical requirementsmatch analytical requirements

Bridge to micro analytical developmentsBridge to micro analytical developmentsReaction monitoringReaction monitoring

Microreactors and continuous flow reactorsMicroreactors and continuous flow reactorsBatch reactors (with fast loop)Batch reactors (with fast loop)

Sample PreparationSample PreparationGas handling (mixing, generation, delivery)Gas handling (mixing, generation, delivery)Liquid handling (mixing, dilution, conditioning, etc.)Liquid handling (mixing, dilution, conditioning, etc.)

AgilentAgilent NeSSI™ Dielectric SensorNeSSI™ Dielectric Sensor

Cable to Agilent Network Analyzer

Dielectric Probe

Inner Body

O-ring (inside)

Outer Body

Exploded View

Close up of

Coaxial Probe

Tip

Swagelok2-Port Valve Base

Vapochromic Sensor InterfaceVapochromic Sensor InterfaceOptical sensor based on vapochromatic Optical sensor based on vapochromatic compoundscompounds

Responds to different analytes by intensity and Responds to different analytes by intensity and wavelength shifts in fluorescence signalwavelength shifts in fluorescence signalOptical detection using simple spectrometerOptical detection using simple spectrometer

LED excitation light sourceLED excitation light sourceSimple reflectance 2 fiber optical measurementSimple reflectance 2 fiber optical measurement

Use of Use of BallProbeBallProbe™ to provide single™ to provide single--sided sided optical interfaceoptical interface

Vapochrome coated on ball surfaceVapochrome coated on ball surfaceInserted into standard NeSSI™ tube fitting blockInserted into standard NeSSI™ tube fitting block

NeSSI™ system provides controlled delivery NeSSI™ system provides controlled delivery and mixing of gas streams to sensorand mixing of gas streams to sensor

NeSSI™ Gas Mixing SystemNeSSI™ Gas Mixing SystemUsing a customized Using a customized BallprobeBallprobe™ reflectance probe ™ reflectance probe for vapochromic detectionfor vapochromic detection

Ocean optics USB VIS spectrometerOcean optics USB VIS spectrometerBallprobeBallprobe™™ coated with vapochromeSwagelok NeSSINeSSI™™ systemsystem

Brooks Brooks MFC’sMFC’s and controllercoated with vapochrome

and controller

Vapochromic OVapochromic O22 Sensor ResponseSensor Response

New Gas Sensor Testing SystemNew Gas Sensor Testing SystemMore capability to generate analytical vapors, gas blending, andMore capability to generate analytical vapors, gas blending, andonon--line dilution of vapor streams for method development workline dilution of vapor streams for method development work

Vapor generation initially offVapor generation initially off--system system –– research opportunity for research opportunity for integrating onto NeSSI™ platformintegrating onto NeSSI™ platformSerial dilution possibilities allows wide concentration range toSerial dilution possibilities allows wide concentration range to be be investigatedinvestigated

NeSSI Raman Sampling BlockNeSSI Raman Sampling Block

Parker Parker IntraflowIntraflow NeSSI substrateNeSSI substrateSample conditioning to induce backpressure to Sample conditioning to induce backpressure to reduce bubble formation and the heated reduce bubble formation and the heated substrate allows analysis at reactor conditionssubstrate allows analysis at reactor conditions

NeSSI™ Microreactor DeliveryNeSSI™ Microreactor Delivery/Calibration System/Calibration System

Reactor Feed 1

Reactor Feed 2

Product Stream

Real-timeCalibration

waste

prod

RamanProbe

Pump 1

Pump 2

Parker Parker IntraflowIntraflow™™ SystemSystem

IMM Microreactors and IMM Microreactors and MicroMixersMicroMixers

Caterpillar Mixer

Heat Exchanger

Liquid Microreactor Micro Mixer

NeSSI™ AdapterBackbone Block

Mixer-Heat Exchanger

Fuel Cell ResearchFuel Cell ResearchGoal: to study the water uptake properties of Goal: to study the water uptake properties of NafionNafion 112 112 by varying the relative humidity of the input gas streams by varying the relative humidity of the input gas streams to better understand membrane hydration and its effects to better understand membrane hydration and its effects on fuel cell performance. on fuel cell performance. NeSSI™ System for gas flow and humidity sensingNeSSI™ System for gas flow and humidity sensing

PEM Fuel Cell

Fan/BlowerOr Pump

Both Streams Purge to outside environment

3 Voltmeters,1 AmmeterThermocouple and Humidity sensor

Tank (might run system without a tank)

Thermocouple and Humidity sensors

H2 in

Air in

Where Are We Now?Where Are We Now?Development continues on control systemDevelopment continues on control system

Data I/O, comm., and control hardwareData I/O, comm., and control hardwareSoftware for DAQ, automation and control Software for DAQ, automation and control

NeSSI microreactor system becoming reality NeSSI microreactor system becoming reality Parker Parker IntraflowIntraflow™™ fluidic system designed and being builtfluidic system designed and being builtIMM, IMM, MicroglassMicroglass, CPC mixers and reactor components here or , CPC mixers and reactor components here or coming sooncoming soonLC, Raman, dielectric, RI detection demonstrated or close toLC, Raman, dielectric, RI detection demonstrated or close to

Headspace and media sampling systemsHeadspace and media sampling systemsRGA analyzer, Thermo MS systems runningRGA analyzer, Thermo MS systems runningFilter system from CIRCOR functionally testedFilter system from CIRCOR functionally tested

Vapochromatic sensor test and development platform Vapochromatic sensor test and development platform operational and providing good resultsoperational and providing good results

Large improvement over traditional lab gas handling systemsLarge improvement over traditional lab gas handling systemsNeSSI™ flexibility allows for evolutionary improvementsNeSSI™ flexibility allows for evolutionary improvements

What’s AheadWhat’s AheadContinue gas sensing work with focus on Continue gas sensing work with focus on application development application development

Vapochromatic BTEX sensor (array)Vapochromatic BTEX sensor (array)Vapochromatic humidity sensor for fuel cellsVapochromatic humidity sensor for fuel cellsFermentation headspace/offFermentation headspace/off--gas monitoringgas monitoring

Continue development of control and acquisition Continue development of control and acquisition softwaresoftwareBegin characterizing flows and dispersion in the Begin characterizing flows and dispersion in the NeSSI™ systemsNeSSI™ systems

Important for analytical and mixing applicationsImportant for analytical and mixing applicationsContinue developing analytical interfaces to Continue developing analytical interfaces to bring more instrumentation to NeSSI™bring more instrumentation to NeSSI™

Working with Vendors of new technologyWorking with Vendors of new technologyInIn--house fiber optic flow cell for NeSSI™ house fiber optic flow cell for NeSSI™

AcknowledgementsAcknowledgementsSwagelokSwagelok, CIRCOR, and Parker (NeSSI™ , CIRCOR, and Parker (NeSSI™ systems and components)systems and components)Brooks Instruments and Brooks Instruments and FlowmatrixFlowmatrix ((MFCsMFCs))Thermo and Thermo and MerkMerk/Horiba (Mass Spec.)/Horiba (Mass Spec.)AgilentAgilent (Dielectric)(Dielectric)IMM, IMM, MicroglassMicroglass, and CPC (microreactors) , and CPC (microreactors) UOP (server for NeSSI™ web sites)UOP (server for NeSSI™ web sites)ExxonMobil, Kraft, others (applications)ExxonMobil, Kraft, others (applications)NeSSI™ Steering TeamNeSSI™ Steering TeamCPACCPAC