Brian Marquardt and Dave Veltkamp Brian Marquardt and Dave Veltkamp

Applied Physics LaboratoryApplied Physics LaboratoryCenter for Process Analytical ChemistryCenter for Process Analytical ChemistryUniversity of WashingtonUniversity of WashingtonSeattle, WA 98105 Seattle, WA 98105

Combining Analytical Sensors and NeSSI to Improve PAT

What is NeSSI™?What is NeSSI™?

Industry-driven effort to Industry-driven effort to define and promote a new define and promote a new standardized alternative to standardized alternative to sample conditioning systems sample conditioning systems for analyzers and sensorsfor analyzers and sensors Standard fluidic interface for Standard fluidic interface for

modular surface-mount modular surface-mount components components

Standard wiring and Standard wiring and communications interfacescommunications interfaces

Standard platform forStandard platform formicro analyticsmicro analytics

What does NeSSI™ ProvideWhat does NeSSI™ Provide

Simple “Lego-like” assemblySimple “Lego-like” assembly Easy to re-configureEasy to re-configure No special tools or skills requiredNo special tools or skills required

Standardized flow componentsStandardized flow components ““Mix-and-match” compatibility between vendorsMix-and-match” compatibility between vendors Growing list of componentsGrowing list of components

Standardized electrical and communication (Gen II)Standardized electrical and communication (Gen II) ““Plug-and-play” integration of multiple devicesPlug-and-play” integration of multiple devices Simplified interface for programmatic I/O and controlSimplified interface for programmatic I/O and control

Advanced analytics (Gen III)Advanced analytics (Gen III) Micro-analyzersMicro-analyzers Integrated analysis or “smart” systemsIntegrated analysis or “smart” systems

Where Does NeSSI™ Fit in the LabWhere Does NeSSI™ Fit in the Lab

Instrument/Sensor InterfacesInstrument/Sensor Interfaces Design standards make development simplerDesign standards make development simpler

Reduced toolset to be masteredReduced toolset to be masteredReduced sample variability to account forReduced sample variability to account for

Calibration/validation built-inCalibration/validation built-inConsistent physical environment for measurementConsistent physical environment for measurementStream switching and/or mixing allow generation of standards to match Stream switching and/or mixing allow generation of standards to match analytical requirementsanalytical requirements

Reaction monitoringReaction monitoring Microreactors and continuous flow reactorsMicroreactors and continuous flow reactors Batch reactors (with fast loop)Batch reactors (with fast loop)

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

The NeSSI Could Become the Base for The NeSSI Could Become the Base for a Micro-Analytical Laba Micro-Analytical Lab

‘A DEVELOPMENT PLATFORM’‘A DEVELOPMENT PLATFORM’

NeSSI with an Array of Micro-NeSSI with an Array of Micro-Analytical Techniques will Impact Analytical Techniques will Impact

Many IndustriesMany Industries

Process ControlProcess Control

Process Process OptimizationOptimization

Product Product DevelopmentDevelopment

Sensing TechnologiesSensing Technologies

Gas ChromatographyGas Chromatography Thermal Desorption (Thermal Desorption (??))

Dielectric (Dielectric (√√))SpectroscopiesSpectroscopies IR (IR (++)), NIR (, NIR (++)) UV- Vis (UV- Vis (++)) Raman (Raman (√√)) Fluorescence (Fluorescence (++))

Impedance (Impedance (++))Conductivity (Conductivity (√√))Refractive Index (Refractive Index (√√))

Vapochromic SensorsVapochromic Sensors ( (++))GLRSGLRS ( (++))Particle SizingParticle Sizing Light scattering (Light scattering (??))

TurbidityTurbidity ( (++))pHpH ( (√√))RGARGA ( (++))

Mass SpectrometryMass Spectrometry ( (√√))

LC, SEC, ICLC, SEC, IC ( (++))

Terrahertz Terrahertz ((??))

NeSSI™:NeSSI™: Enabler for MicroAnalyticalEnabler for MicroAnalytical

(the “rail” concept)(the “rail” concept)

Standard Mechanical Interface “Rail”

Standard Electrical (Digital) Interface “Rail”

Anyone’s Sensor Anyone’s Actuator

SAM*

Standard “hockey-puckPC”

P

V

*Sensor/Actuator Manager

Standard“connectivit

y”

What technologies are availableSuitability for modular sampling systems

Phased Micro Gas AnalyzerPhased Micro Gas Analyzer

Substrate Substrate

On/Off and On/Off and Modulating valvesModulating valves

Flow Sensor w/ Flow Sensor w/ Temp, Pressure Temp, Pressure w/ Tempw/ Temp

Substrate

Moisture in Moisture in Dry GasesDry Gases

PHASED *PHASED * Micro GC Micro GC

Other Analytical:Other Analytical:Ion, Nox. OIon, Nox. O2, 2, pHpHConductivity, Conductivity, NOx, Turbidity,NOx, Turbidity,Density, OpacityDensity, OpacityRefractive Index,Refractive Index,OthersOthers

ChemometricChemometricSensors for Sensors for Complex AnalyticalComplex AnalyticalMeasurements.Measurements.

ModValve

D/A

Network

Press/Temp

A/D

Network

*PHASED: Courtesy of Honeywell

PHASED microGCPHASED microGC

MICRO-GC MICRO-GC SLSSLSGCM 5000GCM 5000

< 20 W Power< 20 W Power

3 x 2 x 0.6 inches3 x 2 x 0.6 inches

100 gm / 3 oz.100 gm / 3 oz.

www.slsmt.comwww.slsmt.com

V

ABB Natural Gas ChromatographABB Natural Gas Chromatograph

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)

Dimensions: 6.75“ dia. × 16'' long × 9.00'' tallWeight: Approximately 28 lb. (12.7 Kg)

Siemens microSAM GCSiemens microSAM GC

Valveless live injection with Valveless live injection with software-adjustable injection software-adjustable injection volume volume Maintenance-free column Maintenance-free column switching and electronic switching and electronic pressure control pressure control Accurate measuring results by Accurate measuring results by multiple parallel micro-multiple parallel micro-detectorsdetectorsCan be mounted directly at the Can be mounted directly at the sample extraction point sample extraction point because only a single auxiliary because only a single auxiliary gas and very little electrical gas and very little electrical power is required power is required Simple remote control with Simple remote control with Windows-based software and Windows-based software and Ethernet communicationEthernet communication

Agilent 3000 Micro GCAgilent 3000 Micro GCCustom configurations with 1 to 4 Custom configurations with 1 to 4 replaceable chromatographic replaceable chromatographic channels. Choose from various micro-channels. Choose from various micro-machined injectors, columns, sample machined injectors, columns, sample conditioners, and application-specific conditioners, and application-specific reports. reports. The modular GC design maximizes The modular GC design maximizes uptime, with repair as simple as uptime, with repair as simple as exchanging one module for another. exchanging one module for another. Increase sensitivity, maintain high Increase sensitivity, maintain high precision, remove unwanted precision, remove unwanted contaminants from your sample, or contaminants from your sample, or speed up analysis with variable, fixed speed up analysis with variable, fixed or backflush injection options. or backflush injection options. Digital pneumatics control carrier gas Digital pneumatics control carrier gas flow electronically, enhancing flow electronically, enhancing reliability and precision while further reliability and precision while further simplifying operation.simplifying operation.

Dimensions: 5.9” x 9.8” x 16.1” Wt: 18 – 37 lbs (portable)

Applied Analytics Inc. Diode Array Applied Analytics Inc. Diode Array

OMA-300 OMA-300 A  Fiber-optics-diode-A  Fiber-optics-diode-array process analyzerarray process analyzerFor on-line concentration For on-line concentration monitoringmonitoring

Applied Analytics Microspec IRApplied Analytics Microspec IR

FEATURESFEATURES

Ideal for monitoring Ideal for monitoring PPM PPM level level WATER WATER in various solventsin various solvents

In stream quantitative measurementsIn stream quantitative measurements

Contains no moving parts andContains no moving parts and

Extremely robust allowing for Extremely robust allowing for installations in process stream installations in process stream environmentsenvironments

Replaces analyzers such as process Replaces analyzers such as process spectrometers in the process plant.spectrometers in the process plant.

NeSSI IR Gas CellNeSSI IR Gas Cell

Removable TipVersion

Sentelligence Current NIR SensorsSentelligence Current NIR Sensors

- NIR Sensors

IR Microsystems Microarray 64 IR Microsystems Microarray 64

                                                                                                                                                                                                            Board Dimensions: 66 x 53 Board Dimensions: 66 x 53 mm mm 22

     

Wilks Enterprise InfraSpec Variable Filter Array

Agilent NeSSI Dielectric SensorAgilent NeSSI Dielectric Sensor

Cable to Agilent

Network Analyzer

Swagelok 2-Port

Valve Base

Dielectric Probe

Inner Body

O-ring (insid

e)

Outer Body

Exploded View

Close up of

Coaxial Probe

Tip

Liquid Chromatography for NeSSI™Liquid Chromatography for NeSSI™

micromixer

diluent in

column

mobile phase in

sample in

Scott Gilbert, CPAC Visiting ScholarScott Gilbert, CPAC Visiting ScholarCrystal Vision Microsystems LLCCrystal Vision Microsystems LLCAtofluidic Technologies, LLCAtofluidic Technologies, LLC

Split flow approach to samplingSplit flow approach to sampling

-fluidic LC Chip for On-line -fluidic LC Chip for On-line Sample PretreatmentSample Pretreatment

Pulsed electrochemical Pulsed electrochemical

detection (on-chip)detection (on-chip)

Liters per minute

microliters per minute

nanoliters per minute

Aspectrics EP-IR with Gas CellAspectrics EP-IR with Gas Cell

Glow source

Gas cell

Spectrometer

15”

7”

5.2”

Interfacing NeSSI™ to ASI Interfacing NeSSI™ to ASI micromicroFast GCFast GC™™

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

GC sipper port

EP-IR gas cell

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

CPAC Funded Technology CPAC Funded Technology DevelopmentsDevelopments

Development of a Micro-NMR System

NMR spectrum of a 3 micro liter NMR spectrum of a 3 micro liter water sample using a RF micro-coilwater sample using a RF micro-coilM. McCarthy, UC Davis

Spreeta SPR sensing componentsSpreeta SPR sensing components

Each Spreeta chip contains all of the optical components needed for sensitive SPR measurement of biomolecular interactions

SPIRIT system performs SPR SPIRIT system performs SPR detection using Texas detection using Texas Instruments’ Spreeta SPR Instruments’ Spreeta SPR chipschips

Chips are mass-produced by Chips are mass-produced by TI, cost ~$4 in large quantitiesTI, cost ~$4 in large quantities

Each chip can perform three Each chip can perform three simultaneous measurementssimultaneous measurements

Systems contain 8 chips, for Systems contain 8 chips, for 24 total sensing channels24 total sensing channels

Clem Furlong, et al, UW

Fringing Field Dielectric NeSSI SensorFringing Field Dielectric NeSSI Sensor

Alex Mamishev EE and Marquardt CPAC, UW

Raman/NIR/UV-Vis Sensor ModuleRaman/NIR/UV-Vis Sensor Module

NeSSI Raman Sampling BlockNeSSI Raman Sampling Block

• Reactor NeSSI substrate• Sample conditioning to induce

backpressure to reduce bubble formation and the heated substrate allows analysis at reactor conditions

PtOPtO22 NeSSI Sensor NeSSI Sensor

Fiber optic cable to Ocean Optics

Spectrometer

Swagelok 2-Port

Valve Base

Fiber-optic

Probe(405 nm LED)

Inner Body

O-ring (insid

e)

Outer Body

Exploded View

Close up of Outer Body Tip

VapochromicTip

Calibrated Gas GenerationCalibrated Gas Generation

Application of Permeation ApparatusApplication of Permeation Apparatus

AcknowledgmentsAcknowledgmentsCenter for Process Analytical ChemistryCenter for Process Analytical Chemistry

Students – Charles Branham and Wes Thompson, UWStudents – Charles Branham and Wes Thompson, UW

Professor Kent Mann, Univ. of MinnesotaProfessor Kent Mann, Univ. of Minnesota

Clem Furlong – UW Medical GeneticsClem Furlong – UW Medical Genetics

Mike McCarthy and group – UC DavisMike McCarthy and group – UC Davis

Scott Gilbert – UW Visiting scholarScott Gilbert – UW Visiting scholar

Swagelok, Parker and Circor Swagelok, Parker and Circor

ABB, Agilent, Aspectrics, Honeywell, ExxonMobilABB, Agilent, Aspectrics, Honeywell, ExxonMobil