brian marquardt and dave veltkamp applied physics laboratory center for process analytical chemistry...
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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