application of nessi to fundamental measurements for modeling and process development michelle j....
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Application of NeSSI to Application of NeSSI to Fundamental Measurements for Fundamental Measurements for
Modeling and Process DevelopmentModeling and Process Development
Michelle J CohnMichelle J Cohn
uop uop LLCLLC
copy 2004 UOP LLC All Rights Reserved
UOP LLC Who We AreUOP LLC Who We Are Global company with Global company with
11 manufacturing sites 11 manufacturing sites and offices in 25 countriesand offices in 25 countries
More than 3000 highly trained More than 3000 highly trained employeesemployees
90 years of innovative solutions for 90 years of innovative solutions for the hydrocarbon processing the hydrocarbon processing industryindustry
UOPrsquos customers are located in UOPrsquos customers are located in more than 200 countries more than 200 countries
Worldrsquos largest supplier of Worldrsquos largest supplier of molecular sieve adsorbentsmolecular sieve adsorbents
What We DoWhat We Do Develop technology that Develop technology that
provides solutions to problemsprovides solutions to problems License design engineerLicense design engineer
and service process technologyand service process technology Develop and manufacture Develop and manufacture
catalysts molecular sieves catalysts molecular sieves adsorbents and specialized adsorbents and specialized equipmentequipment
Transfer technology to Transfer technology to customers who achieve high customers who achieve high yield of high quality productsyield of high quality products
Some Process Development NeedsSome Process Development Needs- Reaction Kinetics- Reaction Kinetics
CH3
CH3
H+
CH3
CH3
CH3
CH3
+2
RTEa
PMA
R
PMA
Aek
PPK
KP
PKk
r
2
2
2 1
Needs for Fundamental Understanding-
Decision for Process Intensification
bull Reaction mechanismpathwaysReaction mechanismpathwaysbull Kinetic constantsKinetic constants - adsorption constant - adsorption constant - activation energy - activation energy - heats of adsorption - heats of adsorption - pre-exponentials - pre-exponentials
Some Process Development NeedsSome Process Development Needs- Reaction Fundamentals- Reaction Fundamentals
Bimolecular Reaction Pathways
Monomolecular Reaction Pathways
Needs for Fundamental Understanding
bull Reaction mechanismpathwaysReaction mechanismpathways
Some Process Development NeedsSome Process Development Needs- Other Parameters- Other Parameters
Needs for Fundamental Understanding
bull Reaction mechanismpathwaysReaction mechanismpathwaysbull Kinetic constantsKinetic constants - adsorption constant - adsorption constant - activation energy - activation energy - heats of adsorption - heats of adsorption - pre-exponentials - pre-exponentialsbull DiffusionDiffusionbull DeactivationDeactivation
Application to Process Intensification
Applying Atmospheric MicroreactorsApplying Atmospheric Microreactors
o -Xylene Isomerization
0102030405060708090
100
350 400 450 500
Temperature (C)
o-X
Co
nv
ers
ion
(w
t)
Sample A Sample B
EQuilibrium
062
0625
063
0635
064
0645
065
0655
066
0665
300 350 400 450 500
T(C)
(k1 m
Xlt
=gt
pX)
(k2 o
Xlt
=gt
mX
)
Activity Comparison Kinetic Modeling of Data
Catalyst screeningQuality controlCatalyst modification
Insight into mechanistic changesFirst pass at kinetic constants - Activation Energy - Pre-exponential - Adsorption ConstantsEnsure proper process conditions
Temperature Scanning Reactor Temperature Scanning Reactor (TSR)Methodology(TSR)Methodology
Feed Product
Fractional Catalyst Volum e ----gt
Feed
Fractional Catalyst Volum e ----gt
Product
Desired Information
Measure ConversionThroughout Reactor
Rate = FdXdVRate = FdXdV----gt Rate = FdXdTaugt Rate = FdXdTau
Information from Typical Reactivity Test
ldquoI know what I put in and I know what I got outrdquo
Modeling TSR Data
Feed 4
TSRModeling Methodologybull Handles wide range of feeds and conditionsbull Incorporates deactivationbull Uses fundamental constants
Possible Impactsbull Differentiating materialsbull Incorporate into yield estimatingbull Help focus pilot plant test conditions
Feed 3
Feed 2Feed 1
Process Analytical Technology (PAT)Process Analytical Technology (PAT)
Diversity in process conditions for all unit operationsbull Continuous Modeling Neededbull Diversity in phase microstructure particle characteristicsbull Applied to synthesis preparation testing and characterization bull Requires detailed characterization
design monitoring control and modeling design monitoring control and modeling of materials and process conditionsof materials and process conditions
PAT in Heterogeneous Catalysis Product and Process Control
Very similar to Pharma Needs
NIRNIR FTIRFTIR QMSQMS RAMANRAMAN GCGC
UltrasoundUltrasound
LAMIMSLAMIMS
Micro-calorimetryMicro-calorimetry
FTIRFTIR
EtcEtc
Enablers for PATEnablers for PAT
Online Online ProcessProcess
AnalyticsAnalytics
Data Analysis
ModelBuilding
SamplingFeedbackFeedbackControlControl
Reactor
SensorT
Time
NESSI
VTP
A
PS
NESSI
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
UOP LLC Who We AreUOP LLC Who We Are Global company with Global company with
11 manufacturing sites 11 manufacturing sites and offices in 25 countriesand offices in 25 countries
More than 3000 highly trained More than 3000 highly trained employeesemployees
90 years of innovative solutions for 90 years of innovative solutions for the hydrocarbon processing the hydrocarbon processing industryindustry
UOPrsquos customers are located in UOPrsquos customers are located in more than 200 countries more than 200 countries
Worldrsquos largest supplier of Worldrsquos largest supplier of molecular sieve adsorbentsmolecular sieve adsorbents
What We DoWhat We Do Develop technology that Develop technology that
provides solutions to problemsprovides solutions to problems License design engineerLicense design engineer
and service process technologyand service process technology Develop and manufacture Develop and manufacture
catalysts molecular sieves catalysts molecular sieves adsorbents and specialized adsorbents and specialized equipmentequipment
Transfer technology to Transfer technology to customers who achieve high customers who achieve high yield of high quality productsyield of high quality products
Some Process Development NeedsSome Process Development Needs- Reaction Kinetics- Reaction Kinetics
CH3
CH3
H+
CH3
CH3
CH3
CH3
+2
RTEa
PMA
R
PMA
Aek
PPK
KP
PKk
r
2
2
2 1
Needs for Fundamental Understanding-
Decision for Process Intensification
bull Reaction mechanismpathwaysReaction mechanismpathwaysbull Kinetic constantsKinetic constants - adsorption constant - adsorption constant - activation energy - activation energy - heats of adsorption - heats of adsorption - pre-exponentials - pre-exponentials
Some Process Development NeedsSome Process Development Needs- Reaction Fundamentals- Reaction Fundamentals
Bimolecular Reaction Pathways
Monomolecular Reaction Pathways
Needs for Fundamental Understanding
bull Reaction mechanismpathwaysReaction mechanismpathways
Some Process Development NeedsSome Process Development Needs- Other Parameters- Other Parameters
Needs for Fundamental Understanding
bull Reaction mechanismpathwaysReaction mechanismpathwaysbull Kinetic constantsKinetic constants - adsorption constant - adsorption constant - activation energy - activation energy - heats of adsorption - heats of adsorption - pre-exponentials - pre-exponentialsbull DiffusionDiffusionbull DeactivationDeactivation
Application to Process Intensification
Applying Atmospheric MicroreactorsApplying Atmospheric Microreactors
o -Xylene Isomerization
0102030405060708090
100
350 400 450 500
Temperature (C)
o-X
Co
nv
ers
ion
(w
t)
Sample A Sample B
EQuilibrium
062
0625
063
0635
064
0645
065
0655
066
0665
300 350 400 450 500
T(C)
(k1 m
Xlt
=gt
pX)
(k2 o
Xlt
=gt
mX
)
Activity Comparison Kinetic Modeling of Data
Catalyst screeningQuality controlCatalyst modification
Insight into mechanistic changesFirst pass at kinetic constants - Activation Energy - Pre-exponential - Adsorption ConstantsEnsure proper process conditions
Temperature Scanning Reactor Temperature Scanning Reactor (TSR)Methodology(TSR)Methodology
Feed Product
Fractional Catalyst Volum e ----gt
Feed
Fractional Catalyst Volum e ----gt
Product
Desired Information
Measure ConversionThroughout Reactor
Rate = FdXdVRate = FdXdV----gt Rate = FdXdTaugt Rate = FdXdTau
Information from Typical Reactivity Test
ldquoI know what I put in and I know what I got outrdquo
Modeling TSR Data
Feed 4
TSRModeling Methodologybull Handles wide range of feeds and conditionsbull Incorporates deactivationbull Uses fundamental constants
Possible Impactsbull Differentiating materialsbull Incorporate into yield estimatingbull Help focus pilot plant test conditions
Feed 3
Feed 2Feed 1
Process Analytical Technology (PAT)Process Analytical Technology (PAT)
Diversity in process conditions for all unit operationsbull Continuous Modeling Neededbull Diversity in phase microstructure particle characteristicsbull Applied to synthesis preparation testing and characterization bull Requires detailed characterization
design monitoring control and modeling design monitoring control and modeling of materials and process conditionsof materials and process conditions
PAT in Heterogeneous Catalysis Product and Process Control
Very similar to Pharma Needs
NIRNIR FTIRFTIR QMSQMS RAMANRAMAN GCGC
UltrasoundUltrasound
LAMIMSLAMIMS
Micro-calorimetryMicro-calorimetry
FTIRFTIR
EtcEtc
Enablers for PATEnablers for PAT
Online Online ProcessProcess
AnalyticsAnalytics
Data Analysis
ModelBuilding
SamplingFeedbackFeedbackControlControl
Reactor
SensorT
Time
NESSI
VTP
A
PS
NESSI
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
What We DoWhat We Do Develop technology that Develop technology that
provides solutions to problemsprovides solutions to problems License design engineerLicense design engineer
and service process technologyand service process technology Develop and manufacture Develop and manufacture
catalysts molecular sieves catalysts molecular sieves adsorbents and specialized adsorbents and specialized equipmentequipment
Transfer technology to Transfer technology to customers who achieve high customers who achieve high yield of high quality productsyield of high quality products
Some Process Development NeedsSome Process Development Needs- Reaction Kinetics- Reaction Kinetics
CH3
CH3
H+
CH3
CH3
CH3
CH3
+2
RTEa
PMA
R
PMA
Aek
PPK
KP
PKk
r
2
2
2 1
Needs for Fundamental Understanding-
Decision for Process Intensification
bull Reaction mechanismpathwaysReaction mechanismpathwaysbull Kinetic constantsKinetic constants - adsorption constant - adsorption constant - activation energy - activation energy - heats of adsorption - heats of adsorption - pre-exponentials - pre-exponentials
Some Process Development NeedsSome Process Development Needs- Reaction Fundamentals- Reaction Fundamentals
Bimolecular Reaction Pathways
Monomolecular Reaction Pathways
Needs for Fundamental Understanding
bull Reaction mechanismpathwaysReaction mechanismpathways
Some Process Development NeedsSome Process Development Needs- Other Parameters- Other Parameters
Needs for Fundamental Understanding
bull Reaction mechanismpathwaysReaction mechanismpathwaysbull Kinetic constantsKinetic constants - adsorption constant - adsorption constant - activation energy - activation energy - heats of adsorption - heats of adsorption - pre-exponentials - pre-exponentialsbull DiffusionDiffusionbull DeactivationDeactivation
Application to Process Intensification
Applying Atmospheric MicroreactorsApplying Atmospheric Microreactors
o -Xylene Isomerization
0102030405060708090
100
350 400 450 500
Temperature (C)
o-X
Co
nv
ers
ion
(w
t)
Sample A Sample B
EQuilibrium
062
0625
063
0635
064
0645
065
0655
066
0665
300 350 400 450 500
T(C)
(k1 m
Xlt
=gt
pX)
(k2 o
Xlt
=gt
mX
)
Activity Comparison Kinetic Modeling of Data
Catalyst screeningQuality controlCatalyst modification
Insight into mechanistic changesFirst pass at kinetic constants - Activation Energy - Pre-exponential - Adsorption ConstantsEnsure proper process conditions
Temperature Scanning Reactor Temperature Scanning Reactor (TSR)Methodology(TSR)Methodology
Feed Product
Fractional Catalyst Volum e ----gt
Feed
Fractional Catalyst Volum e ----gt
Product
Desired Information
Measure ConversionThroughout Reactor
Rate = FdXdVRate = FdXdV----gt Rate = FdXdTaugt Rate = FdXdTau
Information from Typical Reactivity Test
ldquoI know what I put in and I know what I got outrdquo
Modeling TSR Data
Feed 4
TSRModeling Methodologybull Handles wide range of feeds and conditionsbull Incorporates deactivationbull Uses fundamental constants
Possible Impactsbull Differentiating materialsbull Incorporate into yield estimatingbull Help focus pilot plant test conditions
Feed 3
Feed 2Feed 1
Process Analytical Technology (PAT)Process Analytical Technology (PAT)
Diversity in process conditions for all unit operationsbull Continuous Modeling Neededbull Diversity in phase microstructure particle characteristicsbull Applied to synthesis preparation testing and characterization bull Requires detailed characterization
design monitoring control and modeling design monitoring control and modeling of materials and process conditionsof materials and process conditions
PAT in Heterogeneous Catalysis Product and Process Control
Very similar to Pharma Needs
NIRNIR FTIRFTIR QMSQMS RAMANRAMAN GCGC
UltrasoundUltrasound
LAMIMSLAMIMS
Micro-calorimetryMicro-calorimetry
FTIRFTIR
EtcEtc
Enablers for PATEnablers for PAT
Online Online ProcessProcess
AnalyticsAnalytics
Data Analysis
ModelBuilding
SamplingFeedbackFeedbackControlControl
Reactor
SensorT
Time
NESSI
VTP
A
PS
NESSI
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Some Process Development NeedsSome Process Development Needs- Reaction Kinetics- Reaction Kinetics
CH3
CH3
H+
CH3
CH3
CH3
CH3
+2
RTEa
PMA
R
PMA
Aek
PPK
KP
PKk
r
2
2
2 1
Needs for Fundamental Understanding-
Decision for Process Intensification
bull Reaction mechanismpathwaysReaction mechanismpathwaysbull Kinetic constantsKinetic constants - adsorption constant - adsorption constant - activation energy - activation energy - heats of adsorption - heats of adsorption - pre-exponentials - pre-exponentials
Some Process Development NeedsSome Process Development Needs- Reaction Fundamentals- Reaction Fundamentals
Bimolecular Reaction Pathways
Monomolecular Reaction Pathways
Needs for Fundamental Understanding
bull Reaction mechanismpathwaysReaction mechanismpathways
Some Process Development NeedsSome Process Development Needs- Other Parameters- Other Parameters
Needs for Fundamental Understanding
bull Reaction mechanismpathwaysReaction mechanismpathwaysbull Kinetic constantsKinetic constants - adsorption constant - adsorption constant - activation energy - activation energy - heats of adsorption - heats of adsorption - pre-exponentials - pre-exponentialsbull DiffusionDiffusionbull DeactivationDeactivation
Application to Process Intensification
Applying Atmospheric MicroreactorsApplying Atmospheric Microreactors
o -Xylene Isomerization
0102030405060708090
100
350 400 450 500
Temperature (C)
o-X
Co
nv
ers
ion
(w
t)
Sample A Sample B
EQuilibrium
062
0625
063
0635
064
0645
065
0655
066
0665
300 350 400 450 500
T(C)
(k1 m
Xlt
=gt
pX)
(k2 o
Xlt
=gt
mX
)
Activity Comparison Kinetic Modeling of Data
Catalyst screeningQuality controlCatalyst modification
Insight into mechanistic changesFirst pass at kinetic constants - Activation Energy - Pre-exponential - Adsorption ConstantsEnsure proper process conditions
Temperature Scanning Reactor Temperature Scanning Reactor (TSR)Methodology(TSR)Methodology
Feed Product
Fractional Catalyst Volum e ----gt
Feed
Fractional Catalyst Volum e ----gt
Product
Desired Information
Measure ConversionThroughout Reactor
Rate = FdXdVRate = FdXdV----gt Rate = FdXdTaugt Rate = FdXdTau
Information from Typical Reactivity Test
ldquoI know what I put in and I know what I got outrdquo
Modeling TSR Data
Feed 4
TSRModeling Methodologybull Handles wide range of feeds and conditionsbull Incorporates deactivationbull Uses fundamental constants
Possible Impactsbull Differentiating materialsbull Incorporate into yield estimatingbull Help focus pilot plant test conditions
Feed 3
Feed 2Feed 1
Process Analytical Technology (PAT)Process Analytical Technology (PAT)
Diversity in process conditions for all unit operationsbull Continuous Modeling Neededbull Diversity in phase microstructure particle characteristicsbull Applied to synthesis preparation testing and characterization bull Requires detailed characterization
design monitoring control and modeling design monitoring control and modeling of materials and process conditionsof materials and process conditions
PAT in Heterogeneous Catalysis Product and Process Control
Very similar to Pharma Needs
NIRNIR FTIRFTIR QMSQMS RAMANRAMAN GCGC
UltrasoundUltrasound
LAMIMSLAMIMS
Micro-calorimetryMicro-calorimetry
FTIRFTIR
EtcEtc
Enablers for PATEnablers for PAT
Online Online ProcessProcess
AnalyticsAnalytics
Data Analysis
ModelBuilding
SamplingFeedbackFeedbackControlControl
Reactor
SensorT
Time
NESSI
VTP
A
PS
NESSI
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Some Process Development NeedsSome Process Development Needs- Reaction Fundamentals- Reaction Fundamentals
Bimolecular Reaction Pathways
Monomolecular Reaction Pathways
Needs for Fundamental Understanding
bull Reaction mechanismpathwaysReaction mechanismpathways
Some Process Development NeedsSome Process Development Needs- Other Parameters- Other Parameters
Needs for Fundamental Understanding
bull Reaction mechanismpathwaysReaction mechanismpathwaysbull Kinetic constantsKinetic constants - adsorption constant - adsorption constant - activation energy - activation energy - heats of adsorption - heats of adsorption - pre-exponentials - pre-exponentialsbull DiffusionDiffusionbull DeactivationDeactivation
Application to Process Intensification
Applying Atmospheric MicroreactorsApplying Atmospheric Microreactors
o -Xylene Isomerization
0102030405060708090
100
350 400 450 500
Temperature (C)
o-X
Co
nv
ers
ion
(w
t)
Sample A Sample B
EQuilibrium
062
0625
063
0635
064
0645
065
0655
066
0665
300 350 400 450 500
T(C)
(k1 m
Xlt
=gt
pX)
(k2 o
Xlt
=gt
mX
)
Activity Comparison Kinetic Modeling of Data
Catalyst screeningQuality controlCatalyst modification
Insight into mechanistic changesFirst pass at kinetic constants - Activation Energy - Pre-exponential - Adsorption ConstantsEnsure proper process conditions
Temperature Scanning Reactor Temperature Scanning Reactor (TSR)Methodology(TSR)Methodology
Feed Product
Fractional Catalyst Volum e ----gt
Feed
Fractional Catalyst Volum e ----gt
Product
Desired Information
Measure ConversionThroughout Reactor
Rate = FdXdVRate = FdXdV----gt Rate = FdXdTaugt Rate = FdXdTau
Information from Typical Reactivity Test
ldquoI know what I put in and I know what I got outrdquo
Modeling TSR Data
Feed 4
TSRModeling Methodologybull Handles wide range of feeds and conditionsbull Incorporates deactivationbull Uses fundamental constants
Possible Impactsbull Differentiating materialsbull Incorporate into yield estimatingbull Help focus pilot plant test conditions
Feed 3
Feed 2Feed 1
Process Analytical Technology (PAT)Process Analytical Technology (PAT)
Diversity in process conditions for all unit operationsbull Continuous Modeling Neededbull Diversity in phase microstructure particle characteristicsbull Applied to synthesis preparation testing and characterization bull Requires detailed characterization
design monitoring control and modeling design monitoring control and modeling of materials and process conditionsof materials and process conditions
PAT in Heterogeneous Catalysis Product and Process Control
Very similar to Pharma Needs
NIRNIR FTIRFTIR QMSQMS RAMANRAMAN GCGC
UltrasoundUltrasound
LAMIMSLAMIMS
Micro-calorimetryMicro-calorimetry
FTIRFTIR
EtcEtc
Enablers for PATEnablers for PAT
Online Online ProcessProcess
AnalyticsAnalytics
Data Analysis
ModelBuilding
SamplingFeedbackFeedbackControlControl
Reactor
SensorT
Time
NESSI
VTP
A
PS
NESSI
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Some Process Development NeedsSome Process Development Needs- Other Parameters- Other Parameters
Needs for Fundamental Understanding
bull Reaction mechanismpathwaysReaction mechanismpathwaysbull Kinetic constantsKinetic constants - adsorption constant - adsorption constant - activation energy - activation energy - heats of adsorption - heats of adsorption - pre-exponentials - pre-exponentialsbull DiffusionDiffusionbull DeactivationDeactivation
Application to Process Intensification
Applying Atmospheric MicroreactorsApplying Atmospheric Microreactors
o -Xylene Isomerization
0102030405060708090
100
350 400 450 500
Temperature (C)
o-X
Co
nv
ers
ion
(w
t)
Sample A Sample B
EQuilibrium
062
0625
063
0635
064
0645
065
0655
066
0665
300 350 400 450 500
T(C)
(k1 m
Xlt
=gt
pX)
(k2 o
Xlt
=gt
mX
)
Activity Comparison Kinetic Modeling of Data
Catalyst screeningQuality controlCatalyst modification
Insight into mechanistic changesFirst pass at kinetic constants - Activation Energy - Pre-exponential - Adsorption ConstantsEnsure proper process conditions
Temperature Scanning Reactor Temperature Scanning Reactor (TSR)Methodology(TSR)Methodology
Feed Product
Fractional Catalyst Volum e ----gt
Feed
Fractional Catalyst Volum e ----gt
Product
Desired Information
Measure ConversionThroughout Reactor
Rate = FdXdVRate = FdXdV----gt Rate = FdXdTaugt Rate = FdXdTau
Information from Typical Reactivity Test
ldquoI know what I put in and I know what I got outrdquo
Modeling TSR Data
Feed 4
TSRModeling Methodologybull Handles wide range of feeds and conditionsbull Incorporates deactivationbull Uses fundamental constants
Possible Impactsbull Differentiating materialsbull Incorporate into yield estimatingbull Help focus pilot plant test conditions
Feed 3
Feed 2Feed 1
Process Analytical Technology (PAT)Process Analytical Technology (PAT)
Diversity in process conditions for all unit operationsbull Continuous Modeling Neededbull Diversity in phase microstructure particle characteristicsbull Applied to synthesis preparation testing and characterization bull Requires detailed characterization
design monitoring control and modeling design monitoring control and modeling of materials and process conditionsof materials and process conditions
PAT in Heterogeneous Catalysis Product and Process Control
Very similar to Pharma Needs
NIRNIR FTIRFTIR QMSQMS RAMANRAMAN GCGC
UltrasoundUltrasound
LAMIMSLAMIMS
Micro-calorimetryMicro-calorimetry
FTIRFTIR
EtcEtc
Enablers for PATEnablers for PAT
Online Online ProcessProcess
AnalyticsAnalytics
Data Analysis
ModelBuilding
SamplingFeedbackFeedbackControlControl
Reactor
SensorT
Time
NESSI
VTP
A
PS
NESSI
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Applying Atmospheric MicroreactorsApplying Atmospheric Microreactors
o -Xylene Isomerization
0102030405060708090
100
350 400 450 500
Temperature (C)
o-X
Co
nv
ers
ion
(w
t)
Sample A Sample B
EQuilibrium
062
0625
063
0635
064
0645
065
0655
066
0665
300 350 400 450 500
T(C)
(k1 m
Xlt
=gt
pX)
(k2 o
Xlt
=gt
mX
)
Activity Comparison Kinetic Modeling of Data
Catalyst screeningQuality controlCatalyst modification
Insight into mechanistic changesFirst pass at kinetic constants - Activation Energy - Pre-exponential - Adsorption ConstantsEnsure proper process conditions
Temperature Scanning Reactor Temperature Scanning Reactor (TSR)Methodology(TSR)Methodology
Feed Product
Fractional Catalyst Volum e ----gt
Feed
Fractional Catalyst Volum e ----gt
Product
Desired Information
Measure ConversionThroughout Reactor
Rate = FdXdVRate = FdXdV----gt Rate = FdXdTaugt Rate = FdXdTau
Information from Typical Reactivity Test
ldquoI know what I put in and I know what I got outrdquo
Modeling TSR Data
Feed 4
TSRModeling Methodologybull Handles wide range of feeds and conditionsbull Incorporates deactivationbull Uses fundamental constants
Possible Impactsbull Differentiating materialsbull Incorporate into yield estimatingbull Help focus pilot plant test conditions
Feed 3
Feed 2Feed 1
Process Analytical Technology (PAT)Process Analytical Technology (PAT)
Diversity in process conditions for all unit operationsbull Continuous Modeling Neededbull Diversity in phase microstructure particle characteristicsbull Applied to synthesis preparation testing and characterization bull Requires detailed characterization
design monitoring control and modeling design monitoring control and modeling of materials and process conditionsof materials and process conditions
PAT in Heterogeneous Catalysis Product and Process Control
Very similar to Pharma Needs
NIRNIR FTIRFTIR QMSQMS RAMANRAMAN GCGC
UltrasoundUltrasound
LAMIMSLAMIMS
Micro-calorimetryMicro-calorimetry
FTIRFTIR
EtcEtc
Enablers for PATEnablers for PAT
Online Online ProcessProcess
AnalyticsAnalytics
Data Analysis
ModelBuilding
SamplingFeedbackFeedbackControlControl
Reactor
SensorT
Time
NESSI
VTP
A
PS
NESSI
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Temperature Scanning Reactor Temperature Scanning Reactor (TSR)Methodology(TSR)Methodology
Feed Product
Fractional Catalyst Volum e ----gt
Feed
Fractional Catalyst Volum e ----gt
Product
Desired Information
Measure ConversionThroughout Reactor
Rate = FdXdVRate = FdXdV----gt Rate = FdXdTaugt Rate = FdXdTau
Information from Typical Reactivity Test
ldquoI know what I put in and I know what I got outrdquo
Modeling TSR Data
Feed 4
TSRModeling Methodologybull Handles wide range of feeds and conditionsbull Incorporates deactivationbull Uses fundamental constants
Possible Impactsbull Differentiating materialsbull Incorporate into yield estimatingbull Help focus pilot plant test conditions
Feed 3
Feed 2Feed 1
Process Analytical Technology (PAT)Process Analytical Technology (PAT)
Diversity in process conditions for all unit operationsbull Continuous Modeling Neededbull Diversity in phase microstructure particle characteristicsbull Applied to synthesis preparation testing and characterization bull Requires detailed characterization
design monitoring control and modeling design monitoring control and modeling of materials and process conditionsof materials and process conditions
PAT in Heterogeneous Catalysis Product and Process Control
Very similar to Pharma Needs
NIRNIR FTIRFTIR QMSQMS RAMANRAMAN GCGC
UltrasoundUltrasound
LAMIMSLAMIMS
Micro-calorimetryMicro-calorimetry
FTIRFTIR
EtcEtc
Enablers for PATEnablers for PAT
Online Online ProcessProcess
AnalyticsAnalytics
Data Analysis
ModelBuilding
SamplingFeedbackFeedbackControlControl
Reactor
SensorT
Time
NESSI
VTP
A
PS
NESSI
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Modeling TSR Data
Feed 4
TSRModeling Methodologybull Handles wide range of feeds and conditionsbull Incorporates deactivationbull Uses fundamental constants
Possible Impactsbull Differentiating materialsbull Incorporate into yield estimatingbull Help focus pilot plant test conditions
Feed 3
Feed 2Feed 1
Process Analytical Technology (PAT)Process Analytical Technology (PAT)
Diversity in process conditions for all unit operationsbull Continuous Modeling Neededbull Diversity in phase microstructure particle characteristicsbull Applied to synthesis preparation testing and characterization bull Requires detailed characterization
design monitoring control and modeling design monitoring control and modeling of materials and process conditionsof materials and process conditions
PAT in Heterogeneous Catalysis Product and Process Control
Very similar to Pharma Needs
NIRNIR FTIRFTIR QMSQMS RAMANRAMAN GCGC
UltrasoundUltrasound
LAMIMSLAMIMS
Micro-calorimetryMicro-calorimetry
FTIRFTIR
EtcEtc
Enablers for PATEnablers for PAT
Online Online ProcessProcess
AnalyticsAnalytics
Data Analysis
ModelBuilding
SamplingFeedbackFeedbackControlControl
Reactor
SensorT
Time
NESSI
VTP
A
PS
NESSI
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Process Analytical Technology (PAT)Process Analytical Technology (PAT)
Diversity in process conditions for all unit operationsbull Continuous Modeling Neededbull Diversity in phase microstructure particle characteristicsbull Applied to synthesis preparation testing and characterization bull Requires detailed characterization
design monitoring control and modeling design monitoring control and modeling of materials and process conditionsof materials and process conditions
PAT in Heterogeneous Catalysis Product and Process Control
Very similar to Pharma Needs
NIRNIR FTIRFTIR QMSQMS RAMANRAMAN GCGC
UltrasoundUltrasound
LAMIMSLAMIMS
Micro-calorimetryMicro-calorimetry
FTIRFTIR
EtcEtc
Enablers for PATEnablers for PAT
Online Online ProcessProcess
AnalyticsAnalytics
Data Analysis
ModelBuilding
SamplingFeedbackFeedbackControlControl
Reactor
SensorT
Time
NESSI
VTP
A
PS
NESSI
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
NIRNIR FTIRFTIR QMSQMS RAMANRAMAN GCGC
UltrasoundUltrasound
LAMIMSLAMIMS
Micro-calorimetryMicro-calorimetry
FTIRFTIR
EtcEtc
Enablers for PATEnablers for PAT
Online Online ProcessProcess
AnalyticsAnalytics
Data Analysis
ModelBuilding
SamplingFeedbackFeedbackControlControl
Reactor
SensorT
Time
NESSI
VTP
A
PS
NESSI
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Combinatorial VisionCombinatorial Vision
1 2 3
DiscoveryDiscovery Research Research(1000s of ideas)(1000s of ideas)
FocusFocus ResearchResearch(100s of ideas)(100s of ideas)
Successful Successful CommercialCommercial
OperationOperation (1 prototype)(1 prototype)
Catalyst PreparationCatalyst PreparationCatalyst TestingCatalyst Testing
ModelingModelingInformaticsInformatics
Process DevelopmentProcess Development (2-5 leads)(2-5 leads)
Combi is a Step in theTechnology Delivery Process
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Enablers of Combinatorial ChemistryEnablers of Combinatorial Chemistry Efficient ways of materials synthesisEfficient ways of materials synthesis Parallel preparation of experimental catalystsParallel preparation of experimental catalysts Availability and development of high-speed Availability and development of high-speed
characterization tools characterization tools Parallel and high throughput testing of catalytic Parallel and high throughput testing of catalytic
propertiesproperties Data analysis techniques - informaticsData analysis techniques - informatics
Accelerated processes of discovery andAccelerated processes of discovery and technology delivery technology delivery
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
High Throughput High Throughput Characterization ToolsCharacterization Tools
HT RamanHT RamanActive Site Active Site Phase IDPhase ID
LAMIMSLAMIMSReactivityReactivity
IR ThermographyIR ThermographyTPD AdsorptionTPD Adsorption
HT Adsorption HT Adsorption Surface Area PoreSurface Area PoreSize DistributionSize Distribution Full spectrum of toolsFull spectrum of tools
Ultra-fast collection timesUltra-fast collection times 100rsquos to 1000rsquos samples day100rsquos to 1000rsquos samples day
GoalsGoals
Characterization is Key to SuccessCharacterization is Key to SuccessFrom Data From Data
StructureFunction Models StructureFunction Models = Knowledge= Knowledge
HT XRDHT XRDStructuralStructuralPhase IDPhase ID
HT SEMHT SEMMorphology Particle SizeMorphology Particle Size
HT XRFHT XRFElementElementAnalysisAnalysis
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
High Throughput ScreeningLAMIMS
Laser Activated Membrane IntroductionMass Spectrometry
Micro reactivity test Closed environment (realistic catalyst
exposure) Very broad temperature application Full QMS product analysis Real world catalysts
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
The LAMIMS Screening System
System Components LAMIMS reactant delivery
system A 25 watt CO2 barcode writing
laser LAMIMS reactor Quadrupole mass spectrometer
(QMS) NeSSI reactant feed system
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
LAMIMS SystemLAMIMS System
Laser heats samplesLaser heats samples Large array of Large array of
samples in reactorsamples in reactor Mass spec monitors Mass spec monitors
product streamproduct stream Dehydrogenation test Dehydrogenation test
for metal activityfor metal activity
1000 samples tested per 1000 samples tested per dayday
MCH Toluene
Catalyst Spot
To QMA
Silicone Rubber MembraneHeat
Cartridge Well
Tripod Base
ZnSe window
flow distributor
Sample Inlet
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Data from Reactor System45 samples
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
The visionhellipThe visionhellip
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Applying NeSSI TechnologyApplying NeSSI Technology
Used Ethernet and DeviceNet networks and commercially available Gen I LabView software on PC for configuration control data and diagnostics Proved the need for low power small size actuators and valves Exceptional diagnostic control and data collection capabilities 1048708 Remote monitoring and control via standard internet tools 10487081048708 Fast and easy configuration using LabView
Honeywell sensors Parker Hannifin Intraflow
substrate and components GO pressure regulators Parker valves and actuators Brooks mass flow controllers
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Automated System Components DescriptionDescription
33 Device Net Flow controllersDevice Net Flow controllers
33 Back Pressure RegulatorsBack Pressure Regulators
22 4 port two position valves4 port two position valves
11 3 port two position valve3 port two position valve
6 6 24VDC bellows sealed 24VDC bellows sealed valvesvalves
6 6 Pressure IndicatorsPressure Indicators
3 3 Pressure reducing Pressure reducing regulatorsregulators
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
LAMIMS Gas Handling System Construction and Demonstration Accelerated with NeSSI
Mass Spectrometer installed Mass Spectrometer installed
Laser installedLaser installed
NESSI gas manifold installed NESSI gas manifold installed
Lab View Automation software completedLab View Automation software completed
Safety review completedSafety review completedResourcesResources WNeSSIWNeSSI TypicalTypical
Elapsed timeElapsed time 4months4months 6 months6 months
Personnel timePersonnel time 2months2months 4months4months
Manifold costManifold cost +10+10 baselinebaseline
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Second NESSI systemSecond NESSI system
Flexible system for gas conditioning sensor evaluation
Honeywell ParkerHoneywell Parker
IntegrationIntegration
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Some of the Current NESSI Control Some of the Current NESSI Control Systems at UOPSystems at UOP
LAMIMS system operating since March 2004LAMIMS system operating since March 2004ndash Thousands of samples tested- Thousands of samples tested- ndash No operational issuesNo operational issues
Samplingpretreatment system in use Samplingpretreatment system in use ndash Overall installed savings again about 30Overall installed savings again about 30
System using Swagelock modular system ldquoheatedrdquondash online hydrogen System using Swagelock modular system ldquoheatedrdquondash online hydrogen sensing systemsensing system
ndash Demonstrated in house Demonstrated in house New high pressure system for High throughput Hydrogen storage New high pressure system for High throughput Hydrogen storage
assay DOE project- Need to evaluate 50-100 samplesdayassay DOE project- Need to evaluate 50-100 samplesday- NESSI system besides providing automation can be reliably NESSI system besides providing automation can be reliably
shipped to and from our collaborator in Norway SINTEF for shipped to and from our collaborator in Norway SINTEF for - allows Sintef not only to test the final configuration but also test allows Sintef not only to test the final configuration but also test
and integrate the automation of this systemand integrate the automation of this system
WORKING PRESSURE is 1800psigWORKING PRESSURE is 1800psigSeveral other non-controlling systems in use at UOPSeveral other non-controlling systems in use at UOP
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
H2
To Desorb
To Glovebox
To Glovebox
Vent
N2
N2Ar
To Liquid N2 Dewar
Vent
1377rdquo
1912rdquo
LP
HPHP
HPHP
HP
HP
HP
HP
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Item Qty Description
2 IntraFlow standard pegboard w 6 mounting brackets
8Parker B series manual 2-way ball valve mini lever handle
5Parker CO series check valve specify cracking pressure
1 Parker HR series needle valve specify flow rate range
2Parker RL4 series relief valve specify cracking pressure range
1Parker SM930 NC pneumatic diaphragm valve (125psig max)
8Parker SM945 NC pneumatic diaphragm valve (3000psig max)
5Parker SMSQ pressure reducing regulator 3000 psig max inlet 0-250psig max outlet range
1 Porter rotometer w needle valve specify flow range
3Parker restricted orifice holder with standard orifice plate (sandwiched between fitting and surface mount device specify orifice size
9 Wika pressure indicator specify range
1 Honeywell pressure transmitter specify range
PI
LP
HP
PT
Ordered from Parker Honeywell Alliance- they are integrators
Again components from multiple vendors
Came in around 15 more in costsExpect savings in shakedown- also new capability of High Pressure
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
PAT SummaryPAT Summary
Technology and industry needs are converging for Technology and industry needs are converging for PAT and NESSIPAT and NESSI
ndash In-situ measurementsIn-situ measurements
ndash Sensor integrationSensor integration
ndash Computational capacity and modelsComputational capacity and models
ndash Understanding of mechanismsUnderstanding of mechanisms
Demonstrated success in refining and Demonstrated success in refining and petrochemicalspetrochemicals
Opportunities for cross-industry fertilizationOpportunities for cross-industry fertilization
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
Mechanism ToolsMechanism Tools
LAMIMSLAMIMS AtmAtmMRXMRX TSRTSR TEOMTEOM
TAPTAPPulsePulseMRXMRX
Reactivity Testing
ZLCZLC
CalorimetryCalorimetry Isotopic Isotopic LabelingLabeling
SSITKASSITKA
ProcessProcessModelModel
RxnRxnMechanismMechanism
Heat of AdsHeat of AdsCapacityCapacity
Number of Number of IntermediatesIntermediates
LifetimeLifetimeDiffusionDiffusion
Characterization
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-
NESSINESSIPATPAT
AdvancedAdvancedCharacterizationCharacterization InformaticsInformatics
SummarySummary
Enabling Step Changes In Technology Enabling Step Changes In Technology
Innovation and growth driven by enabler toolboxInnovation and growth driven by enabler toolbox Opportunities PAT and NESSIOpportunities PAT and NESSI
ndash Seek enhanced understanding of process variables and Seek enhanced understanding of process variables and relationship to performancerelationship to performance
Enabling technologies cut across industriesEnabling technologies cut across industries
- Application of NeSSI to Fundamental Measurements for Modeling and Process Development
- Slide 22
-