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