February 2, 2012

Evolving Applications that Demonstrate the Value of the NeSSITM Platform

Sampling System Development for the Field and Laboratory

Process Analytical Systems: The Big Picture Sample Conditioning

Sample Disposal Vent Master™

Sample Extraction

Key System Performance

Information To Analyzer Network

Hub

Analyzer

Clean Gas DBB Probe Sample Transport

Heat Trace

R-Max™

Intertec (enclosure & heat)

Honeywell Alliance (pressure & flow sensing)

Gas Generators

Carrier & Cal Gas Delivery

Control

Sensor Monitoring

DCS/Unit Control

The Conventional Approach

3 Picture Courtesy ExxonMobil Chemical

Sample Conditioning Systems: * Custom designed, engineered and built * Lots of tubing/fittings * Many man-hours designing/building it * Lots of discrete components Cost Issue – Irritates the Bean Counters

* Typically not Smart (Smart = knowing if p,t,f of sample are normal, i.e. validating representative sample)

“Quality of Measurement Issue” - Credibility of analysis

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

• Standardized flow components • “Mix-and-match” compatibility between vendors • Growing list of components

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

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

What Is NeSSI? New Sample/Sensor Initiative

Gen I: Fluid Handling Systems Mostly Mechanical Components

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Gen II: Electrically Networked Systems

IS Serial Bus, miniTransducers, local wireless

Gen III: Microanalytical

Systems Platform for microAnalytical, remote

wireless, advanced gas & liquid sensors

NeSSITM – Modular Sampling System Initiative: Technology Roadmap

Modular Component Suppliers

6 Parker - IntraflowTM

Swagelok Circor

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Modular Hardware Functionality • Three Suppliers: Parker, Swagelok and Circor • Parker Design Incorporates a Taper connection between substrates • Swagelok Design Utilizes a channeled tube design • Circor Design models Swagelok but uses welded joint connections

Parker Intraflow

Swagelok

Circor

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IntraflowTM Parker Modular (NeSSITM) Systems: Gen I Foundation of Modular Approach

Slip-fit intra-fitting connectors

Same screw size throughout

ISA/ANSI SP76.00.02 Compliant

Mounting “Pegboard”

Field connectors (top or end)

Same plane flowpaths

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•Design Drivers • Simplicity Overcomes Limitations

IntraFlow™ Fitting IntraFlow™ System

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IntraflowTM Substrates/Flowpath Options: The Library is Has Become Much Larger to Accommodate

Laboratory and Process Applications (over 100 flow options)

IntraFlow™ Fitting

Modular Sampling System “Tool Box”

• Full range of valves (Library) • Full range of pressure control hardware • Flow control – Volumetric and Mass • Flow/Pressure Monitoring (Local/Remote) • Temperature Control – Convective/Conductive • Sample Eductors/Pumps • Sample Cylinders • Analytical Systems (pH, Cond., O2, GC, RAMAN, FTIR, etc.)

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"When men got structural steel, they did not use

it to build steel copies of wooden bridges."

Ayn Rand. Atlas Shrugged. 1957.

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Modular System vs. Conventional Tubing

Conventional Flow System

Modular System Applications: Where and How are They Used?

• Typical process analyzer sample conditioning applications – liquids and gases (HF non-SP76 standard system to accommodate higher viscosity liquids)

• Fluidic control for laboratory and R&D reaction systems • Mixing/blending of standard gases for supplying variable

concentration ranges • Platform for supplying controlled sample to on-board

analytical systems – Gen. III • Implementation of gas purifying hardware • Sample conditioning upstream of bench-top analytical

systems

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IntraflowTM Process Sample Conditioning

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Complete smart sample system integration

• Mono-ethylene glycol liquid service • Flow & pressure sensing • Conductive heating • Conventional grab sample & system functionalities

10-Stream Natural Gas BTU Analysis System

• Coalescing & Membrane Separator Drain Header • Restricted Orifice Header Pressure Control • Freeze Protection Heating • Sample pressure 1,500 – 3,000psig

High Pressure Applications

Common Drain

NeSSI™ and Raman Probe Reactor Application

NeSSI™ Sampling System for Reactor

Raman Probe

monitor

bypass

clean

NeSSITM and MicroReactor Performance Analysis

19 U.S. Food and Drug Administration

0 500 1000 1500 2000 2500 3000 35000

0.2

0.4

0.6

0.8

1

1.2

Raman Shift (cm-1)

No

rmal

ized

Inte

nsi

ty (

Arb

. Un

its)

Normalized Standard Spectra

Courtesy of Brian Marquardt

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NeSSITM :Reactor Monitoring and Control

Upstream reactor control and monitoring

Product monitoring

Micro Reactor Fluid Control with IntraflowTM

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Courtesy of Brian Marquardt – UW APL

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Sampling, Vaporization and Injection Integrated

6-port VICI Valve and Actuator

Parker Vaporizing Regulator

Remote Stream Isolation

Pre-heated carrier gas

To GC

Advantage of NeSSI:

Helium

Reactor Feed 1

Reactor Feed 2

Product Stream

Real-time Calibration

waste

prod

Analyzer Suite

Pump 1

Pump 2

NeSSITM Reactor Sampling/Calibration

• Application of sampling systems and analytics to optimize and control reactor

Small-Scale Lab Fermenter Applications

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1 Liter Fermentation Vessel

Pump for liquid recirculation

Parker IntraflowTM for Fluidic Control and Sensor Interface

BioTech Applications: On-line Fermenter Monitoring

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• Hardware used to transport, control and manage fluidic delivery to the analytical system • Calibration media also mounted to hardware and engineered to deliver calibration gas to GC

Integration of Sophisticated Analytics to Modular Sampling Systems

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RAMAN Probe

Analytical Probe-Based Measurement on ISA SP76 Platforms

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H2 Measurement

Parker IntraflowTM – A Platform for Experimentation

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• R&D Sensors for Experimentation • Simple fluid control hardware implemented easily • Complete flexibility for changing flow and pressure

Custom R&D Sensor

Courtesy of Brian Marquardt – UW APL

NeSSITM SP76 and Transportable Analytical Applications

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Courtesy of Carl Rechsteiner - Chevron

MicroGC (Falcon Analytical) with IntraflowTM Sample Conditioning System Mobile Unit with Support Equipment Mounted

NeSSITM Lab Calibration/Dilution System with On-board Analytics

30 Real-time monitoring of pressure, flow and component concentration

Courtesy of Brian Marquardt – UW APL

• Easy removal of heat exchanger

Patent Pending

Conventional Sample Extraction Modularized

Intraflow™ Vaporizing Regulator • CFD modeling of the

vaporizer indicates that room temp water vaporizes at around 80% through the heat exchanger

°C

Number of Tetrahedral Elements = .42 million Pressure Inlet: 25 psi Pressure outlet : 5 psi Temperature input to aluminum block: 190 oC All other external walls are considered as adiabatic walls Fluid: Water Solver: Segregated 3D steady solver with SIMPLE pressure-velocity coupling with standard k-e turbulence model.

Location of Post

Processing Plane

°C°C

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Calibration from NeSSITM -Permeation Tube System

Conceptual Design

Alternative Prototype Testing

4000 3800 3600 3400 3200 3000 2800 2600 2400 2200 2000-5

0

5

10

15

20x 10-3

Wavenumber (cm-1)

Ab

sorb

ance

(A

rbit

rary

Un

its)

Flow Rate Results: Ethanol Permeation Tube Trial

H2O

Ethanol CO2

As Flow Rate Increases the Signal Decrease

10 mL/min

60 mL/min

4000 3800 3600 3400 3200 3000 2800 2600 2400 2200 2000-2

-1

0

1

2

3

4

5x 10-3

Wavenumber (cm-1)

Ab

sorb

ance

(A

rbit

rary

Un

its)

H2O Ethanol

CO2

As Temp Decreases the Signal Decreases

85˚C

65˚C

Temperature Range Test: Ethanol Permeation Tube Trial

Sample Introduction Flexibility for microAnalytics is Available

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Inject valves for GC or LC

Dilution/Mixing Systems

Expensive Blended Gas Cylinder (H2S, CH4, CO, CO2, etc.) $$$$

Pure gas cylinders $

Gas Calibration System – Yields blended gas cylinder results

Analytics – GC, FTIR, O2, etc.

The NeSSITM Platform Accommodates Sampling ‘At The Process Extraction Point’

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Astute System with C2V Micro GC and H2Scan hydrogen analyzer

Courtesy of E.I.F (www.eif-filters.com)

microGC H2 Sensor

NeSSITM: ‘Clean’ Sampling?

Courtesy of Brian Marquardt – UW APL

Sterilization Method Sterilized Sterile Water Rinse ~ 500mL 120 °C for 15 min

Filled Sterile growth media is pumped by head pressure of compressed gas

Incubated 37°C for 72 hours

Swabbed Substrates sampled onto bacterial streak plates

Courtesy of Brian Marquardt – UW APL

Growth Study

1. End piece (Start Flow) 2. Valve substrate 1 3. Substrate 3 4. Top mount 3 5. Substrate 4 6. Substrate 5 7. Valve substrate 6 8. End piece (End Flow)

1

2 3 5 7 4 6

8

contaminated

Note: Contamination only found in starting and ending components. Most likely due to insufficient sterilization of the sealing caps placed during incubation.

Courtesy of Brian Marquardt – UW APL

• Demonstrated sterilization of NeSSI components • Possibly contaminated by residual cells trapped in threads of end

caps • Steam sterilization is a valid method of sterilization for NeSSI

components • O-rings and tubing are compatible with autoclave conditions • Ensures a sterile flow path without exposing external parts to hot

and humid conditions • Next step – Top mount components

• Sterilization of top mount components will be dependent on the materials and flow path of the components themselves

• Next step – Full integration to NeSSI System • Integrate rinse stream and boiler system to NeSSI fast loop

sampling system • Create digital control system for automatic sterilization

What may be Concluded?

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Gen I: Fluid Handling Systems Mostly Mechanical Components

Gen II: Electrically Networked Systems

IS Serial Bus, miniTransducers, local wireless

Gen III: Microanalytical

Systems Platform for microAnalytical, remote

wireless, advanced gas & liquid sensors

NeSSITM – Modular Sampling System Initiative

Sensors for NeSSI

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Pressure Transmitters: • Dwyer (Series 626) • Ashcroft (Series A2X, A4) • GE Sensing (PTX1200,DPS4000) • Brooks Instruments (SS2 series) • SensorsONE (PD33X,DMP331i) • Mensor (series 6000) • StellarTech (GTX2511)

Flow Controllers: • Porter Instruments (3261) • Brooks model (SLA5850) • Horiba (STEC) (SEC-G100) • Sierra Instruments • MKS Instruments • Alicat Scientific (316L MCS/MCRS)

Area Classification: • Intrinsically Safe • Intrinsically safe, Class I Div. II • Class I Div. II, Class I Div. I, IS, GP • Class I Div. II • GP and IS • GP • Class I Div I & II

Area Classification: • Class I Div. II • Class I Div. II • GP • GP • GP • Class I Div. II, ATEX

Signal Output: • 4-20mA • 4-20mA • 4-20mA, RS485, CanBus • 4-20mA • 4-20mA, RS-485, USB • RS-485 • RS-232, RS485, CanBus

Signal Output: • 0-10vdc, 4-20mA • 0-5vdc,4-20mA, RS485, DeviceNet, Profibus • 0-5vdc, DeviceNet •0-5vdc, DeviceNet •0-5vdc, DeviceNet • 0-5vdc, 4-20mA, RS-232, RS-485, DeviceNet, Profibus

Flow Meters: • Porter Instruments (3261) • Brooks (SLA5850) • FCI (FS10A (FM, FS)) • Sierra Instruments • MKS Instruments • Alicat Scientific (M Series)

Signal Output: • 4-20mA • 0-5vdc,4-20mA, RS485, DeviceNet, Profibus • 4-20mA • 4-20mA • 4-20mA • 0-5vdc, 4-20mA, RS-232, RS-485, DeviceNet, Profibus

Area Classification: • Class I Div. II • Class I Div. II • Class I Div. II • GP • GP • Class I Div. II, ATEX

Parker: Sensor, Analyzer, Valve Actuation Management

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SAM Valve Control Valve “On/Off” Indication

Ethernet Comm.

Gen II Model Architecture

Future Modular Sampling Hardware Developments for the Lab and Process Markets?

• Mixing Systems – Liquid and Gas Dynamic/Static

• Permeation/Calibration Hardware • Inject Valve Integration for Microanalytics • Solvent Delivery System • Modified Interface Hardware for RAMAN,

FTIR, pH and other probe-based analytics • Alternative Material Applications - PEEK

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Acknowledgments

• Brian Marquadt, Charlie Branham, Wes Thompson, Michael Roberto, Lauren Hughs and Thomas Dearing– Applied Physics Laboratory University of Washington

• Kin – Tek Laboratories • CPAC –University of Washington

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Thank You!!