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Advanced Gas Measurement of Bio-Pharma Processes

IFPAC 2004 Presentation

January 15, 2004

Advanced Gas Measurement of Bio-Pharma Processes

IFPAC 2004 Presentation

January 15, 2004

Ronald R. Rich, PresidentRonald R. Rich, PresidentAtmosphere Recovery, Inc.Atmosphere Recovery, Inc.

15800 32nd Avenue North, Suite 11015800 32nd Avenue North, Suite 110Plymouth, MN 55447Plymouth, MN 55447

Ph: (763) 557-8675 Fax: (763) 557-8668Ph: (763) 557-8675 Fax: (763) 557-8668Web: www.atmrcv.com E-mail: rrr@atmrcv.comWeb: www.atmrcv.com E-mail: rrr@atmrcv.com

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Company BackgroundCompany Background

Founded 1994Founded 1994 - Dana Corporation & DOE R&D - Dana Corporation & DOE R&D Heat Treating Furnace ProcessesHeat Treating Furnace Processes Grant & Contract FundingGrant & Contract Funding

1995-19981995-1998 - Process Gas Recycling System - Process Gas Recycling System Development Development

1997-20001997-2000 - Laser Raman Gas Analyzer & - Laser Raman Gas Analyzer & Gas Processing Development Gas Processing Development

2000-20012000-2001 – Analyzer/Controller Field Trials – Analyzer/Controller Field Trials 2002- 2002- – Furnace Analyzer Offerings – Furnace Analyzer Offerings 2003- 2003- – Bio-Pharma Analyzer Offerings – Bio-Pharma Analyzer Offerings

Significant Process Industries - Gas Based

Significant Process Industries - Gas Based

Metal Processing – Initial SuccessMetal Processing – Initial Success Automotive & Aerospace Heat TreatingAutomotive & Aerospace Heat Treating Metal Refining & Powdered MetalMetal Refining & Powdered Metal

Many Others – Ready for TrialsMany Others – Ready for Trials Bio-PharmaBio-Pharma PetrochemicalPetrochemical SemiconductorSemiconductor Energy UtilitiesEnergy Utilities Glass & CeramicGlass & Ceramic Continuous Emission MonitoringContinuous Emission Monitoring

Bio-Pharma Process Goals – General

Bio-Pharma Process Goals – General

Lower Production CostsLower Production Costs Higher Productivity and Product YieldsHigher Productivity and Product Yields Reduced Feedstock UseReduced Feedstock Use Improved Consistency & QualityImproved Consistency & Quality Capital Avoidance (Lower Vessel Numbers)Capital Avoidance (Lower Vessel Numbers)

Other FactorsOther Factors New Processes & MaterialsNew Processes & Materials Lower Analyzer Cost of OperationLower Analyzer Cost of Operation Reduced Process Air Emissions & EnergyReduced Process Air Emissions & Energy

12 Month Payback (Max.)12 Month Payback (Max.)

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Process Gas Conceptual Needs –Process Gas Conceptual Needs –Better Control, Less UseBetter Control, Less UseProcess Gas Conceptual Needs –Process Gas Conceptual Needs –Better Control, Less UseBetter Control, Less Use

Off-Line Analysis

High Use (H)

Std. Infrared Adds Control Med. Use (M)

Complete Gas Control/Reuse

Low Use (L)

Biological Process Reactor

Feedstock Liquids &

Solids

Process Gases

(O2) and Liquids (Vapors)

Off Gases & VaporsAnalysis & ControlAnalysis & Control

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Metal Processing Gases – Similar Constituents

Metal Processing Gases – Similar Constituents

Carburizing, Carbonitriding, FNC & NitridingCarburizing, Carbonitriding, FNC & Nitriding NN22, CO, H, CO, H22, CO, CO22, H, H22O, CHO, CH44, O, O22, NH, NH33, CH, CH33OHOH

Atmosphere Tempering and Annealing Atmosphere Tempering and Annealing NN22, H, H22, CO, CO, CO, CO22, H, H22O, CHO, CH44, O, O22, NH, NH33, Ar , Ar

Steel, Copper and Aluminum BrazingSteel, Copper and Aluminum Brazing NN22, H, H22, CO, CO, CO, CO22, H, H22O, CHO, CH44, O, O22, NH, NH33, Ar , Ar

Powdered Metal Sintering and AnnealingPowdered Metal Sintering and Annealing HH22, N, N22, CO, CO, CO, CO22, H, H22O, CHO, CH44, O, O22,, NHNH33, H, H22SS

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Bio-Pharma Off-Gas Applications –Similar Needs

Bio-Pharma Off-Gas Applications –Similar Needs

COCO22, O, O22, - Routinely Sampled, - Routinely Sampled

NN22, H, H22, NH, NH33 – Sometimes Desired Now – Sometimes Desired Now

Organic Vapors – Very ImportantOrganic Vapors – Very Important Alcohols, Ketones, Aldehydes, Etc. Alcohols, Ketones, Aldehydes, Etc.

Other Inorganics – Determine Rates Other Inorganics – Determine Rates S, N, P and Other CompoundsS, N, P and Other Compounds

Water Vapor – Determines BalanceWater Vapor – Determines Balance

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Typical Process Gas Control - Measures Only One or Two Species

Typical Process Gas Control - Measures Only One or Two Species

Example TypesExample Types Paramagnetic Oxygen Probe – Measures OxygenParamagnetic Oxygen Probe – Measures Oxygen Infrared – Measures Carbon DioxideInfrared – Measures Carbon Dioxide Electrochemical Cells – Low Range Single GasesElectrochemical Cells – Low Range Single Gases Thin Film Technologies – Too Many InterferencesThin Film Technologies – Too Many Interferences

BenefitsBenefits Proven Technology (Typically)Proven Technology (Typically) Lower Capital Cost Lower Capital Cost Low Complexity? (Two Analyzers Needed)Low Complexity? (Two Analyzers Needed)

DisadvantagesDisadvantages Other Gas Constituents Assumed (Guessed)Other Gas Constituents Assumed (Guessed) Assumptions Often WrongAssumptions Often Wrong Least Accurate Process Control OptionLeast Accurate Process Control Option Limits Process Control Options & ImprovementsLimits Process Control Options & Improvements

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Improved Process Gas Control –Absorption-Based Optical (IR)

Improved Process Gas Control –Absorption-Based Optical (IR)

Can Measure Multiple Gas SpeciesCan Measure Multiple Gas Species Carbon DioxideCarbon Dioxide MethaneMethane Alcohols (Some)Alcohols (Some) Ketones (Maybe)Ketones (Maybe) Aldehydes (?)Aldehydes (?)

BenefitsBenefits Proven Technology and VendorsProven Technology and Vendors Can be Used to Reduce Feedstock Use SomewhatCan be Used to Reduce Feedstock Use Somewhat

DisadvantagesDisadvantages Cannot Measure Diatomics (OCannot Measure Diatomics (O22, H, H22, N, N22, Etc.), Etc.) Detectors Have Limited Measurement RangeDetectors Have Limited Measurement Range Requires Frequent CalibrationRequires Frequent Calibration Species Measurement Has Significant OverlapSpecies Measurement Has Significant Overlap Restricts Optimal ControlRestricts Optimal Control

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Other Gas Analysis Technologies –Higher Cost of Ownership

Other Gas Analysis Technologies –Higher Cost of Ownership

Gas Chromatography (GC)Gas Chromatography (GC) High Installed Capital Cost ($25,000 - $60,000+)High Installed Capital Cost ($25,000 - $60,000+) Slow (2 Minutes+)Slow (2 Minutes+) Complex – Use Requires TrainingComplex – Use Requires Training Carrier Gas and Frequent CalibrationCarrier Gas and Frequent Calibration Laboratory and Petrochemical Processes PredominateLaboratory and Petrochemical Processes Predominate

Mass Spectroscopy (MS)Mass Spectroscopy (MS) Higher Capital Cost ($50,000 - $120,000)Higher Capital Cost ($50,000 - $120,000) Requires Vacuum PumpRequires Vacuum Pump Gas Mixtures Often Require Second Analysis MethodGas Mixtures Often Require Second Analysis Method Ionizer Susceptible to Water DamageIonizer Susceptible to Water Damage Expensive Sampling SystemExpensive Sampling System Expensive to MaintainExpensive to Maintain

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Ultimate Process Control Goal –Practical Complete Gas AnalyzerUltimate Process Control Goal –Practical Complete Gas Analyzer Measure All Reactive Gas SpeciesMeasure All Reactive Gas Species Detector Range - Low PPM to 100%Detector Range - Low PPM to 100% Work with Elevated Sample TemperaturesWork with Elevated Sample Temperatures Fast ResponseFast Response Compact and Operator FriendlyCompact and Operator Friendly Rugged, Reliable, Easy to ServiceRugged, Reliable, Easy to Service Minimal CalibrationMinimal Calibration Low Cost of OwnershipLow Cost of Ownership Potential for MiniaturizationPotential for Miniaturization

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Unique Frequency “Shift” for Each Chemical BondUnique Frequency “Shift” for Each Chemical Bond Little Interference Between Most GasesLittle Interference Between Most Gases Measures Gases of All Types (Except Inerts)Measures Gases of All Types (Except Inerts) Rapid “Real Time” Response Rates PossibleRapid “Real Time” Response Rates Possible Signal Directly Proportional to Number of Gas Atoms Signal Directly Proportional to Number of Gas Atoms PPM-100% Gas Concentrations with One DetectorPPM-100% Gas Concentrations with One Detector Resolution and Accuracy Depends On:Resolution and Accuracy Depends On:

Laser Power and Optics Variation Laser Power and Optics Variation Gas Concentration and PressureGas Concentration and Pressure Molecular Bond TypeMolecular Bond Type Background and Scattered RadiationBackground and Scattered Radiation Optical and Electronic Detector CircuitryOptical and Electronic Detector Circuitry

Laser Raman Gas Spectroscopy - Features

Laser Raman Gas Spectroscopy - Features

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Core of Laser Gas Control – Unique 8 Gas Detector Module

Core of Laser Gas Control – Unique 8 Gas Detector Module

Mirror Polarizer Prism & Mirror

Laser BeamGas Sample Tube

Gas Out

8 Optical Filters/Sensors (1 for Each Gas Measured)

Detector AssemblyDetector Assembly

Gas Out

Special Particle Filter

Plasma Cell

Gas to be Analyzed In

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Detector Module Features Detector Module Features Internal Cavity-Based RamanInternal Cavity-Based Raman

Low Power Laser (Helium-Neon Plasma)Low Power Laser (Helium-Neon Plasma) Sample Gas Flows Through InstrumentSample Gas Flows Through Instrument Higher Inherent AccuracyHigher Inherent Accuracy

Discrete Optical Filtering and QuantifyingDiscrete Optical Filtering and Quantifying Any 8 Gases Detected Per ModuleAny 8 Gases Detected Per Module Process Specific Configurations & Module #s Process Specific Configurations & Module #s Simultaneous Detection of All Gas SpeciesSimultaneous Detection of All Gas Species Fast Detector Updates (50 milliseconds)Fast Detector Updates (50 milliseconds) Only High Nitrogen Dioxide Levels InterfereOnly High Nitrogen Dioxide Levels Interfere Array Based Interference Computations Array Based Interference Computations

10 Minute Module Exchange10 Minute Module Exchange

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Typical Gas Constituents Monitored and Detection Limits

Typical Gas Constituents Monitored and Detection Limits

Gas Species Lower Limit

Hydrogen - H2 10-50 ppm*

Nitrogen - N2 50 ppm

Oxygen - O2 50 ppm

Water Vapor - H2O 10-50 ppm*

Carbon Monoxide - CO 50 ppm

Carbon Dioxide - CO2 25 ppm

Organics - CxHy 10-50 ppm*

Ammonia - NH3 10-50 ppm*

*Customer Selectable – Selecting Lower Value Limits The Upper Range to 30%; Other Gas Species Substitutable as Options

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Gas Analyzer – Current SubsystemGas Analyzer – Current Subsystem

Detector AssemblyDetector Assembly

Integrated ComputerIntegrated Computer& Control System& Control System

Sample Pump, ValvesSample Pump, Valvesand Pressure Controland Pressure Control

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Subsystem FeaturesSubsystem Features Integrated Sampling and Calibration SystemIntegrated Sampling and Calibration System

Internal Pump and ValvesInternal Pump and Valves Low Volume Sample Gas Flows (200 ml/minute) Low Volume Sample Gas Flows (200 ml/minute) Multiple Sample Port OptionsMultiple Sample Port Options Automated Zero and Span CalibrationAutomated Zero and Span Calibration Automated Sample Line Monitoring (Flow & Pressure)Automated Sample Line Monitoring (Flow & Pressure)

Integrated Electronics & SoftwareIntegrated Electronics & Software Pentium III Computer w/ HMI and Data TrendingPentium III Computer w/ HMI and Data Trending Customizable Process Deviation AnalysisCustomizable Process Deviation Analysis Local and Remote Displays and InterfacesLocal and Remote Displays and Interfaces OPC Server and Client for ConnectivityOPC Server and Client for Connectivity Available Analog and Digital I/O OptionsAvailable Analog and Digital I/O Options Multiple Configurable Process and PLC InterfacesMultiple Configurable Process and PLC Interfaces

NeSSI Integration NowNeSSI Integration Now NeSSI Generation II Potential NeSSI Generation II Potential

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Example Main Control ScreenExample Main Control Screen

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Remote Analyzer/Controller – 4 Port Bio-Pharma Product

Remote Analyzer/Controller – 4 Port Bio-Pharma Product

Model 4FM Fermentation

Off-Gas Analyzer

Inside ViewInside ViewOutside ViewOutside View

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Mobile Process Audit Analyzer – 4 Samples, 8 Pressures, 8 Temperatures

Mobile Process Audit Analyzer – 4 Samples, 8 Pressures, 8 Temperatures

Bio-Pharma Commissioning

Performance Problem Resolution

Advanced Control Demonstration and Testing

ARI ConsultingService

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Analyzer/Controller – Eight Gases, Four Process Tanks

Analyzer/Controller – Eight Gases, Four Process Tanks

Inside ViewInside ViewOutside ViewOutside View

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Analyzer/Controller – 16 Gases, 16 Process Tanks

Analyzer/Controller – 16 Gases, 16 Process Tanks

Inside ViewInside ViewOutside ViewOutside View

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Products Integrate Sampling System & Fully Automated Operation

Products Integrate Sampling System & Fully Automated Operation

Fully Integrated Sample System (1-16 Ports) “Real Time” On-Line Monitoring and Control

(1 to 15 Second to Update Each Sample Location)

Operates with Existing PLCs and Sensors Low Volume Sample Gas Flows (200 ml/minute) Electronic Flow and Pressure Monitoring Optics Protection and Enclosure Inerting Sample Line Pre-Purge and Back-flush Options Automatic Condensate Removal Precision Temp. Controlled NEMA Enclosures Self-Monitoring of Critical Functions Many Wired and Wireless Communication Options

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Economic Benefits of High-SpeedGas Process Analysis and ControlEconomic Benefits of High-SpeedGas Process Analysis and Control Multiple Gas Analysis Capability

= System Versatility

Economic Paybacks in Many Ways Increase Production Capacity Improve Product Quality Improve Product Consistency Reduce Analysis Costs Reduce Instrumentation and Control Reduce Instrumentation and Control

ComplexityComplexity Reduce Lost Batch Costs Better Process Documentation Maintenance Early Warnings Enhanced Process Safety Reduce Energy Costs

DependsDependson Systemon SystemFunctionsFunctions

UsedUsed

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Thank You For ListeningThank You For Listening

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