Advanced Gas Measurement of Bio-Pharma Processes IFPAC 2004 Presentation January 15, 2004

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Advanced Gas Measurement of Bio-Pharma Processes
IFPAC 2004 PresentationJanuary 15, 2004

• Ronald R. Rich, President
• Atmosphere Recovery, Inc.
• 15800 32nd Avenue North, Suite 110
• Plymouth, MN 55447
• Ph [phone] Fax [phone]
• Web www.atmrcv.com E-mail rrr_at_atmrcv.com

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Company Background

• Founded 1994 - Dana Corporation DOE RD
• Heat Treating Furnace Processes
• Grant Contract Funding
• 1995-1998 - Process Gas Recycling System
  Development
• 1997-2000 - Laser Raman Gas Analyzer
  Gas Processing Development
• 2000-2001 Analyzer/Controller Field Trials
• 2002- Furnace Analyzer Offerings
• 2003- Bio-Pharma Analyzer Offerings

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Significant Process Industries - Gas Based

• Metal Processing Initial Success
• Automotive Aerospace Heat Treating
• Metal Refining Powdered Metal
• Many Others Ready for Trials
• Bio-Pharma
• Petrochemical
• Semiconductor
• Energy Utilities
• Glass Ceramic
• Continuous Emission Monitoring

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Bio-Pharma Process Goals General

• Lower Production Costs
• Higher Productivity and Product Yields
• Reduced Feedstock Use
• Improved Consistency Quality
• Capital Avoidance (Lower Vessel Numbers)
• Other Factors
• New Processes Materials
• Lower Analyzer Cost of Operation
• Reduced Process Air Emissions Energy
• 12 Month Payback (Max.)

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Process Gas Conceptual Needs Better Control,
Less Use
Off Gases Vapors
Analysis Control
Feedstock Liquids Solids
Off-Line Analysis High Use (H)
Std. Infrared Adds Control Med. Use (M)
Biological Process Reactor
Process Gases (O2) and Liquids (Vapors)
Complete Gas Control/Reuse Low Use (L)
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Metal Processing Gases Similar Constituents

• Carburizing, Carbonitriding, FNC Nitriding
• N2, CO, H2, CO2, H2O, CH4, O2, NH3, CH3OH
• Atmosphere Tempering and Annealing
• N2, H2, CO, CO2, H2O, CH4, O2, NH3, Ar
• Steel, Copper and Aluminum Brazing
• N2, H2, CO, CO2, H2O, CH4, O2, NH3, Ar
• Powdered Metal Sintering and Annealing
• H2, N2, CO, CO2, H2O, CH4, O2, NH3, H2S

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Bio-Pharma Off-Gas Applications Similar Needs

• CO2, O2, - Routinely Sampled
• N2, H2, NH3 Sometimes Desired Now
• Organic Vapors Very Important
• Alcohols, Ketones, Aldehydes, Etc.
• Other Inorganics Determine Rates
• S, N, P and Other Compounds
• Water Vapor Determines Balance

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Typical Process Gas Control - Measures Only One
or Two Species

• Example Types
• Paramagnetic Oxygen Probe Measures Oxygen
• Infrared Measures Carbon Dioxide
• Electrochemical Cells Low Range Single Gases
• Thin Film Technologies Too Many Interferences
• Benefits
• Proven Technology (Typically)
• Lower Capital Cost
• Low Complexity? (Two Analyzers Needed)
• Disadvantages
• Other Gas Constituents Assumed (Guessed)
• Assumptions Often Wrong
• Least Accurate Process Control Option
• Limits Process Control Options Improvements

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Improved Process Gas Control Absorption-Based
Optical (IR)

• Can Measure Multiple Gas Species
• Carbon Dioxide
• Methane
• Alcohols (Some)
• Ketones (Maybe)
• Aldehydes (?)
• Benefits
• Proven Technology and Vendors
• Can be Used to Reduce Feedstock Use Somewhat
• Disadvantages
• Cannot Measure Diatomics (O2, H2, N2, Etc.)
• Detectors Have Limited Measurement Range
• Requires Frequent Calibration
• Species Measurement Has Significant Overlap
• Restricts Optimal Control

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Other Gas Analysis Technologies Higher Cost of
Ownership

• Gas Chromatography (GC)
• High Installed Capital Cost (25,000 - 60,000)
• Slow (2 Minutes)
• Complex Use Requires Training
• Carrier Gas and Frequent Calibration
• Laboratory and Petrochemical Processes
  Predominate
• Mass Spectroscopy (MS)
• Higher Capital Cost (50,000 - 120,000)
• Requires Vacuum Pump
• Gas Mixtures Often Require Second Analysis Method
• Ionizer Susceptible to Water Damage
• Expensive Sampling System
• Expensive to Maintain

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Ultimate Process Control Goal Practical
Complete Gas Analyzer

• Measure All Reactive Gas Species
• Detector Range - Low PPM to 100
• Work with Elevated Sample Temperatures
• Fast Response
• Compact and Operator Friendly
• Rugged, Reliable, Easy to Service
• Minimal Calibration
• Low Cost of Ownership
• Potential for Miniaturization

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Laser Raman Gas Spectroscopy - Features

• Unique Frequency Shift for Each Chemical Bond
• Little Interference Between Most Gases
• Measures Gases of All Types (Except Inerts)
• Rapid Real Time Response Rates Possible
• Signal Directly Proportional to Number of Gas
  Atoms
• PPM-100 Gas Concentrations with One Detector
• Resolution and Accuracy Depends On
• Laser Power and Optics Variation
• Gas Concentration and Pressure
• Molecular Bond Type
• Background and Scattered Radiation
• Optical and Electronic Detector Circuitry

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Core of Laser Gas Control Unique 8 Gas
Detector Module
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Detector Module Features

• Internal Cavity-Based Raman
• Low Power Laser (Helium-Neon Plasma)
• Sample Gas Flows Through Instrument
• Higher Inherent Accuracy
• Discrete Optical Filtering and Quantifying
• Any 8 Gases Detected Per Module
• Process Specific Configurations Module s
• Simultaneous Detection of All Gas Species
• Fast Detector Updates (50 milliseconds)
• Only High Nitrogen Dioxide Levels Interfere
• Array Based Interference Computations
• 10 Minute Module Exchange

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Typical Gas Constituents Monitored and Detection
Limits
Customer Selectable Selecting Lower Value
Limits The Upper Range to 30 Other Gas
Species Substitutable as Options
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Gas Analyzer Current Subsystem
Integrated Computer Control System
Detector Assembly
Sample Pump, Valves and Pressure Control
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Subsystem Features

• Integrated Sampling and Calibration System
• Internal Pump and Valves
• Low Volume Sample Gas Flows (200 ml/minute)
• Multiple Sample Port Options
• Automated Zero and Span Calibration
• Automated Sample Line Monitoring (Flow
  Pressure)
• Integrated Electronics Software
• Pentium III Computer w/ HMI and Data Trending
• Customizable Process Deviation Analysis
• Local and Remote Displays and Interfaces
• OPC Server and Client for Connectivity
• Available Analog and Digital I/O Options
• Multiple Configurable Process and PLC Interfaces
• NeSSI Integration Now
• NeSSI Generation II Potential

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Example Main Control Screen
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Remote Analyzer/Controller 4 Port Bio-Pharma
Product
Model 4FM Fermentation Off-Gas Analyzer
Inside View
Outside View
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Mobile Process Audit Analyzer 4 Samples, 8
Pressures, 8 Temperatures

• Bio-Pharma Commissioning
• Performance Problem Resolution
• Advanced Control Demonstration and Testing
• ARI Consulting
• Service

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Analyzer/Controller Eight Gases, Four Process
Tanks
Inside View
Outside View
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Analyzer/Controller 16 Gases, 16 Process Tanks
Inside View
Outside View
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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 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 Complexity
• Reduce Lost Batch Costs
• Better Process Documentation
• Maintenance Early Warnings
• Enhanced Process Safety
• Reduce Energy Costs

Depends on System Functions Used
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Thank You For Listening

• Looking for Demonstration Sites
• Looking for Technology, Marketing Financial
  Partners
• Brochures if Interested
• Questions?