Advanced Gas Measurement of Bio-Pharma Processes IFPAC 2004

Advanced Gas Measurement of Bio-Pharma Processes IFPAC 2004 Presentation January 15, 2004 Ronald R. Rich, President Atmosphere Recovery, Inc. 15800 32 nd Avenue North, Suite 110 Plymouth, MN 55447 Ph: (763) 557 -8675 Fax: (763) 557 -8668 Web: www. atmrcv. com E-mail: rrr@atmrcv. com 1

Company Background ® Founded 1994 - Dana Corporation & DOE R&D ® 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 2

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

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. )

Process Gas Conceptual Needs – Better Control, Less Use Feedstock Liquids & Solids Process Gases (O 2) and Liquids (Vapors) Analysis & Control Off-Line Analysis High Use (H) Std. Infrared Adds Control Med. Use (M) Complete Gas Control/Reuse Low Use (L) Off Gases & Vapors Biological Process Reactor 5

Metal Processing Gases – Similar Constituents ® Carburizing, Carbonitriding, FNC & Nitriding ® N 2, CO, H 2, CO 2, H 2 O, CH 4, O 2, NH 3, CH 3 OH ® Atmosphere Tempering and Annealing ® N 2, H 2, CO 2, H 2 O, CH 4, O 2, NH 3, Ar ® Steel, Copper and Aluminum Brazing ® N 2, H 2, CO 2, H 2 O, CH 4, O 2, NH 3, Ar ® Powdered Metal Sintering and Annealing ® H 2, N 2, CO 2, H 2 O, CH 4, O 2, NH 3, H 2 S 6

Bio-Pharma Off-Gas Applications – Similar Needs ® CO 2, - Routinely Sampled ® N 2, H 2, NH 3 – 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 7

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 8

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 (O 2, H 2, N 2, Etc. ) ® Detectors Have Limited Measurement Range ® Requires Frequent Calibration ® Species Measurement Has Significant Overlap ® Restricts Optimal Control 9

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 10

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 11

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 12

Core of Laser Gas Control – Unique 8 Gas Detector Module Gas to be Analyzed In Special Particle Filter 8 Optical Filters/Sensors (1 for Each Gas Measured) Detector Assembly Plasma Cell Mirror Polarizer Gas Sample Tube Laser Beam Prism & Mirror Gas Out 13

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 14

Typical Gas Constituents Monitored and Detection Limits Gas Species Hydrogen - H 2 Nitrogen - N 2 Oxygen - O 2 Water Vapor - H 2 O Carbon Monoxide - CO Carbon Dioxide - CO 2 Organics - Cx. Hy Ammonia - NH 3 Lower Limit 10 -50 ppm* 50 ppm 25 ppm 10 -50 ppm* *Customer Selectable – Selecting Lower Value Limits The Upper Range to 30%; Other Gas Species Substitutable as Options 15

Gas Analyzer – Current Subsystem Integrated Computer & Control System Detector Assembly Sample Pump, Valves and Pressure Control 16

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 Ne. SSI Integration Now ® Ne. SSI Generation II Potential ® 17

Example Main Control Screen 18

Remote Analyzer/Controller – 4 Port Bio-Pharma Product Model 4 FM Fermentation Off-Gas Analyzer Outside View Inside View 19

Mobile Process Audit Analyzer – 4 Samples, 8 Pressures, 8 Temperatures ® Bio-Pharma Commissioning ® Performance Problem Resolution ® Advanced Control Demonstration and Testing ® ARI Consulting Service 20

Analyzer/Controller – Eight Gases, Four Process Tanks Outside View Inside View 21

Analyzer/Controller – 16 Gases, 16 Process Tanks Outside View Inside View 22

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 23

Economic Benefits of High-Speed Gas Process Analysis and Control ® Multiple Gas Analysis Capability = System Versatility ® Economic Paybacks in Many Ways ® Increase Production Capacity Depends ® Improve Product Quality on System ® Improve Product Consistency ® Reduce Analysis Costs Functions ® Reduce Instrumentation and Control Used Complexity ® Reduce Lost Batch Costs ® Better Process Documentation ® Maintenance Early Warnings ® Enhanced Process Safety ® Reduce Energy Costs 24

Thank You For Listening ® Looking for Demonstration Sites ® Looking for Technology, Marketing & Financial Partners ® Brochures if Interested ® Questions? 25