1. 1 Enhanced Rate Chemical Processing Using Non-equilibrium Reactions Controlled with High Speed Gas Analysis IFPAC 2004 Presentation January 14, 2004 Ronald R. Rich, President Atmosphere Recovery, Inc. 15800 32nd Avenue North, Suite 110 Plymouth, MN 55447 Ph: (763) 557-8675 Fax: (763) 557-8668 Web: www.atmrcv.com E-mail: rrr@atmrcv.com

2. 2 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

3. Manufacturing Process Goals – General  Lower Production Costs  Higher Productivity and Yields  Improved Quality  Capital Avoidance  Reduced Feedstock & Energy Use  Other Factors  New Processes & Materials  Lower Analyzer Cost of Operation  Reduced Process Air Emissions  12 Month Payback (Max.)

4. 4 Process Gas Conceptual Needs – Better Control, Less Use Fixed Flow or Single Gas High Use (H) Std. Multi-Gas Adds Control Med. Use (M) Complete Gas Control/Reuse Low Use (L) Gas- Based Process Reactor Natural Gas and Liquid Fuels Process Gases and Liquids (Vapors) Waste Gas Amounts H M L

5. 5 Metal Processing Atmospheres – 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, CO 2, H 2 O, CH 4, O 2, NH 3, Ar  Steel, Copper and Aluminum Brazing  N 2, H 2, CO, CO 2, H 2 O, CH 4, O 2, NH 3, Ar  Powdered Metal Sintering and Annealing  H 2, N 2, CO, CO 2, H 2 O, CH 4, O 2, NH 3, H 2 S

6. 6 Typical Atmosphere Control - Measures Only One Gas Species  Types  Zirconia Oxygen Probe – Measures Oxygen  Dew Point Meters – Measures Water Vapor  Electrochemical Cells – Low Range Single Gases  Benefits  Proven Technology  Lower Capital Cost  Low Complexity  Disadvantages  Other Gas Constituents Assumed (Guessed)  Assumptions Often Wrong  Limits Process Control & Improvement Options  Requires High Process Atmosphere Flows

7. 7 Improved Atmosphere Control – Single Gas Plus Infra-Red  Economically Measures Three More Gases  Carbon Monoxide  Carbon Dioxide  Methane  Benefits  Proven Technology and Vendors  Can be Used to Reduce Atmosphere Use  Disadvantages  Cannot Measure Hydrogen, Nitrogen and Inerts  Expensive to Measure Other Significant Gases  Limited Measurement Range  Requires Frequent Calibration  Limits High Efficiency Atmosphere Gas Mixtures  Can’t Significantly Reduce Atmosphere Use

8. 8 Other Gas Analysis Technologies – Less Applicable to Atmospheres  Gas Chromatography (GC)  High Installed Capital Cost ($15,000 - $60,000)  Slow (2 Minutes+)  Complex – Use Requires Training  Carrier Gas and Frequent Calibration  Few Used for Atmosphere Control  Mass Spectroscopy (MS)  Higher Installed Capital Cost ($50,000 - $120,000)  Best Applied on Vacuum Processes  Ionizer Susceptible to Water Damage  Expensive to Maintain  Many Gases Hard to Determine (Equal Charge-Mass)

9. 9 Atmosphere Control Goal – High-Rate Complete Gas Analyzer  Measure All Reactive Gases  Monitor Any Industrial Atmosphere  Fast Analyzer Response  Compact and Operator Friendly  Rugged, Reliable, Easy to Service  Minimal Calibration  Cost-Effective  Allows Advanced Atmosphere Control

10. 10  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 Laser Raman Gas Spectroscopy - Features

11. 11 Core of Laser Gas Control – Unique 8 Gas Detector Mirror Polarizer Prism & Mirror Laser Beam Gas Sample Tube Gas Out 8 Optical Filters/Sensors (1 for Each Gas Measured) Detector Assembly Gas Out Special Particle Filter Plasma Cell Gas to be Analyzed In

12. 12 Laser Gas Detector Module – Features  Low Power Laser Insures Safety  Sample Gas Flows Analyzed Inside Instrument for Higher Inherent Accuracy  Discrete Optical Filtering and Quantifying  8 Gases Detected – Can be Process Specific  Simultaneous Detection of Each Gas Species  Fast Detector Response (50 milliseconds)  Array Based Interference Computations  Most Cost-Effective Approach

13. 13 Standard Furnace Constituents Monitored and Detection Limits Gas SpeciesLower Limit Hydrogen - H 2 10-50 ppm* Nitrogen - N 2 50 ppm Oxygen - O 2 50 ppm Water Vapor - H 2 O10-50 ppm* Carbon Monoxide - CO50 ppm Carbon Dioxide - CO 2 25 ppm Organics - C x H y 10-50 ppm* Ammonia - NH 3 10-50 ppm* *Customer Selectable – Selecting Lower Value Limits The Upper Range to 30%; Other Gas Species Optional

14. 14 Gas Analyzer – Subsystem View Detector Assembly Integrated Computer & Control System Sample Pump, Valves and Pressure Control

15. 15 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 Compatible

16. 16 Example Main Control Screen

17. 17 Mobile Furnace Process Control – 4 Samples, 8 Pressures, 8 Temperatures  Furnace Tuning & Commissioning  Furnace Performance Problem Resolution  Advanced Atmosphere Demonstration and Testing  ARI/APCI Consulting Service

18. 18 Advanced Carburizing Control – 2 Batch Furnaces Inside View Outside View

19. 19 Analyzer/Controller – 16 Zone Continuous Furnace Inside View Outside View

20. 20 Current Product Integrates Sampling System & Added Features  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

21. 21 Economic Benefits of Laser Gas Atmosphere Analysis and Control  Multiple Gas Analysis Capability = System Versatility  Economic Paybacks in Many Ways  Reduce Energy Costs  Increase Production Capacity  Improve Component Quality  Improve Component Consistency  Reduce Destructive Analysis Costs  Reduce Re-Work Costs  Better Process Documentation  Maintenance Early Warnings  Enhanced Furnace Safety Depends on System FunctionsUsed

22. 22 Rapid Carburizing and Atmosphere Recovery Demonstrated at Dana

23. 23 System Location in Plant “Explosion Resistant” Test Area “Explosion Resistant” Test Area

24. 24  Improves Steel Wear Resistance on Part Surfaces  Maintains Steel “Toughness” at Part Depth  Parts Heated in a Gas “Atmosphere”  Atmosphere Provides Reactive Chemistry Typical Parts (Gears) Typical Furnace (Batch) Carburizing Use & Purpose

25. 25 Traditional Carburizing Atmosphere Endogas Air Natural Gas Composition: CO~20%, N 2 ~39%, H 2 ~39%, 1% CH 4, Balance: CO 2, H 2 O, O 2 At Metal Surface: 2H 2 +2CO+3Fe  Fe 3 C+2H 2 O+CO 2 3Fe+CH 4  Fe 3 C+2H 2 Exhaust Stack

26. 26 Typical Carburizing Operation (Slow - Approaches Equilibrium)

27. 27 Benefits of Laser Gas Analysis - Conventional Heat Treating  Atmosphere Gas Consumption Reduced Endothermic Example – 90%+ Exothermic Example – 50%+  Extra Gas Generators Turned Off  Shorter Cycle Times Inherent Carburizing Example – Up to 20%  Process Energy Savings Significant Carburizing Example – 25% of Total Furnace Use Exothermic Example – 15% of Total Furnace Use

28. 28 Example 96% Endo Savings Surface Combustion All-Case Furnace (Shown Under Standard Operation) Stack and Flare Shut Off Door and Burner Leaks Reduced

29. 29 Initial Demonstration – Atmosphere Recovery Process IR-GC First - Later Laser Gas Analyzer

30. 30 Atmosphere Recovery – Prototype System  Prototype Development, Assembly and Testing  First Full Scale Operation - Aug. 6, 1997  Finding - Process Worked and Increased Productivity IR-GC (Later Replaced by Laser Analyzer)

31. 31 ARI Effluent Control System Detector Module & Controller Sampling System (Composition, Pressure & Temperature) ARI Pressure Control & Safety System Furnace Chamber Vestibule Existing PLC Furnace Control Existing Over Temperature Controller Burner Valves Existing N2 Safety System Gas CGas BGas A Calibration Gases Sample gas and pressure line(s) plus optional temperature probe(s) Furnace Atmosphere Supply Existing Batch Furnace Bulk N 2 Natural Gas for Burners Existing IRI Gas Train O 2 Probe KEY: Control Signals Burner Natural Gas ARI Rapid Carburizing Process Control Diagram ARI Flow Monitoring & Control Assembly ARI Laser Gas Analyzer Calibration Gases

32. 32 Example Rapid Carburizing Trial

33. 33 Benefits of Laser Gas Control – In-Situ Rapid Carburizing (Non-Equilibrium)  Greatly Increased Production Capacity Example: Cycle time for ~1mm case reduced 50%  Up to 40% Energy Savings  Elimination of Endo Generators  Further Improved Product Quality  Reduced Sooting and Furnace Maintenance

34. 34 System Paybacks in Less Than 12 Months * Includes Furnaces, Atmosphere Generators, and Ancillary Equipment if Plant New or Near Capacity Benefit Standard Carburizing Rapid Carburizing Exothermic Annealing Productivity Improvement Reduced Processing Times Improved Quality Up to 20%Up to 50% Reduced Energy Consumption25%40%Up to 30% Reduced Process Gas UseUp to 90%Up to 98%Up to 90% Reduced Regulated EmissionsOver 90%Over 98%Over 90% System Price (Typical)$40-100K$70-150K$40-90K Example Customer Gear Manufacturer Axle Manufacturer Non-Ferrous Annealer Cost Benefits Capital Savings (Avoiding Conventional Equipment)* Operation & Maintenance Cost Reduction $150K $100K/year $250K $200K/year $90K $100K/year

35. 35 Rapid Carburizing – Metallurgical Findings Summary  Batch Cycle Times Faster (Load to Unload)  Same Process Temperature (Typically 1750 Deg. F.)  Case Depth of.040” – 35% to 50% Faster  Case Depth of.065 – 20-30% Faster  Less Case Depth Variation Though the Load  Controllable Carbon Content/Hardness Profile  Controllable Retained Austenite Levels  Controllable Iron Carbide Levels  Wide Variation in Atmosphere Constituents Tolerated  Soot Control Algorithms Do Not Affect Parts  All Parts Released for Production

36. 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

37. 37 Thank You For Listening  Looking for Demonstration Sites  Looking for Technology, Marketing & Financial Partners  Brochures if Interested  Questions?