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Introducing the SA-9600 Flowing Gas BET Surface Area Analyzer

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Dr. Michael Pohl of HORIBA Particle presents information about the SA-9600 series of surface area analyzers.

Dr. Michael Pohl of HORIBA Particle presents information about the SA-9600 series of surface area analyzers.

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  • 1. State-of-the-Art BET Surface Area An Introduction to the SA-9600 Technology Mike Pohl mike.pohl@horiba.com www.horiba.com/us/particle© 2010 HORIBA, Ltd. All rights reserved.
  • 2. Outline Surface Area Basics The BET Technique Measurement Workflow Recent Advancements© 2010 HORIBA, Ltd. All rights reserved.
  • 3. Surface Area Basics© 2010 HORIBA, Ltd. All rights reserved.
  • 4. Why Surface Area? Rates of… Dissolution Reaction Absorption/adsorption Combustion Hydration© 2010 HORIBA, Ltd. All rights reserved.
  • 5. Porosity Non-porous solid Porous solid Low specific surface area High specific surface area Low specific pore volume High specific pore volume Porous materials have highly developed internal surface area that can be used to perform a specific function. Almost all solids have some amount of porosity.© 2010 HORIBA, Ltd. All rights reserved.
  • 6. Porosity There are three parameters used to measure porosity; specific surface area, specific pore volume or porosity, and pore size and its distribution. Total surface area, m2 Specific Surface Area, m 2/g = Mass of the solid, g Porosity, % = Volume of pores X 100 Porosity Volume of solid (including pores)Pore size andits distribution Specific Pore volume, cm3/g Total pore volume, cm3 = Mass of the solid, g© 2010 HORIBA, Ltd. All rights reserved.
  • 7. Pore Size Micropores Mesopores MacroporesZeolite, Mesoporous silica, Sintered metalsActivated Activated carbon and ceramicscarbon,Metal organicframework 2 nm 50 nm© 2010 HORIBA, Ltd. All rights reserved.
  • 8. Definitions ABsorption Gas molecules penetrate mass of a solid ADsorption ABsorption Gas molecules condense on free surfaces Physisorption Physical adsorption - van der Waals forces ADsorption Chemisorption Chemical adsorption – chemical bonding Note: Flowing-gas method uses physisorption© 2010 HORIBA, Ltd. All rights reserved.
  • 9. Comparison Physisorption Chemisorption Weak, long-range Strong, short-range Not surface specific Surface specific Lower energy of Ads. Higher energy of Ads. Desorption increases Adsorption can with increasing temp. increase with temp. Non-reactive at Potentially reactive at surface surface Multilayer adsorption Monolayer adsorption (BET used to model) (Langmuir model)© 2010 HORIBA, Ltd. All rights reserved.
  • 10. Physisorption Behavior© 2010 HORIBA, Ltd. All rights reserved.
  • 11. © 2010 HORIBA, Ltd. All rights reserved.
  • 12. Isotherm Types Type 1 Type 2 Type 3W t W t W t Non-porous Chemisorption or macropore powders P / P0 P / P0 P / P0 Type 4 Type 5 W t W t Porous Powders P / P0 P / P0© 2010 HORIBA, Ltd. All rights reserved.
  • 13. Type IV Isotherm© 2010 HORIBA, Ltd. All rights reserved.
  • 14. The BET Technique© 2010 HORIBA, Ltd. All rights reserved.
  • 15. BET Calculation© 2010 HORIBA, Ltd. All rights reserved.
  • 16. BET Calculation© 2010 HORIBA, Ltd. All rights reserved.
  • 17. Effect of Multipoint Single-point method offers the advantage of simplicity and speed, with acceptable accuracy. V = V 1− P P m a o (m ) i.e. V = 1/slope A relative pressure of 0.3 gives good general agreement with the multi- point method. Correction of single point “error” at P/P0 = 0.3 by multiplying the single point BET value by C/C-2 decreases the difference. Sample Multi-point Uncorrected Uncorrected Corrected Corrected No. BET single-point difference single – difference (m2/g) (m2/g) (%) point (%) (m2/g) 1 4.923 4.241 -13.9 4.948 0.51 2 4.286 3.664 -14.5 4.275 -0.26 3 8.056 6.867 -14.8 8.011 -0.56 4 5.957 5.194 -12.8 6.060 +1.73© 2010 HORIBA, Ltd. All rights reserved.
  • 18. Method Comparison Dynamic Static-Volumetric (Flowing-Gas) Faster Slower Easy to use Easy to use Increased sensitivity Low SSA longer to low SSA materials measurement times Higher throughput Lower throughput Lower operating costs Higher operating costs Lower service costs Higher service costs© 2010 HORIBA, Ltd. All rights reserved.
  • 19. Measurement Workflow© 2010 HORIBA, Ltd. All rights reserved.
  • 20. The SA-9600 Surface Area Analyzer Outgassing station Analysis stations Liquid nitrogen bath© 2010 HORIBA, Ltd. All rights reserved.
  • 21. What You’ll Need Gases 99.999% pure Helium 99.999% pure Nitrogen Dry gas Liquid Nitrogen Cools material surface for adsorption Mass Balance Instrument measures total surface area, sample mass is used to convert to SSA© 2010 HORIBA, Ltd. All rights reserved.
  • 22. Workflow Preparation Check gas flow Confirm temperature and pressure Weigh sample (know how much) Degas sample (prepare clean surfaces) Measurement Automatic calibration Automatic adsorption and desorption Automatic calculation of specific surface area Save, Export, Print report© 2010 HORIBA, Ltd. All rights reserved.
  • 23. Recent Advancements© 2010 HORIBA, Ltd. All rights reserved.
  • 24. SA-9600 Software Easy to Use Software Multi-tasking – View, Edit and Print Data while Measuring. Measure and Display Window – Similar to LA Products© 2010 HORIBA, Ltd. All rights reserved.
  • 25. SA-9600 Software 5 Measurement Types 3 Gas Mixture Points 6 Gas Mixture Points 13 point Pore Size Dist. Pore Volume – Multiple Runs Single Point – Multiple Runs Data Graphed on Screen and Reports© 2010 HORIBA, Ltd. All rights reserved.
  • 26. Real-time Measurement Adsorption Desorption Calibration© 2010 HORIBA, Ltd. All rights reserved.
  • 27. SA-9600 Security Module User Name and Password to Login to Software Built-in Security with Users and Groups Setup Security Settings Horiba Provides Master System Administration Key to Unlock System© 2010 HORIBA, Ltd. All rights reserved.
  • 28. 21 CFR Part 11 Compliance Audit Trail capability Electronic Signature on reports Analyzer must be controlled from computer Certain events require a User name and Password© 2010 HORIBA, Ltd. All rights reserved.
  • 29. Electronic Signature Electronic Signature is the information printed at the Bottom of the report that is automatically generated based on information stored in the file and the current user.© 2010 HORIBA, Ltd. All rights reserved.
  • 30. Audit Trail Audit Trail contains all events related to the creation of data files, editing conditions, printing, etc. It also logs system access information such as login name, login time, and bad passwords.© 2010 HORIBA, Ltd. All rights reserved.
  • 31. For More Details Visit www.horiba.com/us/particle Contact us directly at labinfo@horiba.com Visit the Download Center to find this recorded presentation and many more on other topics© 2010 HORIBA, Ltd. All rights reserved.

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