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ASTM Committee D-32 on Catalysts

ASTM Committee D-32 on Catalysts. Developing Standards for Catalytic Materials Since 1975 Thomas Szymanski Saint-Gobain Norpro Corporation L. D. Irish Emeritus, United Catalyst Inc. Jeffrey Elks ExxonMobil Process Research Labs. What Is ASTM?. American Society for Testing & Materials

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ASTM Committee D-32 on Catalysts

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  1. ASTM Committee D-32on Catalysts Developing Standards for Catalytic Materials Since 1975 Thomas Szymanski Saint-Gobain Norpro Corporation L. D. Irish Emeritus, United Catalyst Inc. Jeffrey Elks ExxonMobil Process Research Labs

  2. What Is ASTM? • American Society for Testing & Materials • A non-commercial organization • Founded in 1898 • Headquartered in Pennsylvania • Coordinates >10,000 written standards • Involves 132 standards-writing committees • Has 32,000 volunteer members worldwide • Dedicated to promoting testing excellence - 2 -

  3. Who Are ASTM's Members? • Producers • Companies who make a product • Users • Companies who use a product • General interest • Academics, government laboratories and other interested individuals - 3 -

  4. ASTM Standard Test Methods • What is an ASTM standard? • Developed by a technical committee • Composed of detailed instructions • Evaluated by multiple users • Approved by a consensus of ASTM members • Who develops ASTM standards? • Anyone can suggest the need for a method • A technical committee considers options • Methods are developed by concensus - 4 -

  5. Why Are ASTM Standards Needed? • ASTM standards provide • Robust methods for general use • A common ground to discuss materials manufacturing specifications • Impartial methods to resolve disputes • A tested introduction to a subject or characterization methodology - 5 -

  6. What Do ASTM Standards Deal With? • ASTM standards include: • Chemical analysis techniques • Physical property methods • Sampling protocols • Catalyst utilization methods • Instrumental methods • Technical definitions • Editorial guidance - 6 -

  7. What Is the ASTM D-32 Committee on Catalysts? • The D-32 Committee • Was established January, 1975 • Resulted from an AICHE meeting on catalytic standards • Has published more than 41 standards • Consists of more than 41 volunteers - 7 -

  8. Who Are Members of D-32? • Our members span the global catalyst and materials producer/user communities • Chemical companies • Refining companies • Catalyst suppliers • Carrier suppliers • Equipment vendors • Technology licensors • Academic researchers • Government laboratory scientists - 8 -

  9. All D-32 Test Methods Contain Several Key Elements • Safety considerations • Sampling plan • Required sample pretreatment • Required reagent quality • Inter-lab round-robin testing protocol • Data reduction information • Statistical evaluation/validation - 9 -

  10. How Does D-32 Function? • Members meet for two days, twice a year • Sites rotate within North America • Eleven subcommittees meet as needed • Task groups coordinate efforts • Members develop draft test method(s) • Formulate testing plans and conduct tests • Evaluate results • Submit test method(s) for Society approval - 10 -

  11. The D-32 Committee’s Mission/Scope • Our Committee's Scope: • The development of test methods, classifications, practices and terminology pertaining to catalysts, zeolites and related materials used in their manufacture, and the stimulation of research related thereto. The work of this Committee will be coordinated with other ASTM committees and other organizations having mutual interests. - 11 -

  12. What Are Typical Standard Test Methods for Catalysts? • Physical-mechanical test methods include: • Crush strength • Abrasion and attrition resistance • Powder and particle packing density • Vibratory methods • Mechanically tapped methods • Particle size distribution by sieving, laser-light scattering and electronic counting • Catalyst bulk-crush strength • Total pore volume by Hg porosimetry and He pycnometry - 12 -

  13. What Are Typical Standard Test Methods for Catalysts? • Instrumental test methods include: • ZSM-5 crystallinity by XRD • Zeolite content of a catalyst by XRD • Zeolite crystallinity and U-cell dimensions by XRD • BET surface area • Micropore volume and zeolite surface area • Pore size distribution by N2 physisorption • Pore size distribution by Hg porosimetry - 13 -

  14. What Are Typical Standard Test Methods for Catalysts? • Physical-chemical test methods include: • Nickel content in alumina-base catalysts • Nickel and vanadium in equilibrium FCC catalysts • Palladium in molecular sieve catalysts • Platinum in reforming catalysts • Cobalt and molybdenum in alumina-based catalysts • Metals dispersion by H2 chemisorption - 14 -

  15. What Are Typical Standard Test Methods for Catalysts? • Catalytic test methods include: • Standard microactivity method for FCC catalysts • FCC catalyst activity and selectivity • Deactivation of fresh FCC catalysts • Steam • Addition of metals - 15 -

  16. What Standard Test Methods Are Being Developed? • Standard test methods under development include: • Water pore volume by centrifugation • Rare earth metals analysis by ICP • Rare earth metals in FCC by XRF • Surface acidity by ammonia TPD • Surface acidity by amine TPD • Metal dispersion in bimetallic catalysts by CO chemisorption • Catalytic material pore volume • Particle size by sedimentation - 16 -

  17. What New Test Methods Are Being Considered? • Standard test methods under consideration or in development include: • Micropore size distribution • Chemisorption techniques • Metals distribution • Catalyst metallation and deactivation • Zeolite sorption properties • Zeolite beta crystallinity - 17 -

  18. Why Join D-32? • Promote quality assurance • Participate in development of new methods • Learn from colleagues with similar problems • Recognize potential hazards • Access new methodology from industry experts • Encourage international participation • Expand personal technical network A "ground floor" opportunity to guide technology - 18 -

  19. Appendix - 19 -

  20. General Use and Catalyst Methods Developed by D-32 • D 3663 TM for Surface Area of Catalysts • D 4365 TM for Determination of Micropore Volume and Zeolite Surface Area of a Catalyst • D 4567 TM for Single-Point Determination of Specific Surface Area of Catalysts Using Nitrogen Adsorption by Continuous Flow Method • D 4780 TM for Determination of Low Surface Area of Catalysts by Multipoint Krypton Adsorption • D 4222 TM for Determination of Nitrogen Adsorption and Desorption Isotherms of Catalysts by Static Volumetric Measurements • D 4641 Practice Calculation of Pore Size Distributions of Catalysts from Nitrogen Desorption Isotherms • D 4284 TM for Determination of Pore Volume Distribution of Catalysts by Mercury Intrusion Porosimetry • D 3908 TM for Hydrogen Chemisorption on Supported Platinum on Alumina Catalysts by Volumetric Vacuum Method - 20 -

  21. General Use and Catalyst Methods Developed by D-32 • D 4824 TM for Determination of Catalyst Acidity by Ammonia Chemisorption • D 4058 TM for Attrition and Abrasion of Catalysts and Catalyst Carriers • D 4164 TM for Mechanically Tapped Packing Density of Formed Catalyst and Catalyst Carriers • D 4180 TM for Vibratory Packing Density of Formed Catalyst Particles and Catalyst Carriers • D 4512 TM for Vibrated Apparent Packing Density of Fine Catalyst Particles and Powder • D 4699 TM for Vibratory Packing Density of Large Formed Catalyst Particles • D 4781 TM for Mechanically Tapped Packing Density of Fine Catalyst Particles and Catalyst Carrier Particles • D 6761 TM for Determination of Total Pore Volume of Catalysts and Catalyst Carriers by Mercury Porosimetry and Helium Pycnometry - 21 -

  22. General Use and Catalyst Methods Developed by D-32 • D 4179 TM for Sinple Pellet Crush Strength of Formed Catalyst Shapes • D 6175 TM for Radial Crush Strength of Extruded Catalyst Particles • D 4438 TM for Particle Size Distribution of Catalytic Material by Electronic Counting • D 4464 TM for Particle Size Distribution of Catalytic Materials by Laser Light Scattering • D 4513 TM for Particle Size Distribution of Catalytic Material by Sieving • D 5757 TM for Determination of Attrition and Abrasion of Powdered Catalysts by Air Jets • D 4642 TM for Platinum in Reforming Catalysts by Wet Chemistry • D 4782 TM for Palladium in Molecular Sieve Catalyst by Wet Chemistry • D 5153 TM for Palladium in Molecular Sieve Catalyst by Atomic Spectroscopy • D 1977 TM for Determination of Nickel and Vanadium in FCC Equilibrium Catalysts by Hydrofluoric and Sulfuric Acid Decomposition and Atomic Spectroscopic Analysis - 22 -

  23. General Use and Catalyst Methods Developed by D-32 • D 3610 TM for Determination of Total Cobalt in Alumina-Base Cobalt-Molybdenum Catalyst by Potentiometric Titration • D 3943 TM for Determination of Total Molybdenum in Fresh Alumina-Base Catalyst • D 4481 TM for Determination of Total Nickel in Fresh Alumina-Base Catalyst • D 3907 TM for Testing of FCC Catalysts by Microactivity Test • D 5154 TM for Determination of Activity and Selectivity of FCC Catalysts by Microactivity Test • D 4463 TM for Metals Free Steam Deactivation of Fresh Fluid Cracking Catalysts • D 3906 TM for Determination of Relative Zeolite Diffraction Intensities • D 3942 TM for Determination of the Unit Cell Dimension of a Faujasite-Type Zeolite • D 5357 TM for Determination of Relative Crystallinity of Zeolite Sodium by X-Ray Diffraction - 23 -

  24. General Use and Catalyst Methods Developed by D-32 • D 5758 TM for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray Diffraction • D 4926 TM for Gamma Alumina Content in Catalysts Containing Silica and Alumina by X-Ray Powder Diffraction • D 3766 Catalysts and Catalysis Nomenclature • D 7084 TM for Determination of Bulk Crush Strength of Catalysts and Catalyst Carriers • D 7085 Standard Guide for Determination of Chemical Elements in Fluid Catalytic Cracking Catalysts by X-Ray Fluorescence Spectrometry • D 7206 Standard Guide for Cyclic Deactivation of Fluid Catalytic Cracking (FCC) Catalysts with Metals - 24 -

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