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?
Committee D-32 on Catalysts 

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

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government laboratories and other interested individuals -3- .Who Are ASTM's Members? Committee D-32 on Catalysts  Producers Companies who make a product  Users Companies who use a product  General interest Academics.

ASTM Standard Test Methods Committee D-32 on Catalysts  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- .

Committee D-32 on Catalysts 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- .

Committee D-32 on Catalysts 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- .

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

Who Are Members of D-32? Committee D-32 on Catalysts  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- .

Committee D-32 on Catalysts 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- .

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

12 -  Physical-mechanical test methods include: .Committee D-32 on Catalysts What Are Typical Standard Test Methods for Catalysts? 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 .

Committee D-32 on Catalysts 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 - .Committee D-32 on Catalysts 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 .

Committee D-32 on Catalysts 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 - .Committee D-32 on Catalysts 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 .

Committee D-32 on Catalysts 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 - .

Why Join D-32? Committee D-32 on Catalysts  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 - .

9- .Committee D-32 on Catalysts Appendix .

20 - .Committee D-32 on Catalysts 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 .

Committee D-32 on Catalysts 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 - .

Committee D-32 on Catalysts 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 - .

Committee D-32 on Catalysts General Use and Catalyst Methods Developed by D-32 D 3610 TM for Determination of Total Cobalt in Alumina-Base CobaltMolybdenum Catalyst by Potentiometric Titration D 3943 TM for Determination of Total Molybdenum in Fresh AluminaBase 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 FaujasiteType Zeolite D 5357 TM for Determination of Relative Crystallinity of Zeolite Sodium by X-Ray Diffraction .23 - .

Committee D-32 on Catalysts 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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