Committee D-32 on Catalysts

ASTM Committee D-32on Catalysts

Developing Standards for Catalytic Materials Since

1975

Thomas SzymanskiSaint-Gobain Norpro Corporation

L. D. IrishEmeritus, United Catalyst Inc.

Jeffrey ElksExxonMobil Process Research Labs

Committee D-32 on Catalysts

What Is ASTM?

American Society for Testing & Materials A non-commercial organization Founded in 1898Headquartered in PennsylvaniaCoordinates >10,000 written standardsInvolves 132 standards-writing committeesHas 32,000 volunteer members worldwideDedicated to promoting testing excellence

- 2 -

Committee D-32 on Catalysts

Who Are ASTM's Members?

Producers Companies who make a product

UsersCompanies who use a product

General interestAcademics, government laboratories and other interested individuals

- 3 -

Committee D-32 on Catalysts

ASTM Standard Test Methods

What is an ASTM standard?Developed by a technical committeeComposed of detailed instructionsEvaluated by multiple usersApproved by a consensus of ASTM members

Who develops ASTM standards?Anyone can suggest the need for a methodA technical committee considers optionsMethods are developed by concensus

- 4 -

Committee D-32 on Catalysts

Why Are ASTM Standards Needed?

ASTM standards provideRobust methods for general useA common ground to discuss materials manufacturing specificationsImpartial methods to resolve disputesA 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 techniquesPhysical property methodsSampling protocolsCatalyst utilization methodsInstrumental methodsTechnical definitionsEditorial guidance

- 6 -

Committee D-32 on Catalysts

What Is the ASTM D-32

Committee on Catalysts?

The D-32 CommitteeWas established January, 1975Resulted from an AICHE meeting on catalytic standardsHas published more than 41 standardsConsists of more than 41 volunteers

- 7 -

Committee D-32 on Catalysts

Who Are Members of D-32?

Our members span the global catalyst and materials producer/user communities

Chemical companiesRefining companiesCatalyst suppliersCarrier suppliersEquipment vendorsTechnology licensorsAcademic researchers Government laboratory scientists

- 8 -

Committee D-32 on Catalysts

All D-32 Test Methods Contain Several Key

Elements

Safety considerationsSampling planRequired sample pretreatmentRequired reagent quality Inter-lab round-robin testing

protocolData reduction informationStatistical evaluation/validation

- 9 -

Committee D-32 on Catalysts

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 effortsMembers develop draft test method(s) Formulate testing plans and conduct testsEvaluate resultsSubmit test method(s) for Society approval

- 10 -

Committee D-32 on Catalysts

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 -

Committee D-32 on Catalysts

What Are Typical Standard Test Methods

for Catalysts? Physical-mechanical test methods

include:Crush strengthAbrasion and attrition resistancePowder and particle packing densityVibratory methodsMechanically tapped methodsParticle size distribution by sieving, laser-light scattering and electronic countingCatalyst bulk-crush strengthTotal pore volume by Hg porosimetry and He pycnometry

- 12 -

Committee D-32 on Catalysts

Instrumental test methods include:ZSM-5 crystallinity by XRDZeolite content of a catalyst by XRDZeolite crystallinity and U-cell dimensions by XRDBET surface areaMicropore volume and zeolite surface areaPore size distribution by N2 physisorption

Pore size distribution by Hg porosimetry

What Are Typical Standard Test Methods

for Catalysts?

- 13 -

Committee D-32 on Catalysts

Physical-chemical test methods include:

Nickel content in alumina-base catalystsNickel and vanadium in equilibrium FCC catalystsPalladium in molecular sieve catalystsPlatinum in reforming catalystsCobalt and molybdenum in alumina-based catalystsMetals dispersion by H2 chemisorption

What Are Typical Standard Test Methods

for Catalysts?

- 14 -

Committee D-32 on Catalysts

Catalytic test methods include:Standard microactivity method for FCC catalystsFCC catalyst activity and selectivityDeactivation of fresh FCC catalysts+Steam+Addition of metals

What Are Typical Standard Test Methods

for Catalysts?

- 15 -

Committee D-32 on Catalysts

What Standard Test Methods Are Being

Developed?Standard test methods under

development include:Water pore volume by centrifugationRare earth metals analysis by ICPRare earth metals in FCC by XRFSurface acidity by ammonia TPDSurface acidity by amine TPDMetal dispersion in bimetallic catalysts by CO chemisorptionCatalytic material pore volume Particle size by sedimentation

- 16 -

Committee D-32 on Catalysts

What New Test Methods Are Being

Considered?Standard test methods under

consideration or in development include:

Micropore size distributionChemisorption techniquesMetals distributionCatalyst metallation and deactivationZeolite sorption propertiesZeolite beta crystallinity

- 17 -

Committee D-32 on Catalysts

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 -

Committee D-32 on Catalysts

Appendix

- 19 -

Committee D-32 on Catalysts

General Use and Catalyst Methods

Developed by D-32D 3663 TM for Surface Area of CatalystsD 4365 TM for Determination of Micropore Volume and Zeolite Surface Area of a CatalystD 4567 TM for Single-Point Determination of Specific Surface Area of Catalysts Using Nitrogen Adsorption by Continuous Flow MethodD 4780 TM for Determination of Low Surface Area of Catalysts by Multipoint Krypton AdsorptionD 4222 TM for Determination of Nitrogen Adsorption and Desorption Isotherms of Catalysts by Static Volumetric MeasurementsD 4641 Practice Calculation of Pore Size Distributions of Catalysts from Nitrogen Desorption IsothermsD 4284 TM for Determination of Pore Volume Distribution of Catalysts by Mercury Intrusion PorosimetryD 3908 TM for Hydrogen Chemisorption on Supported Platinum on Alumina Catalysts by Volumetric Vacuum Method

- 20 -

Committee D-32 on Catalysts

General Use and Catalyst Methods

Developed by D-32D 4824 TM for Determination of Catalyst Acidity by Ammonia ChemisorptionD 4058 TM for Attrition and Abrasion of Catalysts and Catalyst CarriersD 4164 TM for Mechanically Tapped Packing Density of Formed Catalyst and Catalyst CarriersD 4180 TM for Vibratory Packing Density of Formed Catalyst Particles and Catalyst CarriersD 4512 TM for Vibrated Apparent Packing Density of Fine Catalyst Particles and PowderD 4699 TM for Vibratory Packing Density of Large Formed Catalyst ParticlesD 4781 TM for Mechanically Tapped Packing Density of Fine Catalyst Particles and Catalyst Carrier ParticlesD 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-32D 4179 TM for Sinple Pellet Crush Strength of Formed Catalyst ShapesD 6175 TM for Radial Crush Strength of Extruded Catalyst ParticlesD 4438 TM for Particle Size Distribution of Catalytic Material by Electronic CountingD 4464 TM for Particle Size Distribution of Catalytic Materials by Laser Light ScatteringD 4513 TM for Particle Size Distribution of Catalytic Material by SievingD 5757 TM for Determination of Attrition and Abrasion of Powdered Catalysts by Air JetsD 4642 TM for Platinum in Reforming Catalysts by Wet ChemistryD 4782 TM for Palladium in Molecular Sieve Catalyst by Wet ChemistryD 5153 TM for Palladium in Molecular Sieve Catalyst by Atomic SpectroscopyD 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-32D 3610 TM for Determination of Total Cobalt in Alumina-Base Cobalt-Molybdenum Catalyst by Potentiometric TitrationD 3943 TM for Determination of Total Molybdenum in Fresh Alumina-Base CatalystD 4481 TM for Determination of Total Nickel in Fresh Alumina-Base CatalystD 3907 TM for Testing of FCC Catalysts by Microactivity TestD 5154 TM for Determination of Activity and Selectivity of FCC Catalysts by Microactivity TestD 4463 TM for Metals Free Steam Deactivation of Fresh Fluid Cracking CatalystsD 3906 TM for Determination of Relative Zeolite Diffraction IntensitiesD 3942 TM for Determination of the Unit Cell Dimension of a Faujasite-Type ZeoliteD 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-32D 5758 TM for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray DiffractionD 4926 TM for Gamma Alumina Content in Catalysts Containing Silica and Alumina by X-Ray Powder DiffractionD 3766 Catalysts and Catalysis NomenclatureD 7084 TM for Determination of Bulk Crush Strength of Catalysts and Catalyst CarriersD 7085 Standard Guide for Determination of Chemical Elements in Fluid Catalytic Cracking Catalysts by X-Ray Fluorescence SpectrometryD 7206 Standard Guide for Cyclic Deactivation of Fluid Catalytic Cracking (FCC) Catalysts with Metals

- 24 -