Download October 2003 - ASTM International

OCTOBER 2003
ASTM D32 CATALYST COMMITTEE NEWS

The committee has about 40 approved methods (published in ASTM methods volume 05.05) under its
jurisdiction and others under development. Technical discussions from recent meetings are
summarized below in section 2. Please contact the appropriate sub-committee chair for more
information.

The committee is comprised of nearly seventy members representing over forty international users,
producers, and academics interested in catalysis

We welcome new members to help develop new methods and participate in inter-laboratory round
robins. Please join us at our next meeting; we have methods under development needing your
participation. Please see the ASTM home page for membership information.

Membership is not necessary for you to contribute ideas, participate in round-robin testing, etc. Contact
any officer or sub-committee chairs if you’re interested in working with us.

D32 Publications:
“Characterization and Catalyst Development. An Interactive Approach”, ACS Symposium
Series 411 (1989)
Section 1.
Meeting Highlights & Committee Activities
The fall meeting of ASTM committee D-32 met October 20-22, 2003 in Tampa, FL. Committee minutes are available
to D32 members via the web site.
Committee Officers:
Chairman:
Vice Chairman – User:
Vice Chairman – Producer:
Secretary:
Membership Secretary:
Thomas Szymanski, Saint Gobain
Jefrey T. Elks, Exxon Mobil
Steven A. Bradley, UOP Research Center
Marshall J. Margolis, ABB Lummus Global Inc.
Thomas E. Block, Azko Nobel Catalysts LLC
Future D32 Meetings (cw) = ASTM Committee Weeks; See the ASTM web site for registration information
Next Meeting 
April 19-21, 2004
October 4-5, 2004
April 18-20, 2005
October 17-19, 2005
April 24-26, 2006
October 23-25, 2006
Salt Lake City, UT (cw)
Washington DC (cw)
Reno, NV (cw)
Dallas, TX (cw)
Toronto, Ontario (cw)
Atlanta, GA (cw)
FCC Workshop: This has been proposed for the October 2005 Dallas meeting. A task force has been
established to define the structure, content, and potential collaborators. Interested individuals should
contact the D32 ASTM staff manager, Diane Rehiel ([email protected]), for further information
Strategies for Growth: Various proposals are under discussion to expand the committee’s methods
development scope and to develop synergistic relationships other with groups having common interests.
Possibilities include: Gulf Coast Conference, North American Catalyst Association, CATCON, and other
ASTM Committees.
Section 2.
Summary of our current technical activities
Physical-Chemical Properties (D32.01)
Chair: Jeffrey C. Kenvin / Micromeritics / tel: 770-662-3665
Methods successfully balloted and released for publication:

D 3663: "Test Method for Surface Area of Catalysts"

D 3908: "Test Method for Hydrogen Chemisorption on Supported Platinum in Alumina Catalysts by
Volumetric Vacuum Method"

D 4222: "Test Method for Determination of Nitrogen Adsorption and Desorption Isotherms of Catalysts
by Static Volumetric Measurements"

D 4567: "Test Method for Single Point Determination of Specific Surface Area of Catalysts Using
Nitrogen Adsorption by Continuous Flow"

D 4824: "Test Method for Determination of Catalyst Acidity by Ammonia Chemisorption"
Methods Under Development (round robin/input by interested parties needed)

Z 9864: "CO Chemisorption by Continuous and Static Volumetric Techniques for Monometallic and
Bimetallic Noble Metals Catalysts"

Z 6347: "Standard Test Method for the Determination of Acid Strength and Acid Site Density By
Ammonia Temperature Programmed Desorption" - Inadvertently dropped from the D32.01 work list.
This will be registered as a new work item after the method is further reviewed. A second round robin
may be required based on review of the method.

Catalyst Acidity and Acid Strength Distribution by Ammonia Temperature Programmed Desorption

"External" or "Matrix" Acidity of Catalysts by Temperature Programmed Desorption

Determination of Lewis and Bronsted acidity using TMPO, IPA, Pyridine

Oxygen/hydrogen titration method
Physical-Mechanical Properties (D32.02)
Chair: Jeffrey T. Elks / ExxonMobil Research & Development Labs / tel: 908-730-2201
Method to be revised/reballoted:

D 6761-02: "Standard Test Method for the Determination of the Total Pore Volume of Catalysts and
Catalyst Carriers" - Negatives and comments deemed persuasive. Some revisions were not reflected in
the balloted document. Corrected version will be re-balloted in next cycle.
Methods successfully balloted and released for publication:
 D 4164-99: "Standard Test Method for Mechanically Tapped Packing Density of Formed Catalyst and
Catalyst Carriers"

D 4180-99: "Standard Test Method for Vibratory Packing Density of Formed Catalyst Particles and
Catalyst Carriers"

D 4512-99: "Standard Test Method for Vibrated Apparent Packing Density of Fine Catalyst and Catalyst
Carrier Particles and Powder"

D 4699-99: "Standard Test Method for Vibratory Packing Density of Large Formed Catalyst and
Catalyst Carrier Particles"

D 4781-99: "Standard Test Method for Mechanically Tapped Packing Density of Fine Catalyst Particles
and Catalyst Carrier Particles"

D 6175: "Method of Radial Crush Strength of Extruded Catalyst Particles" - Round robin planned to
provide compatibility testing, define sample preparation. Research report to be reviewed with
statistician to determine if smaller population can be used. Review of past data suggests possible
calcination effects. Expand reported results to include number of particles tested and number of
particles excluded from sample (too weak or strong to be measured by device)
Under Development (round robin/input by interested parties needed)
 Z 8216: "Standard Test Method for Determination of Water Pore Volume of Catalyst and Catalyst
Carriers by Centrifugation" - Status of round robin and task group activity underway.

Z 4448: "Standard Test Method for Determination of Attrition and Abrasion of Powdered Catalyst by Jet
Cup" - volunteer participants continue to change.

Proposed Practice for the determination of “Bulk Crush of Catalyst and Catalyst Carriers” (rather than a
standard test method) will remain as a STM since "reportable" data are generated.

Proposed Guide for the determination of particle strength using accepted techniques including bulk
crush, individual particle, drop testing, etc. - a compendium document of pertinent literature references
and guidelines for conducting these measurements. Recent compilation of individual particle strength
data from different devices and with different jaw configurations to be included.

Z 8477: "Standard Test Method for Determination of Crush Strength of Low Surface Area Catalysts and
Catalyst Carriers by Drop Test into a Container" - Potential materials for suitability testing identified,
scoping results to be developed along with worksheet prior to round robin testing.

Z 8478: "Standard Test Method for Determination of Individual Particle Strength of Low Surface Area
Catalysts and Catalyst Carriers by Drop Test onto a Steel Plate" - Potential materials for suitability
testing identified, scoping results to be developed along with worksheet prior to round robin testing.

Proposed Method for Determination of Length to Diameter Ratio of Small Extruded Catalyst Particles Round robin materials selected and testing protocol developed, round robin activity delayed pending
draft of optical imaging method for concurrent testing with physical measurement method.

Proposed method for the Determination of Particle Strength Using a Single Point of Contact is under
evaluation to determine technical applicability before advancement to draft status and/or round robin
testing. Data generated comparing 1/8-inch anvil, full plate and half-cylinder jaw designs was reviewed.
Using samples prepared concurrently using a common sampling procedure, data obtained suggested
certain designs favor improved strength discrimination. Additional data presented and available in
D32.02 minutes. Discussion to resume at Fall 2003 meeting.

Need Identified for Possible Practice/Guide/Method for Determination of Reactor Density Using
Measured Catalyst Properties.

Need identified for development of a method to test for “Attrition in Slurry Phase Systems” - generic
draft provided to task group chair and under review.

Interest in developing method for measuring sphericity of catalysts and catalyst particles. Several
instrument vendors currently offering devices to measure oblate vs. prolate dimensions of large
particles. This is more a measure of flowability rather than sphericity.
Chemical Composition (D32.03)
Chair: Raymond L. Jordan / W. R. Grace / tel 410-354-8524
Methods successfully balloted and released for publication:
 D 1997: “Standard Test Method for Nickel and Vanadium in FCC Equilibrium Catalysts by Hydrofluoric/Sulfuric Acid
Decomposition and Atomic Spectroscopic Analysis”
Under Development (round robin/input by interested parties needed)
 Determination of rhenium in reforming catalysts

Method for determination of major rare earth elements in FCC catalysts by ICP

Method for determination of rare earth elements in FCC catalysts by XRF

Guide for the measurement of 29 Elements in FCC Catalysts

Guide for the preparation of samples for ICPES analysis by dissolution or fusion techniques

Method for determination of ultra-trace precious metals (from additives) in FCC catalysts
Catalytic Properties (D32.04)
Chair: Robert Andrews / Engelhard / 732-205-5133
Workshop Presentations
 October, 1998: “Fluid-Bed Testing for FCC” presented by J.C. Kayser and J. O. Cozard
 October, 1999: Siauw Ng / CANMET made a presentation on use of fluid bed methods for FCC
evaluations
Ballot Items / Revisions in Progress

D3907-92, Standard Method for Testing Fluid Catalytic Cracking (FCC) Catalysts by Microactivity Test successfully reinstated with original STM number

D5154-91, Standard Test Method for Determining the Activity and Selectivity of fluid Catalytic Cracking
(FCC) Catalysts by Microactivity - successfully reinstated with original STM number
Under Development (round robin/input by interested parties needed)
 Methodology for FCC catalyst metals impregnation and deactivation

Standard guide for Determination of the Metals Tolerance of Fresh Fluid Cracking Catalysts

Interest in developing a fixed fluidized bed Microactivity method for evaluation of FCC catalysts

Development of fixed fluidized bed Microactivity testing workshop; date to be determined.
Zeolites (D32-05)
Chair: George E. McKedy / Multisorb Technologies Inc / tel 716-824-8900

This sub-committee needs more active members. Please contact ASTM or sub-committee chair if you
are interested in participating.
Under Development (round robin/input by interested parties needed)
 A draft method has been prepared for determination of relative crystallinity of mordenite zeolite by x-ray
diffraction. Participants included UOP, United Catalyst, Shell, Arco, Akzo, and W.R. Grace

A test method to determine relative crystallinty of zeolite Beta by X-ray diffraction
Section 3.
Technical questions for the catalyst characterization community
Seeking Methods:

Does anyone have a method for the in situ determination of bulk density of a packed catalyst bed within
a reactor?

What techniques are used for determining catalyst attrition in a liquid phase?

What metals deactivation procedures are in use for FCC catalyst testing?

Determination “roundness” of packed bed size spherical particles

Other than steaming, with or without metals, what methods are in use for deactivation of FCC catalysts
for laboratory performance testing?

Are users of fluid bed “MAT” reactors interested in developing a standard method for this type of FCC
catalyst performance testing?

A method for determination of bulk crush strength
Seeking Information:
 Does anyone use a synthetic hydrocarbon blend for either standard or fluid bed “MAT” evaluation of
FCC catalysts? Any suggestions or comments on this approach?

What companies or organizations might be interested in distributing reference materials used to develop
ASTM methods?

Is there a source for 1/32” trilobe catalyst supports?