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Standardization Of Catalyst Test Methods
767
G. Poncelet, P. Grange and P.A. Jacobs (Editors), Preparation of Catalysts III
© 1983 Elsevier Science Publishers B.V., Amsterdam - Printed in The Netherlands
STANDARDIZATION OF CATALYST TEST METHODS R. J. BERTOLACINIl and ARTHUR NEAL2 lAmoco Oil Company, P. O. Box 400, Naperville, Illinois
60566, U.S.A.
2Exxon Corporation, P. O. Box 2226, Baton Rouge, Louisiana
70821, U.S.A.
ABSTRACT This is a report on the progress made by ASTM Committee D-32 on Catalysts since the last paper given at this meeting in 1978. The main committee has seven subcommittees of people with interest and expertise in specific areas related to the main committee. subcommittees is reviewed.
Progress of the
These include catalytic properties, chemical
analysis, physical-chemical properties, physical-mechanical properties, and nomenclature.
Eight standards have been published and approximately 23 others
are at various stages of development in the task groups.
INTRODUCTION Previous speakers at this symposium (ref. 1-2) reviewed the early history of the American Society for Testing Materials, Committee D-32 on Catalysts. The scope of ASTM D-32 is to develop test methods, classifications, recommended practices, and definitions pertaining to catalysts and materials used in their manufacture, and stimulation of research related to catalysts.
For the present,
the catalysts considered have been heterogeneous, but if an interest or demand existed in standards for homogeneous or heterogenized catalysts it would be appropriate for D-32 to consider these system? Since its organization on January 14, 1975, ·the membership has steadily increased and today is 121.
Each member must be classified as having a voting
interest or not and identified as representatives of producers, users, or general interest.
Users represent organizations which either purchase or use
catalysts, and who could not be classified as producers. companies which make and sell catalysts. neither user nor producer.
Producers represent
The general interest category
~s
This category includes private consultants,
instrument and equipment companies, independent laboratories, consumer groups, and university researchers. of D-32.
Table 1 shows the classification for the membership
Only a single vote is allowed to representatives of one institution
or major separate functional division of it. dominate.
We are in good balance.
No interest can be allowed to
768 TABLE 1 Membership classification Users Producers General Interest Unclassified Total
45 52 23 1 121
Fourteen of the 121 members represent eleven foreign countries; n1ne are Europeans, two South Americans, two Canadians, and one Australian.
In addition
to representatives from these countries, we have had contacts with interested researchers in the USSR, Japan, and India. Table 2 shows the current officers of D-32. balance of interest.
Even here, we must maintain a
The chairman cannot be a producer of catalysts.
vice chairmen represent both users and producers.
The two
Committee D-32 has a liaison
chairman who has contact with other organizations and researchers outside the United States who are interested in standardization.
Each committee has an
ASTM-assigned staff manager to assist the committee and provide liaison to the parent organization. TABLE 2 D-32 Officers Chairman - R. J. Bertolacini, Amoco oil R&D Producer Vice Chairman - K. I. Jagel, Engelhard User Vice Chairman - R. M. Koros, Exxon R&D General Secretary - D. E. Gross, Monsanto Membership Secretary - F. G. Young, Union Carbide Liaison Chairman - A. H. Neal, Exxon R&D ASTM Staff Manager - A. Cavallero ASTM Committee D-32 is subdivided into four technical subcommittees and three support subcommittees.
These are shown in Table 3.
TABLE 3 Subcommittees Technical Physical-Chemical Properties Physical-Mechanical Properties Chemical Analyses Catalytic Properties Support Nomenclature Editorial Statistics and Data Handling Subcommittee officers are either appointed or elected for each group. The officers include a chairman and vice chairman. subdivided into task groups.
Each subcommittee is fUrther
Their fUnction is to initiate draft standards
769 and revisions.
This is where the work begins.
elected, appointed, or volunteer.
The task group leader can be
As a member of D-32, one chooses the
subcommittee and task groups of interest, and then becomes involved in the standardization process. Previous papers (ref. 1-3) have described the standardization procedure, so we will only briefly review the process. works is illustrated in Figure 1.
How the standardization process
The members of a task group, let's say 1n
the subcommittee on Physical-Chemical Properties, decide that the determination of surface area by a static single-point procedure is an important catalyst characterization method.
Each member is then solicited for a possible proce-
dure to be considered by the task group.
After tentative selection of a method,
reference samples are circulated and each active member tests the samples using the selected procedure.
The resulting data are analyzed and a draft
method written; the method 1S reviewed by the subcommittee through a balloting procedure.
If approved in two-thirds of the ballots returned (a minimum of
60% of the eligible subcommittee voters must return ballots), the document moves on to the full D-32 Committee.
At the committee level, the proposed
document must be approved by 90% of those balloting and again a 60% return is required.
If approved, it moves on to the full ASTM Society ballot.
each member of ASTM has an opportunity to vote on the document.
Now,
Of those
voting, 90% must approve; but before final, official sanction as an ASTM method, the document must be submitted to the Committee on Standards of ASTM.
If the
Committee on Standards of ASTM determines all the Society requirements have been met,
the document is now an approved ASTM standard.
At each step,
from subcommittee through ASTM Society ballot, any negative
ballot must be rigorously considered and reconciled before proceeding.
The
minority opinion must be heard, and only after concensus is reached is the document allowed to proceed to the next step.
The process is deliberate, but
has resulted in over 6,000 ASTM standards.
Fig. 1. Standardization process Now we will concentrate on the methods which have been published and others
770 which are now being evaluated by each subcommittee.
Eight methods have been
standardized and these are conveniently published in a brochure (ref. 4). This is available at nominal cost from ASTM.
In addition, the eight standard
methods are published in Part 25 of the 1982 annual book of standards (ref. 5). This volume includes standards on petroleum and lubricants as well as aerospace materials, so it is considerably more expensive than the brochure; however, the volume 1S available free to ASTM members.
SUBCOMMITTEE ACTIVITIES Physical-Chemical Properties This subcommi ttee has publ i sh ed four standards:
D3663-78, Test for Sur face
Area of Catalysts; D3906-80, Test for Relative Zeolite Diffraction Intensities; D3908-80, Test for Hydrogen Chemisorption on Supported Platinum on Alumina Catalyst by Volumetric Vacuum Method; and D3942-80, Test for Determination of the Unit Cell Dimension of a Faujasite-Type Zeolite.
Currently, the subcom-
mittee is working to improve the precision and accuracy method.
0
f the sur face area
A revision has also been made to the precision and accuracy statement
on the procedure for hydrogen-chemisorption by platinum on alumina catalysts. Several test procedures are in various stages of development.
A test method
for pore-size distribution by mercury intrusion is in the final approval stage. A second test method for measuring pore-size distribution by nitrogen adsorption desorption isotherms is undergoing revision for committee approval. Five procedures are in the early development stage and the subcommittee members are evaluating test procedures and testing reference samples.
These
methods are: (1) Procedure for oxygen chemisorption of silver catalysts on alpha alumina. (2) A dynamic (pulse) procedure for carbon monoxide on platinum-alumina. (3) Nitrogen adsorption for determining effective zeolite content
0
f a catalyst.
(4) X-ray diffraction to estimate gamma-alumina in cracking catalysts. (5) Methods for determining surface acidity of catalysts. Physical-Mechanical Properties This committee has just completed development of a rotating-drum method for measuring attrition-abrasion of formed catalysts. Final revisions are being made on a method for determining the crushing strength of single pellets and spheres. for extruded catalysts.
The method is also being evaluated
Reference samples are being sent to participating
laboratories. Problems in obtaining reproducible results for a test of bulk crushing strength are being resolved by modifications to the procedure.
Interlaboratory
samples incorporating the new modifications are now being tested.
771 The committee 1S also revising methods for vibratory and tapped bulk density for formed catalysts and introducing a project to extend the method to powders. Methods for measuring particle-size distribution using two commercially available automated counting units are now being drafted.
A third method for
evaluating a sonic sifter technique will be circulated next.
The committee is
also reactivating a study for methods to measure the attrition-abrasion of powdered catalyst by jet stream attrition techniques. Chemical Analysis This subcommittee has issued two standards:
D36l0-77, Test for Total Cobalt
1n Alumina-Base Cobalt-Molybdenum Catalysts; and D3943-80, Test for Molybdenum in Fresh Alumina-Base Catalysts.
The group is redrafting a procedure for
determining high nickel concentrations 1n alumina-base catalysts and a method based on atomic absorption for low (up to 6%) concentrations of nickel.
Two
reforming catalysts are being used in interlaboratory tests to develop a procedure for analyzing platinum in fresh alumina-base catalysts. Catalytic Properties This group has issued one standard method, D3907-80, Testing Fluid Cracking Catalysts by Microactivity Test.
They are now working to develop a procedure
for measuring individual component yields (gas, liquid, and coke) microactivity test to determine catalyst selectivity. a companion to the microactivity test.
from the
This procedure would be
Because steaming is a normal pretreat-
ment before measuring fluid cracking catalyst activity, the committee is in the initial stages of developing a procedure to measure steam deactivation. Interlaboratory tests are defining important variables such as temperature, fixed versus fluid bed, and the advisability of using thermal shock.
Several
zeolitic cracking catalysts have been tested and the evaluation is continuing. Nomenclature This group has issued one standard, D3766-80, Definitions of Terms Relating to Catalysts and Catalysis. In addition to the four technical standards subcommittees, D-32 has two special support subcommittees which serve as advisors to the others.
An
Editorial subcommittee holds periodic workshops to diacuss writing formats, research reports, metrication, and other timely topics to assist the other subcommittees in publishing their reports.
A subcommittee on Statistics and
Data Handling works with task groups to advise them on data processing, precision and accuracy statements, and computer programs for data handling. The statistics subcommittee has also developed a computer program to design experiments for interlaboratory testing.
772 Committee D-32 also has an ad hoc committee on Liaison with other ASTM committees and with foreign groups with similar interest in standardization and characterization methods for catalyst testing.
SUMMARY since its organization 1n 1975, ASTM Committee D-32 on Catalysts has expanded its membership from about 70 to 121.
Liaison has been established with others
interested in standardization, including groups in Canada, USSR, Europe, South America, Japan,
Au~tralia
and India.
ASTM encourages this participation by
either active membership in ASTM or cooperation through the liaison chairman. Eight methods have been approved and published as standards. methods are in either the evaluation or development stage.
About 23 test
If the usual time-
table for acceptance is followed, about six of these will be approved as standards during 1982.
Thus far, Committee D-32 has concentrated its efforts
in the area of heterogeneous catalysts closely related to petroleum refining and petrochemicals processing.
However, if there is interest in either other
heterogeneous systems or homogeneous catalysts, the committee 1S willing to develop test procedures to fit these needs. consider any catalyst test procedure.
The committee is willing to
We welcome participation in this work
as active members, cooperating in the tests, or as interested catalytic scientists.
REFERENCES 1 J.R. Kiovsky, Oral communications, Proceedings of the International Symposium on the Relations Between Heterogeneous and Homogeneous Catalytic Phenomena, Brussels, October 23, 1974. 2 A.H. Neal, "Preparation of Catalysts II," B. Delmon, et al., Ed., p.719, Elsevier, Amsterdam, 1979. 3 R.J. Bertolacini, et al., Papers 8a-8e, American Institute of Chemical Engineers, Chicago, November 18, 1980. 4 "ASTM Standard on Catalysts," PCN 06-432080-12, ASTM, 1916 Race Street, Philadelphia, Pennsylvania, 19103. 5 American Society for Testing Materials, 1981 Annual Book of Standards, Part 25, p.1103-1143.
773 DISCUSSION W. RODER: Are there any intentions up to now, to standardize catalytic properties of other catalysts than fluid-cracking-catalysts (for instance hydrocarbon oxidation or methanation ? R.J. BERTOLACINI: There is at present no interest in the USA for developing standard test procedures for hydrocarbon oxidation or methanation. We have discussed the possibility of developing standardized tests for HDS and catalytic reforming but to date, there has been no interest. ASTM Committee D-32 is currently working on a method for measuring selectivity for cracking catalysts, an adaptation of the MAT test. The selectivity testing is in progress and I estimate a standardized procedure should be published in the latter part of 1983 or early 1984. M.F.L. JOHNSON ASTM consciously attempts to write procedures in such a way that it will encompass commercially available equipment as well as home-constructed equipment. R.J. BERTOLACINI Yes, ASTM doe not specify a single commercial unit but rather writes broad apparatus specifications so as to eliminate any conflict of interest M.M. BHASIN: In standardization of catalyst/carrier test methods, are you developing a library of primary standard test samples? Also would you elaborate on how they are stored to ensure they remain primary standards? R.J. BERTOLACINI: Yes, we have a number of reference samples for all of our procedures. These are stored by the supplier under proper conditions to assure their quality. We are attempting to interest commercial specialty chemical supply firms to catalog and sell these items. If this approach does not work out, we have indications that the USA-National Bureau of Standards would be interested in storing and cataloging the samples as reference materials. If the Bureau catalogues the materials, the samples would be available at a nominal cost.
G. Poncelet, P. Grange and P.A. Jacobs (Editors), Preparation of Catalysts III
© 1983 Elsevier Science Publishers B.V., Amsterdam - Printed in The Netherlands
STANDARDIZATION OF CATALYST TEST METHODS R. J. BERTOLACINIl and ARTHUR NEAL2 lAmoco Oil Company, P. O. Box 400, Naperville, Illinois
60566, U.S.A.
2Exxon Corporation, P. O. Box 2226, Baton Rouge, Louisiana
70821, U.S.A.
ABSTRACT This is a report on the progress made by ASTM Committee D-32 on Catalysts since the last paper given at this meeting in 1978. The main committee has seven subcommittees of people with interest and expertise in specific areas related to the main committee. subcommittees is reviewed.
Progress of the
These include catalytic properties, chemical
analysis, physical-chemical properties, physical-mechanical properties, and nomenclature.
Eight standards have been published and approximately 23 others
are at various stages of development in the task groups.
INTRODUCTION Previous speakers at this symposium (ref. 1-2) reviewed the early history of the American Society for Testing Materials, Committee D-32 on Catalysts. The scope of ASTM D-32 is to develop test methods, classifications, recommended practices, and definitions pertaining to catalysts and materials used in their manufacture, and stimulation of research related to catalysts.
For the present,
the catalysts considered have been heterogeneous, but if an interest or demand existed in standards for homogeneous or heterogenized catalysts it would be appropriate for D-32 to consider these system? Since its organization on January 14, 1975, ·the membership has steadily increased and today is 121.
Each member must be classified as having a voting
interest or not and identified as representatives of producers, users, or general interest.
Users represent organizations which either purchase or use
catalysts, and who could not be classified as producers. companies which make and sell catalysts. neither user nor producer.
Producers represent
The general interest category
~s
This category includes private consultants,
instrument and equipment companies, independent laboratories, consumer groups, and university researchers. of D-32.
Table 1 shows the classification for the membership
Only a single vote is allowed to representatives of one institution
or major separate functional division of it. dominate.
We are in good balance.
No interest can be allowed to
768 TABLE 1 Membership classification Users Producers General Interest Unclassified Total
45 52 23 1 121
Fourteen of the 121 members represent eleven foreign countries; n1ne are Europeans, two South Americans, two Canadians, and one Australian.
In addition
to representatives from these countries, we have had contacts with interested researchers in the USSR, Japan, and India. Table 2 shows the current officers of D-32. balance of interest.
Even here, we must maintain a
The chairman cannot be a producer of catalysts.
vice chairmen represent both users and producers.
The two
Committee D-32 has a liaison
chairman who has contact with other organizations and researchers outside the United States who are interested in standardization.
Each committee has an
ASTM-assigned staff manager to assist the committee and provide liaison to the parent organization. TABLE 2 D-32 Officers Chairman - R. J. Bertolacini, Amoco oil R&D Producer Vice Chairman - K. I. Jagel, Engelhard User Vice Chairman - R. M. Koros, Exxon R&D General Secretary - D. E. Gross, Monsanto Membership Secretary - F. G. Young, Union Carbide Liaison Chairman - A. H. Neal, Exxon R&D ASTM Staff Manager - A. Cavallero ASTM Committee D-32 is subdivided into four technical subcommittees and three support subcommittees.
These are shown in Table 3.
TABLE 3 Subcommittees Technical Physical-Chemical Properties Physical-Mechanical Properties Chemical Analyses Catalytic Properties Support Nomenclature Editorial Statistics and Data Handling Subcommittee officers are either appointed or elected for each group. The officers include a chairman and vice chairman. subdivided into task groups.
Each subcommittee is fUrther
Their fUnction is to initiate draft standards
769 and revisions.
This is where the work begins.
elected, appointed, or volunteer.
The task group leader can be
As a member of D-32, one chooses the
subcommittee and task groups of interest, and then becomes involved in the standardization process. Previous papers (ref. 1-3) have described the standardization procedure, so we will only briefly review the process. works is illustrated in Figure 1.
How the standardization process
The members of a task group, let's say 1n
the subcommittee on Physical-Chemical Properties, decide that the determination of surface area by a static single-point procedure is an important catalyst characterization method.
Each member is then solicited for a possible proce-
dure to be considered by the task group.
After tentative selection of a method,
reference samples are circulated and each active member tests the samples using the selected procedure.
The resulting data are analyzed and a draft
method written; the method 1S reviewed by the subcommittee through a balloting procedure.
If approved in two-thirds of the ballots returned (a minimum of
60% of the eligible subcommittee voters must return ballots), the document moves on to the full D-32 Committee.
At the committee level, the proposed
document must be approved by 90% of those balloting and again a 60% return is required.
If approved, it moves on to the full ASTM Society ballot.
each member of ASTM has an opportunity to vote on the document.
Now,
Of those
voting, 90% must approve; but before final, official sanction as an ASTM method, the document must be submitted to the Committee on Standards of ASTM.
If the
Committee on Standards of ASTM determines all the Society requirements have been met,
the document is now an approved ASTM standard.
At each step,
from subcommittee through ASTM Society ballot, any negative
ballot must be rigorously considered and reconciled before proceeding.
The
minority opinion must be heard, and only after concensus is reached is the document allowed to proceed to the next step.
The process is deliberate, but
has resulted in over 6,000 ASTM standards.
Fig. 1. Standardization process Now we will concentrate on the methods which have been published and others
770 which are now being evaluated by each subcommittee.
Eight methods have been
standardized and these are conveniently published in a brochure (ref. 4). This is available at nominal cost from ASTM.
In addition, the eight standard
methods are published in Part 25 of the 1982 annual book of standards (ref. 5). This volume includes standards on petroleum and lubricants as well as aerospace materials, so it is considerably more expensive than the brochure; however, the volume 1S available free to ASTM members.
SUBCOMMITTEE ACTIVITIES Physical-Chemical Properties This subcommi ttee has publ i sh ed four standards:
D3663-78, Test for Sur face
Area of Catalysts; D3906-80, Test for Relative Zeolite Diffraction Intensities; D3908-80, Test for Hydrogen Chemisorption on Supported Platinum on Alumina Catalyst by Volumetric Vacuum Method; and D3942-80, Test for Determination of the Unit Cell Dimension of a Faujasite-Type Zeolite.
Currently, the subcom-
mittee is working to improve the precision and accuracy method.
0
f the sur face area
A revision has also been made to the precision and accuracy statement
on the procedure for hydrogen-chemisorption by platinum on alumina catalysts. Several test procedures are in various stages of development.
A test method
for pore-size distribution by mercury intrusion is in the final approval stage. A second test method for measuring pore-size distribution by nitrogen adsorption desorption isotherms is undergoing revision for committee approval. Five procedures are in the early development stage and the subcommittee members are evaluating test procedures and testing reference samples.
These
methods are: (1) Procedure for oxygen chemisorption of silver catalysts on alpha alumina. (2) A dynamic (pulse) procedure for carbon monoxide on platinum-alumina. (3) Nitrogen adsorption for determining effective zeolite content
0
f a catalyst.
(4) X-ray diffraction to estimate gamma-alumina in cracking catalysts. (5) Methods for determining surface acidity of catalysts. Physical-Mechanical Properties This committee has just completed development of a rotating-drum method for measuring attrition-abrasion of formed catalysts. Final revisions are being made on a method for determining the crushing strength of single pellets and spheres. for extruded catalysts.
The method is also being evaluated
Reference samples are being sent to participating
laboratories. Problems in obtaining reproducible results for a test of bulk crushing strength are being resolved by modifications to the procedure.
Interlaboratory
samples incorporating the new modifications are now being tested.
771 The committee 1S also revising methods for vibratory and tapped bulk density for formed catalysts and introducing a project to extend the method to powders. Methods for measuring particle-size distribution using two commercially available automated counting units are now being drafted.
A third method for
evaluating a sonic sifter technique will be circulated next.
The committee is
also reactivating a study for methods to measure the attrition-abrasion of powdered catalyst by jet stream attrition techniques. Chemical Analysis This subcommittee has issued two standards:
D36l0-77, Test for Total Cobalt
1n Alumina-Base Cobalt-Molybdenum Catalysts; and D3943-80, Test for Molybdenum in Fresh Alumina-Base Catalysts.
The group is redrafting a procedure for
determining high nickel concentrations 1n alumina-base catalysts and a method based on atomic absorption for low (up to 6%) concentrations of nickel.
Two
reforming catalysts are being used in interlaboratory tests to develop a procedure for analyzing platinum in fresh alumina-base catalysts. Catalytic Properties This group has issued one standard method, D3907-80, Testing Fluid Cracking Catalysts by Microactivity Test.
They are now working to develop a procedure
for measuring individual component yields (gas, liquid, and coke) microactivity test to determine catalyst selectivity. a companion to the microactivity test.
from the
This procedure would be
Because steaming is a normal pretreat-
ment before measuring fluid cracking catalyst activity, the committee is in the initial stages of developing a procedure to measure steam deactivation. Interlaboratory tests are defining important variables such as temperature, fixed versus fluid bed, and the advisability of using thermal shock.
Several
zeolitic cracking catalysts have been tested and the evaluation is continuing. Nomenclature This group has issued one standard, D3766-80, Definitions of Terms Relating to Catalysts and Catalysis. In addition to the four technical standards subcommittees, D-32 has two special support subcommittees which serve as advisors to the others.
An
Editorial subcommittee holds periodic workshops to diacuss writing formats, research reports, metrication, and other timely topics to assist the other subcommittees in publishing their reports.
A subcommittee on Statistics and
Data Handling works with task groups to advise them on data processing, precision and accuracy statements, and computer programs for data handling. The statistics subcommittee has also developed a computer program to design experiments for interlaboratory testing.
772 Committee D-32 also has an ad hoc committee on Liaison with other ASTM committees and with foreign groups with similar interest in standardization and characterization methods for catalyst testing.
SUMMARY since its organization 1n 1975, ASTM Committee D-32 on Catalysts has expanded its membership from about 70 to 121.
Liaison has been established with others
interested in standardization, including groups in Canada, USSR, Europe, South America, Japan,
Au~tralia
and India.
ASTM encourages this participation by
either active membership in ASTM or cooperation through the liaison chairman. Eight methods have been approved and published as standards. methods are in either the evaluation or development stage.
About 23 test
If the usual time-
table for acceptance is followed, about six of these will be approved as standards during 1982.
Thus far, Committee D-32 has concentrated its efforts
in the area of heterogeneous catalysts closely related to petroleum refining and petrochemicals processing.
However, if there is interest in either other
heterogeneous systems or homogeneous catalysts, the committee 1S willing to develop test procedures to fit these needs. consider any catalyst test procedure.
The committee is willing to
We welcome participation in this work
as active members, cooperating in the tests, or as interested catalytic scientists.
REFERENCES 1 J.R. Kiovsky, Oral communications, Proceedings of the International Symposium on the Relations Between Heterogeneous and Homogeneous Catalytic Phenomena, Brussels, October 23, 1974. 2 A.H. Neal, "Preparation of Catalysts II," B. Delmon, et al., Ed., p.719, Elsevier, Amsterdam, 1979. 3 R.J. Bertolacini, et al., Papers 8a-8e, American Institute of Chemical Engineers, Chicago, November 18, 1980. 4 "ASTM Standard on Catalysts," PCN 06-432080-12, ASTM, 1916 Race Street, Philadelphia, Pennsylvania, 19103. 5 American Society for Testing Materials, 1981 Annual Book of Standards, Part 25, p.1103-1143.
773 DISCUSSION W. RODER: Are there any intentions up to now, to standardize catalytic properties of other catalysts than fluid-cracking-catalysts (for instance hydrocarbon oxidation or methanation ? R.J. BERTOLACINI: There is at present no interest in the USA for developing standard test procedures for hydrocarbon oxidation or methanation. We have discussed the possibility of developing standardized tests for HDS and catalytic reforming but to date, there has been no interest. ASTM Committee D-32 is currently working on a method for measuring selectivity for cracking catalysts, an adaptation of the MAT test. The selectivity testing is in progress and I estimate a standardized procedure should be published in the latter part of 1983 or early 1984. M.F.L. JOHNSON ASTM consciously attempts to write procedures in such a way that it will encompass commercially available equipment as well as home-constructed equipment. R.J. BERTOLACINI Yes, ASTM doe not specify a single commercial unit but rather writes broad apparatus specifications so as to eliminate any conflict of interest M.M. BHASIN: In standardization of catalyst/carrier test methods, are you developing a library of primary standard test samples? Also would you elaborate on how they are stored to ensure they remain primary standards? R.J. BERTOLACINI: Yes, we have a number of reference samples for all of our procedures. These are stored by the supplier under proper conditions to assure their quality. We are attempting to interest commercial specialty chemical supply firms to catalog and sell these items. If this approach does not work out, we have indications that the USA-National Bureau of Standards would be interested in storing and cataloging the samples as reference materials. If the Bureau catalogues the materials, the samples would be available at a nominal cost.