ASTM D4463/D4463M-19
(Guide)Standard Guide for Metals Free Steam Deactivation of Fresh Fluid Cracking Catalysts
Standard Guide for Metals Free Steam Deactivation of Fresh Fluid Cracking Catalysts
SIGNIFICANCE AND USE
4.1 In general, steam treatment of FCC catalyst can be used either to compare a series of cracking catalysts at a simulated equilibrium condition or conditions, or to simulate the equilibrium condition of a specific cracking unit and a specific catalyst. This guide gives an example for the first purpose and an approach for the latter purpose.
SCOPE
1.1 This guide covers the deactivation of fresh fluid catalytic cracking (FCC) catalyst by hydrothermal treatment prior to the determination of the catalytic cracking activity in the microactivity test (MAT) or the Advanced Cracking Evaluation (ACE) test.
1.2 The hydrothermal treatment of fresh FCC catalyst, prior to the MAT or the ACE test, is important because the catalytic activity of the catalyst in its fresh state is an inadequate measure of its true commercial performance. During operation in a commercial cracking unit, the catalyst is deactivated by thermal, hydrothermal, and chemical degradation. Therefore, to maintain catalytic activity, fresh catalyst is added (semi) continuously to the cracking unit, to replace catalyst lost through the stack or by withdrawal, or both. Under steady state conditions, the catalyst inventory of the unit is called equilibrium catalyst. This catalyst has an activity level substantially below that of fresh catalyst. Therefore, artificially deactivating a fresh catalyst prior to determination of its cracking activity should provide more meaningful catalyst performance data.
1.3 Due to the large variations in properties among fresh FCC catalyst types as well as between commercial cracking unit designs or operating conditions, or both, no single set of steam deactivation conditions is adequate to artificially simulate the equilibrium catalyst for all purposes.
1.3.1 In addition, there are many other factors that will influence the properties and performance of the equilibrium catalyst. These include, but are not limited to: deposition of heavy metals such as Ni, V, and Cu; deposition of light metals such as Na; and contamination from attrited refractory linings of vessel walls. Furthermore, commercially derived equilibrium catalyst represents a distribution of catalysts of different ages (from fresh to >300 days). Despite these apparent problems, it is possible to obtain reasonably close agreement between the performances of steam deactivated and equilibrium catalysts. It is also recognized that it is possible to steam deactivate a catalyst so that its properties and performance poorly represent the equilibrium. It is therefore recommended that when assessing the performance of different catalyst types, a common steaming condition be used. Catalyst deactivation by metals deposition is not addressed in this guide, but is addressed in Guide D7206/D7206M.
1.4 This guide offers two approaches to steam deactivate fresh catalysts. The first part provides specific sets of conditions (time, temperature, and steam pressure) that can be used as general pre-treatments prior to comparison of fresh FCC catalyst MAT activities (Test Method D3907) or activities plus selectivities (Test Methods D5154 and D7964).
1.4.1 The second part provides guidance on how to pretreat catalysts to simulate their deactivation in a specific FCCU and suggests catalyst properties which can be used to judge adequacy of the simulation. This technique is especially useful when examining how different types of catalyst may perform in a specific FCCU, provided no other changes (catalyst addition rate, regenerator temperature, contaminant metals levels, etc.) occur. This approach covers catalyst physical properties that can be used as monitors to indicate the closeness to equilibrium catalyst properties.
1.5 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each s...
General Information
- Status
- Published
- Publication Date
- 31-Mar-2019
- Technical Committee
- D32 - Catalysts
- Drafting Committee
- D32.04 - Catalytic Properties
Relations
- Effective Date
- 01-Apr-2022
- Refers
ASTM D4365-19 - Standard Test Method for Determining Micropore Volume and Zeolite Area of a Catalyst - Effective Date
- 01-Jul-2019
- Effective Date
- 01-Apr-2019
- Effective Date
- 01-Apr-2019
- Effective Date
- 01-Oct-2017
- Effective Date
- 01-Oct-2017
- Effective Date
- 01-May-2014
- Effective Date
- 01-Dec-2013
- Effective Date
- 15-Nov-2013
- Effective Date
- 15-Nov-2013
- Effective Date
- 15-Nov-2013
- Effective Date
- 15-Nov-2013
- Effective Date
- 15-Aug-2013
- Effective Date
- 01-May-2013
- Effective Date
- 01-May-2013
Overview
ASTM D4463/D4463M-19 is the standard guide for the metals-free steam deactivation of fresh fluid catalytic cracking (FCC) catalysts. Issued by ASTM International, this guide provides crucial methodology for simulating the deactivation of FCC catalysts through controlled hydrothermal treatment with steam. The aim is to create representative catalyst conditions closely resembling those found in commercial fluid catalytic cracking units, enabling more accurate and relevant performance testing.
In commercial FCC operations, catalysts undergo significant changes due to thermal, hydrothermal, and chemical stresses, leading to decreased activity over time. Since fresh catalyst performance does not reflect the real-world environment of an FCC unit, pre-treatment by steam deactivation is essential for reliable evaluations using standard industry tests such as the Microactivity Test (MAT) and Advanced Cracking Evaluation (ACE) test.
Key Topics
- Hydrothermal Deactivation Methods: The guide outlines procedures for both fixed bed and fluid bed reactors to partially deactivate fresh FCC catalyst samples using steam at elevated temperatures, typically between 700°C and 850°C.
- Simulation of Equilibrium Catalyst: Two main approaches are emphasized:
- General pre-treatment for comparative testing between catalysts.
- Custom deactivation to simulate specific commercial equilibrium catalyst conditions from a particular FCC unit.
- Impact Factors: The standard recognizes the influence of factors such as unit design, operating parameters, and catalyst composition, making it clear that no single set of steaming conditions suits all purposes.
- Exclusions: The guide specifically excludes deactivation by metals contamination, referring users to ASTM D7206/D7206M for those protocols.
- Physical Property Indicators: Key properties for evaluating the match between steamed and equilibrium catalysts include MAT conversion (activity), selectivity to by-products, zeolite unit cell size, and surface area measurements.
Applications
ASTM D4463/D4463M-19 is heavily utilized in the petroleum refining industry and catalyst manufacturing sector. Its primary applications include:
- Pre-Treatment for Testing: Artificial deactivation of fresh FCC catalysts prior to laboratory activity tests ensures that performance evaluations reflect real-world, steady-state operation in FCC units.
- Catalyst Comparison: Enables fair and meaningful comparison of candidate catalysts by subjecting all to consistent steam deactivation conditions before performance testing.
- Performance Simulation: Assists refiners in predicting how new or modified catalysts will perform in their specific FCC unit by matching hydrothermal treatment parameters to those experienced in the plant.
- Quality Control: Provides repeatable procedures that help laboratories and manufacturers maintain consistency and reliability in FCC catalyst assessment.
These uses support improved decision-making for catalyst selection, process optimization, and technological innovation in fluid catalytic cracking operations.
Related Standards
ASTM D4463/D4463M-19 references and complements several other ASTM standards, including:
- ASTM D3907 - Microactivity Test for FCC Catalysts
- ASTM D5154, D7964 - Methods for Determining Activity and Selectivity in FCC Catalysts
- ASTM D3663, D3942, D4365 - Surface area and micropore volume measurements for catalysts
- ASTM D7206/D7206M - Guide for cyclic deactivation of FCC catalysts with metals
- ASTM E105, E177, E456, E691 - Sampling and statistical terms and methods relevant to quality and reliability in laboratory testing
By adhering to these interconnected standards, laboratories and refineries can ensure data accuracy, improved representativeness, and compliance with international best practices for FCC catalyst evaluation.
Keywords: fluid catalytic cracking, FCC catalyst, hydrothermal treatment, steam deactivation, equilibrium catalyst, MAT test, catalyst pre-treatment, ASTM D4463/D4463M, catalyst performance testing, petroleum refining.
Buy Documents
ASTM D4463/D4463M-19 - Standard Guide for Metals Free Steam Deactivation of Fresh Fluid Cracking Catalysts
REDLINE ASTM D4463/D4463M-19 - Standard Guide for Metals Free Steam Deactivation of Fresh Fluid Cracking Catalysts
Get Certified
Connect with accredited certification bodies for this standard
ECOCERT
Organic and sustainability certification.
Eurofins Food Testing Global
Global leader in food, environment, and pharmaceutical product testing.
Intertek Bangladesh
Intertek certification and testing services in Bangladesh.
Sponsored listings
Frequently Asked Questions
ASTM D4463/D4463M-19 is a guide published by ASTM International. Its full title is "Standard Guide for Metals Free Steam Deactivation of Fresh Fluid Cracking Catalysts". This standard covers: SIGNIFICANCE AND USE 4.1 In general, steam treatment of FCC catalyst can be used either to compare a series of cracking catalysts at a simulated equilibrium condition or conditions, or to simulate the equilibrium condition of a specific cracking unit and a specific catalyst. This guide gives an example for the first purpose and an approach for the latter purpose. SCOPE 1.1 This guide covers the deactivation of fresh fluid catalytic cracking (FCC) catalyst by hydrothermal treatment prior to the determination of the catalytic cracking activity in the microactivity test (MAT) or the Advanced Cracking Evaluation (ACE) test. 1.2 The hydrothermal treatment of fresh FCC catalyst, prior to the MAT or the ACE test, is important because the catalytic activity of the catalyst in its fresh state is an inadequate measure of its true commercial performance. During operation in a commercial cracking unit, the catalyst is deactivated by thermal, hydrothermal, and chemical degradation. Therefore, to maintain catalytic activity, fresh catalyst is added (semi) continuously to the cracking unit, to replace catalyst lost through the stack or by withdrawal, or both. Under steady state conditions, the catalyst inventory of the unit is called equilibrium catalyst. This catalyst has an activity level substantially below that of fresh catalyst. Therefore, artificially deactivating a fresh catalyst prior to determination of its cracking activity should provide more meaningful catalyst performance data. 1.3 Due to the large variations in properties among fresh FCC catalyst types as well as between commercial cracking unit designs or operating conditions, or both, no single set of steam deactivation conditions is adequate to artificially simulate the equilibrium catalyst for all purposes. 1.3.1 In addition, there are many other factors that will influence the properties and performance of the equilibrium catalyst. These include, but are not limited to: deposition of heavy metals such as Ni, V, and Cu; deposition of light metals such as Na; and contamination from attrited refractory linings of vessel walls. Furthermore, commercially derived equilibrium catalyst represents a distribution of catalysts of different ages (from fresh to >300 days). Despite these apparent problems, it is possible to obtain reasonably close agreement between the performances of steam deactivated and equilibrium catalysts. It is also recognized that it is possible to steam deactivate a catalyst so that its properties and performance poorly represent the equilibrium. It is therefore recommended that when assessing the performance of different catalyst types, a common steaming condition be used. Catalyst deactivation by metals deposition is not addressed in this guide, but is addressed in Guide D7206/D7206M. 1.4 This guide offers two approaches to steam deactivate fresh catalysts. The first part provides specific sets of conditions (time, temperature, and steam pressure) that can be used as general pre-treatments prior to comparison of fresh FCC catalyst MAT activities (Test Method D3907) or activities plus selectivities (Test Methods D5154 and D7964). 1.4.1 The second part provides guidance on how to pretreat catalysts to simulate their deactivation in a specific FCCU and suggests catalyst properties which can be used to judge adequacy of the simulation. This technique is especially useful when examining how different types of catalyst may perform in a specific FCCU, provided no other changes (catalyst addition rate, regenerator temperature, contaminant metals levels, etc.) occur. This approach covers catalyst physical properties that can be used as monitors to indicate the closeness to equilibrium catalyst properties. 1.5 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each s...
SIGNIFICANCE AND USE 4.1 In general, steam treatment of FCC catalyst can be used either to compare a series of cracking catalysts at a simulated equilibrium condition or conditions, or to simulate the equilibrium condition of a specific cracking unit and a specific catalyst. This guide gives an example for the first purpose and an approach for the latter purpose. SCOPE 1.1 This guide covers the deactivation of fresh fluid catalytic cracking (FCC) catalyst by hydrothermal treatment prior to the determination of the catalytic cracking activity in the microactivity test (MAT) or the Advanced Cracking Evaluation (ACE) test. 1.2 The hydrothermal treatment of fresh FCC catalyst, prior to the MAT or the ACE test, is important because the catalytic activity of the catalyst in its fresh state is an inadequate measure of its true commercial performance. During operation in a commercial cracking unit, the catalyst is deactivated by thermal, hydrothermal, and chemical degradation. Therefore, to maintain catalytic activity, fresh catalyst is added (semi) continuously to the cracking unit, to replace catalyst lost through the stack or by withdrawal, or both. Under steady state conditions, the catalyst inventory of the unit is called equilibrium catalyst. This catalyst has an activity level substantially below that of fresh catalyst. Therefore, artificially deactivating a fresh catalyst prior to determination of its cracking activity should provide more meaningful catalyst performance data. 1.3 Due to the large variations in properties among fresh FCC catalyst types as well as between commercial cracking unit designs or operating conditions, or both, no single set of steam deactivation conditions is adequate to artificially simulate the equilibrium catalyst for all purposes. 1.3.1 In addition, there are many other factors that will influence the properties and performance of the equilibrium catalyst. These include, but are not limited to: deposition of heavy metals such as Ni, V, and Cu; deposition of light metals such as Na; and contamination from attrited refractory linings of vessel walls. Furthermore, commercially derived equilibrium catalyst represents a distribution of catalysts of different ages (from fresh to >300 days). Despite these apparent problems, it is possible to obtain reasonably close agreement between the performances of steam deactivated and equilibrium catalysts. It is also recognized that it is possible to steam deactivate a catalyst so that its properties and performance poorly represent the equilibrium. It is therefore recommended that when assessing the performance of different catalyst types, a common steaming condition be used. Catalyst deactivation by metals deposition is not addressed in this guide, but is addressed in Guide D7206/D7206M. 1.4 This guide offers two approaches to steam deactivate fresh catalysts. The first part provides specific sets of conditions (time, temperature, and steam pressure) that can be used as general pre-treatments prior to comparison of fresh FCC catalyst MAT activities (Test Method D3907) or activities plus selectivities (Test Methods D5154 and D7964). 1.4.1 The second part provides guidance on how to pretreat catalysts to simulate their deactivation in a specific FCCU and suggests catalyst properties which can be used to judge adequacy of the simulation. This technique is especially useful when examining how different types of catalyst may perform in a specific FCCU, provided no other changes (catalyst addition rate, regenerator temperature, contaminant metals levels, etc.) occur. This approach covers catalyst physical properties that can be used as monitors to indicate the closeness to equilibrium catalyst properties. 1.5 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each s...
ASTM D4463/D4463M-19 is classified under the following ICS (International Classification for Standards) categories: 71.040.30 - Chemical reagents. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM D4463/D4463M-19 has the following relationships with other standards: It is inter standard links to ASTM E456-13a(2022)e1, ASTM D4365-19, ASTM D3942-19, ASTM D7206/D7206M-19, ASTM E456-13A(2017)e1, ASTM E456-13A(2017)e3, ASTM E177-14, ASTM D3942-03(2013), ASTM E456-13a, ASTM E456-13ae3, ASTM E456-13ae1, ASTM E456-13ae2, ASTM E456-13, ASTM E691-13, ASTM E177-13. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM D4463/D4463M-19 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4463/D4463M − 19
Standard Guide for
Metals Free Steam Deactivation of Fresh Fluid Cracking
Catalysts
This standard is issued under the fixed designation D4463/D4463M; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope rium catalysts. It is also recognized that it is possible to steam
deactivate a catalyst so that its properties and performance
1.1 This guide covers the deactivation of fresh fluid cata-
poorly represent the equilibrium. It is therefore recommended
lytic cracking (FCC) catalyst by hydrothermal treatment prior
thatwhenassessingtheperformanceofdifferentcatalysttypes,
to the determination of the catalytic cracking activity in the
a common steaming condition be used. Catalyst deactivation
microactivitytest(MAT)ortheAdvancedCrackingEvaluation
by metals deposition is not addressed in this guide, but is
(ACE) test.
addressed in Guide D7206/D7206M.
1.2 The hydrothermal treatment of fresh FCC catalyst, prior
1.4 This guide offers two approaches to steam deactivate
to the MAT or theACE test, is important because the catalytic
fresh catalysts. The first part provides specific sets of condi-
activity of the catalyst in its fresh state is an inadequate
tions (time, temperature, and steam pressure) that can be used
measure of its true commercial performance. During operation
as general pre-treatments prior to comparison of fresh FCC
in a commercial cracking unit, the catalyst is deactivated by
catalyst MAT activities (Test Method D3907) or activities plus
thermal, hydrothermal, and chemical degradation. Therefore,
selectivities (Test Methods D5154 and D7964).
to maintain catalytic activity, fresh catalyst is added (semi)
1.4.1 The second part provides guidance on how to pretreat
continuously to the cracking unit, to replace catalyst lost
catalysts to simulate their deactivation in a specific FCCU and
through the stack or by withdrawal, or both. Under steady state
suggests catalyst properties which can be used to judge
conditions, the catalyst inventory of the unit is called equilib-
adequacy of the simulation. This technique is especially useful
rium catalyst. This catalyst has an activity level substantially
whenexamininghowdifferenttypesofcatalystmayperformin
below that of fresh catalyst. Therefore, artificially deactivating
a specific FCCU, provided no other changes (catalyst addition
a fresh catalyst prior to determination of its cracking activity
rate, regenerator temperature, contaminant metals levels, etc.)
should provide more meaningful catalyst performance data.
occur. This approach covers catalyst physical properties that
1.3 Due to the large variations in properties among fresh
canbeusedasmonitorstoindicatetheclosenesstoequilibrium
FCC catalyst types as well as between commercial cracking
catalyst properties.
unit designs or operating conditions, or both, no single set of
steam deactivation conditions is adequate to artificially simu- 1.5 The values stated in either SI units or inch-pound units
late the equilibrium catalyst for all purposes. are to be regarded separately as standard. The values stated in
1.3.1 In addition, there are many other factors that will each system are not necessarily exact equivalents; therefore, to
influence the properties and performance of the equilibrium ensure conformance with the standard, each system shall be
catalyst. These include, but are not limited to: deposition of used independently of the other, and values from the two
heavy metals such as Ni, V, and Cu; deposition of light metals systems shall not be combined.
such as Na; and contamination from attrited refractory linings
1.6 This standard does not purport to address all of the
of vessel walls. Furthermore, commercially derived equilib-
safety concerns, if any, associated with its use. It is the
rium catalyst represents a distribution of catalysts of different
responsibility of the user of this standard to establish appro-
ages (from fresh to >300 days). Despite these apparent
priate safety, health, and environmental practices and deter-
problems, it is possible to obtain reasonably close agreement
mine the applicability of regulatory limitations prior to use.
between the performances of steam deactivated and equilib-
1.7 This international standard was developed in accor-
dance with internationally recognized principles on standard-
This guide is under the jurisdiction ofASTM Committee D32 on Catalysts and
ization established in the Decision on Principles for the
is the direct responsibility of Subcommittee D32.04 on Catalytic Properties.
Development of International Standards, Guides and Recom-
Current edition approved April 1, 2019. Published April 2019. Originally
mendations issued by the World Trade Organization Technical
approved in 1985. Last previous edition approved in 2013 as D4463/
ɛ1
D4463M–96(2013) . DOI: 10.1520/D4463_D4463M-19. Barriers to Trade (TBT) Committee.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4463/D4463M − 19
2. Referenced Documents 5.3 Temperature control during steam treatment is critical,
2 as temperature variations of 62°C [63.6 °F] can lead to
2.1 ASTM Standards:
61 mass % conversion changes or more, especially at higher
D3663 Test Method for Surface Area of Catalysts and
temperatures.
Catalyst Carriers
D3907 Test Method for Testing Fluid Catalytic Cracking 5.4 In fixed bed steaming, the temperature gradient through
(FCC) Catalysts by Microactivity Test the catalyst bed should be kept as small as possible and should
D3942 Test Method for Determination of the Unit Cell not exceed 4 °C [7.2 °F]. In fluid bed steaming the bed
Dimension of a Faujasite-Type Zeolite temperature must be homogeneous.
D4365 Test Method for Determining Micropore Volume and
5.5 Heating and cooling of the catalyst must be performed
Zeolite Area of a Catalyst
in the reactor under a flow of dry nitrogen.
D5154 TestMethodforDeterminingActivityandSelectivity
5.6 Precautions must be taken to achieve uniform contact of
of Fluid Catalytic Cracking (FCC) Catalysts by Microac-
the steam with the bed.
tivity Test
D7206/D7206M Guide for Cyclic Deactivation of Fluid
6. Sampling
Catalytic Cracking (FCC) Catalysts with Metals
D7964 Test Method for DeterminingActivity of Fluid Cata-
6.1 Asuitable sampling procedure is needed. Practice E105
lytic Cracking (FCC) Catalysts in a Fluidized Bed
is appropriate.
E105 Practice for Probability Sampling of Materials
E177 Practice for Use of the Terms Precision and Bias in
7. Sample Preparation
ASTM Test Methods
7.1 No sample preparation is necessary if the catalyst is
E456 Terminology Relating to Quality and Statistics
heated slowly during preheating (non-shock steaming).
E691 Practice for Conducting an Interlaboratory Study to
7.2 If the sample is introduced directly into a preheated
Determine the Precision of a Test Method
steaming reactor (shock-steaming), it is desirable to predry the
sample for about 1 h at about 550 °C [1022 °F] to prevent
3. Summary of Guide
excessive catalyst loss.
3.1 A sample of fresh fluid cracking catalyst is placed in a
reactor, either fixed bed or preferably fluid bed, and is
8. Procedure
contacted with steam at elevated temperature. This treatment
8.1 Procedure for Fluid Bed and Fixed Bed Steam Treat-
causes partial deactivation of the catalyst.
ment (Non-shock Steaming):
NOTE 1—In a fixed bed reactor, material containing sulfates, chlorides,
8.1.1 With the reactor heated to 300 °C [572 °F] or lower,
etc. can result in significant additional chemical deactivation.
load the reactor with catalyst.
3.2 The catalyst is withdrawn from the reactor and may be
8.1.2 Start nitrogen flow to the reactor at a flow velocity of
subjected to an activity or activity plus selectivity
3 cm/s [0.1 ft/s].
determination, by using the microactivity test (Test Methods
8.1.3 Heat the reactor at the maximum rate until a tempera-
D3907 or D5154) or ACE test (Test Method D7964).
ture of 600 °C [1112 °F] is reached.
8.1.4 Keep the temperature constant at 600 °C [1112 °F] for
4. Significance and Use
30 min in order to remove volatile material from the catalyst.
8.1.5 Heat the reactor at the maximum rate until the desired
4.1 In general, steam treatment of FCC catalyst can be used
either to compare a series of cracking catalysts at a simulated steaming temperature is reached; for example, at 760, 788, or
800 °C [1400, 1450, or 1472 °F] 62°C[63.6 °F].
equilibrium condition or conditions,
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D4463/D4463M − 96 (Reapproved 2013) D4463/D4463M − 19
Standard Guide for
Metals Free Steam Deactivation of Fresh Fluid Cracking
Catalysts
This standard is issued under the fixed designation D4463/D4463M; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Editorially changed 1.3.1 and 2.1 in March 2013.
1. Scope
1.1 This guide covers the deactivation of fresh fluid catalytic cracking (FCC) catalyst by hydrothermal treatment prior to the
determination of the catalytic cracking activity in the microactivity test (MAT).(MAT) or the Advanced Cracking Evaluation (ACE)
test.
1.2 The hydrothermal treatment of fresh FCC catalyst, prior to the MAT, MAT or the ACE test, is important because the catalytic
activity of the catalyst in its fresh state is an inadequate measure of its true commercial performance. During operation in a
commercial cracking unit, the catalyst is deactivated by thermal, hydrothermal, and chemical degradation. Therefore, to maintain
catalytic activity, fresh catalyst is added (semi) continuously to the cracking unit, to replace catalyst lost through the stack or by
withdrawal, or both. Under steady state conditions, the catalyst inventory of the unit is called equilibrium catalyst. This catalyst
has an activity level substantially below that of fresh catalyst. Therefore, artificially deactivating a fresh catalyst prior to
determination of its cracking activity should provide more meaningful catalyst performance data.
1.3 Due to the large variations in properties among fresh FCC catalyst types as well as between commercial cracking unit
designs or operating conditions, or both, no single set of steam deactivation conditions is adequate to artificially simulate the
equilibrium catalyst for all purposes.
1.3.1 In addition, there are many other factors that will influence the properties and performance of the equilibrium catalyst.
These include, but are not limited to: deposition of heavy metals such as Ni, V, and Cu; deposition of light metals such as Na; and
contamination from attrited refractory linings of vessel walls. Furthermore, commercially derived equilibrium catalyst represents
a distribution of catalysts of different ages (from fresh to >300 days). Despite these apparent problems, it is possible to obtain
reasonably close agreement between the performances of steam deactivated and equilibrium catalysts. It is also recognized that it
is possible to steam deactivate a catalyst so that its properties and performance poorly represent the equilibrium. It is therefore
recommended that when assessing the performance of different catalyst types, a common steaming condition be used. Catalyst
deactivation by metals deposition is not addressed in this guide, but is addressed in Guide D7206/D7206M.
1.4 This guide offers two approaches to steam deactivate fresh catalysts. The first part provides specific sets of conditions (time,
temperature, and steam pressure) that can be used as general pre-treatments prior to comparison of fresh FCC catalyst MAT
activities (Test Method D3907) or activities plus selectivities (Test MethodMethods D5154 and D7964).
1.4.1 The second part provides guidance on how to pretreat catalysts to simulate their deactivation in a specific FCCU and
suggests catalyst properties which can be used to judge adequacy of the simulation. This technique is especially useful when
examining how different types of catalyst may perform in a specific FCCU, provided no other changes (catalyst addition rate,
regenerator temperature, contaminant metals levels, etc.) occur. This approach covers catalyst physical properties that can be used
as monitors to indicate the closeness to equilibrium catalyst properties.
1.5 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each
system mayare not benecessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used
independently of the other. Combiningother, and values from the two systems may result in non-conformance with the
standard.shall not be combined.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
This guide is under the jurisdiction of ASTM Committee D32 on Catalysts and is the direct responsibility of Subcommittee D32.04 on Catalytic Properties.
Current edition approved March 1, 2013April 1, 2019. Published March 2013April 2019. Originally approved in 1985. Last previous edition approved in 20122013 as
ɛ1
D4463/D4463M–96(2012)D4463/D4463M–96(2013) e1. DOI: 10.1520/D4463_D4463M-96R13E01.10.1520/D4463_D4463M-19.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4463/D4463M − 19
1.7 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D3663 Test Method for Surface Area of Catalysts and Catalyst Carriers
D3907 Test Method for Testing Fluid Catalytic Cracking (FCC) Catalysts by Microactivity Test
D3942 Test Method for Determination of the Unit Cell Dimension of a Faujasite-Type Zeolite
D4365 Test Method for Determining Micropore Volume and Zeolite Area of a Catalyst
D5154 Test Method for Determining Activity and Selectivity of Fluid Catalytic Cracking (FCC) Catalysts by Microactivity Test
D7206/D7206M Guide for Cyclic Deactivation of Fluid Catalytic Cracking (FCC) Catalysts with Metals
D7964 Test Method for Determining Activity of Fluid Catalytic Cracking (FCC) Catalysts in a Fluidized Bed
E105 Practice for Probability Sampling of Materials
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Summary of Guide
3.1 A sample of fresh fluid cracking catalyst is placed in a reactor, either fixed bed or preferably fluid bed, and is contacted with
steam at elevated temperature. This treatment causes partial deactivation of the catalyst.
NOTE 1—In a fixed bed reactor, material containing sulfates, chlorides, etc. can result in significant additional chemical deactivation.
3.2 The catalyst is withdrawn from the reactor and may be subjected to an activity or activity plus selectivity determination,
by using the microactivity test (Test Methods D3907 or D5154) or ACE test (Test Method D7964).
4. Significance and Use
4.1 In general, steam treatment of FCC catalyst can be used either to compare a series of cracking catalysts at a simulated
equilibrium condition or conditions, or to simulate the equilibrium condition of a specific cracking unit and a specific catalyst. This
guide gives an example for the first purpose and an approach for the latter purpose.
5. Apparatus
5.1 Fixed bed or fluid bed steaming reactors can be used for the hydrothermal treatment of FCC catalyst.
5.2 In the steaming reactor, temperatures of the catalyst can be maintained at selected constant mean levels between 700°C
[1292°F] and 850°C [1562°F] 62°C [63.6°F]700 °C [1292 °F] and 850 °C [1562 °F] 62 °C [63.6 °F] during the steam
treatment.
5.3 Temperature control during steam treatment is critical, as temperature variations of 62°C [63.6°F]62 °C [63.6 °F] can
lead to 61 wt. % 61 mass % conversion changes or more, especially at higher temperatures.
5.4 In fixed bed steaming, the temperature gradient through the catalyst bed should be kept as small as possible and should not
exceed 4°C [7.2°F].4 °C [7.2 °F]. In fluid bed steaming the bed temperature must be homogeneous.
5.5 Heating and cooling of the catalyst must be performed in the reactor under a flow of dry nitrogen.
5.6 Precautions must be taken to achieve uniform contact of the steam with the bed.
6. Sampling
6.1 A suitable sampling procedure is needed. Practice E105 is appropriate.
7. Sample Preparation
7.1 No sample preparation is necessary if the catalyst is heated slowly during preheating (non-shock steaming).
7.2 If the sample is introduced directly into a preheated steaming reactor, (shock-steaming)reactor (shock-steaming), it is
desirable to predry the sample for about one hour 1 h at about 550°C [1022°F]550 °C [1022 °F] to prevent excessive catalyst loss.
8. Procedure
8.1 Procedure for fluid bed and fixed bed s
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.
Loading comments...