ASTM D5154/D5154M-18

Standard Test Method for Determining Activity and Selectivity of Fluid Catalytic Cracking (FCC) Catalysts by Microactivity Test

SIGNIFICANCE AND USE
5.1 The microactivity test provides data to assess the relative performance of FCC catalysts. Because results are affected by catalyst pretreatment, feedstock characteristics, test equipment, and operating parameters, adherence to this test method is a prerequisite for correct interpretation of results. Apparatus, test conditions, and analytical procedures actually used should closely resemble those described in this test method. Significant variations in apparatus, test conditions and/or analytical procedures may result in activity and selectivity data which do not correlate with data developed by other laboratories on identical catalyst/feedstock samples.  
5.2 The standard method reaction temperature is 516 °C [960 °F]. Other reaction temperatures can be used; however, catalyst selectivity data developed at temperatures other than 516 °C [960 °F] may not correlate with selectivity data developed at 516 °C [960 °F]. Also, precision at other reaction temperatures may change compared to data obtained at 516 °C [960 °F].
SCOPE
1.1 This test method covers determining the activity and selectivity of either equilibrium or laboratory deactivated fluid catalytic cracking (FCC) catalysts. The activity is evaluated on the basis of mass percent conversion of gas oil feed in a microactivity unit. The selectivities are evaluated on the basis of mass percent yields of specifically defined products resulting from the catalytic cracking of gas oil feed.  
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

General Information

• Status: Published
• Publication Date: 30-Apr-2018
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.04 - Catalytic Properties

Relations

• Refers: ASTM D2887-23 - Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography
• Effective Date: 01-Jul-2023
• Refers: ASTM E456-13a(2022)e1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Apr-2022
• Refers: ASTM D2887-19 - Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography
• Effective Date: 01-Jul-2019
• Refers: ASTM E456-13A(2017)e3 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Oct-2017
• Refers: ASTM E456-13A(2017)e1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Oct-2017
• Refers: ASTM D2887-15 - Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography
• Effective Date: 01-Jul-2015
• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM E456-13a - Standard Terminology Relating to Quality and Statistics
• Effective Date: 15-Nov-2013
• Refers: ASTM E456-13ae1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 15-Nov-2013
• Refers: ASTM E456-13ae3 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 15-Nov-2013
• Refers: ASTM E456-13ae2 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 15-Nov-2013
• Refers: ASTM E456-13 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 15-Aug-2013
• Refers: ASTM D2887-13 - Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography
• Effective Date: 01-May-2013
• Refers: ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• Refers: ASTM E177-13 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2013

Overview

ASTM D5154/D5154M-18 is the internationally recognized standard test method for determining the activity and selectivity of fluid catalytic cracking (FCC) catalysts using a microactivity test. Developed by ASTM, this method provides a uniform procedure for evaluating both equilibrium and laboratory-deactivated FCC catalysts under controlled conditions. The microactivity test yields quantitative data on catalyst performance, focusing on mass percent conversion of gas oil and the yield distribution among key products. Consistent application of this standard is essential for correct interpretation and reliable comparison of results across different laboratories.

Key Topics

• FCC Catalyst Evaluation: The method guides the determination of catalyst activity based on the conversion rate of gas oil feed in a microactivity unit, and selectivity by identifying the mass percent yield of important products such as gasoline, light cycle oil (LCO), heavy cycle oil (HCO), dry gas, and coke.
• Standard Test Conditions: The reaction is typically performed at 516 °C (960 °F) to ensure comparable data, as alternative temperatures may affect precision and correlation of selectivity values.
• Product Analysis: Analytical procedures specify the use of techniques like gas chromatography for liquid and gas phase separation, ensuring accurate measurement of gasoline, LCO, HCO, and other product fractions.
• Normalization and Mass Balance: The standard emphasizes the importance of mass balance (recovery) within 96 to 101% to validate each test, requiring normalization of yields when necessary.
• Reproducibility: The method stresses the need for strict adherence to apparatus and procedures to achieve reproducible activity and selectivity data across laboratories.
• Sampling and Preparation: Recommendations are given for the proper sampling, decoking, and steam treatment of catalysts prior to testing, critical for ensuring valid comparisons.

Applications

ASTM D5154/D5154M-18 finds wide application in:

• Refinery R&D: Assisting in the development and selection of FCC catalysts for improved conversion efficiency and product yield distribution.
• Quality Control: Ensuring consistent performance of FCC catalysts during production and prior to industrial deployment in petroleum refining.
• Interlaboratory Comparisons: Facilitating meaningful comparison of catalyst data between different organizations by providing a reference procedure less influenced by variations in local equipment or analysis methods.
• Performance Benchmarking: Offering a standardized approach for benchmarking new or modified catalysts against industry reference materials.
• Troubleshooting: Supporting process engineers in diagnosing changes in process yields by correlating with standardized catalyst microactivity data.

Related Standards

• ASTM D2887 - Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography
• ASTM D3907 - Test Method for Testing Fluid Catalytic Cracking (FCC) Catalysts by Microactivity Test
• ASTM D4463 - Guide for Metals Free Steam Deactivation of Fresh Fluid Cracking Catalysts
• ASTM D7964 - Test Method for Determining Activity of FCC Catalysts in a Fluidized Bed
• ASTM E105 - Practice for Probability Sampling of Materials
• ASTM E177 - Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• ASTM E456 - Terminology Relating to Quality and Statistics
• ASTM E691 - Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method

Practical Value

This test method delivers high practical value by:

• Standardizing FCC catalyst performance assessment, yielding reliable, comparable results for regulatory, development, and commercial purposes.
• Improving refinery process efficiency by informing catalyst selection and usage with robust microactivity and selectivity data.
• Supporting quality assurance throughout the catalyst supply chain, from manufacturing to industrial use.

Keywords: FCC catalyst microactivity test, ASTM D5154, catalyst activity, catalyst selectivity, fluid catalytic cracking, petroleum refinery standards, ASTM catalyst testing.

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: D5154/D5154M − 18
Standard Test Method for
Determining Activity and Selectivity of Fluid Catalytic
Cracking (FCC) Catalysts by Microactivity Test
This standard is issued under the fixed designation D5154/D5154M; 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 D4463 Guide for Metals Free Steam Deactivation of Fresh
Fluid Cracking Catalysts
1.1 This test method covers determining the activity and
D7964 Test Method for DeterminingActivity of Fluid Cata-
selectivity of either equilibrium or laboratory deactivated fluid
lytic Cracking (FCC) Catalysts in a Fluidized Bed
catalytic cracking (FCC) catalysts. The activity is evaluated on
E105 Practice for Probability Sampling of Materials
the basis of mass percent conversion of gas oil feed in a
E177 Practice for Use of the Terms Precision and Bias in
microactivity unit. The selectivities are evaluated on the basis
ASTM Test Methods
ofmasspercentyieldsofspecificallydefinedproductsresulting
E456 Terminology Relating to Quality and Statistics
from the catalytic cracking of gas oil feed.
E691 Practice for Conducting an Interlaboratory Study to
1.2 The values stated in either SI units or inch-pound units
Determine the Precision of a Test Method
are to be regarded separately as standard. The values stated in
each system may not be exact equivalents; therefore, each
3. Terminology
system shall be used independently of the other. Combining
3.1 Definitions of Terms Specific to This Standard:
values from the two systems may result in non-conformance
3.1.1 activity—calculated as conversion divided by the dif-
with the standard.
ference of 100 minus conversion.
1.3 This standard does not purport to address all of the
3.1.2 ASTM reference catalysts—a set of equilibrium FCC
safety concerns, if any, associated with its use. It is the
catalysts within the useful range of this test method is used to
responsibility of the user of this standard to establish appro-
improve the reproducibility of test results between different
priate safety, health, and environmental practices and deter-
laboratories. Each catalyst has a consensus mean conversion
mine the applicability of regulatory limitations prior to use.
value assigned to it by Committee D32. Samples of theASTM
1.4 This international standard was developed in accor-
reference catalysts can be obtained through NIST.
dance with internationally recognized principles on standard-
3.1.3 ASTMstandardfeed—aspecificbatchofgasoilthatis
ization established in the Decision on Principles for the
used as feedstock in the described test method.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical 3.1.4 catalyst/oil (C/O) ratio—the mass of catalyst used in
Barriers to Trade (TBT) Committee. the test divided by the mass of feed fed to the reactor. In
practice, the mass of catalyst is usually maintained at a
2. Referenced Documents
constant value and the total mass of feed is varied.
2.1 ASTM Standards: 3.1.5 contacttime—calculated as 3600/(WHSV· C/O).This
D2887 Test Method for Boiling Range Distribution of Pe-
is the delivery time, in seconds, during which feed is intro-
troleum Fractions by Gas Chromatography duced to the reactor.
D3907 Test Method for Testing Fluid Catalytic Cracking
3.1.6 conversion—calculated as the difference between the
(FCC) Catalysts by Microactivity Test
mass of feed used and the mass of unconverted material
divided by the mass of feed used times 100 %. The uncon-
verted material is defined as all liquid product with a boiling
This test method is under the jurisdiction of ASTM Committee D32 on
point above 216 °C [421 °F].
Catalysts and is the direct responsibility of Subcommittee D32.04 on Catalytic
Properties.
3.1.7 gasoline—C compounds through compounds boiling
Current edition approved May 1, 2018. Published May 2018. Originally
at 216 °C [421° F].
approved in 1991. Last previous edition approved in 2010 as D5154–10. DOI:
10.1520/D5154_D5154M-18.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Formerly available from National Institute of Standards and Technology
Standards volume information, refer to the standard’s Document Summary page on (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://
the ASTM website. www.nist.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5154/D5154M − 18
3.1.8 HCO—the heavy cycle oil product defined to have a
minimum boiling point of 343 °C [650 °F].
3.1.9 LCO—the light cycle oil product defined to have a
boiling point range of 216 °C to 343 °C [421°F to 650 °F].
3.1.10 liquid product—all products formed in the catalytic
reaction that can be condensed in the chiller bath afterward,
usually a combination of gasoline, LCO, and HCO, but can
contain a trace of C and C minus compounds.
4 4
3.1.11 normalized product yield—the result obtained when
each product yield has been corrected for non-perfect mass
balances. For a run to be judged acceptable, the total recovery,
mass % of feed, should be in the range of 96 to 101 % prior to
normalization. If the recovery is outside this range the test data
should be discarded.
3.1.12 product yield—one hundred times the mass of a
specific product divided by the mass of feed used in the test.
3.1.13 reactionseverity—an indication of the severity of the
cracking reaction which allows a range of conversions to be
obtained from any particular catalyst without changing reactor
temperature. Changing reaction severity is achieved by chang-
ing WHSV or C/O ratio or both.
3.1.14 selectivity—same as yield. Selectivity generally re-
fers to how much of a particular product, such as coke, is
formed during a chemical reaction; selectivity is related to, but
different from, conversion, which is the total amount of all
NOTE 1—This drawing is not to scale. For engineering details, see other
products formed during the reaction.
drawings.
FIG. 1 Microactivity Flow Chart
3.1.15 weight hourly space velocity (WHSV)—the oil feed
rateingramsperhourdividedbythemassofcatalystingrams.
-1
Units are hr .
4. Summary of Test Method
method is a prerequisite for correct interpretation of results.
Apparatus, test conditions, and analytical procedures actually
4.1 At least two samples of FCC catalysts, one of which is
used should closely resemble those described in this test
chosen as a reference, are separately contacted with gas oil
method. Significant variations in apparatus, test conditions
feed (ASTM Standard Feed or other suitable feedstock) in a
and/or analytical procedures may result in activity and selec-
fixed bed reactor at a specified reaction temperature and at
tivity data which do not correlate with data developed by other
morethanonereactionseverity.Reactionproducts(liquid,gas,
laboratories on identical catalyst/feedstock samples.
and coke on catalyst) are analyzed. Conversion, activity, and
product yields are calculated for each experiment.
5.2 The standard method reaction temperature is 516 °C
4.2 Following analysis of the products, the total recovery [960 °F]. Other reaction temperatures can be used; however,
(that is, mass balance) of the feed as converted and uncon- catalyst selectivity data developed at temperatures other than
verted products is determined. If the recovery is less than 96 % 516 °C [960 °F] may not correlate with selectivity data devel-
or greater than 101 %, the test is rejected as unsatisfactory (an oped at 516 °C [960 °F]. Also, precision at other reaction
outlier). temperatures may change compared to data obtained at 516 °C
[960 °F].
4.3 For each catalyst tested, normalized product yields are
plotted against conversion or activity to generate a yield curve.
6. Apparatus
The data comprising the yield curve may be used to obtain the
parameters of an appropriate mathematical expression for the
6.1 The apparatus of this test method is essentially that
curve. Comparisons among catalysts can be made by interpo-
described in Test Method D3907, as shown in Figs. 1-4, with
lating the yield curves to obtain the product yields at some
the addition of a gas collection system on the effluent gas vent
specified conversion.
line. In a typical gas collection system, water is displaced by
the collected gas and the volume of displaced water provides a
5. Significance and Use
quantitative measurement of the amount of gas collected. To
5.1 The microactivity test provides data to assess the rela- minimize the solubility of gases like H and H S in the fluid,
2 2
tiveperformanceofFCCcatalysts.Becauseresultsareaffected a saturated brine (NaCl) solution is recommended. Other gas
by catalyst pretreatment, feedstock characteristics, test collection systems can be used, such as the water-free gasom-
equipment, and operating parameters, adherence to this test eter (consisting of two gas chambers in series, each with a
D5154/D5154M − 18
FIG. 2 Microactivity Reactor
4 6
piston inside) which is more ideal for H S quantification. Research Report RR:D32-1030 who can provide specific
Some publications have appeared which give example flow equipment for performing this test. However, Committee D32
schematics and more detailed descriptions of typical appara- can only suggest and will not recommend nor certify any
tus. Alternatively, there are several vendors as listed in specific vendor. Significant variations from the test apparatus
of this method most likely will result in significantly different
activity and selectivity data from identical catalyst samples.
Ng, S.H., Shi,Y., Heshka, N.E., Zhang,Y., Little, E. “Laboratory Production of
Biofuels and Biochemicals from a Rapeseed Oil through Catalytic Cracking
Conversion”, J. Vis. Exp. e54390, doi:10.3791/54390.
5 6
Campagna, R. J., Wick, J. P., Brady, M. F., and Fort, D. L., “ Fresh FCC Supporting data have been filed at ASTM International Headquarters and may
Catalyst Tests Predict Performance,” OGJ, March 24, 1986, p. 85. be obtained by requesting Research Report RR:D32-1030.
D5154/D5154M − 18
FIG. 3 Reactor Feed Tube Insert
D5154/D5154M − 18
the furnace to burn the sample free of coke. Insufficient coke
removal is indicated by a difference in color of the top and
bottom layers. The hot crucible is cooled in a desiccator to
prevent moisture pickup.
NOTE 1—Heavily coked samples may be damaged by sintering or
deactivation if oxidation is allowed to occur too rapidly, leading to
artificially low catalytic activity and surface area.
8.2 Fresh Catalysts—Fresh catalyst samples should be
steam treated prior to selectivity testing. Steaming procedures
suchasthosespecifiedinGuideD4463maybeused.However,
specific conditions (temperature, partial pressure of steam, and
time) should be chosen such that the steamed catalyst proper-
ties (activity, zeolite and matrix surface areas, and unit cell
size) approximate those found in equilibrium FCC catalysts of
the same type.
9. Procedure
9.1 Reactor Preparation:
9.1.1 Rinse feed line with acetone or other suitable solvent
and dry with air. Periodic cleaning of the insert is recom-
FIG. 4 Liquid Product Receiver
mended by air purge at 550 °C [1022 °F] for one hour at least
once every 12 tests.
6.2 Chromatographic Equipment:
9.1.2 Washthereactorandproductreceiverthoroughlywith
6.2.1 Liquid product analyses should be performed using
acetone or other suitable solvent and dry. If necessary, burn out
Test Method D2887 on a gas chromatograph (GC) equipped
any coke deposited in the reactor by heating in air at 516 °C
with a flame ionization detector.
[960 °F] prior to washing.
6.2.2 Gas product analyses may be accomplished in two
9.1.3 Insert a plug of quartz or borosilicate glass wool
parts. First, a GC equipped with a thermal conductivity
(about 20 mm length) until it reaches the constricted region of
detector is needed for quantitative identification of H and N .
2 2
thereactor.Optionally,areactorwithafritteddiscmaybeused
H S can optionally be detected, but will not be quantitative in
to position the catalyst. Add 4.00 to 4.05 g of catalyst in a
units that collect gas by water displacement. Second, an
free-flowing manner. Tap the reactor lightly to ensure good
analysis using a GC equipped with a FID or TCD, employing
radial distribution (do not pack). Insert another plug of quartz
He as a carrier gas and using a column that permits the
or glass wool and add approximately 10 cc of 80 to 100 mesh
separation and quantitative identification of methane, ethane,
glass microspheres or crushed glass particles. These act as a
ethylene, propane, propylene, n-butane, iso-butane, 1-butene
preheat bed and aid in feed dispersion, especially at higher
and iso-butene, cis-2-butene, and trans-2-butene, C ’s (C
5 5
+
WHSV’s.
saturates, i.e., i-pentane and n-pentane) and a C lump
9.1.4 Inspect the oil insert needle to ensure it is clear of
(including C olefins, i.e., i-pentenes and n-pentenes, and C +,
5 6
+
deposits. Place insert in reactor and adjust if necessary so that
i.e., C to C ) that is not resolved. The C ’s and the C group
6 9 5 5
thebottomoftheoilinsertneedleisjusttouchingthetopofthe
are included as part of the gasoline fraction.
glassmicrospherepreheatbed(about20mmabovethecatalyst
6.3 Carbon analysis of a representative sample of the spent
bed).Inspectthereactorinsertbeforeusingtobesurethetipof
catalyst (that is, the catalyst after the cracking reaction) may be
the thermocouple (see Fig. 3, Detail 2) is bent under the tip of
accomplished using a commercially available carbon analyzer
the syringe needle. (This is necessary to control the oil preheat
if the microactivity unit being used does not have catalyst
temperature accurately.) Place the reactor in the furnace that
regeneration capability. If the microactivity unit is a model that
hasbeenpreheatedto516 °C[960 °F]andconnectthenitrogen
does have regeneration capability, then the carbon on catalyst
purge line directly to the reactor feed line. Purge with 30
is back calculated from the CO evolved in the flue gas during
mL/min [30 sccm] of nitrogen for at least 30 min.
the regeneration cycle.
9.1.5 Make electrical connections on the integral oil feed
preheater and connect the thermocouple to the recorder.
7. Sampling
9.2 Preparation of Syringe and Liquid Product Receiver:
7.1 A sampling procedure is needed. Practice E105 is
9.2.1 Preheat the gas oil feedstock to 40 6 5 °C [104 6
appropriate.
9 °F]toallowfillingofthesyringe.Beforetesting,calibratethe
syringe pump to the correct feed rate by collecting the oil,
8. Sample Preparation
preheated to 40 6 5 °C [104 6 9 °F], outside the reactor and
8.1 Equilibrium Catalysts—Dry samples and remove coke
weighing the oil or by weighing the syringe before and after
by heating a shallow (less than 10 mm thick) bed of catalyst in
delivery to assure the appropriate mass of oil delivered over
a porcelain crucible at 590 6 20 °C [1094 6 36 °F] for a
unit time.
length of time sufficient to remove any coke. This typically
requiresapproximately3h.Sufficientairshouldbeavailablein NOTE 2—If heavier feedstocks are used, a syringe temperature of 70 6
D5154/D5154M − 18
5 °C [158 6 9 °F] should be used for obtaining accurate feed rates.
9.3.7 Immediately after the oil addition, restart the nitrogen
flow at 30 mL/min. [30 sccm] by switching the multiport valve
9.2.2 Fill the syringe with preheated feedstock and invert to
to purge the reactor and product recovery system.
allow air to rise. Remove the air bubbles. The syringe should
contain a small amount of oil in excess of the nominal volume 9.3.8 Remove the syringe from the reactor and reweigh it.
to be charged.
Recordthemassofoilfeed(W ).W shouldvarynomorethan
F F
9.2.3 Afterthesyringeisfilledandthevalveisinthecorrect
60.03 g from the desired feed mass.
position, blow excess oil out of the valve and clean the outside
9.3.9 After 4 6 0.25 min of nitrogen purge, remove the
o
...

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.
Designation: D5154 − 10 D5154/D5154M − 18
Standard Test Method for
Determining Activity and Selectivity of Fluid Catalytic
Cracking (FCC) Catalysts by Microactivity Test
This standard is issued under the fixed designation D5154;D5154/D5154M; 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
1.1 This test method covers determining the activity and selectivity of either equilibrium or laboratory deactivated fluid catalytic
cracking (FCC) catalysts. The activity is evaluated on the basis of mass percent conversion of gas oil feed in a microactivity unit.
The selectivities are evaluated on the basis of mass percent yields of specifically defined products resulting from the catalytic
cracking of gas oil.oil feed.
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values given in
parentheses are mathematical conversions to SI units that are provided for information only and are not considered stated in each
system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the
two systems may result in non-conformance with the standard.
1.2.1 Exception—SI units have been retained in some of the figures.
1.3 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.
1.4 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:
D2887 Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography
D3907 Test Method for Testing Fluid Catalytic Cracking (FCC) Catalysts by Microactivity Test
D4463 Guide for Metals Free Steam Deactivation of Fresh Fluid Cracking Catalysts
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. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 activity—calculated as conversion divided by the difference of 100 minus conversion.
3.1.2 ASTM reference catalysts—a set of equilibrium FCC catalysts within the useful range of this test method is used to
improve the reproducibility of test results between different laboratories. Each catalyst has a consensus mean conversion value
assigned to it by Committee D32. Samples of the ASTM reference catalysts can be obtained through NIST.
3.1.3 ASTM standard feed—a specific batch of gas oil that is used as feedstock in the described test method.
This test method 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 April 1, 2010May 1, 2018. Published May 2010May 2018. Originally approved in 1991. Last previous edition approved in 20052010 as
D5154–05.–10. DOI: 10.1520/D5154-10.10.1520/D5154_D5154M-18.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available Formerly available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070,
http://www.nist.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5154/D5154M − 18
3.1.4 catalyst/oil (C/O) ratio—the mass of catalyst used in the test divided by the mass of feed fed to the reactor. In practice,
the mass of catalyst is usually maintained at a constant value and the total mass of feed is varied.
3.1.5 contact time—calculated as 3600/(WHSV · C/O). This is the delivery time, in seconds, during which feed is introduced
to the reactor.
3.1.6 HCO—the heavy cycle oil product defined to have a minimum boiling point of 650°F (343°C).
3.1.7 LCO—the light cycle oil product defined to have a boiling point range of 421 to 650°F (216 to 343°C).
3.1.6 measured conversion—calculated as the difference between the mass of feed used and the mass of unconverted material
divided by the mass of feed used times 100 %. The unconverted material is defined as all liquid product with a boiling point above
42°F (216°C).216 °C [421 °F].
3.1.7 gasoline—C compounds through compounds boiling at 216 °C [421° F].
3.1.8 HCO—the heavy cycle oil product defined to have a minimum boiling point of 343 °C [650 °F].
3.1.9 LCO—the light cycle oil product defined to have a boiling point range of 216 °C to 343 °C [421°F to 650 °F].
3.1.10 liquid product—all products formed in the catalytic reaction that can be condensed in the chiller bath afterward, usually
a combination of gasoline, LCO, and HCO, but can contain a trace of C and C minus compounds.
4 4
3.1.11 normalized product yield—the result obtained when each product yield has been corrected for non-perfect mass balances.
For a run to be judged acceptable, the total recovery, wt %mass % of feed, should be in the range of 96 to 101 % prior to
normalization. If the recovery is outside this range the test data should be discarded.
3.1.12 product yield—one hundred times the mass of a specific product divided by the mass of feed used in the test.
3.1.13 reaction severity—an indication of the severity of the cracking reaction which allows a range of conversions to be
obtained from any particular catalyst without changing reactor temperature. Changing reaction severity is achieved by changing
WHSV or C/O ratio or both.
3.1.14 selectivity—same as yield. Selectivity generally refers to how much of a particular product, such as coke, is formed
during a chemical reaction; selectivity is related to, but different from, conversion, which is the total amount of all products formed
during the reaction.
3.1.15 weight hourly space velocity (WHSV)—the oil feed rate in grams per hour divided by the mass of catalyst in grams. Units
-1
are hr .
4. Summary of Test Method
4.1 At least two samples of FCC catalysts, one of which is chosen as a reference, are separately contacted with gas oil feed
(ASTM Standard Feed or other suitable feedstock) in a fixed bed reactor at a specified reaction temperature and at more than one
reaction severity. Reaction products (liquid, gas, and coke on catalyst) are analyzed. Conversion, activity, and product yields are
calculated for each experiment.
4.2 Following analysis of the products, the total recovery (that is, mass balance) of the feed as converted and unconverted
products is determined. If the recovery is less than 96 % or greater than 101 %, the test is rejected as unsatisfactory.unsatisfactory
(an outlier).
4.3 For each catalyst tested, normalized product yields are plotted against conversion or activity to generate a yield curve. The
data comprising the yield curve may be used to obtain the parameters of an appropriate mathematical expression for the curve.
Comparisons among catalysts can be made by interpolating the yield curves to obtain the product yields at some specified
conversion.
5. Significance and Use
5.1 The microactivity test provides data to assess the relative performance of FCC catalysts. Because results are affected by
catalyst pretreatment, feedstock characteristics, test equipment, and operating parameters, adherence to this test method is a
prerequisite for correct interpretation of results. Apparatus, test conditions, and analytical procedures actually used should closely
resemble those described in this test method. Significant variations in apparatus, test conditions and/or analytical procedures may
result in activity and selectivity data which do not correlate with data developed by other laboratories on identical
catalyst/feedstock samples.
5.2 The standard method reaction temperature is 960°F (516°C).516 °C [960 °F]. Other reaction temperatures can be used;
however, catalyst selectivity data developed at temperatures other than 960°F (516°C)516 °C [960 °F] may not correlate with
selectivity data developed at 960°F (516°C).516 °C [960 °F]. Also, precision at other reaction temperatures may change compared
to data obtained at 960°F (516°C).516 °C [960 °F].
D5154/D5154M − 18
NOTE 1—This drawing is not to scale. For engineering details, see other drawings.
FIG. 1 Microactivity Flow Chart
6. Apparatus
6.1 The apparatus of this test method is essentially that described in Test Method D3907, as shown in Figs. 1-4, with the addition
of a gas collection system on the effluent gas vent line. In a typical gas collection system, a fluid water is displaced by the collected
gas and the volume of displaced liquidwater provides a quantitative measurement of the amount of gas collected. To minimize the
solubility of gases like H and H S in the fluid, a saturated brine (NaCl) solution is recommended. Other gas collection systems
2 2
can be used, such as the water-free gasometer (consisting of two gas chambers in series, each with a piston inside) which is more
ideal for H S quantification. Some publications have appeared which give example flow schematics and more detailed
5 6
descriptions of typical apparatus. Alternatively, there are several vendors as listed in Research Report RR:D32-1030 who can
provide specific equipment for performing this test. However, Committee D32 can only suggest and will not recommend nor certify
any specific vendor. Significant variations from the test apparatus of this method most likely will result in significantly different
activity and selectivity data from identical catalyst samples.
6.2 Chromatographic Equipment:
6.2.1 Liquid product analyses should be performed using Test Method D2887 on a gas chromatograph (G.C.)(GC) equipped
with a flame ionization detector.
6.2.2 Gas product analyses may be accomplished in two parts. First, an analysis using a G.C.a GC equipped with a thermal
conductivity detector, employing Ndetector is needed as a carrier gas, andfor quantitative identification of H using aand N G.C.
2 2 2
H column that permits the separation and quantitative identification of HS can optionally be detected, but will not be quantitative
in and Hunits that S. collect gas by water displacement. Second, an analysis using a G.C.GC equipped with a FID or TCD,
2 2
employing He as a carrier gas and using a column that permits the separation and quantitative identification of methane, ethane,
ethylene, propane, propylene, n-butane, iso-butane, 1-butene and iso-butene, cis-2-butene, and trans-2-butene, C ’s (C and
5 5
+
saturates, i.e., i-pentane and n-pentane) and a C lump (including C olefins, i.e., i-pentenes and n-pentenes, and C +, i.e., C to
5 5 6 6
+
C ) that is not resolved. The C ’s and the C group are included as part of the gasoline fraction.
9 5 5
Ng, S.H., Shi, Y., Heshka, N.E., Zhang, Y., Little, E. “Laboratory Production of Biofuels and Biochemicals from a Rapeseed Oil through Catalytic Cracking Conversion”,
J. Vis. Exp. e54390, doi:10.3791/54390.
Campagna, R. J., Wick, J. P., Brady, M. F., and Fort, D. L., “ Fresh FCC Catalyst Tests Predict Performance,” OGJ, March 24, 1986, p. 85.
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D32-1030.
D5154/D5154M − 18
FIG. 2 Microactivity Reactor
6.3 Carbon analysis of a representative sample of the spent catalyst (that is, the catalyst after the cracking reaction has been
completed) reaction) may be accomplished using a commercially available carbon analyzer.analyzer if the microactivity unit being
used does not have catalyst regeneration capability. If the microactivity unit is a model that does have regeneration capability, then
the carbon on catalyst is back calculated from the CO evolved in the flue gas during the regeneration cycle.
7. Sampling
7.1 A sampling procedure is needed. Practice E105 is appropriate.
8. Sample Preparation
8.1 Equilibrium Catalysts—Dry samples or decoke, or both, and remove coke by heating a shallow (less than 10 mm thick) bed
of catalyst in a porcelain crucible at 1094590 6 36°F (59020 °C [1094 6 20°C)36 °F] for a length of time sufficient to remove
D5154/D5154M − 18
FIG. 3 Reactor Feed Tube Insert
D5154/D5154M − 18
FIG. 4 Liquid Product Receiver
any coke. This typically requires approximately three hours.3 h. Sufficient air should be available in the furnace to burn the sample
free of coke. Insufficient decoking coke removal is indicated by a difference in color of the top and bottom layers. The hot crucible
is cooled in a desiccator to prevent moisture pickup.
NOTE 1—Heavily coked samples may be damaged by sintering or deactivation if oxidation is allowed to occur too rapidly, leading to artificially low
catalytic activity and surface area.
8.2 Fresh Catalysts—Fresh catalyst samples should be steam treated prior to selectivity testing. Steaming procedures such as
those specified in Guide D4463 may be used. However, specific conditions (temperature, partial pressure of steam, and time)
should be chosen such that the steamed catalyst properties (activity, zeolite and matrix surface areas, and unit cell size)
approximate those found in equilibrium FCC catalysts of the same type.
9. Procedure
9.1 Reactor Preparation:
9.1.1 Rinse feed line with acetone or other suitable solvent and dry with air. Periodic cleaning of the insert is recommended by
air purge at 1022°F (550°C)550 °C [1022 °F] for one hour at least once every 12 tests.
9.1.2 Wash the reactor and product receiver thoroughly with acetone or other suitable solvent and dry. If necessary, burn out
any coke deposited in the reactor by heating in air at 960°F (516°C)516 °C [960 °F] prior to washing.
9.1.3 Insert a plug of quartz or borosilicate glass wool (about 20 mm length) until it reaches the constricted region of the reactor.
Optionally, a reactor with a fritted disc may be used to position the catalyst. Add 4.00 to 4.05 g of catalyst in a free-flowing manner.
Tap the reactor lightly to ensure good radial distribution (do not pack). Insert another plug of quartz or glass wool and add
approximately 10 cc of 80 to 100 mesh glass microspheres or crushed glass particles. These act as a preheat bed and aid in feed
dispersion, especially at higher WHSV’s.
9.1.4 Inspect the oil insert needle to ensure it is clear of deposits. Place insert in reactor and adjust if necessary so that the bottom
of the oil insert needle is just touching the top of the glass microsphere preheat bed (about 20 mm above the catalyst bed). Inspect
the reactor insert before using to be sure the tip of the thermocouple (see Fig. 3, Detail 2) is bent under the tip of the syringe needle.
(This is necessary to control the oil preheat temperature accurately.) Place the reactor in the furnace that has been preheated to
960°F (516°C)516 °C [960 °F] and connect the nitrogen purge line directly to the reactor feed line. Purge with 30 seem (30
mL/min)mL/min [30 sccm] of nitrogen for at least 30 min.
9.1.5 Make electrical connections on the integral oil feed preheater and connect the thermocouple to the recorder.
9.2 Preparation of Syringe and Liquid Product Receiver:
9.2.1 Preheat the gas oil feedstock to 10440 6 9°F (405 °C [104 6 5°C)9 °F] to allow filling of the syringe. Before testing,
calibrate the syringe pump to the correct feed rate by collecting the oil, preheated to 10440 6 9°F (405 °C [104 6 5°C),9 °F],
outside the reactor and weighing the oil or by weighing the syringe before and after delivery to assure the appropriate mass of oil
delivered over unit time.
NOTE 2—If heavier feedstocks are used, a syringe temperature of 15870 6 9°F (705 °C [158 6 5°C)9 °F] should be used for obtaining accurate feed
rates.
D5154/D5154M − 18
9.2.2 Fill the syringe with preheated feedstock and invert to allow air to rise. Remove the air bubbles. The syringe should
contain a small amount of oil in excess of the nominal volume to be charged.
9.2.3 After the syringe is filled and the valve is in the correct position, blow excess oil out of the valve and clean the outside
of the syringe.
9.2.4 Weigh the syringe assembly and record the mass.
9.2.5 Attach the syringe and syringe valve to the reactor making sure the valve is in the nitrogen flow position. A thermocouple
may be placed on the syringe body to monitor the syringe temperature during oil injection.
+
9.2.6 A small plug of g
...