ASTM D8414/D8414M-21

Standard Test Method for Measurement of Jet Cup Attrition Index of Catalytic Materials

SIGNIFICANCE AND USE
5.1 The jet cup attrition test will provide an estimate of the relative attrition resistance of fluid catalytic cracking (FCC) catalyst, catalyst additives, and catalytic materials.  
5.2 The test is designed to simulate the attrition a catalyst or additive undergoes in a fluid catalytic cracking unit but at an accelerated rate.  
5.3 The data from this test can be used to rank catalyst according to attrition rate.  
5.4 The test requires a relatively small sample size of 5 g [0.175 oz] and a relatively short analysis time of 40 min. This test should be useful to quality control facilities that require fast turnaround time and research and development (R&D) facilities that have limited sample material.
SCOPE
1.1 The jet cup attrition test is applicable to fluid catalytic cracking (FCC) catalysts, catalyst additives, and catalytic materials.  
1.2 Applications for other powdered catalysts have been reported in the literature. The round robin test samples included two FCC catalysts and one powdered alumina.  
1.3 Units—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 system shall be used independently of the other, and values from the two systems shall not be combined.  
1.4 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.  
1.5 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-Sep-2021
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.02 - Physical-Mechanical Properties

Relations

• 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 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
• Refers: ASTM E691-11 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2011
• Refers: ASTM E177-10 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2010
• Refers: ASTM E691-08 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Oct-2008
• Refers: ASTM E177-08 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2008
• Refers: ASTM E177-06b - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 15-Nov-2006
• Refers: ASTM E177-06a - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2006
• Refers: ASTM E691-05 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2005
• Refers: ASTM E177-04e1 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-04 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-06 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-90a(2002) - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 10-Jan-2002
• Refers: ASTM E691-99 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 10-May-1999

Overview

ASTM D8414/D8414M-21: Standard Test Method for Measurement of Jet Cup Attrition Index of Catalytic Materials is an international standard developed by ASTM International. This test method provides a reliable procedure for measuring the Jet Cup Attrition Index (JCI) to estimate the relative attrition resistance of fluid catalytic cracking (FCC) catalysts, catalyst additives, and other catalytic materials. The test is widely used in the petroleum refining and chemical processing industries for quality control and research and development due to its efficiency, small sample requirement, and ability to simulate real-world catalyst attrition at an accelerated rate.

Key Topics

• Jet Cup Attrition Index (JCI): The JCI quantifies the weight percent of fines (particles under 20 µm) generated per hour when a sample is subjected to high-velocity, humidified air in a jet cup apparatus. This provides an index of how resistant the catalyst is to attrition.
• Sample Requirements: The method only requires approximately 5 grams of sample and a 40-minute analysis time, making it suited to both routine quality control and R&D with limited sample availability.
• Simulated Conditions: The process simulates the particle collisions and breakage experienced by catalysts in a fluid catalytic cracking unit, providing relevant performance data.
• Ranking and Control: Results can be used to rank different catalysts and additives by their attrition rates, supporting material selection and process optimization efforts.

Applications

• Fluid Catalytic Cracking (FCC): The test is especially applicable to FCC catalysts commonly used in petroleum refineries for breaking down complex hydrocarbons. It ensures that catalysts chosen for operations can withstand process conditions and maintain activity over time.
• Catalyst Additives: Manufacturers and users of catalyst additives can assess attrition properties to ensure the additives will not unduly contribute to fines generation and operational problems.
• Powdered Catalysts: While the focus is on FCC materials, the method is also referenced for other powdered catalyst types, providing a basis for consistent attrition resistance evaluation.
• Quality Control in Manufacturing: The rapid turnaround and small sample size make the method ideal for routine checks in catalyst production facilities, helping to monitor and uphold product consistency.
• Research and Development: With minimal sample requirements, laboratories developing new catalytic materials can use this method during early-stage screening or optimization phases.

Related Standards

• ASTM E177: Practice for Use of the Terms Precision and Bias in ASTM Test Methods, cited for method validation.
• ASTM E691: Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method, relevant for test precision measurement.
• International Standardization: ASTM D8414/D8414M-21 aligns with internationally recognized principles per the World Trade Organization Technical Barriers to Trade (TBT) Committee guidelines.

Practical Value

Implementing ASTM D8414/D8414M-21 enables catalyst manufacturers and end-users to:

• Optimize Catalyst Performance: Select and design catalyst formulations with the desired attrition resistance for operational longevity.
• Minimize Fines Generation: Reduce operational costs and equipment fouling caused by excess fines generation.
• Benchmark Products: Objectively compare and benchmark catalyst products within and across organizations.
• Support Regulatory Compliance: Adhere to standardized test methods recognized internationally, ensuring credible and traceable results.

Keywords

Fluid catalytic cracking, FCC catalyst, catalyst additives, catalytic materials, jet cup attrition index, JCI, powdered catalyst, attrition resistance, quality control, ASTM D8414/D8414M-21.

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: D8414/D8414M − 21
Standard Test Method for
Measurement of Jet Cup Attrition Index of Catalytic
Materials
This standard is issued under the fixed designation D8414/D8414M; 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 3. Terminology
3.1 Definitions of Terms Specific to This Standard:
1.1 The jet cup attrition test is applicable to fluid catalytic
cracking (FCC) catalysts, catalyst additives, and catalytic 3.1.1 control factor, CF, n—unitlessvaluedeterminedbythe
repetitive analysis of a standard material; it is equal to the
materials.
(initial value of the control standard)/ (current value of the
1.2 Applications for other powdered catalysts have been
control standard) = CF.
reported in the literature. The round robin test samples in-
3.1.1.1 Discussion—Refer to 12.1 for details on the stan-
cluded two FCC catalysts and one powdered alumina.
dard.
1.3 Units—The values stated in either SI units or inch-
3.1.1.2 Discussion—The values used in the calculations are
pound units are to be regarded separately as standard. The
monthly averages.
values stated in each system are not necessarily exact equiva-
3.1.2 jet cup index, JCI, n—unitless value equal to the
lents; therefore, to ensure conformance with the standard, each
“weight percent of 0- to 20-µm [0- to 787-µin.] fines generated
system shall be used independently of the other, and values
per hour” under test conditions.
from the two systems shall not be combined.
1.4 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 Of the sample to be tested, 5 g [0.175 oz] is placed into
responsibility of the user of this standard to establish appro-
the jet cup of the test apparatus where humidified air is passed
priate safety, health, and environmental practices and deter-
through an orifice in the jet cup at high velocity.
mine the applicability of regulatory limitations prior to use.
4.2 The air impinges on the catalyst and causes particles to
1.5 This international standard was developed in accor-
collide with each other and the walls of the jet cup. These
dance with internationally recognized principles on standard-
particle-to-particle and particle-to-wall interactions cause fines
ization established in the Decision on Principles for the
to form via attrition. In addition, weaker particles will fracture
Development of International Standards, Guides and Recom-
and form fines.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
4.3 The jet cup is attached to a fines disengagement cham-
berthatallowsparticleslessthan20µm[787-µin.]topassinto
2. Referenced Documents
a fines collection assembly.
NOTE 1—The fines disengagement chamber is based on theAMINCO-
2.1 ASTM Standards:
Roller air elutriation particle size analyzer, historically used to measure
E177Practice for Use of the Terms Precision and Bias in
the 0-20 micron fraction in catalyst.
ASTM Test Methods
4.4 The JCI is calculated from the mass of fines collected
E691Practice for Conducting an Interlaboratory Study to
and is numerically equivalent to the “weight percent of fines
Determine the Precision of a Test Method
generated per hour” under test conditions.
5. Significance and Use
This test method is under the jurisdiction of ASTM Committee D32 on
Catalysts and is the direct responsibility of Subcommittee D32.02 on Physical-
5.1 The jet cup attrition test will provide an estimate of the
Mechanical Properties.
relative attrition resistance of fluid catalytic cracking (FCC)
Current edition approved Oct. 1, 2021. Published November 2021. DOI:
catalyst, catalyst additives, and catalytic materials.
10.1520/D8414_D8414M-21.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.2 Thetestisdesignedtosimulatetheattritionacatalystor
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
additive undergoes in a fluid catalytic cracking unit but at an
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. accelerated rate.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D8414/D8414M − 21
5.3 The data from this test can be used to rank catalyst 7.15 Ancillary Equipment:
according to attrition rate. 7.15.1 Analytical Balance, 4-place, readable to 0.0001g,
with a minimum range of 30 gms.
5.4 The test requires a relatively small sample size of 5 g
7.15.2 Weigh Boats, small, disposable plastic.
[0.175 oz] and a relatively short analysis time of 40 min. This
7.15.3 Desiccator, with desiccant.
test should be useful to quality control facilities that require
7.15.4 Humidity Probe, with calibration traceable to the
fast turnaround time and research and development (R&D)
National Institutes of Standards and Technology (NIST).
facilities that have limited sample material.
7.15.5 Oven, 225°C [437°F], vented with 1CFH (0.5lpm)
air flow.
6. Interferences
7.15.6 Furnace, muffle, 565°C [1049°F], vented with
6.1 There are no known interferences. Factors such as
1CFH (0.5lpm) air flow.
density, particle size distribution, morphology, and intrinsic
7.15.7 Assorted Borosilicate Glass or Ceramic Dishes and
hardnesswillaffecttheresults.Theseandotherfactorsmustbe
Crucibles.
considered.
8. Reagents and Materials
7. Apparatus
8.1 Instrument Grade Air.
7.1 Pressure Regulator, to reduce the Instrument grade air
supply pressure to 206.8 kPa [30 psig].
8.2 De-ionized Water, 16 meg-Ω, minimum.
7.2 Mass Flow Controller, capable of delivering 21.0 6
8.3 Collection Thimbles, 19 by 90 mm [0.7 by 0.4 in.],
0.05 slpm of air into a system with 34 kPa [5 psig] of
Whatman #2814199®, or equivalent.
backpressure. Mass flow controller should not be affected by
small amounts of moisture in the air supply, changes in room
9. Assembling the Apparatus
temperature, or changes in barometric pressure.
9.1 Refer to the block diagram, Fig. A1.3,in Annex A1.
7.3 Humidification Equipment, capable of humidifying
9.2 Attachtheshutoffvalveandthepressureregulatortothe
21slpm of air to 55 % relative humidity (RH) in a continuous,
source of instrument grade air. No air should be flowing at this
uninterrupted operation. De-ionized water addition, 16 meg-Ω
time.
minimum, can be automatic or manual. The humidifier should
have a 70-kPa [10-psi] pressure-relief valve installed. 9.3 Attachtheinletofthemassflowcontrollertotheexitof
the pressure regulator.
7.4 Backpressure Gauge, 0-100 kPa [0-15 psig].
9.4 The exit of the mass flow controller is attached to the
7.5 Three-way Air Solenoid Valve.
inlet of the humidifier. The humidifier should have a 70-kPa
7.6 Timer.
[10-psi] pressure-relief valve installed. If not, install a tee
fitting and a pressure-relief valve at the exit of the humidifier.
7.7 Jet Cup—See Fig. A1.1 in Annex A1.
7.8 Fines Disengagement Chamber—See Fig. A1.2 in An- 9.5 Install a tee fitting and the backpressure gauge,
0-100kPa [0-15psig].
nexA1. Can be welded steel or solid 2-piece with or without a
fines release coating.
9.6 Next, install the three-way air solenoid valve controlled
7.9 Connector, to attach the jet cup to the fines disengage- by a timer. The inlet of the valve is attached to the tee fitting
ment chamber. Commercially available equipment has the jet used to mount the backpressure gauge. With the timer
cup permanently mounted into a holder that forms a positive deactivated, air should be flowing through the vent. Wire the
connection with the fines disengagement chamber. Lab built solenoidtoatimercapableoftiming20.0min.Attacha10-cm
units use a machined plastic connector with o-rings to make a [4-in.] length of 1.6-mm [ ⁄16-in.] outer diameter (OD) tubing
leak tight seal. The connector can be as simple as a piece of to the vent.
large diameter Tygon® tubing and two hose clamps.
9.7 Attach a hose to the exit of the solenoid valve. Attach
7.10 Rack or Mounting Brackets, to support the fines the other end of the hose to the jet cup. Keep the hose as short
disengagement chamber in an upright position. as possible, usually less than 1m [3ft].
7.11 Tubing, pre-cleaned stainless steel or food grade tub- 9.8 Mount the fines disengagement chamber in an upright
ing.
position.
7.12 Assorted Tubing Fittings.
9.9 Assemble the thimble holders (14.3).
9.9.1 Insert the barb end of the pipe elbow into the rubber
1 3
7.13 Pipe Elbows, 15 mm [ ⁄2in.] NPT × 10 mm [ ⁄8in.]
stopper.
Barb. Light weight plastic.
9.9.2 Prepare a minimum of two thimble holders. Four or
7.14 Rubber Stoppers, number 5.5 with a hole bored with a
more will speed up analysis time.
#7 cork borer.
3 4
Tygon® a registered trademark of Saint-Gobain Corporation, 20 Moores Rd, Whatman® is a registered trademark of Cytiva, 100 ResultsWy, Marlborough,
Malvern, PA 19355. MA 01752.
D8414/D8414M − 21
10. Hazards 12.4.5 Slowly increase the flow on the mass flow controller
until the backpressure gauge reads 41kPa [6psig]. Above
10.1 The main hazard in this test is the formation of
48kPa[7psig],theplugwillblowoutofthechamber.Shutoff
respirable fines. All cleaning of the jet cup, fines disengage-
the air flow at 41kPa [6psig].
ment chamber, thimbles, and thimble holders should be per-
12.4.6 Allow the pressure to stabilize and then begin taking
formed either in a hood rated for this type usage or with a
readingsonthebackpressuregauge.Aleakagerateoflessthan
high-efficiency particulate air (HEPA) vacuum cleaner.
0.7kPa [0.1psig] per minute is allowable.
12.4.7 Above that level, snoop the connections with a leak
11. Sampling
detectorsolution.Donotforgettherubberstopperinthetopof
11.1 This test uses 5-g [0.175-oz] aliquots of catalyst
the fines disengagement chamber. If your chamber is welded
materialfortesting.Themainsourceoferrorinthistestoccurs
steel, snoop the welds.
in the sampling process. Fluid catalytic cracking catalyst, for
12.4.8 If the leakage rate is still unacceptable, isolate
example, is a non-homogeneous material in that it has a
sections of the flow assembly until the leak is found.
particle-size distribution.
12.4.9 Once the leakage rate is below the acceptable level,
slowly and carefully remove the plug from the top of the
11.2 Riffle the sample to obtain a 100-g [3.5-oz.] sub-
chamber.
sample.Ifarifflerisnotavailable,usethefollowingprocedure:
12.4.10 Reset the timer.
11.2.1 Gentlymixtheoriginalsamplecontainertoblendthe
12.4.11 Turn on the air supply and reset the mass flow
sample. This blending shall not cause the sample to attrite or
controller to 21.0slpm.
form fines, or both.
11.2.2 Remove a 100-g [3.5-oz] aliquot and place in a
12.5 Adjusting the Humidification:
borosilicate glass or ceramic dish sized to provide a 1.2-cm
12.5.1 Turn on the power to the humidifier.
[ ⁄2-in.] bed depth.
12.5.2 Adjust the set point to 55% RH.
12.5.3 Wait until the humidity gauge has stabilized near
11.3 If 100 g [3.5-oz] of material is not available, size the
55%RH.
dish to maintain a 1.2-cm [ ⁄2-in.] bed depth. Small aliquots
12.5.4 Depressthetimertodirecttheairflowthroughthejet
such as 6 g [0.2 oz] are generally placed into a crucible.
cup and into the fines disengagement chamber.
11.4 Drythematerialfor1hat225°C[437°F]followedby
12.5.5 Insert a National Institute of Standards and Technol-
2h at 565°C [1049°F].
ogy (NIST) traceable humidity probe into the center of the
11.5 Cool the material in a desiccator. Place in a 125-ml fines disengagement chamber.
12.5.6 Begin recording the % RH every 30 sec. Adjust the
[4-oz] glass bottle when cool.
setpointonthehumidifieruntilaconstantreadingof50%RH
11.6 Store the dried material in a desiccator.
is obtained at the fines disengagement chamber.
11.7 Materialnotanalyzedin24hrequiresreheatingfor1h
12.5.7 Remove the humidity probe and reset the timer.
at 565°C [1049°F].
NOTE 2—The pressure test is only run on initial startup of the system
and whenever the control chart indicates there may be a problem with the
12. Preparation of Apparatus
system.
12.1 Turn on the instrument grade air. Set the mass flow
13. Calibration and Standardization
controller to 21.0slpm.
13.1 Establishing a Control Standard and a Control Chart:
12.2 Air should be flowing through the vent of the solenoid
13.1.1 Select a fresh fluid catalytic cracking (FCC) catalyst
valve. Verify the backpressure is between 28 to 34kPa [4 to
with a normal attrition rate of 3 to 6%. Maintain a sufficient
5psig]. If not, adjust the length of the tubing attached to the
quantity for at least 300 sample preparations and analyses.
vent to obtain the proper backpressure.
13.1.2 Dry 100 g [3.5-oz] of the material as directed in
12.3 Set the timer for 20.0min. Depress the start button on
Section 11.
thetimer.Thesolenoidshouldswitchandairshouldbeflowing
13.1.3 Perform a minimum of seven analyses of the control
through the jet cup.The backpressure should be between 28 to
standard as directed in Section 13. Record these values to two
34kPa [4 to 5psig].
decimal places. Calculate the average and the Relative Stan-
dard Deviation (RSD) for the JCI values. (See Note 3.)
12.4 Pressure Testing the System (see Note 2):
13.1.4 Prepare a control chart with the average value from
12.4.1 Resetthetimersothatairisflowingthroughthevent.
13.1.3 as the center line. Draw in the 2-sigma and 3-sigma
12.4.2 Insert a plug into the exit of the fines disengagement
lines.
chamber. The plug can be made by screwing a large bolt into
13.1.5 Thecontrolstandardisanalyzeddailyandplottedon
a one-hole stopper. Attach a safety cord to the bolt and the
the chart. Any result outside 3-sigma is repeated immediately
frame of the unit.
with a freshly prepared control standard. Whenever there are
12.4.3 Reduce the mass flow controller setting to zero.
two consecutive values beyond 2-sigma, the test is repeated
Verifytheflowreadingiszero.Themassflowcontrollershould
with a freshly prepared control standard.
read zero and the backpressure gauge should read zero.
12.4.4 Depress the timer so that air is directed through the 13.2 Calculating the Control Factor (CF):
jet cup. 13.2.1 The initial CF is set at 1.000.
D8414/D8414M − 21
13.2.2 Forexample,letussaythatthesevenanalyseshadan 14.8 Be certain air is not flowing through the jet cup.
average JCI of 5.00. Transfer the sample to the jet cup.Asmall amount of sample,
approximately 0.05g [0.02oz] will remain in the weigh boat.
13.2.3 Monthly, all of the data on the control chart is
averaged and the 1-sigma standard deviation is calculated for That is acceptable.
the monthly average. One way to record this data is with an
14.9 Reweigh the weigh boat and record as Sw-final, to the
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