ASTM D4699-23

Standard Test Method for Vibratory Packing Density of Large Formed Catalyst and Catalyst Carrier Particles

SIGNIFICANCE AND USE
5.1 This test method is used for measuring the vibratory packing density of formed particles used in fixed bed reactors, driers, and so forth.
SCOPE
1.1 This test method covers the determination of the vibratory packing density of formed catalyst and catalyst carrier particles that will not break up significantly under test conditions. For the purpose of this test, catalyst particles are defined as extrudates, spheres or formed pellets greater than 4.8 mm.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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-Sep-2023
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.02 - Physical-Mechanical Properties

Relations

• Replaces: ASTM D4699-03(2018)e1 - Standard Test Method for Vibratory Packing Density of Large Formed Catalyst and Catalyst Carrier Particles
• Effective Date: 01-Oct-2023
• Refers: ASTM D3766-24a - Standard Terminology Relating to Catalysts and Catalysis
• Effective Date: 01-Feb-2024
• Refers: ASTM D3766-24 - Standard Terminology Relating to Catalysts and Catalysis
• Effective Date: 01-Jan-2024
• Refers: ASTM E456-13a(2022)e1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Apr-2022
• Refers: ASTM E456-13a(2022) - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Apr-2022
• Refers: ASTM D3766-08(2018) - Standard Terminology Relating to Catalysts and Catalysis
• Effective Date: 01-Nov-2018

Overview

ASTM D4699-23: Standard Test Method for Vibratory Packing Density of Large Formed Catalyst and Catalyst Carrier Particles establishes a precise procedure for determining the vibratory packing density of large catalyst and catalyst carrier particles. This standard is developed by ASTM International, ensuring global recognition and compliance. The method specifically targets formed particles, including extrudates, spheres, and formed pellets with diameters greater than 4.8 mm, commonly used in fixed bed reactors and industrial dryers.

The standard emphasizes measurements using SI units and requires that test materials do not significantly disintegrate under test conditions. It plays a critical role in process optimization by providing reliable data on the packing properties of catalysts, contributing to improved reactor design and operational efficiency.

Key Topics

• Vibratory Packing Density Determination: The method involves vibrating a known mass of catalyst particles in a graduated cylinder and measuring the resulting packed volume to calculate the density.
• Sample Conditioning and Handling: Samples must be equilibrated to laboratory conditions and properly dried, especially with materials that may adsorb or lose moisture, ensuring consistent results.
• Apparatus and Equipment: The test specifies the use of a 2000-mL graduated cylinder, vibratory plate, desiccator with molecular sieve, precise balances, and a drying oven.
• Precision and Repeatability: The standard details procedures for interlaboratory comparison and provides statistical guidelines for repeatability, ensuring data reliability across different laboratories.
• Safety and Environmental Considerations: Users of ASTM D4699-23 are required to establish appropriate safety, health, and environmental practices prior to conducting the test.

Applications

The ASTM D4699-23 standard is widely applied in industrial sectors where large formed catalysts and catalyst carriers are used. Key applications include:

• Fixed Bed Reactors: Accurate packing density measurements support optimal catalyst loading, directly impacting reactor efficiency, pressure drop, and conversion rates.
• Industrial Dryers: Understanding how particles pack allows for better design and operation of drying equipment, affecting energy usage and drying consistency.
• Quality Control in Catalyst Manufacturing: Producers utilize this method to monitor batch-to-batch consistency, ensure compliance with customer specifications, and validate new formulations.
• Research and Development: Consistent test procedures provide credible data for performance comparisons among different catalyst shapes or carrier materials.

Related Standards

For robust testing and enhanced quality control, ASTM D4699-23 references and complements several other ASTM standards and guides, including:

• ASTM B215: Practices for Sampling Metal Powders
• ASTM D3766: Terminology Relating to Catalysts and Catalysis
• ASTM E105: Guide for Probability Sampling of Materials
• ASTM E122: Practice for Calculating Sample Size for Estimating Averages
• ASTM E177: Practice for Use of the Terms Precision and Bias
• ASTM E456: Terminology Relating to Quality and Statistics
• ASTM E691: Practice for Interlaboratory Study to Determine Precision
• ASTM E1272: Specification for Laboratory Glass Graduated Cylinders

These related standards help ensure the vibratory packing density measurements are dependable, statistically sound, and compatible with broader material characterization protocols.

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By adhering to ASTM D4699-23, laboratories and manufacturers can achieve accurate, repeatable measurements of catalyst packing density, supporting high-performance industrial operations and quality assurance in catalyst production.

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: D4699 − 23
Standard Test Method for
Vibratory Packing Density of Large Formed Catalyst and
Catalyst Carrier Particles
This standard is issued under the fixed designation D4699; 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 E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This test method covers the determination of the vibra-
E1272 Specification for Laboratory Glass Graduated Cylin-
tory packing density of formed catalyst and catalyst carrier
ders
particles that will not break up significantly under test condi-
tions. For the purpose of this test, catalyst particles are defined
3. Terminology
as extrudates, spheres or formed pellets greater than 4.8 mm.
3.1 Definitions—See Terminology D3766.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Test Method
standard.
4.1 A known sample of environmentally equilibrated
1.3 This standard does not purport to address all of the
formed catalyst or catalyst carrier particles is vibrated in a
safety concerns, if any, associated with its use. It is the
graduated cylinder. The vibratory packing density is deter-
responsibility of the user of this standard to establish appro-
mined for a specified drying condition.
priate safety, health, and environmental practices and deter-
5. Significance and Use
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
5.1 This test method is used for measuring the vibratory
dance with internationally recognized principles on standard-
packing density of formed particles used in fixed bed reactors,
ization established in the Decision on Principles for the
driers, and so forth.
Development of International Standards, Guides and Recom-
6. Apparatus
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
6.1 Graduated Cylinder, capacity 2000-mL.
6.2 Vibratory Plate.
2. Referenced Documents
6.3 Desiccator, with a desiccant grade molecular sieve such
2.1 ASTM Standards:
as 4A.
B215 Practices for Sampling Metal Powders
D3766 Terminology Relating to Catalysts and Catalysis
6.4 Balance, having a sensitivity of 1.0 g.
E105 Guide for Probability Sampling of Materials
6.5 Balance, having a sensitivity of 0.1 g.
E122 Practice for Calculating Sample Size to Estimate, With
6.6 Drying Oven.
Specified Precision, the Average for a Characteristic of a
Lot or Process
7. Sampling
E177 Practice for Use of the Terms Precision and Bias in
7.1 Test sample(s) shall be obtained from larger composites
ASTM Test Methods
by riffling or splitting in accordance with subsection 5.12 of
E456 Terminology Relating to Quality and Statistics
STP 447A with the aim of obtaining a representative sample
that mirrors the shape and size distribution of the larger
This test method is under the jurisdiction of ASTM Committee D32 on
Catalysts and is the direct responsibility of Subcommittee D32.02 on Physical-
Mechanical Properties. The sole source of supply of the Syntron Vibrating Machine, Model V-2-B with
Current edition approved Oct. 1, 2023. Published October 2023. Originally Power Pulse Controller, known to the committee at this time is FMC Technologies,
ɛ1
approved in 1987. Last previous edition approved in 2018 as D4699 – 03 (2018) . 57 Cooper Ave., Homer City, PA 15748–9234. If you are aware of alternative
DOI: 10.1520/D4699-23. suppliers, please provide this information to ASTM International Headquarters.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Your comments will receive careful consideration at a meeting of the responsible
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM technical committee , which you may attend.
Standards volume information, refer to the standard’s Document Summary page on Manual on Test Sieving Methods, ASTM STP 447A,ASTM International,
the ASTM website. 2005.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4699 − 23
FIG. 1 Example of Components of Vibratory Stand for Large Diameter Pellets
composite. Guide E105 provides guidance on constructing a 8.4 Clamp the cylinder to the vibratory plate (see example
sampling plan and Practice E122 assists the analyst with Fig. 1).
determining the representative sample size. The analyst is also
8.5 Start vibrator at a setting at the midpoint of the rheostat
urged to consult Practice B215 w
...

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: D4699 − 03 (Reapproved 2018) D4699 − 23
Standard Test Method for
Vibratory Packing Density of Large Formed Catalyst and
Catalyst Carrier Particles
This standard is issued under the fixed designation D4699; 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—Keywords updated editorially in May 2018.
1. Scope
1.1 This test method covers the determination of the vibratory packing density of formed catalyst and catalyst carrier particles that
will not break up significantly under test conditions. For the purpose of this test, catalyst particles are defined as extrudates, spheres
or formed pellets greater than 4.8 mm.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.
2. Referenced Documents
2.1 ASTM Standards:
B215 Practices for Sampling Metal Powders
D3766 Terminology Relating to Catalysts and Catalysis
E105 Guide for Probability Sampling of Materials
E122 Practice for Calculating Sample Size to Estimate, With Specified Precision, the Average for a Characteristic of a Lot or
Process
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
E1272 Specification for Laboratory Glass Graduated Cylinders
3. Terminology
3.1 Definitions—See Terminology D3766.
This test method is under the jurisdiction of ASTM Committee D32 on Catalysts and is the direct responsibility of Subcommittee D32.02 on Physical-Mechanical
Properties.
Current edition approved May 1, 2018Oct. 1, 2023. Published June 2018October 2023. Originally approved in 1987. Last previous edition approved in 20132018 as
ɛ1
D4699–03(2013).D4699 – 03 (2018) . DOI: 10.1520/D4699-03R18.10.1520/D4699-23.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4699 − 23
4. Summary of Test Method
4.1 A known sample of environmentally equilibrated formed catalyst or catalyst carrier particles is vibrated in a graduated
cylinder. The vibratory packing density is determined for a specified drying condition.
5. Significance and Use
5.1 This test method is used for measuring the vibratory packing density of formed particles used in fixed bed reactors, driers, and
so forth.
6. Apparatus
6.1 Graduated Cylinder, capacity 2000-mL.
6.2 Vibratory Plate.
6.3 Desiccator, with a desiccant grade molecular sieve such as 4A.
6.4 Balance, having a sensitivity of 1.0 g.
6.5 Balance, having a sensitivity of 0.1 g.
6.6 Drying Oven.
7. Sampling
7.1 Test sample(s) shall be obtained from larger composites by riffling or splitting in accordance with subsection 5.12 of STP
447A with the aim of obtaining a representative sample that mirrors the shape and size distribution of the larger composite. Guide
E105 provides guidance on constructing a sampling plan and Practice E122 assists the analyst with determining the representative
sample size. The analyst is also urged to consult Practice B215 which contains excellent sampling guidance.
8. Procedure
8.1 Equilibrate test sample to laboratory environment for 4 h.
8.2 Pour between 1000 to 2000 mL of the test specimen carefully into a tared beaker and weigh to the nearest 1 g. Record as W.
8.3 Separately weigh to the nearest tenth of a gram about 100 g 100 g of additional test sample, W , that will be used for moisture
I
loss. Heat this sample at 400 6 15°C400 °C 6 15 °C for not less than 3 h. 3 h. Normally, this treatment can take place in air;
however, in the case of materials that might react with air at elevated temperature (such as prereduced catalysts) the heat treatment
should tak
...