ASTM D3610-22

Standard Test Method for Total Cobalt in Alumina-Base Cobalt-Molybdenum Catalyst by Potentiometric Titration Method

SIGNIFICANCE AND USE
4.1 This test method sets forth a procedure by which catalyst samples may be compared either on an interlaboratory or intralaboratory basis. It is anticipated that catalyst producers and users will find this test method to be of value.
SCOPE
1.1 This test method covers the determination of cobalt (expressed as the oxide) in fresh cobalt-molybdenum catalyst, in the range of 0.5 to 10 % cobalt oxide.  
1.2 Units—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: 31-Jul-2022
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.03 - Chemical Composition

Relations

• Refers: ASTM E50-17 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 01-Sep-2017
• Refers: ASTM E50-11(2016) - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 01-Aug-2016
• Refers: ASTM E50-11 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 15-Oct-2011
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM E50-00(2005) - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 01-May-2005
• Refers: ASTM E50-00 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 10-Nov-2000
• Refers: ASTM D1193-99e1 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1193-99 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999

Overview

ASTM D3610-22 is the internationally recognized standard test method for determining total cobalt content in alumina-based cobalt-molybdenum catalysts using potentiometric titration. This test method is specifically designed for catalyst samples containing between 0.5% and 10% cobalt oxide (CoO) by weight. Widely used by catalyst producers, laboratories, and users, ASTM D3610-22 provides a reliable and repeatable means for both interlaboratory and intralaboratory comparison of catalyst compositions, supporting quality assurance and regulatory compliance in the catalyst industry.

Key Topics

• Cobalt Determination: The standard outlines potentiometric titration as the preferred method for quantifying cobalt in fresh alumina-base cobalt-molybdenum catalysts.
• Applicable Range: Suitable for samples with cobalt oxide content ranging from 0.5% to 10%.
• Sample Preparation: Requires pulverizing the catalyst, proper dissolution using sulfuric acid, and precise handling under laboratory safety protocols.
• Apparatus and Reagents: Specifies the use of precision analytical balances, burets, standard solutions (potassium ferricyanide and cobalt standard solution), and potentiometric titration equipment.
• Interference: Addresses the impact of common elements present in fresh catalysts-elements like nickel, phosphorus, silicon, aluminum, and molybdenum do not interfere, while iron, chromium, vanadium, and manganese can interfere with accuracy.
• Precision and Repeatability: Designed to provide consistent results across different laboratories and operators, based on participation and statistical evaluation.

Applications

ASTM D3610-22 is crucial for various stakeholders in the catalyst and chemical industries:

• Catalyst Manufacturers: Ensures accurate formulation and quality control of cobalt-molybdenum catalysts used in refining and petrochemical processes.
• Industrial Laboratories: Offers a validated protocol for regular testing of fresh catalysts to monitor production consistency and meet contractual or regulatory specifications.
• Quality Assurance: Supports producers and users in meeting both internal quality metrics and external regulatory requirements.
• Interlaboratory Comparisons: Facilitates data comparability across various sites, providing a standard means to assess and benchmark results.
• Process Optimization: Enables accurate measurement of active ingredients, contributing to better process control and catalyst performance evaluation.

Related Standards

For comprehensive and standardized catalyst analysis, users of ASTM D3610-22 should also be aware of the following relevant ASTM standards:

• ASTM D1193 – Specification for Reagent Water: Ensures the water used in analyses meets the appropriate purity requirements.
• ASTM E50 – Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials: Provides guidelines for analytical best practices and laboratory safety.
• ASTM E173 – Practice for Conducting Interlaboratory Studies of Methods for Chemical Analysis of Metals (Withdrawn): Serves as reference for statistical analysis of laboratory data.

Keywords: alumina-base catalyst, cobalt analysis, molybdenum catalyst, potentiometric titration, catalyst quality control, ASTM D3610, chemical analysis standard.

By following ASTM D3610-22, organizations can be confident in the reliability, accuracy, and consistency of their cobalt content determinations, ultimately supporting higher quality catalyst products and enhanced operational performance.

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: D3610 − 22
Standard Test Method for
Total Cobalt in Alumina-Base Cobalt-Molybdenum Catalyst
by Potentiometric Titration Method
This standard is issued under the fixed designation D3610; 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 solution is diluted with water and transferred to a 250 mL
volumetric flask. An aliquot of this solution containing be-
1.1 This test method covers the determination of cobalt
tween10and30 mgofcobaltistransferredtoa250 mLbeaker
(expressed as the oxide) in fresh cobalt-molybdenum catalyst,
containing measured volumes of potassium ferricyanide and
in the range of 0.5 to 10 % cobalt oxide.
ammonium citrate solutions, ammonia, and petroleum ether.
1.2 Units—The values stated in SI units are to be regarded
The excess of ferricyanide is then back-titrated with a standard
as standard. No other units of measurement are included in this
cobalt solution.
standard.
1.3 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
4.1 This test method sets forth a procedure by which
responsibility of the user of this standard to establish appro-
catalyst samples may be compared either on an interlaboratory
priate safety, health, and environmental practices and deter-
or intralaboratory basis. It is anticipated that catalyst producers
mine the applicability of regulatory limitations prior to use.
and users will find this test method to be of value.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
5. Interferences
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5.1 None of the elements normally found in fresh cobalt-
mendations issued by the World Trade Organization Technical
molybdenum catalysts interferes with this method. (Elements
Barriers to Trade (TBT) Committee.
such as nickel, phosphorus, silicon, aluminum, and molybde-
num do not interfere; elements such as iron, chromium,
2. Referenced Documents
vanadium, and manganese do interfere).
2.1 ASTM Standards:
D1193 Specification for Reagent Water
6. Apparatus
E50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and 6.1 Analytical Balance and Weights—The balance used to
Related Materials weigh the sample shall have a precision of 0.1 mg. Analytical
E173 Practice for Conducting Interlaboratory Studies of weightsshallbeofprecisiongradeorcalibratedagainstasetof
Methods for Chemical Analysis of Metals (Withdrawn certified standard weights.
1997)
6.2 Buret—The 50 mL buret used to deliver the standard
potassiumferricyanideandstandardcobaltsolutionsshallbeof
3. Summary of Test Method
precision grade and shall be read to 0.01 mL by interpolation.
3.1 The sample is decomposed by adding water and sulfuric
acid and then heating until completely dissolved. The cold
6.3 Glassware—Beakers used in the analysis of the sample
shall be of chemical-resistant glass and free of etched surfaces.
This test method is under the jurisdiction of ASTM Committee D32 on
Before using, all glassware shall be cleaned in hot dilute
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
hydrochloric acid and thoroughly rinsed with water.
Composition.
Current edition approved Aug. 1, 2022. Published August 2022. Originally
6.4 Potentiometric Titration Apparatus—Apparatus No. 3B
approved in 1977. Last previous edition approved in 2015 as D3610 – 00(2015).
of Practices E50, or equivalent.
DOI: 10.1520/D3610-22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.5 Hot Plate—Capable of maintaining surface temperature
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
of at least 300 °C.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
6.6 Laboratory fume hood suitable for use with fuming
The last approved version of this historical standard is referenced on
www.astm.org. sulfuric acid.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3610 − 22
7. Reagents
Y = milligrams of CoO per millilitre of standard solution,
and
7.1 Purity of Reagents—Reagent grade chemicals shall be
Z = millilitres of potassium ferricyanide solution.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit- Triplicate values should be obtained for the cobalt oxide
tee onAnalytical Reagents of theAmerican Chemical Society,
equivalent. The values obtained should check within 1 to 2
where such specifications are available. Other grades may be parts per thousand.
used, provided it is first ascertained that the reagent is of
7.8 Sulfuric Acid (sp. gr. 1.84)—Concentrated sulfuric acid
sufficiently high purity to permit its use without lessening the
(H SO ).
2 4
accuracy of the determination.
8. Sample Preparation
7.2 Purity of Water—Unless otherwise indicated, references
8.1 Warning—All grinding and pulverizing of the sample
to water shall be understood to mean reagent water conforming
should be conducted in a fume hood.
to Specification D1193, Type IV.
8.2 Pulverize the analytical sample to pass a No. 100
7.3 Ammonium Citrate Solution (680 g/L)—Dissolve 680 g
(150 µm) sieve. Ignite the pulverized sample for 30 min at
of diammonium hydrogen citrate (NH ) HC H O in 750 mL
4 2 6 5 7
550 °C in a muffle furnace. Allow to cool in a desiccator.
of water and dilute to 1 L.
7.4 Ammonium Hydroxide (sp. gr. 0.90)—Concentrated am-
9. Procedure
monium hydroxide (NH OH).
9.1 Warning—All heating of acid solutions on a hot plate
7.5 Cobalt
...

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: D3610 − 00 (Reapproved 2015) D3610 − 22
Standard Test Method for
Total Cobalt in Alumina-Base Cobalt-Molybdenum Catalyst
by Potentiometric Titration Method
This standard is issued under the fixed designation D3610; 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 the determination of cobalt (expressed as the oxide) in fresh cobalt-molybdenum catalyst, in the range
of 0.5 to 10 % cobalt oxide.
1.2 Units—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 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:
D1193 Specification for Reagent Water
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E173 Practice for Conducting Interlaboratory Studies of Methods for Chemical Analysis of Metals (Withdrawn 1997)
3. Summary of Test Method
3.1 The sample is decomposed by adding water and sulfuric acid and then heating until completely dissolved. The cold solution
is diluted with water and transferred to a 250-mL250 mL volumetric flask. An aliquot of this solution containing between 10 and
30 mg 30 mg of cobalt is transferred to a 250-mL250 mL beaker containing measured volumes of potassium ferricyanide and
ammonium citrate solutions, ammonia, and petroleum ether. The excess of ferricyanide is then back-titrated with a standard cobalt
solution.
4. Significance and Use
4.1 This test method sets forth a procedure by which catalyst samples may be compared either on an interlaboratory or
intralaboratory basis. It is anticipated that catalyst producers and users will find this test method to be of value.
This test method is under the jurisdiction of ASTM Committee D32 on Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical Composition.
Current edition approved Dec. 1, 2015Aug. 1, 2022. Published December 2015August 2022. Originally approved in 1977. Last previous edition approved in 20102015
as D3610–00(2010).D3610 – 00(2015). DOI: 10.1520/D3610-00R15.10.1520/D3610-22.
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.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3610 − 22
5. Interferences
5.1 None of the elements normally found in fresh cobalt-molybdenum catalysts interferes with this method. (Elements such as
nickel, phosphorus, silicon, aluminum, and molybdenum do not interfere; elements such as iron, chromium, vanadium, and
manganese do interfere).
6. Apparatus
6.1 Analytical Balance and Weights—The balance used to weigh the sample shall have a precision of 0.1 mg. Analytical weights
shall be of precision grade or calibrated against a set of certified standard weights.
6.2 Buret—The 50-mL50 mL buret used to deliver the standard potassium ferricyanide and standard cobalt solutions shall be of
precision grade and shall be read to 0.01 mL 0.01 mL by interpolation.
6.3 Glassware—Beakers used in the analysis of the sample shall be of chemical-resistant glass and free of etched surfaces. Before
using, all glassware shall be cleaned in hot dilute hydrochloric acid and thoroughly rinsed with water.
6.4 Potentiometric Titration Apparatus—Apparatus No. 3B of Practices E50, or equivalent.
6.5 Hot Plate—Capable of maintaining surface temperature of at least 300°C.300 °C.
6.6 Laboratory fume hood suitable for use with fuming sulfuric acid.
7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
7.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Specification D1193, Type IV.
7.3 Ammonium Citrate Solution (680 g/L)—Dissolve 680 g of diammonium hydrogen citrate (NH ) HC H O in 750 mL of water
4 2 6 5 7
and dilute to 1 L.
7.4 Ammonium Hydroxide (sp. gr. 0.90)—Concentrated ammonium hydroxide (NH OH).
7.5 Cobalt Standard Solution (1 mL = 1.494 mg of CoO)—Dissolve 5.80 g of cobalt nitrate Co(NO ) ·6H O in 500 mL of water,
3 2 2
transfer to a 1-L1 L volumetric flask, dilute to volume, and mix. Since cobalt nitrate may not always be stoichiometric, its content
may be checked versus high-purity cobalt metal (99.9 % purity).
7.6 Petroleum Ether, b.p. 60 to 110°C.110 °C.
7.7 Potassium Ferricyanide Solution (1 mL ; 1.494 mg of CoO):
7.7.1 Dissolve 6.58 g of potassium ferricyanide K Fe(CN) in water and dilute to 1 L. Store the solution in a dark-colored bottle.
3 6
Standardize the solution just before use as follows: Transfer from a 50-mL50 mL buret approximately 25 mL
...