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

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
1
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
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.
3
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.
1
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.
2
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.
3
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
1

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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 = millilitr
...

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
1
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
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
3
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.
1
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.
2
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.
3
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
1

---------------------- Page: 1 ----------------------
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—Capa
...