ASTM D3610-00(2015)

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 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 30-Nov-2015
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.03 - Chemical Composition

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D3610 − 00 (Reapproved 2015)
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 ammonium citrate solutions, ammonia, and petroleum ether.
The excess of ferricyanide is then back-titrated with a standard
1.1 This test method covers the determination of cobalt
cobalt solution.
(expressed as the oxide) in fresh cobalt-molybdenum catalyst,
in the range of 0.5 to 10 % cobalt oxide.
4. Significance and Use
1.2 The values stated in SI units are to be regarded as
4.1 This test method sets forth a procedure by which
standard. No other units of measurement are included in this
catalyst samples may be compared either on an interlaboratory
standard.
or intralaboratory basis. It is anticipated that catalyst producers
1.3 This standard does not purport to address all of the
and users will find this test method to be of value.
safety concerns, if any associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Interferences
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5.1 None of the elements normally found in fresh cobalt-
molybdenum catalysts interferes with this method. (Elements
2. Referenced Documents
such as nickel, phosphorus, silicon, aluminum, and molybde-
num do not interfere; elements such as iron, chromium,
2.1 ASTM Standards:
vanadium, and manganese do interfere).
D1193 Specification for Reagent Water
E50 Practices for Apparatus, Reagents, and Safety Consid-
6. Apparatus
erations for Chemical Analysis of Metals, Ores, and
Related Materials
6.1 Analytical Balance and Weights—The balance used to
E173 Practice for Conducting Interlaboratory Studies of
weigh the sample shall have a precision of 0.1 mg. Analytical
Methods for Chemical Analysis of Metals (Withdrawn
weightsshallbeofprecisiongradeorcalibratedagainstasetof
1998)
certified standard weights.
6.2 Buret—The 50-mL buret used to deliver the standard
3. Summary of Test Method
potassiumferricyanideandstandardcobaltsolutionsshallbeof
3.1 The sample is decomposed by adding water and sulfuric
precision grade and shall be read to 0.01 mL by interpolation.
acid and then heating until completely dissolved. The cold
solution is diluted with water and transferred to a 250-mL
6.3 Glassware—Beakers used in the analysis of the sample
volumetric flask. An aliquot of this solution containing be-
shall be of chemical-resistant glass and free of etched surfaces.
tween10and30mgofcobaltistransferredtoa250-mLbeaker
Before using, all glassware shall be cleaned in hot dilute
containing measured volumes of potassium ferricyanide and
hydrochloric acid and thoroughly rinsed with water.
6.4 Potentiometric Titration Apparatus—Apparatus No. 3B
of Practices E50, or equivalent.
This test method is under the jurisdiction of ASTM Committee D32 on
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
6.5 Hot Plate—Capable of maintaining surface temperature
Composition.
of at least 300°C.
Current edition approved Dec. 1, 2015. Published December 2015. Originally
approved in 1977. Last previous edition approved in 2010 as D3610–00(2010).
DOI: 10.1520/D3610-00R15.
7. Reagents
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
7.1 Purity of Reagents—Reagent grade chemicals shall be
Standards volume information, refer to the standard’s Document Summary page on
used in all tests. Unless otherwise indicated, it is intended that
the ASTM website.
all reagents shall conform to the specifications of the Commit-
The last approved version of this historical standard is referenced on
www.astm.org. tee onAnalytical Reagents of theAmerican Chemical Society,
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3610 − 00 (2015)
where such specifications are available. Other grades may be Triplicate values should be obtained for the cobalt oxide
used, provided it is first ascertained that the reagent is of equivalent. The values obtained should check within 1 to 2
sufficiently high purity to permit its use without lessening the parts per thousand.
accuracy of the determination.
7.8 Sulfuric Acid (sp. gr. 1.84)—Concentrated sulfuric acid
7.2 Purity of Water—Unless otherwise indicated, references
(H SO ).
2 4
to water shall be understood to mean reagent water conforming
to Specification D1193, Type IV.
8. Sample Preparation
7.3 Ammonium Citrate Solution (680 g/L)—Dissolve 680 g
8.1 Pulverize the analytical sample to pass a No. 100
of diammonium hydrogen citrate (NH ) HC H O in 750 mL
(150-µm) sieve. Ignite the pulverized sample for 30 min at
4 2 6 5 7
of water and dilute to 1 L.
550°C in a muffle furnace. Allow to cool in a desiccator.
7.4 Ammonium Hydroxide (sp. gr. 0.90)—Concentrated am-
9. Procedure
monium hydroxide (NH OH).
9.1 Transfer a 4.5-g sample, weighed to the nearest 1 mg, to
7.5 Cobalt Standard Solution (1 mL = 1.494 mg of CoO)—
a 250-mLbeaker. Moisten with 25 mLof water, add slowly 40
Dissolve 5.80 g of cobalt nitrate Co(NO ) ·6H O in 500 mLof
3 2 2
mLofconcentratedsulfuricacid,andstir.Coverthebeakerand
water, transfer to a 1-L volumetric flask, dilute to volume, and
heat, using a hot plate or a Bunsen burner, until the sample
...

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 2010) D3610 − 00 (Reapproved 2015)
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 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 and health practices and determine the applicability of regulatory
limitations prior to use.
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 1998)
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-mL volumetric flask. An aliquot of this solution containing between 10 and 30 mg
of cobalt is transferred to a 250-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.
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-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 by interpolation.
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 Sept. 1, 2010Dec. 1, 2015. Published November 2010December 2015. Originally approved in 1977. Last previous edition approved in 20042010
as D3610–00(2004).D3610–00(2010). DOI: 10.1520/D3610-00R10.10.1520/D3610-00R15.
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 − 00 (2015)
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.
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
4 2 6 5 7
water 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-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.
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-mL buret approximately 25 mL of K Fe(CN) solution to
3 6
a 250-mL beaker. Record the interpolated buret reading to the nearest 0.01
...