ASTM D3610-00(2010)

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

SIGNIFICANCE AND USE
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: 31-Aug-2010
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.03 - Chemical Composition

Relations

• Replaces: ASTM D3610-00(2004) - Standard Test Method for Total Cobalt In Alumina-Base Cobalt-Molybdenum Catalyst by Potentiometric Titration Method
• Effective Date: 01-Sep-2010

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 2010)
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 Sept. 1, 2010. Published November 2010. Originally
approved in 1977. Last previous edition approved in 2004 as D3610–00(2004).
DOI: 10.1520/D3610-00R10.
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 (2010)
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
8. Sample Preparation
to Specification D1193, Type IV.
8.1 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 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 o
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