ASTM D3610-00(2004)
(Test Method)Standard Test Method for Total Cobalt In Alumina-Base Cobalt-Molybdenum Catalyst by Potentiometric Titration Method
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 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.
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Designation:D3610–00 (Reapproved 2004)
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 or intralaboratory basis. It is anticipated that catalyst producers
and users will find this test method to be of value.
1.1 This test method covers the determination of cobalt
(expressed as the oxide) in fresh cobalt-molybdenum catalyst,
5. Interferences
in the range of 0.5 to 10 % cobalt oxide.
5.1 None of the elements normally found in fresh cobalt-
1.2 This standard does not purport to address all of the
molybdenum catalysts interferes with this method. (Elements
safety concerns, if any associated with its use. It is the
such as nickel, phosphorus, silicon, aluminum, and molybde-
responsibility of the user of this standard to establish appro-
num do not interfere; elements such as iron, chromium,
priate safety and health practices and determine the applica-
vanadium, and manganese do interfere).
bility of regulatory limitations prior to use.
6. Apparatus
2. Referenced Documents
2 6.1 Analytical Balance and Weights—The balance used to
2.1 ASTM Standards:
weigh the sample shall have a precision of 0.1 mg. Analytical
D1193 Specification for Reagent Water
weightsshallbeofprecisiongradeorcalibratedagainstasetof
E50 Practices for Apparatus, Reagents, and Safety Consid-
certified standard weights.
erations for Chemical Analysis of Metals, Ores, and
6.2 Buret—The 50-mL buret used to deliver the standard
Related Materials
potassiumferricyanideandstandardcobaltsolutionsshallbeof
E173 Practice for Conducting Interlaboratory Studies of
3 precision grade and shall be read to 0.01 mL by interpolation.
Methods for Chemical Analysis of Metals
6.3 Glassware—Beakers used in the analysis of the sample
3. Summary of Test Method shall be of chemical-resistant glass and free of etched surfaces.
Before using, all glassware shall be cleaned in hot dilute
3.1 The sample is decomposed by adding water and sulfuric
hydrochloric acid and thoroughly rinsed with water.
acid and then heating until completely dissolved. The cold
6.4 Potentiometric Titration Apparatus—Apparatus No. 3B
solution is diluted with water and transferred to a 250-mL
of Practices E50, or equivalent.
volumetric flask. An aliquot of this solution containing be-
6.5 Hot Plate—Capable of maintaining surface temperature
tween10and30mgofcobaltistransferredtoa250-mLbeaker
of at least 300°C.
containing measured volumes of potassium ferricyanide and
ammonium citrate solutions, ammonia, and petroleum ether.
7. Reagents
The excess of ferricyanide is then back-titrated with a standard
7.1 Purity of Reagents—Reagent grade chemicals shall be
cobalt solution.
used in all tests. Unless otherwise indicated, it is intended that
4. Significance and Use all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
4.1 This test method sets forth a procedure by which
where such specifications are available. Other grades may be
catalyst samples may be compared either on an interlaboratory
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
This test method is under the jurisdiction of ASTM Committee D32 on
accuracy of the determination.
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
Composition.
Current edition approved April 1, 2004. Published April 2004. Originally
approved in 1977. Last previous edition D3610–00. DOI: 10.1520/D3610-00R04. Reagent Chemicals, American Chemical Society Specifications, American
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM listed by the American Chemical Society, see Annual Standards for Laboratory
Standards volume information, refer to the standard’s Document Summary page on Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
the ASTM website. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Withdrawn. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3610–00 (2004)
7.2 Purity of Water—Unless otherwise indicated, references 8. Sample Preparation
to water shall be understood to mean reagent water conforming
8.1 Pulverize the analytical sample to pass a No. 100
to Specification D1193, Type IV.
(150-µm) sieve. Ignite the pulverized sample for 30 min at
7.3 Ammonium Citrate Solution (680 g/L)—Dissolve 680 g
550°C in a muffle furnace. Allow to cool in a desiccator.
of diammonium hydrogen citrate (NH ) HC H O in 750 mL
4 2 6 5 7
of water and dilute to 1 L.
9. Procedure
7.4 Ammonium Hydroxide (sp. gr. 0.90)—Concentrated am-
9.1 Transfer a 4.5-g sample, weighed to the nearest 1 mg, to
monium hydroxide (NH OH).
a 250-mLbeaker. Moisten with 25 mLof water, add slowly 40
7.5 Cobalt Standard Solution (1 mL = 1.494 mg of CoO)—
mLofconcentratedsulfuricacid,andstir.Coverthebeakerand
Dissolve 5.80 g of cobalt nitrate Co(N
...
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