ASTM D3610-00
(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
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 problems, 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: D 3610 – 00
Standard Test Method for
Total Cobalt In Alumina-Base Cobalt-Molybdenum Catalyst
by Potentiometric Titration Method
This standard is issued under the fixed designation D 3610; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 5. Interferences
1.1 This test method covers the determination of cobalt 5.1 None of the elements normally found in fresh cobalt-
(expressed as the oxide) in fresh cobalt-molybdenum catalyst, molybdenum catalysts interferes with this method. (Elements
in the range of 0.5 to 10 % cobalt oxide. such as nickel, phosphorus, silicon, aluminum, and molybde-
1.2 This standard does not purport to address all of the num do not interfere; elements such as iron, chromium,
safety concerns, if any associated with its use. It is the vanadium, and manganese do interfere).
responsibility of the user of this standard to establish appro-
6. Apparatus
priate safety and health practices and determine the applica-
6.1 Analytical Balance and Weights— The balance used to
bility of regulatory limitations prior to use.
weigh the sample shall have a precision of 0.1 mg. Analytical
2. Referenced Documents
weights shall be of precision grade or calibrated against a set of
2.1 ASTM Standards: certified standard weights.
D 1193 Specification for Reagent Water 6.2 Buret—The 50-mL buret used to deliver the standard
E 50 Practices for Apparatus, Reagents, and Safety Precau- potassium ferricyanide and standard cobalt solutions shall be of
tions for Chemical Analysis of Metals precision grade and shall be read to 0.01 mL by interpolation.
E 173 Practice for Conducting Interlaboratory Studies of 6.3 Glassware—Beakers used in the analysis of the sample
Methods for Chemical Analysis of Metals shall be of chemical-resistant glass and free of etched surfaces.
Before using, all glassware shall be cleaned in hot dilute
3. Summary of Test Method
hydrochloric acid and thoroughly rinsed with water.
3.1 The sample is decomposed by adding water and sulfuric 6.4 Potentiometric Titration Apparatus— Apparatus No. 3B
acid and then heating until completely dissolved. The cold
of Practices E 50, or equivalent.
solution is diluted with water and transferred to a 250-mL 6.5 Hot Plate—Capable of maintaining surface temperature
volumetric flask. An aliquot of this solution containing be-
of at least 300°C.
tween 10 and 30 mg of cobalt is transferred to a 250-mL beaker
7. Reagents
containing measured volumes of potassium ferricyanide and
ammonium citrate solutions, ammonia, and petroleum ether. 7.1 Purity of Reagents—Reagent grade chemicals shall be
The excess of ferricyanide is then back-titrated with a standard used in all tests. Unless otherwise indicated, it is intended that
cobalt solution. all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
4. Significance and Use 4
where such specifications are available. Other grades may be
4.1 This test method sets forth a procedure by which used, provided it is first ascertained that the reagent is of
catalyst samples may be compared either on an interlaboratory
sufficiently high purity to permit its use without lessening the
or intralaboratory basis. It is anticipated that catalyst producers accuracy of the determination.
and users will find this test method to be of value.
7.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water conforming
to Specification D 1193, Type IV.
This test method is under the jurisdiction of ASTM Committee D32 on
Catalysts, and is the direct responsibility of Subcommittee D32.03 on Chemical
Analysis. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved April 10, 2000. Published May 2000. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
published as D 3610 – 77. Last previous edition D 3610 – 88 (1993). listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 11.01. Chemicals, BDH Ltd., Poole, Dorset, U.K. and the United States Pharmacopeia and
Annual Book of ASTM Standards, Vol 03.05. National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3610–00
7.3 Ammonium Citrate Solution (680 g/L)—Dissolve 680 g 8. Sample Preparation
of diammonium hydrogen citrate (NH ) HC H O in 750 mL
4 2 6 5 7
8.1 Pulverize the analytical sample to pass a No. 100
of water and dilute to 1 L.
(150-μm) sieve. Ignite the pulverized sample for 30 min at
7.4 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
550°C in a muffle furnace. Allow to cool in a desiccator.
monium hydroxide (NH OH).
9. Procedure
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
3 2 2 9.1 Transfer a 4.5-g sample, weighed to the nearest 1 mg, to
water, transfer to a 1-L volumetric flask, dilute to volume, and
a 250-mL beaker. Moisten with 25 mL of water, add slowly 40
mix. Since cobalt nitrate may not always be stoichiometric, its
mL of concentrated sulfuric
...
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