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ASTM D3943-04

(Test Method)

Standard Test Method for Total Molybdenum in Fresh Alumina-Base Catalysts

Standard Test Method for Total Molybdenum in Fresh Alumina-Base Catalysts

SIGNIFICANCE AND USE
This test method sets forth a procedure by which catalyst samples can be compared either on an interlaboratory or intralaboratory basis. It is anticipated that catalyst producers and users will find this method of value.
SCOPE
1.1 This test method covers the determination of molybdenum in alumina-base catalysts and has been cooperatively tested at molybdenum concentrations from 8 to 18 weight %, expressed as MoO3. Any component of the catalyst other than molybdenum such as iron, tungsten, etc., which is capable of being oxidized by either ferric or ceric ions after being passed through a zinc-amalgam reductor column (Jones reductor) will interfere.
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.

General Information

Status
Historical
Publication Date
31-Mar-2004
ICS
71.040.30 - Chemical reagents
Technical Committee
D32 - Catalysts
Drafting Committee
D32.03 - Chemical Composition
Current Stage
Ref Project

Relations

Replaces
ASTM D3943-00 - Standard Test Method for Total Molybdenum in Fresh Alumina-Base Catalysts
Effective Date
01-Apr-2004
Replaced By
ASTM D3943-10 - Standard Test Method for Total Molybdenum in Fresh Alumina-Base Catalysts
Effective Date
01-Apr-2010

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ASTM D3943-04 - Standard Test Method for Total Molybdenum in Fresh Alumina-Base CatalystsASTM D3943-04 - Standard Test Method for Total Molybdenum in Fresh Alumina-Base Catalysts
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ASTM D3943-04 - Standard Test Method for Total Molybdenum in Fresh Alumina-Base Catalysts
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3943–04
Standard Test Method for
1
Total Molybdenum in Fresh Alumina-Base Catalysts
This standard is issued under the fixed designation D3943; 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.
+3
1. Scope 3.2 The ferrous ion produced (three per Mo oxidized) is
titrated with standard ceric sulfate solution in the presence of
1.1 This test method covers the determination of molybde-
ferroin indicator. The indicator undergoes a color change (pink
num in alumina-base catalysts and has been cooperatively
to colorless or very faint blue-green) in the presence of excess
tested at molybdenum concentrations from 8 to 18 weight %,
+2
ceric ion. The amount of Fe titrated in the reaction
expressed as MoO . Any component of the catalyst other than
3
1 2 1 4 1 3 1 3
molybdenum such as iron, tungsten, etc., which is capable of
Fe 1 Ce → Fe 1 Ce (2)
being oxidized by either ferric or ceric ions after being passed
+6
is a direct measure of Mo concentration.
through a zinc-amalgam reductor column (Jones reductor) will
interfere.
4. Significance and Use
1.2 This standard does not purport to address all of the
4.1 This test method sets forth a procedure by which
safety concerns, if any, associated with its use. It is the
catalyst samples can be compared either on an interlaboratory
responsibility of the user of this standard to establish appro-
or intralaboratory basis. It is anticipated that catalyst producers
priate safety and health practices and determine the applica-
and users will find this method of value.
bility of regulatory limitations prior to use.
5. Interferences
2. Referenced Documents
5.1 Elements such as As, Sb, Cr, Fe, Ti, V, U, or W can
2
2.1 ASTM Standards:
interfere in this analysis. If serious interference occurs, it will
D1193 Specification for Reagent Water
be necessary to isolate the molybdenum from the interfering
E173 Practice for Conducting Interlaboratory Studies of
species prior to measurement.
3
Methods for Chemical Analysis of Metals
5.2 Organics and nitrates can interfere or react with the
E507 Test Method for Analysis of Aluminum in Iron Ores
zinc-amalgam if the sulfuric acid treatment is not properly
by Flame Atomic Absorption Spectrometry
carried out as described in 9.1.
3. Summary of Test Method
6. Apparatus
3.1 The catalyst is digested in hot sulfuric acid to dissolve
6.1 Beakers, 250-mL.
molybdenum, destroy organic matter, and to expel nitrates if
6.2 Jones Reductor Column, 30-cm long by 2 cm in outer
present. The acid solution is diluted and passed through an
4
diameter, with a 100-mL reservoir. Attach a piece of vinyl
amalgamated zinc column (Jones reductor) into a receiving
tubing to the end of the delivery tube long enough to extend to
flask containing an excess of ferric ammonium sulfate. The
the bottom of the filtering flask (see Test Method E507).
+6
column quantitatively reduces the molybdenum (Mo to
6.3 Vacuum Filtering Flask, heavy-walled, 1000-mL.
+3
Mo ) which in turn is reoxidized in the receiving flask
6.4 Buret, 50-mL, Class A (0.1-mL divisions).
according to the reaction:
6.5 Stirring Motor, magnetic, and TFE-fluorocarbon-
13 1 3 1 6 1 2
5 9
Mo 1 3Fe → Mo 1 3Fe (1) covered stirring bars, 7.11 by 14.2 mm ( ⁄16 by 1 ⁄16 in.).
7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be
1
This test method is under the jurisdiction of ASTM Committee D32 on
used in all tests. Unless otherwise indicated, it is intended that
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
all reagents shall conform to the specifications of the Commit-
Composition.
Current edition approved April 1, 2004. Published April 2004. Originally
tee onAnalytical Reagents of theAmerican Chemical Society,
approved in 1980. Last previous edition approved in 2000 as D3943–00. DOI:
10.1520/D3943-04.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or The sole source of supply of the apparatus known to the committee at this time
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM is Part No. 8035-J10 from Thomas Scientific, 99 High Hill Rd. at 295, Swedesboro,
Standards volume information, refer to the standard’s Document Summary page on NJ 08085. If you are aware of alternative suppliers, please provide this information
the ASTM website. to ASTM International Headquarters. Your comments will receive careful consid-
3
1
Withdrawn. eration at a meeting of the responsible technical committee, which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United
...

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