ASTM D4481-04
(Test Method)Standard Test Method for Total Nickel in Fresh Alumina-Base Catalysts
Standard Test Method for Total Nickel 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 nickel in fresh alumina-base catalysts and has been tested at nickel concentrations from 2.5 to 60 weight %, expressed as nickel oxide (NiO).
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 its use.
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Designation:D4481–04
Standard Test Method for
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Total Nickel in Fresh Alumina-Base Catalysts
This standard is issued under the fixed designation D4481; 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 4. Significance and Use
1.1 This test method covers the determination of nickel in 4.1 This test method sets forth a procedure by which
fresh alumina-base catalysts and has been tested at nickel catalyst samples can be compared either on an interlaboratory
concentrations from 2.5 to 60 weight %, expressed as nickel or intralaboratory basis. It is anticipated that catalyst producers
oxide (NiO). and users will find this method of value.
1.2 This standard does not purport to address all of the
5. Interferences
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5.1 Cobalt, molybdenum, and aluminum do not interfere.
Interferences by elements that precipitate as hydroxides, such
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to its use. as iron, chromium, aluminum, lead, tin, manganese, titanium,
and zirconium, are avoided by the addition of ammonium
2. Referenced Documents
citrate before making the solutions ammoniacal. Copper,
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2.1 ASTM Standards: present in the 2 to 10 % range, tends to be co-precipitated with
D1193 Specification for Reagent Water the nickel dimethylglyoxime. The only other metal ions pre-
E105 Practice for Probability Sampling Of Materials cipitated by dimethylglyoxime are palladium, gold, and bis-
E177 Practice for Use of the Terms Precision and Bias in muth.
ASTM Test Methods
6. Apparatus
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to 6.1 Beakers, 600-mL, 150-mL.
6.2 Hotplate.
Determine the Precision of a Test Method
6.3 Furnace, electric muffle. Calibrated and capable of
3. Summary of Test Method
maintaining temperatures of 550 6 25°C, and 950 6 25°C.
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3.1 The test specimen (as received) is treated with concen- 6.4 Platinum Dishes, 100-mL capacity.
trated hydrochloric acid to solubilize the nickel. If necessary, 6.5 Mortar and Pestle, agate, or equivalent mechanical
nickel is recovered from any insoluble residue by potassium grinder.
pyrosulfate fusion, after hydrofluoric-sulfuric acid treatment to 6.6 Crucibles, sintered-glass, 30-mL, medium porosity frit.
remove silica. Ammonium citrate is added to complex the 6.7 Fiberglass Filter, 3.2 cm.
aluminum and buffer the solution. Nickel is precipitated as 6.8 Drying Oven capable of maintaining a temperature of
nickel dimethylglyoxime, Ni (C H O N ) , at a weakly alka- 120°C.
4 7 2 2 2
line pH. The precipitate is washed and weighed as Ni 6.9 Vacuum Filtering Flask, 500-mL.
(C H O N ) after drying at 120°C. 6.10 Filter Holder and Filter Disk, Millipore 0.65 µm-
4 7 2 2 2
3.2 A separate test specimen is taken to determine loss on 47-mm diameter.
ignition (LOI) at 550°C. The value is used to calculate the 6.11 pH Paper to detect a value of 9.
nickel as percent nickel oxide (NiO) on a 550°C dry basis. 6.12 Screen, 250-µm openings, 60-mesh.
6.13 Analytical Balance, capable of weighing to nearest 0.1
mg.
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This test method is under the jurisdiction of Committee D32 on Catalysts and
6.14 Ashless Filter Pulp.
is the direct responsibility of Subcommittee D32.03 on Chemical Composition.
6.15 Desiccator.
Current edition approved April 1, 2004. Published April 2004. Originally
approved in 1985. Last previous edition approved in 1997 as D4481–97. DOI:
10.1520/D4481-04.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
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D4481–04
7. Reagents 9.2 Weigh three 1-g test specimens into platinum dishes or
porcelain crucibles. Record mass to the nearest 0.1 mg as G .
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7.1 Purity of Reagents—Reagent grade chemicals shall be
Calcine for2hina 550°C muffle furnace. Transfer to a
used in all tests. Unless otherwise indicated, it is intended that
desiccator containing freshly activated 4A molecular sieve.
all reagents shall conform to the specifications of the Commit-
Cool, weigh, record mass as G , and calculate percent solids.
tee onAnalytical Reagents of theAmerican Chemical Society, 2
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9.3 To test speci
...
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