ASTM D4481-97
(Test Method)Standard Test Method for Total Nickel in Fresh Alumina-Base Catalysts
Standard Test Method for Total Nickel in Fresh Alumina-Base Catalysts
SCOPE
1.1 This test method covers the determination of nickel in fresh alumina-base catalysts and has been cooperatively 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: D 4481 – 97
Standard Test Method for
Total Nickel in Fresh Alumina-Base Catalysts
This standard is issued under the fixed designation D 4481; 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 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,
2.1 ASTM Standards: present in the 2 to 10 % range, tends to be co-precipitated with
D 1193 Specification for Reagent Water the nickel dimethylglyoxime. The only other metal ions pre-
E 105 Practice for Probability Sampling of Materials cipitated by dimethylglyoxime are palladium, gold, and bis-
E 177 Practice for Use of the Terms Precision and Bias in muth.
ASTM Test Methods
3 6. Apparatus
E 456 Terminology Relating to Quality and Statistics
E 691 Practice for Conducting an Interlaboratory Study to 6.1 Beakers, 600-mL, 150-mL.
6.2 Hotplate.
Determine 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.
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 Fiber-Glass 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.
This test method is under the jurisdiction of Committee D-32 on Catalysts and
6.14 Ashless Filter Pulp.
is the direct responsibility of Subcommittee D32.03 on Chemical Analysis.
6.15 Desiccator.
Current edition approved March 10, 1997. Published October 1997. Originally
published as D 4481 – 85. Last previous edition D 4481 – 92.
Annual Book of ASTM Standards, Vol 11.01
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 4481
7. Reagents 9.2 Weigh three 1-g test specimens into platinum dishes or
procelain crucibles. Record mass to the nearest 0.1 mg as G .
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 on Analytical Reagents of the American Chemical Society, 2
9.3 To test specimens from 9.1, add 20-mL of concentrated
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of hydrochloric acid and heat gently on a hotplate until only a
paste of solids is left. Do not boil the solution. Do not bake
sufficiently high purity to permit its use without lessening the
accuracy of the determination. solids or subsequent re-solution will be difficult.
7.2 Purity of Water—Unless otherwise indicated, references
9.4 Add 20 mL of concentrated hydrochloric acid and warm
to water shall be understood to mean type IV reagent water as
on a hotplate 15 to 30 min to dissolve salts. Cool and dilute to
defined in Specification D 1193.
about 100 mL with deionized water.
7.3 Ammonium citrate, dibasic crystal, (NH ) HC H O .
4 2 6 5 7
9.5 Filter solids on 0.45-μm filter, using a 500-mL filter
7.4 Ammonium Hydroxide, 10 and 25 % solutions.
flask as a receiver. Wash the beaker with four approximately
7.5 Hydrochloric acid, concentrated 38 %.
20-mL portions of deionized water, transferring the washes to
7.6 Hydrofluoric acid concentrated 48 %.
the filter. Wash the solids on the filter with three more 20-mL
7.7 Methyl Red Indicator—-(o-Carboxy benzene azodim-
portions of deionized water. Quantitatively transfer the filtrate
ethylaniline). Dissolve 0.02 g in 60-mL reagent grade ethanol.
plus washes to a 600-mL beaker. Keep the beaker covered until
Add 40.0 mL of distilled water.
ready to precipitate nickel.
7.8 4A Molecular Sieve, activated for2hat 275°C.
9.6 Put a filter disk into a platinum dish and cover with
7.9 Potassium Hydrogen Sulfate, fused power-acid-flux
ashless filter pulp. Carefully char over a gas burner, then ignite
grade.
at red heat until the carbon is essentially burned off. Put the
7.10 Sodium Dimethylglyoxime, 8-Hydrate, crystal,
dish in a muffle furnace at 960°C for 50 min.
CH C:NONaC:NONaCH ·8H O. Prepare a 1 weight % per
3 3 2
9.7 To solids in the platinum dish, add 10 mL of 48 %
volume solution in water.
hydrofluoric acid and 5 mL of 10 % sulfuric acid and evaporate
7.11 Sulfuric Acid, 10 and 50 % solutions.
carefully to dryness on a hotplate. Then, carefully bring to a red
NOTE 1—The sodium salt of dimethylglyoxime is recommended, rather
heat over a gas burner until the sulfur trioxide fumes cease.
than the organic reagent, dimethylglyoxime because the salt is water
Cool and add5gof reagent potassium pyrosulfate and fuse
soluble. Large excesses added to precipitate the nickel do no harm as the
over a gas burner until a clear melt is o
...
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