ASTM D4481-21

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

SIGNIFICANCE AND USE
4.1 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 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-May-2021
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.03 - Chemical Composition

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4481 − 21
Standard Test Method for
1
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 3. Summary of Test Method
1.1 This test method covers the determination of nickel in 3.1 The test specimen (as received) is treated with concen-
fresh alumina-base catalysts and has been tested at nickel trated hydrochloric acid to solubilize the nickel. If necessary,
concentrations from 2.5 to 60 weight %, expressed as nickel
nickel is recovered from any insoluble residue by potassium
oxide (NiO). pyrosulfate fusion, after hydrofluoric-sulfuric acid treatment to
remove silica. Ammonium citrate is added to complex the
1.2 Units—The values stated in SI units are to be regarded
aluminum and buffer the solution. Nickel is precipitated as
as standard. No other units of measurement are included in this
nickel dimethylglyoxime, Ni (C H O N ) , at a weakly alka-
4 7 2 2 2
standard.
line pH. The precipitate is washed and weighed as Ni
1.3 This standard does not purport to address all of the
(C H O N ) after drying at 120 °C.
4 7 2 2 2
safety concerns, if any, associated with its use. It is the
3.2 A separate test specimen is taken to determine loss on
responsibility of the user of this standard to establish appro-
ignition (LOI) at 550 °C. The value is used to calculate the
priate safety, health, and environmental practices and deter-
nickel as percent nickel oxide (NiO) on a 550 °C dry basis.
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
4. Significance and Use
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4.1 This test method sets forth a procedure by which
Development of International Standards, Guides and Recom-
catalyst samples can be compared either on an interlaboratory
mendations issued by the World Trade Organization Technical
or intralaboratory basis. It is anticipated that catalyst producers
Barriers to Trade (TBT) Committee.
and users will find this method of value.
2. Referenced Documents
5. Interferences
2
2.1 ASTM Standards:
5.1 Cobalt, molybdenum, and aluminum do not interfere.
D1193 Specification for Reagent Water
Interferences by elements that precipitate as hydroxides, such
D7442 Practice for Sample Preparation of Fluid Catalytic
as iron, chromium, aluminum, lead, tin, manganese, titanium,
CrackingCatalystsandZeolitesforElementalAnalysisby
and zirconium, are avoided by the addition of ammonium
Inductively Coupled Plasma Optical Emission Spectros-
citrate before making the solutions ammoniacal. Copper, pres-
copy
ent in the 2 to 10 % range, tends to be co-precipitated with the
E105 Guide for Probability Sampling of Materials
nickel dimethylglyoxime. The only other metal ions precipi-
E177 Practice for Use of the Terms Precision and Bias in
tated by dimethylglyoxime are palladium, gold, and bismuth.
ASTM Test Methods
E456 Terminology Relating to Quality and Statistics
6. Apparatus
E691 Practice for Conducting an Interlaboratory Study to
6.1 Beakers, 600-mL, 150-mL.
Determine the Precision of a Test Method
6.2 Hotplate.
6.3 Furnace, electric muffle. Calibrated and capable of
1
This test method is under the jurisdiction of ASTM Committee D32 on
maintaining temperatures of 550 6 25 °C, and 950 6 25 °C.
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
Composition. 3
6.4 Platinum Dishes, 100-mL capacity.
Current edition approved June 1, 2021. Published June 2021. Originally
approved in 1985. Last previous edition approved in 2015 as D4481 – 10(2015).
6.5 Mortar and Pestle, agate, or equivalent mechanical
DOI: 10.1520/D4481-21.
grinder.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
6.6 Crucibles, sintered-glass, 30-mL, medium porosity frit.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 6.7 Fiberglass Filter, 3.2 cm.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D4481 − 21
part of the procedure. The organic reagent, dimethylglyoxime, is not very
6.8 Drying Oven capable of maintaining a t
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4481 − 10 (Reapproved 2015) D4481 − 21
Standard Test Method for
1
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
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 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this
standard.
1.3 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to its use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D7442 Practice for Sample Preparation of Fluid Catalytic Cracking Catalysts and Zeolites for Elemental Analysis by Inductively
Coupled Plasma Optical Emission Spectroscopy
E105 Guide for Probability Sampling of Materials
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Summary of Test Method
3.1 The test specimen (as received) is treated with concentrated hydrochloric acid to solubilize the nickel. If necessary, nickel is
recovered from any insoluble residue by potassium pyrosulfate fusion, after hydrofluoric-sulfuric acid treatment to remove silica.
Ammonium citrate is added to complex the aluminum and buffer the solution. Nickel is precipitated as nickel dimethylglyoxime,
Ni (C H O N ) , at a weakly alkaline pH. The precipitate is washed and weighed as Ni (C H O N ) after drying at 120°C.120 °C.
4 7 2 2 2 4 7 2 2 2
3.2 A separate test specimen is taken to determine loss on ignition (LOI) at 550°C.550 °C. The value is used to calculate the nickel
as percent nickel oxide (NiO) on a 550°C550 °C dry basis.
1
This test method is under the jurisdiction of ASTM Committee D32 on Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical Composition.
Current edition approved Dec. 1, 2015June 1, 2021. Published December 2015June 2021. Originally approved in 1985. Last previous edition approved in 20102015 as
D4481D4481 – 10–10.(2015). DOI: 10.1520/D4481-10R15.10.1520/D4481-21.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4481 − 21
4. Significance and Use
4.1 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.
5. Interferences
5.1 Cobalt, molybdenum, and aluminum do not interfere. Interferences by elements that precipitate as hydroxides, such as iron,
chromium, aluminum, lead, tin, manganese, titanium, and zirconium, are avoided by the addition of ammonium citrate before
making the solutions ammoniacal. Copper, present in the 2 to 10 % range, tends to be co-precipitated with the nickel
dimethylglyoxime. The only other metal ions precipitated by dimethylglyoxime are palladium, gold, and bismuth.
6. Apparatus
6.1 Beakers, 600-mL, 150-mL.
6.2 Hotplate.
6.3 Furnace, electric muffle. Calibrated and capable of maintaining temperatures of 550 6 25°C,25 °C, and 950 6 25°C.25 °C.
3
6.4 Platinum Dishes, 100-mL capacity.
6.5 Mortar and Pestle, agate, o
...