ASTM D1977-22

Standard Test Method for Nickel and Vanadium in FCC Equilibrium Catalysts by Hydrofluoric/Sulfuric Acid Decomposition and Atomic Spectroscopic Analysis

SIGNIFICANCE AND USE
5.1 This test method is a procedure by which catalyst samples may be compared on an inter- or intra-laboratory basis. Catalyst producers and user should find this test method to be of value.
SCOPE
1.1 This test method covers the determination of nickel and vanadium in equilibrium catalysts where the vanadium and nickel concentrations are greater than 50 and 25 mg/kg, respectively.  
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-Jul-2022
• ICS: 77.120.40 - Nickel, chromium and their alloys
• 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:D1977 −22
Standard Test Method for
Nickel and Vanadium in FCC Equilibrium Catalysts by
Hydrofluoric/Sulfuric Acid Decomposition and Atomic
1
Spectroscopic Analysis
This standard is issued under the fixed designation D1977; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope E177Practice for Use of the Terms Precision and Bias in
ASTM Test Methods
1.1 This test method covers the determination of nickel and
E288Specification for Laboratory Glass Volumetric Flasks
vanadium in equilibrium catalysts where the vanadium and
E456Terminology Relating to Quality and Statistics
nickel concentrations are greater than 50 and 25mg⁄kg,
E691Practice for Conducting an Interlaboratory Study to
respectively.
Determine the Precision of a Test Method
1.2 Units—The values stated in SI units are to be regarded
3
2.2 U.S. Federal Specification:
asstandard.Nootherunitsofmeasurementareincludedinthis
Federal Specification NNN-P-395CTolerance for Class A
standard.
Pipets
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
3.1 Definitions—See Terminology D3766.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
4. Summary of Test Method
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
4.1 The test specimen (as received) is decomposed with
ization established in the Decision on Principles for the
hydrofluoricandsulfuricacids.Aftercompletevolatilizationof
Development of International Standards, Guides and Recom-
thehydrofluoricacidandcooling,thesulfatesaltsaredilutedto
mendations issued by the World Trade Organization Technical
the appropriate concentration range for analysis by flame
Barriers to Trade (TBT) Committee.
atomic absorption, direct current plasma emission, or induc-
tivelycoupledplasmaemissionspectroscopies.Theinstrument
2. Referenced Documents
is calibrated with matrix-matched standards. Solutions of the
2
2.1 ASTM Standards:
test specimen are analyzed.
D1193Specification for Reagent Water
D3766Terminology Relating to Catalysts and Catalysis
5. Significance and Use
D4481Test Method forTotal Nickel in FreshAlumina-Base
5.1 This test method is a procedure by which catalyst
Catalysts
samples may be compared on an inter- or intra-laboratory
D7442Practice for Sample Preparation of Fluid Catalytic
basis. Catalyst producers and user should find this test method
CrackingCatalystsandZeolitesforElementalAnalysisby
to be of value.
Inductively Coupled Plasma Optical Emission Spectros-
copy
6. Interferences
E105Guide for Probability Sampling of Materials
6.1 The enhancement of alumina in the samples are over-
1
come by using matrix-matched standards. Any dilutions
This test method is under the jurisdiction of ASTM Committee D32 on
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
needed to achieve the working ranges for vanadium and nickel
Composition.
must contain the sameAl O (7800 ppm) concentration as the
2 3
Current edition approved Aug. 1, 2022. Published August 2022. Originally
standards.
approved in 1991. Last previous edition approved in 2016 as D1977–16. DOI:
10.1520/D1977-22.
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
3
Standards volume information, refer to the standard’s Document Summary page on Available from DLA Document Services, Building 4/D, 700 Robbins Ave.,
the ASTM website. Philadelphia, PA 19111-5094, http://quicksearch.dla.mil.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D1977−22
6.2 If using optical emission, consult tables showing inter- 8.3.8 Reference Standard Solution—1000 mg/L vanadium
fering line near analyte lines; if significant overlap occurs, one (see Note 1).
must apply interelement correction or choose an alternate 8.3.9 Aluminum Chloride, reagent grade, AlCl ·6H O
3 2
emission line. 8.3.10 Aluminum Stock Solution—39000 mg/LAl O , dis-
2 3
solve 184.5 g of AlCl ·6H O in water and dilute to 1 L and
3 2
7. Apparatus store in a polyethylene bottle.
8.3.11 Hydrogen Peroxide—3% solution.
7.1 Analyti
...

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: D1977 − 16 D1977 − 22
Standard Test Method for
Nickel and Vanadium in FCC Equilibrium Catalysts by
Hydrofluoric/Sulfuric Acid Decomposition and Atomic
1
Spectroscopic Analysis
This standard is issued under the fixed designation D1977; 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 and vanadium in equilibrium catalysts where the vanadium and nickel
concentrations are greater than 50 and 2525 mg mg/kg, ⁄kg, respectively.
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 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
D3766 Terminology Relating to Catalysts and Catalysis
D4481 Test Method for Total Nickel in Fresh Alumina-Base Catalysts
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
E288 Specification for Laboratory Glass Volumetric Flasks
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3
2.2 U.S. Federal Specification:
Federal Specification NNN-P-395C Tolerance for Class A Pipets
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 March 1, 2016Aug. 1, 2022. Published April 2016August 2022. Originally approved in 1991. Last previous edition approved in 20082016 as
D1977D1977 – 16.–03 (2008). DOI: 10.1520/D1977-16.10.1520/D1977-22.
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.
3
Available from DLA Document Services, Building 4/D, 700 Robbins Ave., Philadelphia, PA 19111-5094, http://quicksearch.dla.mil.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D1977 − 22
3. Terminology
3.1 Definitions—See Terminology D3766.
4. Summary of Test Method
4.1 The test specimen (as received) is decomposed with hydrofluoric and sulfuric acids. After complete volatilization of the
hydrofluoric acid and cooling, the sulfate salts are diluted to the appropriate concentration range for analysis by flame atomic
absorption, direct current plasma emission, or inductively coupled plasma emission spectroscopies. The instrument is calibrated
with matrix-matched standards. Solutions of the test specimen are analyzed.
5. Significance and Use
5.1 This test method is a procedure by which catalyst samples may be compared on an inter- or intra-laboratory basis. Catalyst
producers and user should find this test method to be of value.
6. Interferences
6.1 The enhancement of alumina in the samples are overcome by using matrix-matched standards. Any dilutions needed to achieve
the working ranges for vanadium and nickel must contain the same Al O (7800 ppm) concentration as the standards.
2 3
6.2 If using optical emission, consult tables showing interfering line near analyte lines; if significant overlap occurs, one must
apply interelement correction or choose an alternate emission line.
7. Apparatus
7.1 Analytical Balance, capable of weighing to nearest 0.1 mg.
...