ASTM D5153-22

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: D5153 − 10 (Reapproved 2016) D5153 − 22
Standard Test Method for
Palladium in Molecular Sieve Catalyst by Atomic Absorption
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Spectrophotometry
This standard is issued under the fixed designation D5153; 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 palladium in molecular sieve-containing fresh catalysts with about 0.5 weight
% of palladium.
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
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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
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
D7442E1272 Practice for Sample Preparation of Fluid Catalytic Cracking Catalysts and Zeolites for Elemental Analysis by
Inductively Coupled Plasma Optical Emission SpectroscopySpecification for Laboratory Glass Graduated Cylinders
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2.2 U.S. Federal Specification:
Federal Spec. NNN-P-395C Tolerance for Class A Pipets
3. Summary of Test Method
3.1 Warning—This test method requires the use of an extremely hazardous substance, hydrofluoric acid. Please refer to Appendix
X1 and Appendix X2 for additional safety requirements.
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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 Jan. 1, 2016Aug. 1, 2022. Published January 2016August 2022. Originally approved in 1991. Last previous edition approved in 20102016 as
D5153D5153 – 10–10.(2016). DOI: 10.1520/D5153-10R16.10.1520/D5153-22.
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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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D5153 − 22
3.2 The test sample is treated with a mixture of sulfuric and hydrofluoric acids. Upon dissolution, the excess hydrofluoric acid is
expelled. Aqua regia and lanthanum chloride are added and the solution is diluted to a specific volume. Palladium concentration
is determined by atomic absorption spectrophotometry. Absorbance of the samples is bracketed using a set of narrow range, matrix
matched standards. A second sample, taken at the same time as the analysis sample, is used to determine loss on ignition.
4. Significance and Use
4.1 This test method provides a means of determining the palladium content in fresh catalysts containing molecular sieves.
4.2 This test method is not intended to cover samples containing precious metals other than palladium.
5. Apparatus
5.1 Analytical Balance, capable of weighing to nearest 0.1 mg.
5.2 Atomic Absorption Spectrophotometer.
5.3 Beakers, TFE-fluorocarbon, 100-mL.100 mL.
5.4 Crucibles, porcelain, 10-mL.10 mL.
5.5 Crucible Cover, porcelain, for 10-mL10 mL crucible.
5.6 Desiccator.
5.7 Flasks, Erlenmeyer, 2000-mL.2000 mL.
5.8 Graduated Cylinders, glass, 5-mL, 10-mL, 25-mL, 50-mL, 250-mL, 500-mL, 1000-mL. 5 m
...