ASTM D5153-22

Standard Test Method for Palladium in Molecular Sieve Catalyst by Atomic Absorption Spectrophotometry

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.
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, 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: 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: D5153 − 22
Standard Test Method for
Palladium in Molecular Sieve Catalyst by Atomic Absorption
1
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.
3
1. Scope 2.2 U.S. Federal Specification:
Federal Spec. NNN-P-395C Tolerance for Class A Pipets
1.1 This test method covers the determination of palladium
in molecular sieve-containing fresh catalysts with about 0.5
3. Summary of Test Method
weight % of palladium.
3.1 Warning—This test method requires the use of an
1.2 Units—The values stated in SI units are to be regarded
extremely hazardous substance, hydrofluoric acid. Please refer
as standard. No other units of measurement are included in this
to Appendix X1 and Appendix X2 for additional safety
standard.
requirements.
1.3 This standard does not purport to address all of the
3.2 The test sample is treated with a mixture of sulfuric and
safety concerns, if any, associated with its use. It is the
hydrofluoric acids. Upon dissolution, the excess hydrofluoric
responsibility of the user of this standard to establish appro-
acid is expelled.Aqua regia and lanthanum chloride are added
priate safety, health, and environmental practices and deter-
and the solution is diluted to a specific volume. Palladium
mine the applicability of regulatory limitations prior to use.
concentration is determined by atomic absorption spectropho-
1.4 This international standard was developed in accor-
tometry.Absorbance of the samples is bracketed using a set of
dance with internationally recognized principles on standard-
narrow range, matrix matched standards. A second sample,
ization established in the Decision on Principles for the
taken at the same time as the analysis sample, is used to
Development of International Standards, Guides and Recom-
determine loss on ignition.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
4. Significance and Use
2. Referenced Documents
4.1 This test method provides a means of determining the
2
palladium content in fresh catalysts containing molecular
2.1 ASTM Standards:
sieves.
D1193 Specification for Reagent Water
D7442 Practice for Sample Preparation of Fluid Catalytic
4.2 This test method is not intended to cover samples
CrackingCatalystsandZeolitesforElementalAnalysisby
containing precious metals other than palladium.
Inductively Coupled Plasma Optical Emission Spectros-
5. Apparatus
copy
E177 Practice for Use of the Terms Precision and Bias in
5.1 Analytical Balance, capable of weighing to nearest
ASTM Test Methods
0.1 mg.
E456 Terminology Relating to Quality and Statistics
5.2 Atomic Absorption Spectrophotometer.
E691 Practice for Conducting an Interlaboratory Study to
5.3 Beakers, TFE-fluorocarbon, 100 mL.
Determine the Precision of a Test Method
E1272 Specification for Laboratory Glass Graduated Cylin-
5.4 Crucibles, porcelain, 10 mL.
ders
5.5 Crucible Cover, porcelain, for 10 mL crucible.
1
This test method is under the jurisdiction of ASTM Committee D32 on 5.6 Desiccator.
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
5.7 Flasks, Erlenmeyer, 2000 mL.
Composition.
Current edition approved Aug. 1, 2022. Published August 2022. Originally
5.8 Graduated Cylinders, glass, 5 mL, 10 mL, 25 mL,
approved in 1991. Last previous edition approved in 2016 as D5153 – 10(2016).
50 mL, 250 mL, 500 mL, 1000 mL (see Specification E1272).
DOI: 10.1520/D5153-22.
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 Standardization Documents Order Desk, DODSSP, Bldg. 4,
the ASTM website. Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D5153 − 22
5.9 Graduated Cylinder, plastic, 10 mL. trated hydrochloric acid (12 M) and 25 mL of distilled water.
Transferthesolutiontoa500mLvolumetricflaskanddiluteto
5.10 Hot Plate.
volume when cool.
5.11 Muffle Furnace, electrically heated, capable of
NOTE 2—A commercially available atomic absorption palladium refer-
1000 °C.
ence solution may be used if it is known to be reliable.
5.12 Pipets,
...

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
1
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
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
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
3
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.
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 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.
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 Standardization Documents Order Desk, DODSSP, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
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
...