ASTM D7442-22

Standard Practice for Sample Preparation of Fluid Catalytic Cracking Catalysts, Catalytic Materials, and Zeolites for Elemental Analysis by Inductively Coupled Plasma Optical Emission Spectroscopy

SIGNIFICANCE AND USE
5.1 The chemical composition of catalyst and catalyst materials is an important indicator of catalyst performance and is a valuable tool for assessing parameters in a FCCU process. This practice will be useful to catalyst manufacturers and petroleum refiners for quality verification and performance evaluation, and to environmental authorities at the state and federal levels for evaluation and verification of various compliance programs.3, 4, 5  
5.2 Catalysts and catalyst type materials are difficult to prepare for analysis by ICP, and although the techniques presented in this practice are common, there is wide variation among laboratories in sample pretreatment and digestion recipes. This practice is intended to standardize these variables in order to facilitate the utility of comparative data among manufacturers, refiners, and regulatory agencies.
SCOPE
1.1 This practice covers uniform dissolution techniques for preparing samples of fluid catalytic cracking catalysts (FCC) and exchanged zeolitic materials for analysis by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). These techniques describe standardized approaches to well-known, widely used laboratory practices of sample preparation utilizing acid digestions and borate salt fusions. This practice is applicable to fresh and equilibrium FCC catalysts, catalytic materials used to manufacture catalyst, and exchanged zeolite materials.  
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: 71.040.50 - Physicochemical methods of analysis
• 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: D7442 − 22
Standard Practice for
Sample Preparation of Fluid Catalytic Cracking Catalysts,
Catalytic Materials, and Zeolites for Elemental Analysis by
Inductively Coupled Plasma Optical Emission
1
Spectroscopy
This standard is issued under the fixed designation D7442; 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* tion of Inductively Coupled Plasma-Atomic Emission
Spectrometry (ICP-AES) for ElementalAnalysis of Petro-
1.1 This practice covers uniform dissolution techniques for
leum Products and Lubricants
preparing samples of fluid catalytic cracking catalysts (FCC)
E1272 Specification for Laboratory Glass Graduated Cylin-
and exchanged zeolitic materials for analysis by Inductively
ders
Coupled Plasma Optical Emission Spectroscopy (ICP-OES).
These techniques describe standardized approaches to well-
3. Terminology
known, widely used laboratory practices of sample preparation
utilizingaciddigestionsandboratesaltfusions.Thispracticeis 3.1 Acronyms: As per Terminology D3766.
3.1.1 FCC—Fluid Catalytic Cracking
applicable to fresh and equilibrium FCC catalysts, catalytic
materials used to manufacture catalyst, and exchanged zeolite
3.1.2 FCCU—Fluid Catalytic Cracking Unit
materials.
3.1.3 ICP-OES—Inductively-Coupled Plasma-Optical
1.2 Units—The values stated in SI units are to be regarded
Emission Spectroscopy
as standard. No other units of measurement are included in this
standard.
4. Summary of Practice
1.3 This standard does not purport to address all of the
4.1 Three preparation techniques are presented for convert-
safety concerns, if any, associated with its use. It is the
ing solid, power samples into clear, dilute acid solutions
responsibility of the user of this standard to establish appro-
suitable for analysis by ICP-OES. The three techniques pre-
priate safety, health, and environmental practices and deter-
sented are PerchloricAcid Digestion, SulfuricAcid Digestion,
mine the applicability of regulatory limitations prior to use.
and Lithium-Borate Fused Dissolution. Other techniques may
1.4 This international standard was developed in accor-
be possible; however, these three approaches are established,
dance with internationally recognized principles on standard-
widely used laboratory techniques for preparing FCC catalyst
ization established in the Decision on Principles for the
and catalytic materials.
Development of International Standards, Guides and Recom-
4.2 Powder samples are heat-treated for 1 to3hto remove
mendations issued by the World Trade Organization Technical
volatilecomponentspriortofurtherpreparationbyanyofthese
Barriers to Trade (TBT) Committee.
three techniques.
2. Referenced Documents 4.3 The Perchloric Acid and Sulfuric Acid techniques in-
2
volve dissolving small aliquots of heat-treated sample in the
2.1 ASTM Standards:
respective acid liquors and diluting the resulting solutions to
D3766 Terminology Relating to Catalysts and Catalysis
the appropriate analytical volume. These techniques require
D7260 Practice for Optimization, Calibration, and Valida-
boiling acid solutions in platinum or polytetrafluoroethylene
(PTFE) labware and shall be used in appropriate fume hoods.
1
ThePerchloricAcidDigestionshall neverbeusedinastandard
This practice is under the jurisdiction of ASTM Committee D32 on Catalysts
and is the direct responsibility of Subcommittee D32.03 on Chemical Composition.
fume hood.
Current edition approved Aug. 1, 2022. Published August 2022. Originally
4.4 The Lithium Borate Fused Dissolution technique in-
approved in 2008. Last previous edition approved in 2016 as D7442 – 16. DOI:
10.1520/D7442-22.
volves dissolving small aliquots of heat-treated sample in a
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
molten flux of lithium metaborate and lithium tetraborate salts,
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
dissolving the resulting flux solution in a dilute nitric acid
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. solution, and diluting the clear, concentrated specimen solution
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D7442 − 22
to an appropriate analytical volume. This techn
...

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: D7442 − 16 D7442 − 22
Standard Practice for
Sample Preparation of Fluid Catalytic Cracking Catalysts
Catalysts, Catalytic Materials, and Zeolites for Elemental
Analysis by Inductively Coupled Plasma Optical Emission
1
Spectroscopy
This standard is issued under the fixed designation D7442; 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 practice covers uniform dissolution techniques for preparing samples of fluid catalytic cracking catalysts (FCC) and
exchanged zeolitic materials for analysis by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). These
techniques describe standardized approaches to well-known, widely used laboratory practices of sample preparation utilizing acid
digestions and borate salt fusions. This practice is applicable to fresh and equilibrium FCC catalysts catalysts, catalytic materials
used to manufacture catalyst, and exchanged zeolite materials.
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:
D3766 Terminology Relating to Catalysts and Catalysis
D7260 Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry
(ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
E1272 Specification for Laboratory Glass Graduated Cylinders
3. Terminology
3.1 Acronyms: As per Terminology D3766.
3.1.1 FCC—Fluid Catalytic Cracking
1
This practice 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 2008. Last previous edition approved in 20082016 as
D7442D7442 – 16.–08a. DOI: 10.1520/D7442-16.10.1520/D7442-22.
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.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7442 − 22
3.1.2 FCCU—Fluid Catalytic Cracking Unit
3.1.3 ICP-OES—Inductively-Coupled Plasma-Optical Emission Spectroscopy
4. Summary of Practice
4.1 Three preparation techniques are presented for converting solid, power samples into clear, dilute acid solutions suitable for
analysis by ICP-OES. The three techniques presented are Perchloric Acid Digestion, Sulfuric Acid Digestion, and Lithium-Borate
Fused Dissolution. Other techniques may be possible; however, these three approaches are established, widely used laboratory
techniques for preparing FCC catalyst and catalyst-like samples.catalytic materials.
4.2 Powder samples are heat-treated for 1 to 3 h to remove volatile components prior to further preparation by any of these three
techniques.
4.3 The Perchloric Acid and Sulfuric Acid techniques involve dissolving small aliquots of heat-treated sample in the respective
acid liquors and diluting the resulting solutions to the appropriate analytical volume. These techniques require boiling acid
solutions in platinum or polytetrafluoroethylene (PTFE) labware and shall be used in appropriate fume hoods. The Perchloric Acid
Digestion shall never be used in a standard fume hood.
4.4 The Lithium Borate Fused Dissolution technique involves dissolving small aliquots of heat-treated
...