ASTM D7442-16

Standard Practice for Sample Preparation of Fluid Catalytic Cracking Catalysts 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 and exchanged zeolite materials.  
1.2 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 29-Feb-2016
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.03 - Chemical Composition

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D7442 − 16
Standard Practice for
Sample Preparation of Fluid Catalytic Cracking Catalysts
and Zeolites for Elemental Analysis by Inductively Coupled
1
Plasma Optical Emission 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* 3.1.3 ICP-OES—Inductively-Coupled Plasma-Optical
Emission Spectroscopy
1.1 This practice covers uniform dissolution techniques for
preparing samples of fluid catalytic cracking catalysts (FCC)
4. Summary of Practice
and exchanged zeolitic materials for analysis by Inductively
4.1 Three preparation techniques are presented for convert-
Coupled Plasma Optical Emission Spectroscopy (ICP-OES).
ing solid, power samples into clear, dilute acid solutions
These techniques describe standardized approaches to well-
suitable for analysis by ICP-OES. The three techniques pre-
known, widely used laboratory practices of sample preparation
sented are PerchloricAcid Digestion, SulfuricAcid Digestion,
utilizingaciddigestionsandboratesaltfusions.Thispracticeis
and Lithium-Borate Fused Dissolution. Other techniques may
applicable to fresh and equilibrium FCC catalysts and ex-
be possible; however, these three approaches are established,
changed zeolite materials.
widely used laboratory techniques for preparing FCC catalyst
1.2 The values stated in SI units are to be regarded as
and catalyst-like samples.
standard. No other units of measurement are included in this
4.2 Powder samples are heat-treated for 1 to3hto remove
standard.
volatilecomponentspriortofurtherpreparationbyanyofthese
1.3 This standard does not purport to address all of the
three techniques.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4.3 The Perchloric Acid and Sulfuric Acid techniques in-
volve dissolving small aliquots of heat-treated sample in the
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. respective acid liquors and diluting the resulting solutions to
the appropriate analytical volume. These techniques require
2. Referenced Documents boiling acid solutions in platinum or polytetrafluoroethylene
2 (PTFE) labware and shall be used in appropriate fume hoods.
2.1 ASTM Standards:
ThePerchloricAcidDigestionshall neverbeusedinastandard
D7260 Practice for Optimization, Calibration, and Valida-
fume hood.
tion of Inductively Coupled Plasma-Atomic Emission
Spectrometry (ICP-AES) for ElementalAnalysis of Petro- 4.4 The Lithium Borate Fused Dissolution technique in-
volves dissolving small aliquots of heat-treated sample in a
leum Products and Lubricants
molten flux of lithium metaborate and lithium tetraborate salts,
dissolving the resulting flux solution in a dilute nitric acid
3. Terminology
solution, and diluting the clear, concentrated specimen solution
3.1 Acronyms:
to an appropriate analytical volume. This technique must be
3.1.1 FCC—Fluid Catalytic Cracking
performed in an operational fume hood and can be performed
3.1.2 FCCU—Fluid Catalytic Cracking Unit
manually or may utilize the advantages of an automated fluxer.
The optimal ratio of flux to sample, as well as fusion
temperature needed, will vary depending on sample matrix.
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.
5. Significance and Use
Current edition approved March 1, 2016. Published April 2016. Originally
5.1 The chemical composition of catalyst and catalyst ma-
approved in 2008. Last previous edition approved in 2008 as D7442–08a. DOI:
10.1520/D7442-16.
terials is an important indicator of catalyst performance and is
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
a valuable tool for assessing parameters in a FCCU process.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
This practice will be useful to catalyst manufacturers and
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. petroleum refiners for quality verification and performance
*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 − 16
evaluation, and to environmental authorities at the state and threetechniques.Ifsamplecontainsorganicmaterials,pretreat-
federal levels for evaluation
...

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 − 08a D7442 − 16
Standard Practice for
Sample Preparation of Fluid Catalytic Cracking Catalysts
and Zeolites for Elemental Analysis by Inductively Coupled
1
Plasma AtomicOptical Emission 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 AtomicOptical Emission Spectroscopy (ICP-AES).(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 and exchanged
zeolite materials.
1.2 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D7260 Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry
(ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
3. Terminology
3.1 Acronyms:
3.1.1 FCC—Fluid Catalytic Cracking
3.1.2 FCCU—Fluid Catalytic Cracking Unit
3.1.3 ICP-AES—ICP-OES—Inductively-Coupled Plasma-AtomicPlasma-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-AES.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.
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.
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 Sept. 1, 2008March 1, 2016. Published September 2008April 2016. Originally approved in 2008. Last previous edition approved in 2008 as
D7442–08.–08a. DOI: 10.1520/D7442-08A.10.1520/D7442-16.
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 − 16
4.4 The Lithium Borate Fused Dissolution technique involves dissolving small aliquots of heat-treated sample in a molten flux
of lithium metaborate and lithium tetraborate salts, dissolving the resulting flux solution in a dilute nitric acid solution, and diluting
the clear, concentrated specimen solution to an appropriate analytical volume. This technique must be performed in an operational
fume hood and can be performed manually or may utilize the advantages of an automated fluxer. The optimal ratio of flux to
sample, as well as fusion temperature needed, will vary depending on sample matrix.
5. Significance and Use
5.1 The chemical composition of catalyst and
...