ASTM D7442-08a
(Practice)Standard Practice for Sample Preparation of Fluid Catalytic Cracking Catalysts and Zeolites for Elemental Analysis by Inductively Coupled Plasma Atomic Emission Spectroscopy
Standard Practice for Sample Preparation of Fluid Catalytic Cracking Catalysts and Zeolites for Elemental Analysis by Inductively Coupled Plasma Atomic Emission Spectroscopy
SIGNIFICANCE AND USE
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.
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 Atomic Emission Spectroscopy (ICP-AES). 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.
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Designation: D7442 − 08a
StandardPractice for
Sample Preparation of Fluid Catalytic Cracking Catalysts
and Zeolites for Elemental Analysis by Inductively Coupled
1
Plasma Atomic 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* widely used laboratory techniques for preparing FCC catalyst
and catalyst-like samples.
1.1 This practice covers uniform dissolution techniques for
preparing samples of fluid catalytic cracking catalysts (FCC) 3.2 Powder samples are heat-treated for 1 to3hto remove
and exchanged zeolitic materials for analysis by Inductively volatilecomponentspriortofurtherpreparationbyanyofthese
Coupled Plasma Atomic Emission Spectroscopy (ICP-AES). three techniques.
These techniques describe standardized approaches to well-
3.3 The Perchloric Acid and Sulfuric Acid techniques in-
known, widely used laboratory practices of sample preparation
volve dissolving small aliquots of heat-treated sample in the
utilizingaciddigestionsandboratesaltfusions.Thispracticeis
respective acid liquors and diluting the resulting solutions to
applicable to fresh and equilibrium FCC catalysts and ex-
the appropriate analytical volume. These techniques require
changed zeolite materials.
boiling acid solutions in platinum or polytetrafluoroethylene
1.2 The values stated in SI units are to be regarded as (PTFE) labware and shall be used in appropriate fume hoods.
standard. No other units of measurement are included in this ThePerchloricAcidDigestionshall neverbeusedinastandard
standard. fume hood.
1.3 This standard does not purport to address all of the
3.4 The Lithium Borate Fused Dissolution technique in-
safety concerns, if any, associated with its use. It is the
volves dissolving small aliquots of heat-treated sample in a
responsibility of the user of this standard to establish appro-
molten flux of lithium metaborate and lithium tetraborate salts,
priate safety and health practices and determine the applica-
dissolving the resulting flux solution in a dilute nitric acid
bility of regulatory limitations prior to use.
solution, and diluting the clear, concentrated specimen solution
to an appropriate analytical volume. This technique must be
2. Terminology
performed in an operational fume hood and can be performed
manually or may utilize the advantages of an automated fluxer.
2.1 Acronyms:
The optimal ratio of flux to sample, as well as fusion
2.1.1 FCC—Fluid Catalytic Cracking
temperature needed, will vary depending on sample matrix.
2.1.2 FCCU—Fluid Catalytic Cracking Unit
4. Significance and Use
2.1.3 ICP-AES—Inductively-Coupled Plasma-Atomic
Emission Spectroscopy
4.1 The chemical composition of catalyst and catalyst ma-
terials is an important indicator of catalyst performance and is
3. Summary of Practice
a valuable tool for assessing parameters in a FCCU process.
This practice will be useful to catalyst manufacturers and
3.1 Three preparation techniques are presented for convert-
petroleum refiners for quality verification and performance
ing solid, power samples into clear, dilute acid solutions
evaluation, and to environmental authorities at the state and
suitable for analysis by ICP-AES. The three techniques pre-
federal levels for evaluation and verification of various com-
sented are Perchloric Acid Digestion, Sulfuric Acid Digestion,
2, 3, 4
pliance programs.
and Lithium-Borate Fused Dissolution. Other techniques may
be possible; however, these three approaches are established,
4.2 Catalysts and catalyst type materials are difficult to
prepare for analysis by ICP, and although the techniques
1 2
This practice is under the jurisdiction of ASTM Committee D32 on Catalysts Dean, John R., Practical Inductively Coupled Plasma Spectroscopy, John
and is the direct responsibility of Subcommittee D32.03 on Chemical Composition. Wiley, New York, 2005.
3
Current edition approved Sept. 1, 2008. Published September 2008. Originally Gaines, Paul, “ICP Operations,” at www.ivstandards.com/tech/icp-ops .
4
approved in 2008. Last previous edition approved in 2008 as D7442–08. DOI: Segal, Eileen B., “First Aid for a Unique Acid: HF,” Chemical Health and
10.1520/D7442-08A. Safety, Vol 5, Sept/Oct 1998, p. 25.
*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
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D7442 − 08a
presented in this practice are common, there is wide variation 8. Hazards
among labora
...
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:D7442–08 Designation: D 7442 – 08a
Standard Practice for
Sample Preparation of Fluid Catalytic Cracking Catalysts
and Zeolites for Elemental Analysis by Inductively Coupled
1
Plasma Atomic Emission Spectroscopy
This standard is issued under the fixed designation D 7442; 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 Atomic Emission Spectroscopy (ICP-AES). 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
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. Terminology
2.1 Acronyms:
2.1.1 FCC—Fluid Catalytic Cracking
2.1.2 FCCU—Fluid Catalytic Cracking Unit
2.1.3 ICP-AES—Inductively-Coupled Plasma-Atomic Emission Spectroscopy
3. Summary of Practice
3.1 Three preparation techniques are presented for converting solid, power samples into clear, dilute acid solutions suitable for
analysis by ICP-AES. The three techniques presented are PerchloricAcid Digestion, SulfuricAcid 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.
3.2 Powdersamplesareheat-treatedfor1to3htoremovevolatilecomponentspriortofurtherpreparationbyanyofthesethree
techniques.
3.3 The PerchloricAcid and SulfuricAcid 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 PerchloricAcid
Digestion shall never be used in a standard fume hood.
3.4 The Lithium Borate Fused Dissolution technique involves dissolving small aliquots of heat-treated sample in a molten flux
oflithiummetaborateandlithiumtetraboratesalts,dissolvingtheresultingfluxsolutioninadilutenitricacidsolution,anddiluting
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.
4. Significance and Use
4.1 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
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 April 1, 2008. Published April 2008.
Current edition approved Sept. 1, 2008. Published September 2008. Originally approved in 2008. Last previous edition approved in 2008 as D 7442–08.
*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 ----------------------
D 7442 – 08a
, ,
2 3 4
evaluation and verification of various compliance programs.
4.2 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 w
...
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