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

Relations

• Refers: ASTM D3766-24a - Standard Terminology Relating to Catalysts and Catalysis
• Effective Date: 01-Feb-2024
• Refers: ASTM D3766-24 - Standard Terminology Relating to Catalysts and Catalysis
• Effective Date: 01-Jan-2024
• Refers: ASTM D7260-19 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-May-2019
• Refers: ASTM E1272-02(2019) - Standard Specification for Laboratory Glass Graduated Cylinders
• Effective Date: 01-Jan-2019
• Refers: ASTM D3766-08(2018) - Standard Terminology Relating to Catalysts and Catalysis
• Effective Date: 01-Nov-2018
• Refers: ASTM D3766-08(2013) - Standard Terminology Relating to Catalysts and Catalysis
• Effective Date: 01-Mar-2013
• Refers: ASTM E1272-02(2012) - Standard Specification for Laboratory Glass Graduated Cylinders
• Effective Date: 01-Nov-2012
• Refers: ASTM D3766-08 - Standard Terminology Relating to Catalysts and Catalysis
• Effective Date: 01-Apr-2008
• Refers: ASTM D3766-86(2007) - Standard Terminology Relating to Catalysts and Catalysis
• Effective Date: 15-Nov-2007
• Refers: ASTM E1272-02(2007) - Standard Specification for Laboratory Glass Graduated Cylinders
• Effective Date: 01-Nov-2007
• Refers: ASTM D7260-06 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-May-2006
• Refers: ASTM D3766-86(2002) - Standard Terminology Relating to Catalysts and Catalysis
• Effective Date: 10-Nov-2002
• Refers: ASTM E1272-02 - Standard Specification for Laboratory Glass Graduated Cylinders
• Effective Date: 10-Oct-2002
• Refers: ASTM E1272-95(1999) - Standard Specification for Laboratory Glass Graduated Cylinders
• Effective Date: 10-Dec-1999
• Refers: ASTM D3766-86(1997) - Standard Terminology Relating to Catalysts and Catalysis
• Effective Date: 28-Nov-1986

Overview

ASTM D7442-22 is the international standard practice for the sample preparation of fluid catalytic cracking (FCC) catalysts, catalytic materials, and zeolites for elemental analysis using Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). Developed by ASTM International, this practice specifies standardized dissolution techniques to ensure consistent, accurate, and comparable results across laboratories analyzing catalyst composition. It addresses the needs of catalyst manufacturers, petroleum refiners, and regulatory agencies by facilitating data comparability and supporting quality verification, performance evaluation, and compliance monitoring.

Key Topics

• Standardized Sample Preparation
  ASTM D7442-22 covers three primary methods to convert solid catalyst and zeolite powders into clear, dilute solutions suitable for ICP-OES analysis:

  • Perchloric Acid Digestion
  • Sulfuric Acid Digestion
  • Lithium Borate Fused Dissolution

• Safety Considerations
  The practice outlines extensive safety requirements due to the use of hazardous substances such as perchloric acid and hydrofluoric acid. Proper personal protective equipment (PPE), fume hoods, and emergency response equipment are essential.

• Uniform Sample Dissolution
  The methods ensure thorough removal of moisture and volatile substances, followed by careful chemical dissolution to prevent sample degradation and maintain reliable trace elemental results.

• Quality and Regulatory Importance
  Uniform procedures support laboratory quality assurance, regulatory compliance, and inter-laboratory data correlation for FCC catalyst materials.

Applications

• Catalyst Manufacturing
  Catalyst producers utilize this standard for in-process control and verification of raw and final catalyst compositions. Accurate elemental analysis is critical for quality assurance in FCC catalyst production.

• Petroleum Refining
  Refineries adopt the standard to assess catalyst performance, efficiency, and lifecycle within Fluid Catalytic Cracking Units (FCCUs). It helps optimize catalyst use and monitor process parameters essential for operational success.

• Environmental Compliance
  State and federal environmental authorities employ ASTM D7442-22 to verify data on catalyst and zeolite materials. Consistent preparation methods facilitate transparent compliance verification for environmental regulations.

• Research and Development
  Academic and industrial laboratories benefit from the reproducibility of these sample handling techniques, supporting innovation and new catalyst formulation analysis.

Related Standards

• ASTM D3766 - Terminology Relating to Catalysts and Catalysis: Provides definitions for terms used in catalyst testing and this standard.
• ASTM D7260 - Practice for Optimization, Calibration, and Validation of ICP-AES for Elemental Analysis: Reference standard for conducting the elemental analysis itself.
• ASTM E1272 - Specification for Laboratory Glass Graduated Cylinders: Governs requirements for volumetric measuring equipment.
• ASTM STP 447A - Manual on Test Sieving Methods: Reference for obtaining representative catalyst samples.

Additional safety resources and best practices for handling hazardous acids are strongly recommended, considering the significant risks associated with sample preparation reagents.

Practical Value

Implementing ASTM D7442-22 streamlines laboratory workflows, reduces procedural variability, and improves the reliability of ICP-OES elemental analysis results in catalyst and zeolite testing. By ensuring consistency and safety, this standard underpins robust quality assurance, regulatory compliance, and process optimization in the petrochemical industry and related fields.

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
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-
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.
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
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
D7442 − 22
to an appropriate analytical volume. This technique must be 7.5 Nitric Acid, HNO , concentrated, 65 %.
performed in an operational fume hood and can be performed
7.6 Hydrochloric Acid, 1:1 HCl (concentrated HCl, 38 %,
manually or may utilize the advantages of an automated fluxer.
diluted 1:1).
The optimal ratio of flux to sample, as well as fusion
7.7 Hydrogen Peroxide,3%.
temperature needed, will vary depending on sample matrix.
7.8 Lithium Borate Fluxes, lithium tetraborate, or
5. Significance and Use
metaborate, or both.
5.1 The chemical composition of catalyst and catalyst ma-
7.9 Boric Acid Solution, 2 to 3 %.
terials is an important indicator of catalyst performance and is
a valuable tool for assessing parameters in a FCCU process. 8. Sampling
This practice will be useful to catalyst manufacturers and
8.1 Obtain a representative sample of approximately 50 g of
petroleum refiners for quality verification and performance
material from larger composites by riffling or splitting in
evaluation, and to environmental authorities at the state and
accordance with subsection 5.12 of STP 447A or some other
federal levels for evaluation and verification of various com-
suitable means with the aim of obtaining a sample that
3, 4, 5
pliance programs.
represents the composition of the larger composite.
5.2 Catalysts and catalyst type materials are difficult to
9. Preparation of Powder Samples
prepare for analysis by ICP, and although the techniques
presented in this practice are common, there is wide variation 9.1 Catalysts and catalyst type sample powders contain
among laboratories in sample pretreatment and digestion small amounts of moisture and other volatile materials that
recipes. This practice is intended to standardize these variables must be removed to eliminate potential error in the analysis.
in order to facilitate the utility of comparative data among Typically, 50 g of powder sample are heated in air in a
manufacturers, refiners, and regulatory agencies. laboratory furnace at 538 to 593 °C for 1 to3hto remove
volatilecomponentspriortofurtherpreparationbyanyofthese
6. Apparatus
threetechniques.Ifsamplecontainsorganicmaterials,pretreat-
ment is recommended prior to placing the sample at 538 to
6.1 Muffle Furnace—at 538 to 593 °C.
593 °C.
6.2 Analytical Balance.
9.2 The bed depth of catalyst during the heat treatment
6.3 Digestion Vessels—platinum dish or PTFE beaker.
should typically be 25.4 mm or less.The heat-treated specimen
6.4 Volumetric Flasks—Class A glass, 250 mL.
should be thoroughly blended upon cooling, since some
particle size segregation normally occurs during the heat
6.5 Automated Fusion Machine—alternate to manual proce-
treatment step.
dure.
9.3 The heat-treated specimen should remain in a desiccator
6.6 Crucible—Pt /Au high-form.
95% 5%
until use to prevent re-adsorption of ambient moisture.
6.7 Fume Hood, suitable for materials in use. See Appendix
X1 – Appendix X3.
10. Hazards
6.8 Graduated Cylinders, Class A (see Specification
10.1 Hazards Common to All Mineral Acids:
E1272).
10.1.1 Wear suitable gloves, eye protection, and proper
protectiveclothingtoprotectintheeventofsplashesandspills.
7. Reagents
Dilutions shall be performed by adding acid to water, not the
7.1 All reagents should conform to American Chemical
other way around. Limit quantities in storage to what is needed
Society (ACS) specifications. Ultra high purity standards and for the next few weeks.
reference materials are commercially available from recog-
10.1.2 Boiling acid solutions can be particularly dangerous,
nized vendors. and the elevated temperature typically increases the severity of
the hazardous properties. Particular care and advance prepara-
7.2 Perchloric Acid, concentrated, 69 to 72 %.
tion shall be given to work with tasks involving acid solutions
7.3 Hydrofluoric Acid, concentrated, 48 %.
under these conditions.
7.4 Sulfuric Acid, H SO , concentrated, 94 %.
2 4
10.2 Hazards Specific to Perchloric Acid:
10.2.1 When not handled properly, perchloric acid can be a
very dangerous reagent. Digestions with perchloric acid should
Dean, John R., Practical Inductively Coupled Plasma Spectroscopy, John
be performed only in a fume hood specifically designed for its
Wiley, New York, 2005.
Gaines, Paul, “ICP Operations,” at http://www.ivstandards.com/tech/icp-ops.
unique hazards and properties. This hood shall have a water
Segal, Eileen B., “First Aid for a Unique Acid: HF,” Chemical Health and
washdown system, operated according to the manufacturer’s
Safety, Vol 5, Sept/Oct 1998, p. 25.
6 specifications and instructions. This system is required to
Reagent Chemicals, American Chemical Society Specifications, American
prevent buildup of explosive perchlorate salts in the duct work.
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USP), Rockville, Manual on Test Sieving Methods, ASTM STP 447A, ASTM Internatio
...

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
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
2.1 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
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.
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
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 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 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
3, 4, 5
verification of various compliance programs.
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.
6. Apparatus
6.1 Muffle Furnace—at 538 to 593°C.593 °C.
6.2 Analytical Balance.
6.3 Digestion Vessels—platinum dish or PTFE beaker.
6.4 Volumetric Flasks—Class A glass, 250 mL.
6.5 Automated Fusion Machine—alternate to manual procedure.
6.6 Crucible—Pt /Au high-form.
95% 5%
Dean, John R., Practical Inductively Coupled Plasma Spectroscopy, John Wiley, New York, 2005.
Gaines, Paul, “ICP Operations,” at http://www.ivstandards.com/tech/icp-ops.
Segal, Eileen B., “First Aid for a Unique Acid: HF,” Chemical Health and Safety, Vol 5, Sept/Oct 1998, p. 25.
D7442 − 22
6.7 Fume Hood, suitable for materials in use. See Appendix X1 – Appendix X3.
6.8 Graduated Cylinders, Class A (see Specification E1272).
7. Reagents
7.1 All reagents should conform to American Chemical Society (ACS) specifications. Ultra high purity standards and reference
materials are commercially available from recognized vendors.
7.2 Perchloric Acid, concentrated, 69 to 72 %.
7.3 Hydrofluoric Acid, concentrated, 48 %.
7.4 Sulfuric Acid, H SO , concentrated, 94 %.
2 4
7.5 Nitric Acid, HNO , concentrated, 65 %.
7.6 Hydrochloric Acid, 1:1 HCl (concentrated HCl, 38 %, diluted 1:1).
7.7 Hydrogen Peroxide, 3 %.
7.8 Lithium Borate Fluxes, lithium tetraborate, or metaborate, or both.
7.9 Boric Acid Solution, 2 to 3 %.
8. Sampling
8.1 Obtain a representative sample of approximately 50 g of material from larger composites by riffling or splitting in accordance
with subsection 5.12 of STP 447A or some other suitable means with the aim of obtaining a sample that represents the
composition of the larger composite.
9. Preparation of Powder Samples
9.1 Catalysts and catalyst type sample powders contain small amounts of moisture and other volatile materials that must be
removed to eliminate potential error in the analysis. Typically, 50 g of powder sample are heated in air in a laboratory furnace at
538 to 593°C593 °C for 1 to 3 h to remove volatile components prior to further preparation by any of these three techniques. If
sample contains organic materials, pretreatment is recommended prior to placing the sample at 538 to 593°C.593 °C.
9.2 The bed depth of catalyst during the heat treatment should typically be 25.4 mm or less. The heat-treated specimen should be
thoroughly blended upon cooling, since some particle size segregation normally occurs during the heat treatment step.
9.3 The heat-treated specimen should remain in a desiccator until use to prevent re-adsorption of ambient moisture.
10. Hazards
10.1 Hazards Common to All Mineral Acids:
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed by
the American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USP), Rockville, MD.
Manual on Test Sieving Methods, ASTM STP 447A, ASTM International, 2005.
D7442 − 22
10.1.1 Wear suitable gloves, eye protection, and proper protective clothing to protect in the event of splashes and spills. Dilutions
shall be performed by adding acid to water, not the other way around. Limit quantities in storage to what is needed for the next
few weeks.
10.1.2 Boiling acid solutions can be particularly dangerous, and the elevated temperature typically increases the severity of the
hazardous properties. Particular care and advance preparation shall be given to work with tasks involving acid solutions under these
conditions.
10.2 Hazards Specific to Perchloric Acid:
10.2.1 When not handled properly, perchloric acid can be a very dangerous reagent. Digestions with perchloric acid should be
performed only in a fume hood specifically designed for its unique hazards and properties. This hood shall have a water washdown
system, operated according to the manufacturer’s specifications and instructions. This system is required to preven
...