ASTM D7442-08
(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 inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered 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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Standards Content (Sample)
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Designation:D7442–08
Standard Practice for
Sample Preparation of Fluid Catalytic Cracking Catalysts
and Zeolites for Elemental Analysis by Inductively Coupled
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.2 Powder samples are heat-treated for 1 to3hto remove
volatilecomponentspriortofurtherpreparationbyanyofthese
1.1 This practice covers uniform dissolution techniques for
three techniques.
preparing samples of fluid catalytic cracking catalysts (FCC)
3.3 The Perchloric Acid and Sulfuric Acid techniques in-
and exchanged zeolitic materials for analysis by Inductively
volve dissolving small aliquots of heat-treated sample in the
Coupled Plasma Atomic Emission Spectroscopy (ICP-AES).
respective acid liquors and diluting the resulting solutions to
These techniques describe standardized approaches to well-
the appropriate analytical volume. These techniques require
known, widely used laboratory practices of sample preparation
boiling acid solutions in platinum or polytetrafluoroethylene
utilizingaciddigestionsandboratesaltfusions.Thispracticeis
(PTFE) labware and shall be used in appropriate fume hoods.
applicable to fresh and equilibrium FCC catalysts and ex-
ThePerchloricAcidDigestionshall neverbeusedinastandard
changed zeolite materials.
fume hood.
1.2 The values stated in inch-pound units are to be regarded
3.4 The Lithium Borate Fused Dissolution technique in-
as standard. The values given in parentheses are mathematical
volves dissolving small aliquots of heat-treated sample in a
conversions to SI units that are provided for information only
molten flux of lithium metaborate and lithium tetraborate salts,
and are not considered standard.
dissolving the resulting flux solution in a dilute nitric acid
1.3 This standard does not purport to address all of the
solution, and diluting the clear, concentrated specimen solution
safety concerns, if any, associated with its use. It is the
to an appropriate analytical volume. This technique must be
responsibility of the user of this standard to establish appro-
performed in an operational fume hood and can be performed
priate safety and health practices and determine the applica-
manually or may utilize the advantages of an automated fluxer.
bility of regulatory limitations prior to use.
The optimal ratio of flux to sample, as well as fusion
2. Terminology temperature needed, will vary depending on sample matrix.
2.1 Acronyms:
4. Significance and Use
2.1.1 FCC—Fluid Catalytic Cracking
4.1 The chemical composition of catalyst and catalyst ma-
2.1.2 FCCU—Fluid Catalytic Cracking Unit
terials is an important indicator of catalyst performance and is
2.1.3 ICP-AES—Inductively-Coupled Plasma-Atomic
a valuable tool for assessing parameters in a FCCU process.
Emission Spectroscopy
This practice will be useful to catalyst manufacturers and
3. Summary of Practice petroleum refiners for quality verification and performance
evaluation, and to environmental authorities at the state and
3.1 Three preparation techniques are presented for convert-
federal levels for evaluation and verification of various com-
ing solid, power samples into clear, dilute acid solutions
, ,
2 3 4
pliance programs.
suitable for analysis by ICP-AES. The three techniques pre-
4.2 Catalysts and catalyst type materials are difficult to
sented are PerchloricAcid Digestion, SulfuricAcid Digestion,
prepare for analysis by ICP, and although the techniques
and Lithium-Borate Fused Dissolution. Other techniques may
presented in this practice are common, there is wide variation
be possible; however, these three approaches are established,
among laboratories in sample pretreatment and digestion
widely used laboratory techniques for preparing FCC catalyst
and catalyst-like samples.
Dean, John R., Practical Inductively Coupled Plasma Spectroscopy , John
Wiley, New York, 2005.
This practice is under the jurisdiction of ASTM Committee D32 on Catalysts
Gaines, Paul, “ICP Operations,” at www.ivstandards.com/tech/icp-ops .
and is the direct responsibility of Subcommittee D32.03 on Chemical Composition. Segal, Eileen B., “First Aid for a Unique Acid: HF,” Chemical Health and
Current edition approved April 1, 2008. Published April 2008. Safety, Sept/Oct 1998, Vol 5, p. 25.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7442–08
recipes. This practice is intended to standardize these variables 8.1.2 Boiling acid solutions can be particularly dangerous,
in order to facilitate the utility of comparative data among and the elevated temperature typically increases the severity of
manufacturers, refiners, and regulatory agencies. the hazardous properties. Particular care and advance prepara-
tion shall be given to work with tasks involving acid solutions
5. Apparatus
under these conditions.
5.1 Muffle Furnace—at 1000 to 1100°F (538 to 593°C).
8.2 Hazards Specific to Perchloric Acid:
5.2 Analytical Balance.
8.2.1 When not handled properly, perchloric acid can be a
5.3 Digestion Vessels—platinum dish or PTFE beaker.
very dangerous reagent. Digestions with perchloric acid should
5.4 Volumetric Flasks—Class A glass, 250 mL.
be performed only in a fume hood specifically designed for its
5.5 Automated Fusion Machine—alternate to manual pro-
unique hazards and properties. This hood shall have a water
cedure.
washdown system, operated according to the manufacturer’s
5.6 Crucible—Pt /Au high-form.
95% 5% specifications and instructions. This system is required to
prevent buildup of explosive perchlorate salts in the duct work.
6. Reagents
8.2.2 Solutions with perchloric acid shall never be boiled to
6.1 All reagents should conform to American Chemical
dryness. Careful, attentive observation of techniques using
Society (ACS) specifications. Ultra high purity standards and
perchloric acid is imperative for safe use.
reference materials are commercially available from recog-
8.2.3 Perchloric acid should not be mixed or used with
nized vendors.
organic materials if there is a possibility that the temperature
6.2 Perchloric Acid, concentrated, 69 to 72 %.
will become elevated beyond ambient levels.
6.3 Hydrofluoric Acid, concentrated, 48 %.
8.2.4 In the event of a perchloric acid spill, neutralize with
6.4 Sulfuric Acid,H SO , concentrated, 94 %.
2 4
soda ash or other appropriate neutralizing agent. Soak up with
6.5 Nitric Acid, HNO , concentrated, 65 %.
an inorganic based absorbent. DO NOTuse rags, paper towels,
6.6 Hydrochloric Acid, 1:1 HCl (concentrated HCl, 38 %,
saw dust, or any organic or oxidizable material, as such
diluted 1:1).
material may spontaneously ignite. An approved spill kit for
6.7 Hydrogen Peroxide,3%.
perchloric acid is highly recommended.
6.8 Lithium Borate Fluxes, lithium tetraborate, or metabo-
8.3 Hazards Specific to Hydrofluoric Acid (HF):
rate, or both.
8.3.1 Hydrofluoric acid is an extremely hazardous
...
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