ASTM D5153-04

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Designation:D5153–04
Standard Test Method for
Palladium in Molecular Sieve Catalyst by Atomic
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Absorption
This standard is issued under the fixed designation D5153; 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 4. Significance and Use
1.1 This test method covers the determination of palladium 4.1 This test method provides a means of determining the
in molecular sieve-containing fresh catalysts with about 0.5 palladium content in fresh catalysts containing molecular
weight % of palladium. sieves.
1.2 This standard does not purport to address all of the 4.2 This test method is not intended to cover samples
safety concerns, if any, associated with its use. It is the containing precious metals other than palladium.
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
5.1 Analytical Balance, capable of weighing to nearest 0.1
bility of regulatory limitations prior to use.
mg.
2. Referenced Documents
5.2 Atomic absorption spectrophotometer.
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2.1 ASTM Standards: 5.3 Beakers, TFE-fluorocarbon, 100-mL.
D1193 Specification for Reagent Water 5.4 Crucibles, porcelain, 10-mL.
E177 Practice for Use of the Terms Precision and Bias in 5.5 Crucible Cover, porcelain, for 10-mL crucible.
ASTM Test Methods 5.6 Desiccator.
E456 Terminology Relating to Quality and Statistics 5.7 Flasks, Erlenmeyer, 2000-mL.
E691 Practice for Conducting an Interlaboratory Study to 5.8 Graduated Cylinders, glass, 5-mL, 10-mL, 25-mL, 50-
Determine the Precision of a Test Method mL, 250-mL, 500-mL, 1000-mL.
2.2 U.S. Federal Specification: 5.9 Graduated Cylinder, plastic, 10-mL.
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Federal Spec. NNN-P-395C Tolerance for Class A Pipets 5.10 Hot plate.
5.11 Muffle furnace, electrically heated, capable of 1000°C.
3. Summary of Test Method
5.12 Pipets, 4-mL, 6-mL, 8-mL, 10-mL.
3.1 The test sample is treated with a mixture of sulfuric and
5.13 Volumetric Flasks, 100-mL, 500-mL.
hydrofluoric acids. Upon dissolution, the excess hydrofluoric 5.14 Watch glasses, TFE-fluorocarbon, for 100-mL beaker.
acid is expelled.Aqua regia and lanthanum chloride are added
5.15 Weighing Papers.
and the solution is diluted to a specific volume. Palladium
6. Reagents and Materials
concentration is determined by atomic absorption spectropho-
tometry.Absorbance of the samples is bracketed using a set of 6.1 Purity of Reagents—Reagent grade chemicals shall be
narrow range, matrix matched standards. A second sample, used in all tests. Unless otherwise indicated, it is intended that
taken at the same time as the analysis sample, is used to all reagents shall conform to the specifications of the Commit-
determine loss on ignition. tee onAnalytical Reagents of theAmerican Chemical Society,
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where such specifications are available. Other grades may be
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used provided it is first ascertained that the reagent is of
This test method is under the jurisdiction of ASTM Committee D32 on
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
sufficiently high purity to permit its use without lessening the
Composition.
accuracy of the determination.
Current edition approved April 1, 2004. Published April 2004. Originally
approved in 1991. Last previous edition approved in 1997 as D5153–91(1997).
DOI: 10.1520/D5153-04.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or Reagent Chemicals, American Chemical Society Specifications, American
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
Standards volume information, refer to the standard’s Document Summary page on listed by the American Chemical Society, see Annual Standards for Laboratory
the ASTM website. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
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Available from Standardization Documents Order Desk, DODSSP, Bldg. 4, and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5153–04
NOTE 3—If brown stains do not redissolve, discard sample and prepare
6.2 Purity of Water—Unless otherwise indicated, references
again.
to water shall be understood to mean reagent water as defined
by Specification D1193.
7.1.7 Cool the solutions. Dilute to 70 mL with distilled
6.3 Hydrochloric acid, concentrated, 36.5–38.0 wt. % o
...