ASTM D5153-10(2016)

Standard Test Method for Palladium in Molecular Sieve Catalyst by Atomic Absorption

SIGNIFICANCE AND USE
4.1 This test method provides a means of determining the palladium content in fresh catalysts containing molecular sieves.  
4.2 This test method is not intended to cover samples containing precious metals other than palladium.
SCOPE
1.1 This test method covers the determination of palladium in molecular sieve-containing fresh catalysts with about 0.5 weight % of palladium.  
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: 31-Dec-2015
• ICS: 71.040.30 - Chemical reagents
• 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D5153 − 10 (Reapproved 2016)
Standard Test Method for
Palladium in Molecular Sieve Catalyst by Atomic
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 acid is expelled.Aqua regia and lanthanum chloride are added
and the solution is diluted to a specific volume. Palladium
1.1 This test method covers the determination of palladium
concentration is determined by atomic absorption spectropho-
in molecular sieve-containing fresh catalysts with about 0.5
tometry.Absorbance of the samples is bracketed using a set of
weight % of palladium.
narrow range, matrix matched standards. A second sample,
1.2 The values stated in SI units are to be regarded as
taken at the same time as the analysis sample, is used to
standard. No other units of measurement are included in this
determine loss on ignition.
standard.
1.3 This standard does not purport to address all of the 4. Significance and Use
safety concerns, if any, associated with its use. It is the
4.1 This test method provides a means of determining the
responsibility of the user of this standard to establish appro-
palladium content in fresh catalysts containing molecular
priate safety and health practices and determine the applica-
sieves.
bility of regulatory limitations prior to use.
4.2 This test method is not intended to cover samples
containing precious metals other than palladium.
2. Referenced Documents
2.1 ASTM Standards:
5. Apparatus
D1193 Specification for Reagent Water
5.1 Analytical Balance, capable of weighing to nearest
E177 Practice for Use of the Terms Precision and Bias in
0.1 mg.
ASTM Test Methods
E456 Terminology Relating to Quality and Statistics
5.2 Atomic Absorption Spectrophotometer.
E691 Practice for Conducting an Interlaboratory Study to
5.3 Beakers, TFE-fluorocarbon, 100-mL.
Determine the Precision of a Test Method
5.4 Crucibles, porcelain, 10-mL.
D7442 Practice for Sample Preparation of Fluid Catalytic
CrackingCatalystsandZeolitesforElementalAnalysisby
5.5 Crucible Cover, porcelain, for 10-mL crucible.
Inductively Coupled Plasma Atomic Emission Spectros-
5.6 Desiccator.
copy
5.7 Flasks, Erlenmeyer, 2000-mL.
2.2 U.S. Federal Specification:
Federal Spec. NNN-P-395C Tolerance for Class A Pipets
5.8 Graduated Cylinders, glass, 5-mL, 10-mL, 25-mL,
50-mL, 250-mL, 500-mL, 1000-mL.
3. Summary of Test Method
5.9 Graduated Cylinder, plastic, 10-mL.
3.1 The test sample is treated with a mixture of sulfuric and
5.10 Hot Plate.
hydrofluoric acids. Upon dissolution, the excess hydrofluoric
5.11 Muffle Furnace,electricallyheated,capableof1000°C.
This test method is under the jurisdiction of ASTM Committee D32 on
5.12 Pipets, 4-mL, 6-mL, 8-mL, 10-mL.
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
Composition.
5.13 Volumetric Flasks, 100-mL, 500-mL.
Current edition approved Jan. 1, 2016. Published January 2016. Originally
5.14 Watch Glasses, TFE-fluorocarbon, for 100-mL beaker.
approved in 1991. Last previous edition approved in 2010 as D5153–10. DOI:
10.1520/D5153-10R16.
5.15 Weighing Papers.
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 6. Reagents and Materials
the ASTM website.
3 6.1 Purity of Reagents—Reagent grade chemicals shall be
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098. used in all tests. Unless otherwise indicated, it is intended that
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5153 − 10 (2016)
all reagents shall conform to the specifications of the Commit- 7.1.1 If the concentration of aluminum oxide in the sample
tee onAnalytical Reagents of theAmerican Chemical Society, is unknown, digest a representative sample in acid and deter-
where such specifications are available. Other grades may be mine the aluminum concentration by atomic absorption spec-
used provided it is first ascertained that the reagent is of trophotometry.
sufficiently high purity to permit its use without lessening the
7.1.2 Transfer 30 mL of sulfuric acid (3M) to five TFE-
accuracy of the determination.
fluorocarbon beakers.
7.1.3 Toeachbeakeraddtheequivalentweightofaluminum
6.2 Purity of Water—Unless otherwise indicated, references
oxide that would be present in 0.8000 g of sample as
to water shall be understood to mean reagent water as defined
determined in 7.1.1.
by Specification D1193.
NOTE 3—If it is available, 0.800 g of catalyst base material may be
6.3 Hydrochloric Acid, concentrated, 36.5–38.0 wt. % or 12
substituted for the aluminum oxide.
M, sp gr 1.18.
7.1.4 Transfer 0, 4, 6, 8 and 10 mL of the 500 mg/L
6.4 Hydrofluoric Acid, concentrated, 48.0–51.0 wt. % or
palladium standard to the five TFE-fluorocarbon beakers.
28.9 M, sp gr 1.17.
7.1.5 Add 10 mL of concentrated hydrofluoric acid to each
NOTE 1—Refer to Section 8 of Practice D7442-08 for hazards associ-
beaker.
ated with handling of acids.
7.1.6 Cover the beakers with TFE-fluorocarbon lids and
6.5 NitricAcid,concentrated,69.0–71.0wt.%or15.7M,sp
digest on a hot plate at medium heat until all solid material is
gr 1.41.
in solution (including any brown stains that may appear on the
beaker walls) and light fumes are evolved.
6.6 Sulfuric Acid, concentrated, 95.0–98.0 wt. % or 18 M,
sp gr 1.84.
NOTE 4—If brown stains do not redissolve, discard sample and prepare
again.
6.7 Aluminum Oxide (Al O ).
2 3
7.1.7 Cool the solutions. Dilute to 70 mL with distilled
6.8 Lanthanum Chloride (LaCl ·7H O).
3 2
water.Add 10 mL of aqua regia. Boil gently for a few minutes
6.9 Palladium Wire, 99.99 %.
on a hot plate.
7.1.8 When the solution is cool, transfer quantitatively to a
6.10 Aqua Regia—Mix three parts by volume of concen-
500-mL volumetric flask.
trated hydrochloric acid (12 M) and one part by volume of
7.1.9 Add 5 mL of the lanthanum chloride solution to each
concentrated nitric acid (15.7 M) immediately before use.
flask. Dilute to volume when the solution has reached room
6.11 Sulfuric Acid, 15.8–16.3 wt. % or 3M. Cautiously add
temperature.
250 mL of concentrated sulfuric acid (18 M) to 1250 mL of
7.1.10 The concentration of palladium will be 0, 4, 6, 8 and
water—mix well and allow to cool.
10 mg/L.
6.12 Palladium Standard Solution, 500 mg/L. Dissolve
NOTE 5—The standard solutions are stable for two months.
0.2500 6 0.0001 g of palladium wire (99.99 %) in 25 mL of
aqua regia. Evaporate the solution to dryness on a steam bath.
7.2 Weighing—Prepare a carefully riffled, finely ground
Dissolve the remaining salts by addition of 25 mL of concen- sample of ambient-equilibrated catalyst. For example, the
trated hydrochloric acid (12 M)
...

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: D5153 − 10 D5153 − 10 (Reapproved 2016)
Standard Test Method for
Palladium in Molecular Sieve Catalyst by Atomic
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
1.1 This test method covers the determination of palladium in molecular sieve-containing fresh catalysts with about 0.5 weight
% of palladium.
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
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
D7442 Practice for Sample Preparation of Fluid Catalytic Cracking Catalysts and Zeolites for Elemental Analysis by Inductively
Coupled Plasma Atomic Emission Spectroscopy
2.2 U.S. Federal Specification:
Federal Spec. NNN-P-395C Tolerance for Class A Pipets
3. Summary of Test Method
3.1 The test sample is treated with a mixture of sulfuric and hydrofluoric acids. Upon dissolution, the excess hydrofluoric acid
is expelled. Aqua regia and lanthanum chloride are added and the solution is diluted to a specific volume. Palladium concentration
is determined by atomic absorption spectrophotometry. Absorbance of the samples is bracketed using a set of narrow range, matrix
matched standards. A second sample, taken at the same time as the analysis sample, is used to determine loss on ignition.
4. Significance and Use
4.1 This test method provides a means of determining the palladium content in fresh catalysts containing molecular sieves.
4.2 This test method is not intended to cover samples containing precious metals other than palladium.
5. Apparatus
5.1 Analytical Balance, capable of weighing to nearest 0.1 mg.
5.2 Atomic Absorption Spectrophotometer.
5.3 Beakers, TFE-fluorocarbon, 100-mL.
5.4 Crucibles, porcelain, 10-mL.
This test method 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 Nov. 1, 2010Jan. 1, 2016. Published January 2011 January 2016. Originally approved in 1991. Last previous edition approved in 20042010 as
D5153–04.–10. DOI: 10.1520/D5153-10.10.1520/D5153-10R16.
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.
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5153 − 10 (2016)
5.5 Crucible Cover, porcelain, for 10-mL crucible.
5.6 Desiccator.
5.7 Flasks, Erlenmeyer, 2000-mL.
5.8 Graduated Cylinders, glass, 5-mL, 10-mL, 25-mL, 50-mL, 250-mL, 500-mL, 1000-mL.
5.9 Graduated Cylinder, plastic, 10-mL.
5.10 Hot Plate.
5.11 Muffle Furnace, electrically heated, capable of 1000°C.
5.12 Pipets, 4-mL, 6-mL, 8-mL, 10-mL.
5.13 Volumetric Flasks, 100-mL, 500-mL.
5.14 Watch Glasses, TFE-fluorocarbon, for 100-mL beaker.
5.15 Weighing Papers.
6. Reagents and Materials
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Specification D1193.
6.3 Hydrochloric Acid, concentrated, 36.5–38.0 wt. % or 12 M, sp gr 1.18.
6.4 Hydrofluoric Acid, concentrated, 48.0–51.0 wt. % or 28.9 M, sp gr 1.17.
NOTE 1—Refer to Section 8 of Practice D7442-08 for hazards associated with handling of acids.
6.5 Nitric Acid, concentrated, 69.0–71.0 wt. % or 15.7 M, sp gr 1.41.
6.6 Sulfuric Acid, concentrated, 95.0–98.0 wt. % or 18 M, sp gr 1.84.
6.7 Aluminum Oxide (Al O ).
2 3
6.8 Lanthanum Chloride (LaCl ·7H O).
3 2
6.9 Palladium Wire, 99.99 %.
6.10 Aqua Regia—Mix three parts by volume of concentrated hydrochloric acid (12 M) and one part by volume of concentrated
nitric acid (15.7 M) immediately before use.
6.11 Sulfuric Acid, 15.8–16.3 wt. % or 3M. Cautiously add 250 mL of concentrated sulfuric acid (18 M) to 1250 mL of
water—mix well and allow to cool.
6.12 Palladium Standard Solution, 500 mg/L. Dissolve 0.2500 6 0.0001 g of palladium wire (99.99 %) in 25 mL of aqua regia.
Evaporate the solution to dryness on a steam bath. Dissolve the remaining salts by addition of 25 mL of concentrated hydrochloric
acid (12 M) and 25 mL of distilled water. Transfer the solution to a 500 mL volumetric flask and dilute to volume when cool.
NOTE 2—A commercially available atomic absorption palladium reference solution may be used if it is known to be reliable.
6.13 Lanthanum Chloride Solution—Dissolve 25.5 g of lanthanum chloride (LaCl ·7H O) in distilled water, dilute to 100 mL
3 2
and mix well. This solution serves as an ionization suppressor in atomic absorption.
6.14 Desiccant, molecular sieve, type 4A.
7. Procedure
7.1 Preparation of Calibration Standards:
7.1.1 If the concentration of aluminum oxide in the sample is unknown, digest a representative sample in acid and determine
the aluminum concentration by atomic absorption spectrophotometry.
7.1.2 Transfer 30 mL of sulfuric acid (3M) to five TFE-fluorocarbon beakers.
7.1.3 To each beaker add the equivalent weight of aluminum oxide that would be present in 0.8000 g of sample as determined
in 7.1.1.
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. (USPC), Rockville, MD.
D5153 − 10 (2016
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