ASTM D4782-10

Standard Test Method for Palladium in Molecular Sieve Catalyst by Wet Chemistry

SIGNIFICANCE AND USE
This test method provides a means of determining the palladium content in fresh catalysts containing molecular sieves.
This test method is not intended to cover samples containing 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-Mar-2010
• Technical Committee: D32 - Catalysts
• Drafting Committee: D32.03 - Chemical Composition

Relations

• Replaces: ASTM D4782-04 - Standard Test Method for Palladium in Molecular Sieve Catalyst by Wet Chemistry
• Effective Date: 01-Apr-2010
• Replaced By: ASTM D4782-10(2016) - Standard Test Method for Palladium in Molecular Sieve Catalyst by Wet Chemistry
• Effective Date: 01-Jan-2016

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4782 − 10
StandardTest Method for
1
Palladium in Molecular Sieve Catalyst by Wet Chemistry
This standard is issued under the fixed designation D4782; 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 amount of sodium sulfite is added to the filtrate to reduce any
free iodine to iodide. The excess iodide is titrated with 0.01 N
1.1 This test method covers the determination of palladium
AgNO potentiometrically, using a silver electrode versus a
3
in molecular sieve-containing fresh catalysts with about 0.5
calomel electrode. A second sample taken at the same time is
weight % of palladium.
used to determine loss on ignition.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Significance and Use
standard.
4.1 This test method provides a means of determining the
1.3 This standard does not purport to address all of the
palladium content in fresh catalysts containing molecular
safety concerns, if any, associated with its use. It is the
sieves.
responsibility of the user of this standard to establish appro-
4.2 This test method is not intended to cover samples
priate safety and health practices and determine the applica-
containing metals other than palladium.
bility of regulatory limitations prior to use.
5. Apparatus
2. Referenced Documents
2
5.1 pH Meter with Millivolt Scale or automatic recording
2.1 ASTM Standards:
titrator.
D1193 Specification for Reagent Water
D7442 Practice for Sample Preparation of Fluid Catalytic
5.2 Silver-Sulfide Electrode.
CrackingCatalystsandZeolitesforElementalAnalysisby
5.3 Silver-Silver Chloride Double Junction reference elec-
Inductively Coupled Plasma Atomic Emission Spectros-
trode with 10 % KNO in the outer chamber.
3
copy
E177 Practice for Use of the Terms Precision and Bias in 5.4 Fisher Burner.
ASTM Test Methods
5.5 Low-Temperature Muffle Furnace, 450°C.
E456 Terminology Relating to Quality and Statistics
5.6 High-Temperature Muffle Furnace, 1000°C.
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method 5.7 Hot-Plate, with sand bath as a preferred option.
5.8 Magnetic Stirrer and TFE-Fluorocarbon-Coated Stir-
3. Summary of Test Method
ring Bars.
3.1 The test sample is treated with hydrofluoric acid and
5.9 Burets, 25-mL, with 0.1-mL graduations or an equiva-
evaporated to dryness to remove silica; the residue is fused
lent.
with potassium pyrosulfate, and the cooled melt is dissolved in
5.10 Volumetric Flasks, 1000-mL.
4% H SO . A measured excess of 0.01 N potassium iodide
2 4
(KI) is added to precipitate palladium as palladium iodide
5.11 High-Silica Beakers, 400-mL, with disposable boro-
(PdI ). The precipitate is filtered and washed, and a small
2 silicate beakers as an option. Alternatively, a petri dish can be
used for the fusion step, with polypropylene beakers being
used thereafter.
1
This test method is under the jurisdiction of ASTM Committee D32 on
5.12 Watch Glasses, preferably ribbed, 87 mm.
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
Composition.
5.13 Analytical Balance, capable of weighing to nearest 0.1
Current edition approved April 1, 2010. Published May 2010. Originally
mg.
approved in 1988. Last previous edition approved in 2004 as D4782–04. DOI:
10.1520/D4782-10.
5.14 Weighing Papers.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
5.15 Porcelain Crucibles, 10-mL.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 5.16 Graduated Cylinders, 5-mL, 10-mL, 25-mL, 100-mL.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D4782 − 10
5.17 Filter Paper, Whatman No. 40, 11 cm. min, place in desiccator to cool, and weigh to nearest 0.1 mg.
Transfer approximately 2.0 g of sample to the crucible and
5.18 Funnel, filter.
weigh to the nearest 0.1 mg.
5.19 Desiccator.
7.1.2 For determination of palladium, transfer approxi-
5.20 Crucible Cover, porcelain. mately 1.6 g of sample, weighed to the nearest 0.1 mg, into a
400-mL high-silica beaker.
6. Reagents and Materials
7.2 Loss on Ignition:
6.1 Purity of Reagents—Reagent grade chemicals shall be
7.2.1 Place the porcelain crucible containing the test sample
used in all tests. Unless otherwise indicated, it is intended that
in a muffle furnace maintained at 450°C and heat for 30 min.
all re
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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:D4782–04 Designation:D4782–10
Standard Test Method for
1
Palladium in Molecular Sieve Catalyst by Wet Chemistry
This standard is issued under the fixed designation D4782; 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
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
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D7442 Practice for Sample Preparation of Fluid Catalytic Cracking Catalysts and Zeolites for Elemental Analysis by
Inductively Coupled Plasma Atomic Emission Spectroscopy
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
3. Summary of Test Method
3.1 The test sample is treated with hydrofluoric acid and evaporated to dryness to remove silica; the residue is fused with
potassiumpyrosulfate,andthecooledmeltisdissolvedin4 %H SO .Ameasuredexcessof0.01Npotassiumiodide(KI)isadded
2 4
to precipitate palladium as palladium iodide (PdI ). The precipitate is filtered and washed, and a small amount of sodium sulfite
2
isaddedtothefiltratetoreduceanyfreeiodinetoiodide.Theexcessiodideistitratedwith0.01NAgNO potentiometrically,using
3
a silver electrode versus a calomel electrode. A second sample taken at the same time 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 metals other than palladium.
5. Apparatus
5.1 pH Meter with Millivolt Scale or automatic recording titrator.
5.2 Silver-Sulfide Electrode.
5.3 Silver-Silver Chloride Double Junction reference electrode with 10 % KNO in the outer chamber.
3
5.4 Fisher Burner.
5.5 Low-Temperature Muffle Furnace, 450°C.
5.6 High-Temperature Muffle Furnace, 1000°C.
5.7 Hot-Plate, with sand bath as a preferred option.
5.8 Magnetic Stirrer and TFE-Fluorocarbon-Coated Stirring Bars.
5.9 Burets, 25-mL, with 0.1-mL graduations or an equivalent.
5.10 Volumetric Flasks, 1000-mL.
1
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 April 1, 2004.2010. Published April 2004.May 2010. Originally approved in 1988. Last previous edition approved in 19972004as
D4782–91(1997).D4782–04. DOI: 10.1520/D4782-104.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D4782–10
5.11 High-Silica Beakers, 400-mL, with disposable borosilicate beakers as an option.Alternatively, a petri dish can be used for
the fusion step, with polypropylene beakers being used thereafter.
5.12 Watch Glasses, preferably ribbed, 87 mm.
5.13 Analytical Balance, capable of weighing to nearest 0.1 mg.
5.14 Weighing Papers.
5.15 Porcelain Crucibles, 10-mL.
5.16 Graduated Cylinders, 5-mL, 10-mL, 25-mL, 100-mL.
5.17 Filter Paper, Whatman No. 40, 11 cm.
5.18 Funnel, filter.
5.19 Desiccator.
5.20 Crucible Cover, porcelain.
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
3
such specifications are available. O
...