ASTM D4782-10(2016)
(Test Method)Standard Test Method for Palladium in Molecular Sieve Catalyst by Wet Chemistry
Standard Test Method for Palladium in Molecular Sieve Catalyst by Wet Chemistry
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.
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
Relations
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: D4782 − 10 (Reapproved 2016)
Standard Test Method for
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
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
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.
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.
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 Jan. 1, 2016. Published January 2016. Originally
mg.
approved in 1988. Last previous edition approved in 2004 as D4782–04(2010).
DOI: 10.1520/D4782-10R16.
5.14 Weighing Papers.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. 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
D4782 − 10 (2016)
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 reagents shall conform to the specifications of the Commit-
7.2.2 Transfer the crucible to a muffle furnace maintained at
tee onAnalytical Reagents of theAmerican Chemical Society,
1000°C and heat for at least 1.5 h to constant weight.
where such specifications are available. Other grades may be
7.2.3 Remove the crucible from the furnace, place in des-
used, provided it is first ascertained that the reagent is of
iccator to cool, and weigh to nearest 0.1 mg.
sufficiently high purity to permit its use without lessening the
7.2.4 Calculate weight percent loss on ignition at 1000°C as
accuracy of the determination.
follows:
6.2 Purity of Water—Unless otherwise indicated, references
I 2 F
~ !
to water shall be understood to mean reagent water as defined
Weight % LOI 5 3100 (1)
~I!
by Specification D1193.
where:
6.3 Desiccant Molecular Sieve, type 4A.
I = initial sample weight, and
6.4 Filter Paper Pulp.
F = final sample weight.
NOTE 1—Refer to Section 8 on Hazards in Practice D7442 for hazards
associated with handling of acids. 7.3 Preparation of Test Sample for Titration:
7.3.1 Cautiously add about 3 mL water to the high-silica
6.5 Hydrofluoric Acid (HF), 48 %.
beaker to disperse the test sample.
6.6 Potassium Iodide Solution, 0.01 N—Dissolve 1.66 g of
7.3.2 Add 12 mL hydrofluoric acid (HF) to effect dissolu-
potassiumiodide(KI)indistilledwater,diluteto1000mL,and
tion and evaporate to dryness on the cooler areas of the sand
mix well.
bath to remove silicon dioxide (SiO ).
6.7 Potassium Pyrosulfate (K S O ).
2 2 8
7.3.3 Promptly remove the beaker from the sand bath, cover
residue with9gof potassium pyrosulfate, and heat gently over
6.8 Silver Nitrate Solution, 0.01000 N—Dissolve 1.6989 g
a Fisher burner until all excess hydrofluoric acid (HF) is driven
of silver nitr
...
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