ASTM D4642-04(2016)
(Test Method)Standard Test Method for Platinum in Reforming Catalysts by Wet Chemistry
Standard Test Method for Platinum in Reforming Catalysts by Wet Chemistry
SIGNIFICANCE AND USE
4.1 This test method provides a means of determining the platinum content of fresh reforming catalysts where the platinum is supported on an all alumina substrate.4
4.2 This test method is not intended to cover samples containing metals other than platinum. Palladium, rhenium, and rhodium in particular interfere with the spectrophotometric determination of platinum.
SCOPE
1.1 This test method covers the determination of platinum in nonzeolitic, fresh reforming catalysts containing platinum as the only precious metal, in the range of concentration of 0.200 to 0.700 weight %.
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: D4642 − 04 (Reapproved 2016)
Standard Test Method for
Platinum in Reforming Catalysts by Wet Chemistry
This standard is issued under the fixed designation D4642; 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 at 403 nm by spectrophotometry and the platinum content is
calculated from a previously determined value for the absorp-
1.1 Thistestmethodcoversthedeterminationofplatinumin
tivity.
nonzeolitic, fresh reforming catalysts containing platinum as
the only precious metal, in the range of concentration of 0.200
4. Significance and Use
to 0.700 weight %.
4.1 This test method provides a means of determining the
1.2 The values stated in SI units are to be regarded as
platinum content of fresh reforming catalysts where the plati-
standard. No other units of measurement are included in this
num is supported on an all alumina substrate.
standard.
4.2 This test method is not intended to cover samples
1.3 This standard does not purport to address all of the
containing metals other than platinum. Palladium, rhenium,
safety concerns, if any, associated with its use. It is the
andrhodiuminparticularinterferewiththespectrophotometric
responsibility of the user of this standard to establish appro-
determination of platinum.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Apparatus
5.1 Balance, analytical, capable of weighing to the nearest
2. Referenced Documents
0.1 mg.
2.1 ASTM Standards:
5.2 Beakers, 250-mL, tall form and 600-mL.
D1193 Specification for Reagent Water
E177 Practice for Use of the Terms Precision and Bias in
5.3 Cells, spectrophotometer, 1.0 cm, matched.
ASTM Test Methods
5.4 Crucibles, platinum, or porcelain, 50-mL.
E288 Specification for Laboratory Glass Volumetric Flasks
5.5 Desiccator, vacuum.
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to
5.6 Filter Paper, fine, ashless, slow filtering, 12.5 cm or
Determine the Precision of a Test Method
equivalent.
2.2 U.S. Federal Specification:
5.7 Flasks, volumetric, conforming to tolerances specified
NNN-P-395C Tolerance for Class A Pipets
by Specification E288, 500-mL and 1000-mL.
3. Summary of Test Method
5.8 Funnel, filtering, fluted bowl, 65 mm top diameter, 150
mm stem.
3.1 The ground alumina based reforming catalyst is dis-
solved using dilute hydrochloric acid. Stannous chloride is
5.9 Graduated Cylinders, 10-mL, 25-mL, 50-mL, 250-mL.
added to convert the platinum in solution to a yellowish-
5.10 Pipets, conforming to tolerances specified by Federal
orange-colored platinum stannous hydrochloride complex.The
Specification NNN-P-395C, 5-mL, 10-mL, 15-mL.
absorbance of the resulting solution is measured comparatively
5.11 Muffle Furnace, capable of 1000 6 25°C.
5.12 Spectrophotometer, capable of measuring absorbance
This test method is under the jurisdiction of ASTM Committee D32 on
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical values between 200 to 800 nm with a photometric repeatability
Composition.
of 60.002 absolute at 1.0 absolute.
Current edition approved Jan. 1, 2016. Published January 2016. Originally
approved in 1986. Last previous edition approved in 2010 as D4642–04(2010). 5.13 Watch Glass, flat, 100 mm.
DOI: 10.1520/D4642-04R16.
5.14 Watch Glass, ribbed, 65 mm.
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
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. This test method can be extended to spent reforming catalyst by isolating the
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4, platinum by the methods described in “Assay Procedure for Platinum in Reforming
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098. Catalysts,” Analytical Chemistry , Vol 32, No. 6, May 1960, p. 646.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4642 − 04 (2016)
5.15 Wash Bottle, polyethylene, 500-mL. temperature and readjust carefully to volume with water and
mix. This stock solution contains approximately 1000 ppm of
5.16 Weighing Vial, 25 by 40 mm.
platinum and provides suitable aliquots for platinum standards.
Transfer aliquots of 5 mL, 10 mL, and 15 mL, respectively, to
6. Reagents
3clean500-mLvolumetricflasks.Add175mLofconcentrated
6.1 Purity of Reagents—Reagent grade chemicals shall be
hydrochloric acid, and 30 mL of stannous chloride solution to
used in all tests. Unless otherwise indicated, it is intended that
the 500-mL flask. Add sufficient aluminum chloride solution,
all reagents shall conform to the specifications of the Commit-
(approximately 15 mL), to bring the standard to the same
tee onAnalytical Reagents of theAmerican Chemical Society,
stoichiometric aluminum level as the unknown. Add distilled
where such specifications are available. Other grades may be
water to bring the solution just to the neck of the flask, which
used, provided it is first ascertained that the reagent is of
permits mixing of all components. Prior to taking a portion for
sufficiently high purity to permit its use without lessening the
a spectrophotometric reading, allow the solution to come to
accuracy of the determination.
roomtemperature,addadditionaldistilledwatertoadjusttothe
6.2 Purity of Water—Unless otherwise indicated, all refer-
volumetric mark and mix the solution thoroughly.
ences to water used as a reagent mean deionized or distilled
6.13 Stannous Chloride Reagent—Dissolve 280 g of stan-
water conforming to Specification D1193.
nous chloride (SnCl ·2H O) in 500 mLof concentrated hydro-
2 2
6.3 Aluminum Chloride Solution—Dissolve 453.6 g of
chloric acid with warming on a hot plate. Dilute to 1000 mL
AlCl ·6H O in water and dilute to a litre with water.
with water and mix thoroughly. Filter this solution if it is
3 2
cloudy. This solution should be prepared fresh daily.
6.4 Aqua Regia—Mix three parts concentrated hydrochloric
acid with one part concentrated nitric acid.
6.14 Water, distilled, reagent.
6.5 Formic Acid (HCOOH).
7. Procedure
6.6 Hydrochloric Acid (HCl), concentrated, specific gravity
7.1 Calcination—The platinum level in reforming catalysts
1.19.
is normally reported on a volatile-free basis. The loss on
6.7 Hydrochloric Acid (HCl) Solution, 18 to 19 volume %
ignition (LOI) determination (1000°C) is carried out
or 6 N. Dilute 500 mL of concentrated hydrochloric acid to a
separately, but weighed out at the same time as the ground
litre with water.
sample for digestion. Due to the hygroscopic nature of the
sample, weigh by difference from a weighing vial. Weigh in
6.8 HydrochloricAcid (HCl), 3.7 volume % or 1.2 N. Dilute
triplicate 3 g 6 0.1-mg samples of reforming catalyst in
100 mLof concentrated hydrochloric acid to a litre with water.
platinum or porcelain crucibles,
...
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