ASTM D4642-92(1998)
(Test Method)Standard Test Method for Platinum in Reforming Catalysts by Wet Chemistry
Standard Test Method for Platinum in Reforming Catalysts by Wet Chemistry
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 This standard does not purport to address all of the safety problems, 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.
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Designation: D 4642 – 92 (Reapproved 1998)
Standard Test Method for
Platinum in Reforming Catalysts by Wet Chemistry
This standard is issued under the fixed designation D 4642; 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 (e) 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 platinum in 4.1 This test method provides a means of determining the
nonzeolitic, fresh reforming catalysts containing platinum as platinum content of fresh reforming catalysts where the plati-
the only precious metal, in the range of concentration of 0.200 num is supported on an all alumina substrate.
to 0.700 weight %. 4.2 This test method is not intended to cover samples
1.2 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 and rhodium in particular interfere with the spectrophotometric
responsibility of the user of this standard to establish appro- determination of platinum.
priate safety and health practices and determine the applica-
5. Apparatus
bility of regulatory limitations prior to use.
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.
D 1193 Specification for Reagent Water 5.3 Cells, spectrophotometer, 1.0 cm, matched.
E 177 Practice for Use of the Terms Precision and Bias in 5.4 Crucibles, platinum, or porcelain, 50-mL.
ASTM Test Methods 5.5 Desiccator, vacuum.
E 288 Specification for Laboratory Glass Volumetric 5.6 Filter Paper, fine, ashless, slow filtering, 12.5 cm or
Flasks equivalent.
E 456 Terminology Relating to Quality and Statistics 5.7 Flasks, volumetric, conforming to tolerances specified
E 691 Practice for Conducting an Interlaboratory Study to by Specification E 288, 500-mL and 1000-mL.
Determine the Precision of a Test Method 5.8 Funnel, filtering, fluted bowl, 65 mm top diameter, 150
2.2 U.S. Federal Specification: mm stem.
NNN-P-395C Tolerance for Class A Pipets 5.9 Graduated Cylinders, 10-mL, 25-mL, 50-mL, 250-mL.
5.10 Pipets, conforming to tolerances specified by Federal
3. Summary of Test Method
Specification NNN-P-395C, 5-mL, 10-mL, 15-mL.
3.1 The ground alumina based reforming catalyst is dis- 5.11 Muffle Furnace, capable of 1000°C 6 25°C.
solved using dilute hydrochloric acid. Stannous chloride is
5.12 Spectrophotometer, capable of measuring absorbance
added to convert the platinum in solution to a yellowish- values between 200 to 800 nm with a photometric repeatability
orange-colored platinum stannous hydrochloride complex. The
of 60.002 absolute at 1.0 absolute.
absorbance of the resulting solution is measured comparatively 5.13 Watch Glass, flat, 100 mm.
at 403 nm by spectrophotometry and the platinum content is
5.14 Watch Glass, ribbed, 65 mm.
calculated from a previously determined value for the absorp- 5.15 Wash Bottle, polyethylene, 500-mL.
tivity.
5.16 Weighing Vial,25by40mm.
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be
This test method is under the jurisdiction of ASTM Committee D-32 on
used in all tests. Unless otherwise indicated, it is intended that
Catalysts and is the direct responsibility of Subcommittee D32.03 on Chemical
all reagents shall conform to the specifications of the Commit-
Composition.
tee on Analytical Reagents of the American Chemical Society,
Current edition approved Jan. 15, 1992. Published March 1992. Originally
published as D 4642 – 86. Last previous edition D 4642 – 92.
Annual Book of ASTM Standards, Vol 11.01.
3 5
Annual Book of ASTM Standards, Vol 14.02. The method can be extended to spent reforming catalyst by isolating the
Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 platinum by the methods described in Analytical Chemistry, Vol 32, No. 6, May
Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
1960, p. 646, “Assay Procedure for Platinum in Reforming Catalysts.”
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 4642
where such specifications are available. Other grades may be a spectrophotometric reading, allow the solution to come to
used, provided it is first ascertained that the reagent is of room temperature, add additional distilled water to adjust to the
sufficiently high purity to permit its use without lessening the volumetric mark and mix the solution thoroughly.
accuracy of the determination. 6.13 Stannous Chloride Reagent—Dissolve 280 g of stan-
6.2 Purity of Water—Unless otherwise indicated, all refer- nous chloride (SnCl ·2H O) in 500 mL of concentrated hydro-
2 2
ences to water used as a reagent mean deionized or distilled chloric acid with warming on a hot plate. Dilute to 1000 mL
water conforming to Specification D 1193. with water and mix thoroughly. Filter this solution if it is
6.3 Aluminum Chloride Solution—Dissolve 453.6 g of cloudy. This solution should be prepared fresh daily.
AlCl ·6H O in water and dilute to a litre with water. 6.14 Water, distilled, reagent.
3 2
6.4 Aqua Regia—Mix three parts concentrated hydrochloric
7. Procedure
acid with one part concentrated nitric acid.
7.1 Calcination—The platinum level in reforming catalysts
6.5 Formic Acid (HCOOH).
is normally reported on a volatile-free basis. The loss on
6.6 Hydrochloric Acid (HCl), concentrated, specific gravity
ignition (LOI) determination (1000°C) is carried out sepa-
1.19.
rately, but weighed out at the same time as the ground sample
6.7 Hydrochloric Acid (HCl) Solution, 18 to 19 volume %
for digestion. Due to the hygroscopic nature of the sample,
or 6 N. Dilute 500 mL of concentrated hydrochloric acid to a
weigh by difference from a weighing vial. Weigh in triplicate 3
litre with water.
g 6 0.1-mg samples of reforming catalyst in platinum or
6.8 Hydrochloric Acid (HCl), 3.7 volume % or 1.2 N.
porcelain crucibles, place in a muffle furnace at 1000° 6 25°C,
Dilute 100 mL of concentrated hydrochloric acid to a litre with
and keep at this temperature for 3 h. Remove the crucible from
water.
the muffle and transfer to a desiccator, cool, and weigh 1 h after
6.9 Hydrogen Peroxide (H O ), or chlorine gas.
2 2
removal from the muffle. The desiccant to be loaded in the
6.10 Nitric Acid (HNO ), concentrated specific gravity
desiccator is freshly regenerated Type 4A molecular sieves.
1.42.
7.2 Digestion—Weigh a ground portion of catalyst into a
6.11 Platinum Wire, 99.99 % platinum purity.
600-mL beaker to c
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