ASTM D4893-94(2004)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4893–94 (Reapproved 2004)
Standard Test Method for
Determination of Pitch Volatility
This standard is issued under the fixed designation D4893; 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 inserted into the thermowell No. 1 near the center of the block.
A proportional temperature controller regulates the heat input.
1.1 This test method covers the determination of the percent
Two insulated handles are attached to this part for easy
of pitch volatility.
handling.An additional thermowell No. 2, located in the center
1.2 Since this test method is empirical, strict adherence to
of the block, accommodates another thermocouple used only
the procedure is necessary.
for the determination of the rate of temperature rise of the
1.3 The values stated in SI units are to be regarded as the
pitch. When the screw at the bottom of the No. 2 well is taken
standard.
out, the thermocouple can then be pushed down and inserted in
1.4 This standard does not purport to address all of the
pitch.
safety concerns, if any, associated with its use. It is the
4.1.2 The bottom block has a cavity for the aluminum
responsibility of the user of this standard to establish appro-
weighingdish.Aspiralchannelcutaroundtheperipheryofthis
priate safety and health practices and determine the applica-
part serves for preheating the nitrogen introduced at the
bility of regulatory limitations prior to use.
measured rate (10 cm /min) into the block for purging vola-
2. Summary of Test Method tiles.
4.1.3 The test temperature, the same as that in the top block,
2.1 An aluminum weighing dish with about 15 g of speci-
is maintained by the second proportional temperature control-
men is introduced into the cavity of a metal block heated and
ler according to the signals of a thermocouple inserted in a
maintained at 350°C (662°F). After 30 min 6 10 s during
thermowell No. 3 of the bottom block. There is a hole in the
which the volatiles are swept away from the surface of the
center of the bottom cylinder to accommodate the sample
liquid pitch by preheated nitrogen, the sample is taken out and
platform, a rod with a stainless steel disk welded to its top.The
allowed to cool down in the desiccator. The pitch volatility is
aluminum sample dish containing the sample rests on top of
determined by the sample weight loss and reported as percent
this disk during the test. The aluminum sample dish can be
weight loss.
lifted out of the cavity by raising the disk up to the upper rim
3. Significance and Use
of the cavity.
4.2 Aluminum Weighing Dish.
3.1 This test is useful in evaluating and characterizing pitch
4.3 Flowmeter, 0 to 25-cm /min range.
physical properties in comparing the consistency of shipments
4.4 Nitrogen Cylinder, equipped with a pressure regulator.
and sources of supply.
4.5 Timer, with an alarm.
4. Apparatus
4.6 Aluminum Plate, 5-by-5-in., approximately 20-gage.
4.1 Aluminum Block, 4 ⁄2-in. outside diameter, composed
5. Dehydration of Sample
of two sections (Figs. 1-4).
5.1 Hard Pitch—If the solid bulk sample contains free
4.1.1 The top block is maintained at a chosen constant
water, air-dry a representative portion in a forced-draft oven at
temperature according to the signal from the thermocouple
50°C (122°F).
5.2 Soft Pitch (Softening Point <60°C (<140°F))—If the
This test method is under the jurisdiction of ASTM Committee D02 on
presence of water is indicated by surface foam on heating,
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
maintain a representative portion of the bulk sample at a
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Nov. 1, 2004. Published November 2004. Originally
temperature between 125 and 150°C (251 and 302°F) in an
approved in 1989. Last previous edition approved in 1999 as D4893 – 94 (1999).
open container until the surface is free of foam. Take care not
DOI: 10.1520/D4893-94R04.
2 to overheat, and remove heat source immediately when foam
An aluminum block that may be obtained on special order from Koppers
Company, Inc., 1005 Wm. Pitt Way, Pittsburgh, PA 15238, has been found subsides.
satisfactory for this purpose; or drawings of block will be furnished by Koppers
upon request. If you are aware of alternative suppliers, please provide this
information to ASTM International Headquarters. Your comments will receive
careful consideration at a meeting of the responsible technical committee , which Fisher Catalog Number 08-732 or VWR Scientific Catalog Number 25433-008
you may attend. has been found satisfactory for this purpose.
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D4893–94 (2004)
FIG. 1 Schematic of the Volatility Apparatus
6. Preparation of Working Sample 8.4 Remove top block. Raise the sample platform up
slightly above the rim of heating cavity and support with the
6.1 Crush sample to pass No. 4 mesh (4760 µm).
aluminum plate inserted between the sample platform and top
7. P
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