ASTM D4893-94(1999)

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An American National Standard
Designation:D4893–94 (Reapproved 1999)
Standard Test Method for
Determination of Pitch Volatility
This standard is issued under the fixed designation D 4893; 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 proportional temperature controller regulates the heat input.
Two insulated handles are attached to this part for easy
1.1 This test method covers the determination of the percent
handling.An additional thermowell #2, located in the center of
of pitch volatility.
the block, accommodates another thermocouple used only for
1.2 Since this test method is empirical, strict adherence of
the determination of the rate of temperature rise of the pitch.
the procedure is necessary.
When the screw at the bottom of the #2 well is taken out, the
1.3 This standard does not purport to address all of the
thermocouple can then be pushed down and inserted in 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#3ofthebottomblock.Thereisaholeinthecenter
which the volatiles are swept away from the surface of the
of the bottom cylinder to accommodate the sample platform, a
liquid pitch by preheated nitrogen, the sample is taken out and
rod with a stainless steel disk welded to its top. The aluminum
allowed to cool down in the desiccator. The pitch volatility is
sample dish containing the sample rests on top of this disk
determined by the sample weight loss and reported as percent
during the test. The aluminum sample dish can be lifted out of
weight loss.
the cavity by raising the disk up to the upper rim of the cavity.
3. Significance and Use
4.2 Aluminum Weighing Dish.
4.3 Flowmeter, 0 to 25-cm /min range.
3.1 This test is useful in evaluating and characterizing pitch
4.4 Nitrogen Cylinder, equipped with a pressure regulator.
physical properties in comparing the consistency of shipments
4.5 Timer, with an alarm.
and sources of supply.
4.6 Aluminum Plate, 5-by-5-in., approximately 20-gage.
4. Apparatus
5. Dehydration of Sample
4.1 Aluminum Block, 4 ⁄2-in. outside diameter, composed
5.1 Hard Pitch—If the solid bulk sample contains free
of two sections (Figs. 1-4).
water, air-dry a representative portion in a forced-draft oven at
4.1.1 The top block is maintained at a chosen constant
50°C (122°F).
temperature according to the signal from the thermocouple
5.2 Soft Pitch (Softening Point <60°C (<140°F))—If the
inserted into the thermowell #1 near the center of the block.A
presence of water is indicated by surface foam on heating,
maintain a representative portion of the bulk sample at a
This test method is under the jurisdiction of ASTM Committee D-2 on temperature between 125 and 150°C (251 and 302°F) in an
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
open container until the surface is free of foam. Take care not
D02.05.OF on Industrial Pitches.
to overheat, and remove heat source immediately when foam
Current edition approved Nov. 15, 1994. Published January 1995. Originally
subsides.
published as D 4893 – 89. Last previous edition D 4893 – 89.
An aluminum block that may be obtained on special order from Koppers
Company, Inc., 1005 Wm. Pitt Way, Pittsburgh, PA 15238, has been found
satisfactory for this purpose; or drawings of block will be furnished by Koppers Fisher Catalog Number 08-732 or VWR Scientific Catalog Number 25433-008
upon request. has been found satisfactory for this purpose.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4893–94 (1999)
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. Preparation of Apparatus
rim of the bottom block. Place the aluminum sample dish
7.1 Assemble the apparatus so that the exit opening in the
containing the sample onto the sample p
...