ASTM D4893-94(2009)
(Test Method)Standard Test Method for Determination of Pitch Volatility
Standard Test Method for Determination of Pitch Volatility
SIGNIFICANCE AND USE
This test is useful in evaluating and characterizing pitch physical properties in comparing the consistency of shipments and sources of supply.
SCOPE
1.1 This test method covers the determination of the percent of pitch volatility.
1.2 Since this test method is empirical, strict adherence to the procedure is necessary.
1.3 The values stated in SI units are to be regarded as the standard. The values in parentheses are given for information only.
1.4 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.
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Designation: D4893 − 94(Reapproved 2009)
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 4.1.1 The top block is maintained at a chosen constant
temperature according to the signal from the thermocouple
1.1 This test method covers the determination of the percent
inserted into the thermowell No. 1 near the center of the block.
of pitch volatility.
A proportional temperature controller regulates the heat input.
1.2 Since this test method is empirical, strict adherence to
Two insulated handles are attached to this part for easy
the procedure is necessary.
handling.An additional thermowell No. 2, located in the center
1.3 The values stated in SI units are to be regarded as the of the block, accommodates another thermocouple used only
standard. The values in parentheses are given for information for the determination of the rate of temperature rise of the
only.
pitch. When the screw at the bottom of the No. 2 well is taken
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-
priate safety and health practices and determine the applica- weighingdish.Aspiralchannelcutaroundtheperipheryofthis
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.
2.1 An aluminum weighing dish with about 15 g of speci-
4.1.3 The test temperature, the same as that in the top block,
men is introduced into the cavity of a metal block heated and
is maintained by the second proportional temperature control-
maintained at 350°C (662°F). After 30 min 6 10 s during
ler according to the signals of a thermocouple inserted in a
which the volatiles are swept away from the surface of the
thermowell No. 3 of the bottom block. There is a hole in the
liquid pitch by preheated nitrogen, the sample is taken out and
center of the bottom cylinder to accommodate the sample
allowed to cool down in the desiccator. The pitch volatility is
platform, a rod with a stainless steel disk welded to its top.The
determined by the sample weight loss and reported as percent
aluminum sample dish containing the sample rests on top of
weight loss.
this disk during the test. The aluminum sample dish can be
lifted out of the cavity by raising the disk up to the upper rim
3. Significance and Use
of the cavity.
3.1 This test is useful in evaluating and characterizing pitch
physical properties in comparing the consistency of shipments 4.2 Aluminum Weighing Dish.
and sources of supply.
4.3 Flowmeter, 0 to 25-cm /min range.
4. Apparatus
4.4 Nitrogen Cylinder, equipped with a pressure regulator.
4.1 Aluminum Block, 4 ⁄2-in. outside diameter, composed of
4.5 Timer, with an alarm.
two sections (Figs. 1-4).
4.6 Aluminum Plate, 5-by-5-in., approximately 20-gage.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
5. Dehydration of Sample
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Oct. 1, 2009. Published November 2009. Originally
5.1 Hard Pitch—If the solid bulk sample contains free
approved in 1989. Last previous edition approved in 2004 as D4893–94(2004).
DOI: 10.1520/D4893-94R09. water, air-dry a representative portion in a forced-draft oven at
An aluminum block that may be obtained on special order from Koppers
50°C (122°F).
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
5.2 Soft Pitch (Softening Point <60°C (<140°F ))—If the
upon request. If you are aware of alternative suppliers, please provide this
presence of water is indicated by surface foam on heating,
information to ASTM International Headquarters. Your comments will receive
maintain a representative portion of the bulk sample at a
careful consideration at a meeting of the responsible technical committee, which
you may attend. temperature between 125 and 150°C (251 and 302°F) in an
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4893 − 94 (2009)
FIG. 1 Schematic of the Volatility Apparatus
open container until the surface is free of foam. Take care not 8. Procedure
to overheat, and remove heat source immediately when foam
8.1 Weigh 15 g of prepared sample into a tared aluminum
subsides.
weighing dish with precision of 0.1 mg.
8.2 Start nitrogen purge system at a rate 10 cm /min 6 0.1
6. Preparation of Working Sample
cm /min (10 mL/min 6 0.1 mL/min).
6.1 Crush sample to pass No. 4 mesh (4760 µm).
8.3 Place top block onto bottom block, align the nitrogen
7. Preparation of App
...
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