Standard Test Method for Determination of Pitch Volatility

SIGNIFICANCE AND USE
3.1 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.  
1.3.1 Exceptions—The diameter of a special aluminum block is measured in inches.  
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
´1
Designation: D4893 − 94 (Reapproved 2015)
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.
ε NOTE—SI units formatting was corrected editorially in May 2015.
1. Scope 4. Apparatus
1.1 This test method covers the determination of the percent 4.1 Aluminum Block, 4 ⁄2 in. outside diameter, composed of
of pitch volatility. two sections (Figs. 1-4).
4.1.1 The top block is maintained at a chosen constant
1.2 Since this test method is empirical, strict adherence to
temperature according to the signal from the thermocouple
the procedure is necessary.
inserted into the thermowell No. 1 near the center of the block.
1.3 The values stated in SI units are to be regarded as the
A proportional temperature controller regulates the heat input.
standard. The values in parentheses are given for information
Two insulated handles are attached to this part for easy
only.
handling.An additional thermowell No. 2, located in the center
1.3.1 Exceptions—The diameter of a special aluminum
of the block, accommodates another thermocouple used only
block is measured in inches.
for the determination of the rate of temperature rise of the
1.4 This standard does not purport to address all of the pitch. When the screw at the bottom of the No. 2 well is taken
safety concerns, if any, associated with its use. It is the out, the thermocouple can then be pushed down and inserted in
responsibility of the user of this standard to establish appro- pitch.
priate safety and health practices and determine the applica- 4.1.2 The bottom block has a cavity for the aluminum
bility of regulatory limitations prior to use. weighingdish.Aspiralchannelcutaroundtheperipheryofthis
part serves for preheating the nitrogen introduced at the
2. Summary of Test Method
measured rate (10 cm /min) into the block for purging vola-
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
4.2 Aluminum Weighing Dish.
physical properties in comparing the consistency of shipments
3 3
and sources of supply.
4.3 Flowmeter,0cm /min to 25 cm /min range.
An aluminum block that may be obtained on special order from Koppers
This test method is under the jurisdiction of ASTM Committee D02 on Company, Inc., 1005 Wm. Pitt Way, Pittsburgh, PA 15238, has been found
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of satisfactory for this purpose; or drawings of block will be furnished by Koppers
SubcommitteeD02.05onPropertiesofFuels,PetroleumCokeandCarbonMaterial. upon request. If you are aware of alternative suppliers, please provide this
Current edition approved April 1, 2015. Published May 2015. Originally information to ASTM International Headquarters. Your comments will receive
approved in 1989. Last previous edition approved in 2009 as D4893 – 94 (2009). careful consideration at a meeting of the responsible technical committee, which
DOI: 10.1520/D4893-94R15E01. you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D4893 − 94 (2015)
FIG. 1 Schematic of the Volatility Apparatus
4.4 Nitrogen Cylinder, equipped with a pressure regulator. 7. Preparation of Apparatus
4.5 Timer, with an alarm. 7.1 Assemble the apparatus so that the exit opening in the
upper block is aligned with bottom nitrogen inlet fitting of the
4.6 Aluminum Plate, 127 mm by 127 mm, approximately
bottom block. Both top and bottom blocks are heated to the test
20-gauge.
temperature, 350 °C (662 °F), using the proportional tempera-
ture controllers.Avoid heating the upper block and lower block
5. Dehydration of Sample
when separated from each other.
5.1 Hard Pitch—If the solid bulk sample contains free
water, air-dry a representative portion in a forced-draft oven at
8. Procedure
50 °C (122 °F).
8.1 Weigh 15 g of prepared sample into a tared aluminum
5.2 Soft Pitch (Softening Point <60 °C (<140 °F ))—If the
weighing dish with precision of 0.1 mg.
presence of water is indicated by surface foam on heating,
8.2 Start nitrogen purge system at a rate 10 cm /min 6
maintain a representative portion
...


This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D4893 − 94 (Reapproved 2009) D4893 − 94 (Reapproved 2015)
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.
ε NOTE—SI units formatting was corrected editorially in May 2015.
1. 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.
1.3.1 Exceptions—The diameter of a special aluminum block is measured in inches.
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.
2. Summary of Test Method
2.1 An aluminum weighing dish with about 15 g 15 g of specimen is introduced into the cavity of a metal block heated and
maintained at 350°C (662°F). After 30 min 6 10 s 350 °C (662 °F). After 30 min 6 10 s during which the volatiles are swept away
from the surface of the liquid pitch by preheated nitrogen, the sample is taken out and allowed to cool down in the desiccator. The
pitch volatility is determined by the sample weight loss and reported as percent weight loss.
3. Significance and Use
3.1 This test is useful in evaluating and characterizing pitch physical properties in comparing the consistency of shipments and
sources of supply.
4. Apparatus
4.1 Aluminum Block, 4 ⁄2-in. in. outside diameter, composed of two sections (Figs. 1-4).
4.1.1 The top block is maintained at a chosen constant temperature according to the signal from the thermocouple inserted into
the thermowell No. 1 near the center of the block. A proportional temperature controller regulates the heat input. Two insulated
handles are attached to this part for easy handling. An additional thermowell No. 2, located in the center of the block,
accommodates another thermocouple used only for the determination of the rate of temperature rise of the 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 pitch.
4.1.2 The bottom block has a cavity for the aluminum weighing dish. A spiral channel cut around the periphery of this part
serves for preheating the nitrogen introduced at the measured rate (10 cm(10 cm /min) into the block for purging volatiles.
4.1.3 The test temperature, the same as that in the top block, is maintained by the second proportional temperature controller
according to the signals of a thermocouple inserted in a thermowell No. 3 of the bottom block. There is a hole in the center of the
bottom cylinder to accommodate the sample platform, a rod with a stainless steel disk welded to its top. The aluminum sample
dish containing the sample rests on top of 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 of the cavity.
4.2 Aluminum Weighing Dish.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.
Current edition approved Oct. 1, 2009April 1, 2015. Published November 2009May 2015. Originally approved in 1989. Last previous edition approved in 20042009 as
D4893–94(2004).D4893 – 94 (2009). DOI: 10.1520/D4893-94R09.10.1520/D4893-94R15E01.
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 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 you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D4893 − 94 (2015)
FIG. 1 Schematic of the Volatility Apparatus
3 3
4.3 Flowmeter, 00 cm /min to 25-cm25 cm /min range.
4.4 Nitrogen Cylinder, equipped with a pressure regulator.
4.5 Timer, with an alarm.
4.6 Aluminum Plate, 5-by-5-in., approximately 20-gage.127 mm by 127 mm, approximately 20-gauge.
5. Dehydration of Sample
5.1 Hard Pitch—If the solid bulk sample contains free water, air-dry a representative portion in a forced-draft oven at 50°C
(122°F).50 °C (122 °F).
5.2 Soft Pitch (Softening Point <60°C<60 °C (<140°F<140 °F ))—If the presence of water is indicated by surface foam on
heating, maintain a representative portion of the bulk sample at a temperature between 125125 °C and 150°C (251150 °C (251 °F
and 302°F)302 °F) in an open container until the surface is free of foam. Take care not to overheat, and remove heat source
immediately when foam subsides.
6. Preparation of Working Sample
6.1 Crush sample to pass No. 4 mesh (4760 μm). (4760 μm).
7. Preparation of Apparatus
7.1 Assemble the apparatus so that the exit open
...

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