Standard Test Method for Distillation of Pitch (Withdrawn 2006)

SCOPE
1.1 This test method covers a distillation test for pitch applicable whenever the amount of distillate below 270°C is less than 2.0% by this test method.  
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3  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.
WITHDRAWN RATIONALE
This test method covers a distillation test for pitch applicable whenever the amount of distillate below 270C is less than 2.0 % by this test method.
This test method is being withdrawn due to poor precision and a very broad repeatability and reproducibility.
Formerly under the jurisdiction of Committee D02 on Petroleum Products and Lubricants, this test method was withdrawn without replacement in August 2006.

General Information

Status
Withdrawn
Publication Date
09-Aug-1997
Withdrawal Date
26-Sep-2006
Current Stage
Ref Project

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ASTM D2569-97(2002)e1 - Standard Test Method for Distillation of Pitch (Withdrawn 2006)
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
An American National Standard
e1
Designation:D2569–97 (Reapproved 2002)
Standard Test Method for
Distillation of Pitch
This standard is issued under the fixed designation D2569; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Replaced the word “asbestos” in 8.1.1 editorially in August 2005.
1. Scope 5. Apparatus
1.1 This test method covers a distillation test for pitch 5.1 Flask—Aside-arm distillation flask, as shown in Fig. 1,
applicable whenever the amount of distillate below 270°C is having the following dimensions:
less than 2.0% by this test method.
Diameter of bulb, outside, mm 86.0 6 1.5
Diameter of neck, inside, mm 22.0 6 1.0
1.2 The values stated in SI units are to be regarded as the
Diameter of tubulature, inside, mm 10.06 0.5
standard. The values given in parentheses are for information
Height of flask, outside, mm 131.0 6 1.5
only.
Vertical distance, bottom of bulb, 93.0 6 1.5
outside, to horizontal tangent at
1.3 This standard does not purport to address all of the
tubulature, inside, mm
safety concerns, if any, associated with its use. It is the
Length of tubulature, mm 220 6 5
responsibility of the user of this standard to establish appro-
Angle of tubulature, ° 1.0 to 1.5
Thickness of tubulature wall, mm 75 6 2
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5.2 Condenser Tube—Atapered glass condenser, as shown
in Fig. 2, having the following dimensions:
2. Referenced Documents
Outside diameter of small end, mm 12.5 6 1.5
2.1 ASTM Standards:
Outside diameter of large end, mm 28.5 6 3.0
Length, mm 360 6 4
D140 Practice for Sampling Bituminous Materials
Length of tapered part, mm 100 6 5
E1 Specification for ASTM Thermometers
5.3 Source of Heat—Electric heater, 750-W, with variable
3. Summary of Test Method
transformer control as shown in Fig. 2, with a direct-reading
voltmeter(120V)orammeter(5A).Transformersettingsshall
3.1 A 100-g sample is distilled from an electrically heated
flask in a shield at a designated rate. The weight of distillate be reproducible within 2% on the percent input dial. The
heater shall be fitted with an upper refractory top, with the
fractions at specified temperatures and the time required to
collect the main fraction are recorded. dimensions shown in Fig. 3, and a 110-mm square plate of
6-mm thick non-asbestos containing cement board, having an
4. Significance and Use
80-mm center hole as shown in Fig. 4.
4.1 Inusualpractice,mostoftheoilsdistillingbelow360°C 5.4 Shield—A stainless steel shield with mica windows
are removed in the manufacture of high-softening-point lined with 3-mm thick high temperature cloth, provided with a
pitches. Excessive distillation in this range may indicate an two-piececoverof6-mmthicktransiteboard(non-asbestos)of
abnormalproductwhichcouldcausesomeproblemsoffuming the form and dimensions shown in Fig. 4.
and instability in use.
1 4
This test method is under the jurisdiction of ASTM Committee D02 on The Precision “Ful-Kontrol” heater meets these requirements; it can be
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee purchased through supply houses.
D02.05.OF on Industrial Pitches. The sole source of supply of the mica windows known to the committee at this
Current edition approved Apr. 10, 1997. Published October 1997. Originally time is Humboldt Mfg Co., Inc., 7302 W. Agatite Ave., Chicago, IL 60656. If you
published as D2569–67. Last previous edition D2569–91. are aware of alternative suppliers, please provide this information to ASTM
Annual Book of ASTM Standards, Vol 04.03. International Headquarters. Your comments will receive careful consideration at a
3 1
Annual Book of ASTM Standards, Vol 14.03. 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.
e1
D2569–97 (2002)
FIG. 1 Distillation Flask
FIG. 2 Apparatus Assembly for Pitch Distillation
FIG. 3 Upper Part of Electric Heater
5.5 Receivers—Erlenmeyer flasks or beakers, having a requirements for Thermometer 8C as prescribed in Specifica-
nominalcapacityof50to125mLandtaredtothenearest0.05 tion E1 or a suitable digital thermometer with the same
g. precision as 8C.
5.6 Thermometer—An ASTM High Distillation Thermom- 5.7 Timer—Stop clock or stop watch, calibrated in seconds
eter, having a range from−2 to 400°C and conforming to the or tenths.
e1
D2569–97 (2002)
8. Preparation of Apparatus
8.1 Assemble the apparatus shown in Fig. 2 as follows:
8.1.1 Place the refractory on the heater with the larger
opening facing upwards. Center the heat–resistant refractory
board plate with the hole on the refractory and place the
distillation shield on the plate.
8.1.2 Insert the thermometer through a new, rolled, tightly
fittingcorkintheneckoftheflask,withthebottomofthecork
24to27mmabovethelowestpointofthejuncturebetweenthe
side-arm tubulature and the neck of the flask. The top of the
thermometer bulb must be level with this point.Align the stem
of the thermometer on the axis of the bulb of the flask.
8.1.3 Place the flask within the shield so that it is seated in
the hole in the non-asbestos containing cement board, and
connect the condenser tube to the side arm of the flask with a
tightcorksothatthesidearmprojects30to50mmbeyondthe
cork.Thedistancefromtheneckoftheflasktotheoutletofthe
condenser tube shall be not more than 600 nor less than
500mm.Supporttheflaskandcondensertubesothatthelatter
is aligned with the side arm and the thermometer is vertical.
Place the cover on top of the shield around the neck of the
flask.
9. Procedure
9.1 Weigh 100 6 1 g of the sample into a tared distillation
flask. Assemble the apparatus as described in Section 8.
9.2 Set the control on the electric heater so that the sample
of pitch completely melts, but does not boil, in not less than
10 min nor more than 30 min. Reset the control to provide a
FIG. 4 Shield, Cover, and Non-Asbestos-Cement Plate
voltage or amperage reading which, in past experience on a
similar type of
...

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