ASTM D20-03(2009)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D20 − 03(Reapproved 2009)
Standard Test Method for
Distillation of Road Tars
ThisstandardisissuedunderthefixeddesignationD20;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
adoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope
Diameter of bulb, outside, mm 86.0 ± 1.5
Diameter of neck, inside, mm 22.0 ± 1.0
1.1 This test method covers the distillation of road tars.
Diameter of side-arm, inside, mm 10.0 ± 0.5
Height of flask, outside, mm 131.0 ± 1.5
1.2 The values stated in SI units are to be regarded as
Vertical distance, bottom of bulb, outside, to 93.0 ± 1.5
horizontal
standard. No other units of measurement are included in this
tangent at side-arm, inside, mm
standard.
Length of side-arm, mm 220 ± 5
Angle of side-arm, deg 75 ± 2
1.3 This standard does not purport to address all of the
Thickness of side-arm wall, mm 1.0 to 1.5
safety problems, if any, associated with its use. It is the
5.2 Condenser Tube—Atapered glass condenser, as shown
responsibility of the user of this standard to establish appro-
in Fig. 2 and Fig. 3, having the following dimensions:
priate safety and health practices and determine the applica-
Outside diameter of small end, mm 12.5 ± 1.5
bility of regulatory limitations prior to use.
Outside diameter of large end, mm 28.5 ± 3.0
Length, mm 360 ± 4
Length of uniformly tapered part, mm 100 ± 5
2. Referenced Documents
2 5.3 SourceofHeat—Aheatsourceconsistingofabunsenor
2.1 ASTM Standards:
meker-type burner (Note 1) or an electric heater. The electric
E1Specification for ASTM Liquid-in-Glass Thermometers
heater shall have an output variable of 750 W and an upper
refractorywithdimensionsasshowninFig.4.Thetemperature
3. Summary of Test Method
of the heater shall be controlled by a variable transformer or
3.1 A 100-g sample is distilled at a controlled rate from a
rheostat suitable for the voltage used, and shall be fitted with a
300-mL flask into tared receivers. The masses of distillate
clamp for mounting on a vertical support rod.
fractions at a series of specified temperatures and of residue at
NOTE 1—An artificial gas model used with natural gas has been found
themaximumspecifiedtemperaturearedetermined.Ifdesired,
to give a uniform and easily controlled source of heat.
the residue and distillates may be used for further testing.
5.4 Flask Shield and Cover for Flame Distillation—Asteel
shield (preferably stainless) lined with 3-mm Transite board,
4. Significance and Use
non-asbestos, with two-part cover made from 6-mm Transite
4.1 Thedistillationtestseparatestarintofractionsaccording
board of the form and dimensions shown in Fig. 5.
to a series of specified temperatures.
5.5 Flask Shield and Cover for Electric-Heater
Distillation—A steel shield (preferably stainless) fitted with
5. Apparatus
mica windows, and a cover of the same construction and
dimensions as those for flame distillation (5.4) except for the
5.1 Flask—Aside-arm distillation flask, as shown in Fig. 1,
height of the shield (see Fig. 6).
conforming to the following dimensions:
5.6 Gauze for Flame Distillation—Two sheets of 1.0-mm
opening wire gauze made of 0.56-mm diameter nickel-
1 chromium wire measuring a minimum of 125 mm in diameter
This method is under the jurisdiction of ASTM Committee D04 on Road and
Paving Materials and is the direct responsibility of Subcommittee D04.43 on
or (125 by 125-mm) square.
Specifications and Test for Tar and Tar Products.
Current edition approved Dec. 1, 2009. Published January 2010. Originally
approved in 1911. Last previous edition approved in 2003 as D20–03. DOI: The Precision Ful-Kontrol 750-W heater with built-in variable transformer
10.1520/D0020-03R09. control, available from Precision Scientific Co., Chicago, IL, has been found
For referenced ASTM standards, visit the ASTM website, www.astm.org, or satisfactory. This heater is only available for 115 V. 50/60 Hz. If you are aware of
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM alternative suppliers, please provide this information to ASTM International
Standards volume information, refer to the standard’s Document Summary page on Headquarters.Your comments will receive careful consideration at a meeting of the
the ASTM website. responsible technical committee, which you may attend.
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D20 − 03 (2009)
7.1.3 When using the flame distillation apparatus, place the
flask in the flask shield with its bulb resting on the gauze.
Positiontheburnersothatitisdirectlybeneaththepointwhere
the bulb of the flask contacts the gauze. If the electric heater is
used, place the flask in the flask shield and support the flask so
that its bottom is between 4 and 7 mm above the heating coils.
7.1.4 Connectthecondensertubetotheside-armoftheflask
withatightcorkjoint,havingtheside-armproject30to50mm
throughthecork.Thedistancefromtheneckoftheflasktothe
outlet end of the condenser tube shall be between 500 and 600
mm. Support the condenser tube in a position such that it is in
alignment with the side-arm of the flask, and the thermometer
FIG. 1 Distillation Flask
is vertical. Place the shield cover over the flask shield around
the neck of the flask.
8. Procedure
5.7 Burner Chimney for Flame Distillation—Construct a
8.1 Weigh the flask (along with the thermometer and cork)
cylindricalmetalshieldapproximately100mmhigh,95to105
tothenearest0.1gandthenweigh100.0 60.1gofthesample
mm in diameter, and having a peephole 25 mm in diameter
into the flask.
centered about 32 mm below the ring support. The top of the
shield shall be flanged to permit its being suspended from the
8.2 Apply heat to the flask so that the first drop of distillate
ring support. (oil or water) falls from the end of the condenser tube in 5 to
15 min. Within 2 min after the first drop, adjust the rate of
5.8 Receivers—Erlenmeyerflasksorbeakershavinganomi-
distillation,andsubsequentlymaintaintherate,sothatfrom50
nal capacity of 50 to 125 mL, and tared to the nearest 0.1 g.
to 70 drops per min fall from the end of the condenser. Warm
5.9 Balance and Masses, accurate to 0.1 g.
the condenser tube whenever necessary to prevent accumula-
5.10 Thermometer—AnASTMHighDistillationThermom- tion of solid distillates in the tube.
eterhavingarangefrom−2to+400°Candconformingtothe
8.3 Collect the distillate fractions in tared receivers, chang-
requirements for Thermometer 8C as prescribed in Specifica-
ing receivers as the thermometer indicates the maximum
tion E1.
temperature, corrected as described in 8.4, for each specified
fraction. The following fractions are usually specified.
6. Preparation of Sample
Up to 170°C
6.1 Thoroughly stir or otherwise mix the sample immedi- 170 to 235°C
235 to 270°C
ately before removing the portion for testing, to ensure that
270 to 300°C
suchportionwillberepresentativeofthesample.Ifwarmingis
Residue at 300°C
necessary, take care to avoid loss of volatile material.
Fractions at other temperatures, such as 170 to 200°C and
200 to 235°C, or 300 to 355°C and residue at 355°C, are
7. Preparation of Apparatus
sometimes required.
7.1 Assemble the apparatus as follows (see Fig.
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