Designation: D 255 – 92
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Method for
Steam Distillation of Bituminous Protective Coatings1
This standard is issued under the fixed designation D 255; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 3.3 Source of Heat for the bath, such as a gas burner,
1.1 This is a general method for the separation by steam electric hot plate, or the equivalent. An electric mantle type
distillation and the recovery of solvent and base from bitumi- heater, equipped with a variable resistance transformer of
nous mixtures. suitable size and heat capacity, is a suitable replacement for the
1.2 The following safety hazards caveat pertains only to the bath and heat source.
test methods described in this specification. This standard does 3.4 Distilling Flask, 1000-cm3, heat-resistant glass, with a
not purport to address all of the safety concerns, if any, short ring neck and round bottom. It shall be fitted with a
associated with its use. It is the responsibility of the user of this three-hole rubber stopper, a steam delivery tube that will reach
standard to establish appropriate safety and health practices to within 3⁄8 6 1⁄8 in. (9.5 6 4.7 mm) of the bottom of the flask
and determine the applicability of regulatory limitations prior and project from the top to a convenient distance for
to use. connection to the generator, a vapor outlet tube extending from
beneath the rubber stopper to a point sufficiently above the
2. Referenced Documents distilling flask to permit convenient connection to the
2.1 ASTM Standards: condenser, and a thermometer. The steam tubing shall be not
D 140 Practice for Sampling Bituminous Materials2 less than 2 nor more than 4 mm in internal diameter, and the
E 1 Specification for ASTM Thermometers3 vapor outlet tube shall be not less than 5 mm in internal
diameter.
3. Apparatus 3.5 Thermometer, ASTM Low Distillation, having a range
3.1 Steam Generator, made of either metal or glass, with a of − 2 to + 300°C (30 to 580°F), as specified, and conforming
capacity of approximately 2 gal (7600 cm3), suitable for to the requirements for thermometer 7C or 7F, respectively, as
continued use in the production of steam. If of glass, it shall be prescribed in Specification E 1.
fitted with two outlets having suitable connections for rubber 3.6 Condenser—A glass-jacketed condenser. The following
tubing. In the case of a metal generator, a large opening for dimensions are recommended:
filling and a water gage shall be additional parts of the Length of jacket, excluding the necks 250 6 5 mm
apparatus. The generator shall be supplied with suitable pinch- Length of condenser tube 400 6 25 mm
Outside diameter of condenser tube proper 12.5 6 0.5 mm
cocks or valves so that steam may be blown off to the
Outside diameter of expanded end of tube 23 6 1 mm
atmosphere until the test is ready. Length of expanded end of tube 75 6 1 mm
NOTE 1—The following conversion factors are given for volumetric 3.7 Adapter—A heavy-wall (1 mm) glass adapter, with
glassware graduated in litres:
reinforced top, having an angle of approximately 105°. The
1 L 5 1 dm3 or 1000 cm3 (1) inside diameter at the large end shall be approximately 18 mm
1 mL 5 1 cm 3 and at the small end, not less than 5 mm. The lower surface of
the adapter shall be on a smooth descending curve from the
3.2 Bath, made of metal and having sufficient capacity to larger end to the smaller. The inside line of the outlet end shall
permit immersion of the distilling flask to a depth of not less be vertical and the outlet shall be cut or ground (not fire-
than 4 in. (101.6 mm). polished) at an angle of 45 6 5° to the inside line.
3.8 Receiver—Graduated cylinders of uniform diameter,
with a pressed or molded base and a lipped top. The over-all
1
This method is under the jurisdiction of ASTM Committee D-8 on Roofing, height shall be 10 6 0.250 in. (254 6 6.35 mm). The cylinder
Waterproofing, and Bituminous Materials and is the direct responsibility of
Subcommittee D08.05 on Solvent-Bearing Bituminous Compounds for Roofing and shall be graduated in single millilitres to contain 100 cm3, and
Waterproofing. the graduated portion shall be 7.5 6 0.500 in. (190.5 6 12.70
Current edition approved April 15, 1992. Published June 1992. Originally mm) in length.
published as E 255 – 26. Last previous edition D 255 – 70(82)e1.
2
Annual Book of ASTM Standards, Vol 04.03. 3.9 Separatory Funnel—A separatory funnel having a
3
Annual Book of ASTM Standards, Vol 14.01. capacity of not less than 500 cm3.
1
D 255
4. Sampling Stop the distillation when 100 cm3 of total distillate contains
4.1 Take the samples for laboratory examination from the approximately 0.5 cm 3 of solvent or at a maximum sample
original containers immediately after stirring to a uniform temperature of 400°F (215°C).
condition. Determine the number of containers sampled to 5.2 Combine the total condensates in the separatory funnel
represent a shipment in accordance with Practice D 140. Restir and separate the water from the solvent by withdrawing the
this combined sample immediately before taking out portions lower aqueous phase. In some cases, the water and solvent may
for individual tests. not separate readily; separation can be facilitated by the
addition of sodium chloride, which will result in a sufficient
5. Procedure difference in gravity to produce a clear separation of the two
5.1 Assemble the apparatus as shown in Fig. 1. With layers. Transfer the solvent to clean 100-cm3 graduates. At a
atmospheric outlet open and steam delivery outlet closed, solvent temperature of 55 to 65°F (13 to 18°C), measure the
half-fill the steam generator with water and apply heat. total volume of solvent and record. Retain the solvent for any
Measure a 500 6 0.5-cm 3 sample into the distilling flask. subsequent testing required.
Calculate the weight of the sample, using its specific gravity at 5.3 If solvent and base are required on a mass percent basis,
60°F (15.6°C). Connect the steam generator to the steam determine the specific gravity of the solvent at 60°F (15.6°C).
delivery tube, the end of which shall be within 3⁄8 6 1⁄8 in. (9.5 6. Calculation
6 3.2 mm) of the bottom of the distilling flask. Connect the
6.1 Calculate the volume percent as follows:
outlet from the distilling flask to the condenser and turn on
cooling water. Adjust the adapter over the end of the condenser A 5 B/5 (2)
tube to conduct the distillate into the receiver and closely cover C 5 100 2 A
the top of the receiver during the distillation with a piece of
blotting paper or its equivalent, cut to fit the adapter tightly. where:
A 5 volume percent of solvent,
Extend the adapter into the receiver at least 1 in. (25.4 mm) but
B 5 cubic centimetres of separated solvent, and
not below the 100-cm3 mark. Immerse the receiver up to the C 5 volume percent of base.
100-cm3 mark in a transparent bath maintained between 55 and
6.2 Calculate the mass percent as follows:
65°F (13 and 18°C). Place the end of the bulb of the
thermometer in the distilling flask within 3⁄8 6 1⁄8 in. of the D 5 ~BE 3 100!/F (3)
bottom of the flask. Fill the bath with high-flash oil and apply G 5 100 2 D
heat. When the temperature of the sample in the distilling flask
reaches 266°F (130°C), simultaneously close the atmospheric where:
D 5 mass percent of solvent,
outlet of the steam generator and open the steam delivery outlet
B 5 cubic centimetres of separated solvent,
thus directing the steam to pass through the sample. Adjust the E 5 specific gravity of separated solvent at 60°F (15.6°C),
flow of steam so that the total condensate is collected at the rate F 5 grams of sample used, and
of 6 to 10 cm3/min. Collect successive 100-cm 3 increments of G 5 mass percent of base.
condensate. When 100 cm3 of total condensate contains
approximately 0.5 cm3 of solvent, or less, raise the sample 7. Report
temperature at a rate of 4 to 6°F (2.2 to 3.3°C)/min, 7.1 Report the results as volume percent or mass percent, of
maintaining total condensate rate by controlling steam flow. solvent or of base, as required.
FIG. 1 Assembly of Apparatus for Steam Distillation
2
D 255
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