ASTM D5404-97

Standard Practice for Recovery of Asphalt from Solution Using the Rotary Evaporator

SCOPE
1.1 This test method is intended to recover asphalt from a solvent using the rotary evaporator to ensure that changes in the asphalt properties during the recovery process are minimized.
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.

General Information

• Status: Historical
• Publication Date: 09-Feb-2002
• ICS: 91.100.50 - Binders. Sealing materials
• ICS: 93.080.20 - Road construction materials
• Technical Committee: D04 - Road and Paving Materials
• Drafting Committee: D04.25 - Analysis of Asphalt Mixtures

Relations

• Replaced By: ASTM D5404-02 - Standard Practice for Recovery of Asphalt from Solution Using the Rotary Evaporator
• Effective Date: 10-Feb-2002

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5404 – 97
Standard Practice for
Recovery of Asphalt from Solution Using the Rotary
Evaporator
This standard is issued under the fixed designation D 5404; 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.
1. Scope 4. Significance and Use
1.1 This practice is intended to recover asphalt from a 4.1 In order to determine the characteristics of the asphalt in
solvent using the rotary evaporator to ensure that changes in an asphalt paving mixture, it is necessary to extract the asphalt
the asphalt properties during the recovery process are mini- from the aggregate by means of a suitable solvent and then to
mized. recover the asphalt from the solvent without significantly
1.2 The values stated in SI units are to be regarded as the changing the asphalt’s properties. The asphalt recovered from
standard. The values given in parentheses are provided for the solvent by this practice can be tested using the same
information only. methods as for the original asphalt cement, and comparisons
1.3 This standard does not purport to address all of the between the properties of the original and recovered asphalt
safety concerns, if any, associated with its use. It is the can be made.
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
5.1 Rotary Evaporator (see Fig. 1), equipped with a distil-
bility of regulatory limitations prior to use.
lation flask, a variable speed motor capable of rotating the
2. Referenced Documents
distillation flask at a rate of at least 50 rpm, condenser, solvent
2.1 ASTM Standards: recovery flask, and heated oil bath. The angle of the distillation
D 92 Test Method for Flash and Fire Points by Cleveland flask from the horizontal to the bath is set at approximately 15°.
Open Cup The distillation flask (Note 1), when fully immersed, should be
D 1856 Test Method for Recovery of Asphalt from Solution at a depth of approximately 40 mm (1.5 in.).
by Abson Method
NOTE 1—A flask having a 2000 mL capacity is recommended.
D 2939 Test Methods for Emulsified Bitumens Used as
5.2 Manometer or Vacuum Gage, suitable for measuring the
Protective Coatings
specified vacuum.
2.2 Federal Specification:
5.3 Gas Flowmeter, capable of indicating a gas flow of up to
O-T-634 (latest) Trichloroethylene, Technical
1000 mL/min.
3. Summary of Practice
5.4 Sample Container, having adequate volume to hold the
sample and added solvent.
3.1 The solution of solvent and asphalt from a prior extrac-
5.5 Vacuum System, capable of maintaining a vacuum to
tion is distilled by partially immersing the rotating distillation
within 60.7 kPa (65 mm Hg) of the desired level up to and
flask of the rotary evaporator in a heated oil bath while the
including 80 kPa (600 mm Hg).
solution is subjected to a partial vacuum and a flow of nitrogen
gas or carbon dioxide gas. The recovered asphalt can then be
6. Reagents and Materials
subjected to testing as required.
6.1 Nitrogen Gas or Carbon Dioxide Gas—A pressurized
tank with pressure-reducing valve, or other convenient source.
NOTE 2—Different flow rates may be required depending on whether
nitrogen gas or carbon dioxide gas is used.
This practice is under the jurisdiction of ASTM Committee D-4 on Road and
Paving Materials and is the direct responsibility of Subcommittee D04.25 on 6.2 Oil—The oil for the heated oil bath should be USP
Analysis of Bituminous Mixtures.
White Oil or Silicone Fluid SWS-101 with flash point above
Current edition approved April 10, 1997. Published May 1998. Last previous
215°C (420°F) or an equivalent. The flash point is determined
edition D 5404 – 93.
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 04.03.
4 6
Annual Book of ASTM Standards, Vol 04.04. The Buchi Rotavapor RE-111A, or its equivalent, has been found satisfactory
Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 for this purpose. The Buchi Rotavapor is available from Fischer Scientific,
Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. Pittsburgh, PA.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5404
9.2 Apply a vacuum of 5.3 6 0.7 kPa (40 6 5mmHg)
below atmospheric pressure and draw approximately 600 mL
of asphalt solution from the sample container into the distilla-
tion flask by way of the sample line. Begin a nitrogen or carbon
dioxide flow of approximately 500 mL/min through the system
(Note 3). Begin rotating the distillation flask (at approximately
40 rpm) and lower the flask into the oil bath. Initially the
immersion depth of the flask will be determined by the need to
achieve a controlled solvent evaporation rate. The correct rate
of evaporation can be observed as a steady controlled stream of
condensed solvent being collected in the recovery flask.
FIG. 1 Rotary Evaporator and Recovery System
NOTE 3—The vacuum and nitrogen or carbon dioxide flow values may
need to be adjusted depending on the location. Also, low flow values are
recommended at the beginning of the rotary process when the sample
in accordance with Test Method D 92.
volume is large because of the possibility of back flow into the vacuum
6.3 Solvent—The solvent for extracting the asphalt from system. The possibility of back flow can also be minimized by regulating
the depth of immersion of the flask.
mixtures should be reagent grade trichloroethylene or meth-
ylene chloride.
9.3 When the amount of asphalt solution within the distil-
lation flask appears low enough so that more solution may be
7. Precautions
added, discontinue the nitrogen or carbon dioxide flow. Draw
7.
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