ASTM D5404/D5404M-12(2017)
(Practice)Standard Practice for Recovery of Asphalt from Solution Using the Rotary Evaporator
Standard Practice for Recovery of Asphalt from Solution Using the Rotary Evaporator
SIGNIFICANCE AND USE
4.1 In order to determine the characteristics of the asphalt in an asphalt paving mixture, it is necessary to extract the asphalt from the aggregate by means of a suitable solvent and then to recover the asphalt from the solvent without significantly changing the asphalt's properties. The asphalt recovered from the solvent by this practice can be tested using the same methods as for the original asphalt cement, and comparisons between the properties of the original and recovered asphalt can be made.
Note 1: The quality of the results produced by this standard are dependent on the competence of the personnel performing the procedure and the capability, calibration, and maintenance of the equipment used. Agencies that meet the criteria of Specification D3666 are generally considered capable of competent and objective testing, sampling, inspection, etc. Users of this standard are cautioned that compliance with Specification D3666 alone does not completely ensure reliable results. Reliable results depend on many factors; following the suggestions of Specification D3666 or some similar acceptable guideline provides a means of evaluating and controlling some of those factors.
SCOPE
1.1 This practice 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 either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in nonconformance with the standard.
1.2.1 Residual pressure measurements are shown in both the SI unit of kPa and the commonly used non-standard equivalent unit of “mm of Hg.”
1.2.2 Measurements of volume and mass are only given in SI units because they are the only units typically used in practice when performing this standard practice.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Designation: D5404/D5404M − 12 (Reapproved 2017)
Standard Practice for
Recovery of Asphalt from Solution Using the Rotary
Evaporator
This standard is issued under the fixed designation D5404/D5404M; 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.
1. Scope D1856 Test Method for Recovery of Asphalt From Solution
by Abson Method
1.1 This practice is intended to recover asphalt from a
D2939 Test Methods for Emulsified Bitumens Used as
solvent using the rotary evaporator to ensure that changes in
Protective Coatings (Withdrawn 2012)
the asphalt properties during the recovery process are mini-
D3666 Specification for Minimum Requirements for Agen-
mized.
cies Testing and Inspecting Road and Paving Materials
1.2 The values stated in either SI units or inch-pound units
D6368 Specification for Vapor-Degreasing Solvents Based
are to be regarded separately as standard. The values stated in
on normal-Propyl Bromide and Technical Grade normal-
each system may not be exact equivalents; therefore, each
Propyl Bromide
system shall be used independently of the other. Combining
3. Summary of Practice
values from the two systems may result in nonconformance
with the standard.
3.1 The solution of solvent and asphalt from a prior extrac-
1.2.1 Residualpressuremeasurementsareshowninboththe
tion is distilled by partially immersing the rotating distillation
SI unit of kPa and the commonly used non-standard equivalent
flask of the rotary evaporator in a heated oil bath while the
unit of “mm of Hg.”
solution is subjected to a partial vacuum and a flow of nitrogen
1.2.2 Measurements of volume and mass are only given in
gas or carbon dioxide gas. The recovered asphalt can then be
SI units because they are the only units typically used in
subjected to testing as required.
practice when performing this standard practice.
4. Significance and Use
1.3 This standard does not purport to address all of the
4.1 In order to determine the characteristics of the asphalt in
safety concerns, if any, associated with its use. It is the
an asphalt paving mixture, it is necessary to extract the asphalt
responsibility of the user of this standard to establish appro-
from the aggregate by means of a suitable solvent and then to
priate safety, health, and environmental practices and deter-
recover the asphalt from the solvent without significantly
mine the applicability of regulatory limitations prior to use.
changing the asphalt’s properties. The asphalt recovered from
1.4 This international standard was developed in accor-
the solvent by this practice can be tested using the same
dance with internationally recognized principles on standard-
methods as for the original asphalt cement, and comparisons
ization established in the Decision on Principles for the
between the properties of the original and recovered asphalt
Development of International Standards, Guides and Recom-
can be made.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. NOTE 1—The quality of the results produced by this standard are
dependent on the competence of the personnel performing the procedure
2. Referenced Documents
and the capability, calibration, and maintenance of the equipment used.
2 Agencies that meet the criteria of Specification D3666 are generally
2.1 ASTM Standards:
considered capable of competent and objective testing, sampling,
D92 Test Method for Flash and Fire Points by Cleveland
inspection, etc. Users of this standard are cautioned that compliance with
Open Cup Tester
Specification D3666 alone does not completely ensure reliable results.
Reliable results depend on many factors; following the suggestions of
Specification D3666 or some similar acceptable guideline provides a
This practice is under the jurisdiction of ASTM Committee D04 on Road and
means of evaluating and controlling some of those factors.
Paving Materials and is the direct responsibility of Subcommittee D04.25 on
Analysis of Asphalt Mixtures.
5. Apparatus
Current edition approved Oct. 1, 2017. Published October 2017. Originally
approved in 1993. Last previous edition approved in 2012 as D5404/D5404M – 12.
5.1 Rotary Evaporator (see Fig. 1), equipped with a distil-
DOI: 10.1520/D5404_D5404M-12R17.
lation flask, a variable speed motor capable of rotating the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5404/D5404M − 12 (2017)
NOTE 1—It is important that the needle valve is located as shown instead of being placed ahead of the flowmeter.
FIG. 1 Rotary Evaporator and Recovery System
distillation flask at a rate of at least 50 rpm, condenser, solvent nical grade of trichloroethylene may be used, but it is recom-
recovery flask, and heated oil bath.The angle of the distillation mended that for each new supply of solvent, a blank should be
flaskfromthehorizontaltothebathissetatapproximately15°. run on an asphalt with known properties.
The distillation flask (Note 2), when fully immersed, should be
6.3.2 Normal Propyl Bromides (nPB)—The solvent for
at a depth of approximately 40 mm [1.5 in.].
extracting the asphalt from the mixtures should conform to
Specification D6368. Because there may be some interactions
NOTE 2—A flask having a 2000-mL capacity is recommended.
due to differences in nPB products, it is recommended that for
5.1.1 Thermometric Device—A built-in temperature mea-
a new supply of solvent, a blank should be run on an asphalt
surement device capable of displaying the oil temperatures to
with known properties.
the nearest 1 °C [2 °F].
5.2 ManometerorVacuumGage, suitable for measuring the
7. Precautions
specified vacuum.
7.1 Caution—Thesolventslistedin6.3shouldbeusedonly
5.3 GasFlowmeter,capableofindicatingagasflowofupto
under a hood or with an effective surface exhaust system in a
1000 mL/min.
well-ventilated area, since they are toxic to various degrees.
Consult the current Threshold Limit Concentration Committee
5.4 Sample Container, having adequate volume to hold the
of the American Conference of Governmental Industrial Hy-
sample and added solvent.
gienists for the current threshold limit values.
5.5 Vacuum System, capable of maintaining a vacuum to
7.2 These solvents in the presence of heat and moisture may
within 60.7 kPa [65 mm of Hg] of the desired level up to and
be hydrolyzed to form acids that are extremely corrosive to
including 80 kPa [600 mm of Hg].
certain metals, particularly when subject to contact over
5.6 Oven, capable of maintain a temperature of 165 65°C
lengthy periods of time. Proper precautions should be taken to
[329 6 10 °F].
not allow these solvents to remain in small quantities in the
effluent tanks of aluminum vacuum extractors
...
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.
Designation: D5404/D5404M − 12 D5404/D5404M − 12 (Reapproved 2017)
Standard Practice for
Recovery of Asphalt from Solution Using the Rotary
Evaporator
This standard is issued under the fixed designation D5404/D5404M; 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.
1. Scope
1.1 This practice 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 either SI units or inch-pound units are to be regarded separately as standard. The values stated in each
system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the
two systems may result in non-conformancenonconformance with the standard.
1.2.1 Residual pressure measurements are shown in both the SI unit of kPa and the commonly used non-standard equivalent
unit of “mm of Hg”.Hg.”
1.2.2 Measurements of volume and mass are only given in SI units because they are the only units typically used in practice
when performing this standard practice.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D92 Test Method for Flash and Fire Points by Cleveland Open Cup Tester
D1856 Test Method for Recovery of Asphalt From Solution by Abson Method
D2939 Test Methods for Emulsified Bitumens Used as Protective Coatings (Withdrawn 2012)
D3666 Specification for Minimum Requirements for Agencies Testing and Inspecting Road and Paving Materials
D6368 Specification for Vapor-Degreasing Solvents Based on normal-Propyl Bromide and Technical Grade normal-Propyl
Bromide
3. Summary of Practice
3.1 The solution of solvent and asphalt from a prior extraction is distilled by partially immersing the rotating distillation flask
of the rotary evaporator in a heated oil bath while the solution is subjected to a partial vacuum and a flow of nitrogen gas or carbon
dioxide gas. The recovered asphalt can then be subjected to testing as required.
4. Significance and Use
4.1 In order to determine the characteristics of the asphalt in an asphalt paving mixture, it is necessary to extract the asphalt
from the aggregate by means of a suitable solvent and then to recover the asphalt from the solvent without significantly changing
This practice is under the jurisdiction of ASTM Committee D04 on Road and Paving Materials and is the direct responsibility of Subcommittee D04.25 on Analysis of
BituminousAsphalt Mixtures.
Current edition approved June 1, 2012Oct. 1, 2017. Published May 2013October 2017. Originally approved in 1997.1993. Last previous edition approved in 20112012
as D5404/D5404M – 11.12. DOI: 10.1520/D5404_D5404M-12.10.1520/D5404_D5404M-12R17.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5404/D5404M − 12 (2017)
the asphalt’s properties. The asphalt recovered from the solvent by this practice can be tested using the same methods as for the
original asphalt cement, and comparisons between the properties of the original and recovered asphalt can be made.
NOTE 1—The quality of the results produced by this standard are dependent on the competence of the personnel performing the procedure and the
capability, calibration, and maintenance of the equipment used. Agencies that meet the criteria of Standard Practice Specification D3666 are generally
considered capable of competent and objective testing/sampling/inspection/etc. testing, sampling, inspection, etc. Users of this standard are cautioned that
compliance with PracticeSpecification D3666 alone does not completely assureensure reliable results. Reliable results depend on many factors; following
the suggestions of PracticeSpecification D3666 or some similar acceptable guideline provides a means of evaluating and controlling some of those factors.
5. Apparatus
5.1 Rotary Evaporator (see(see Fig. 1), equipped with a distillation flask, a variable speed motor capable of rotating the
distillation flask at a rate of at least 50 rpm, condenser, solvent recovery flask, and heated oil bath. The angle of the distillation
flask from the horizontal to the bath is set at approximately 15°. The distillation flask (Note 2), when fully immersed, should be
at a depth of approximately 40 mm [1.5 in.].
NOTE 2—A flask having a 2000 mL 2000-mL capacity is recommended.
5.1.1 Thermometric Device—A built-in temperature measurement device capable of displaying the oil temperatures to the
nearest 1°C [2°F].1 °C [2 °F].
5.2 Manometer or Vacuum Gage, suitable for measuring the specified vacuum.
5.3 Gas Flowmeter, capable of indicating a gas flow of up to 1000 mL/min.
5.4 Sample Container, having adequate volume to hold the sample and added solvent.
5.5 Vacuum System, capable of maintaining a vacuum to within 60.7 kPa [65 mm of Hg] of the desired level up to and
including 80 kPa [600 mm of Hg].
5.6 Oven, capable of maintain a temperature of 165 6 5°C5 °C [329 6 10°F].10 °F].
6. Reagents and Materials
6.1 Nitrogen Gas or Carbon Dioxide Gas—A pressurized tank with pressure-reducing valve, or other convenient source.
NOTE 3—Different flow rates may be required depending on whether nitrogen gas or carbon dioxide gas is used.
6.2 Oil—The oil for the heated oil bath should be USP White Oil or Silicone Fluid SWS-101 with flash point above 215°C
[420°F]215 °C [420 °F] or an equivalent. The flash point is determined in accordance with Test Method D92.
6.3 Solvents:
6.3.1 Trichloroethylene and Methylene Chloride—The solvent for extracting the asphalt from mixtures should be reagent grade
reagent-grade trichloroethylene or methylene chloride. A technical grade of trichloroethylene may be used, but it is recommended
that for each new supply of solvent, a blank should be run on an asphalt with known properties.
NOTE 1—It is important that the needle valve is located as shown instead of being placed ahead of the flowmeter.
FIG. 1 Rotary Evaporator and Recovery System
D5404/D5404M − 12 (2017)
6.3.2 Normal Propyl Bromides (nPB)—The solvent for extracting the asphalt from the mixtures should conform to Specification
D6368. Because there may be some interacti
...
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