Designation: D 1856 – 95a (Reapproved 2003)

Standard Test Method for

Recovery of Asphalt From Solution by Abson Method1
This standard is issued under the fixed designation D 1856; 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 test method covers the recovery by the Abson 4.1 The asphalt should be extracted from the aggregate-
method of asphalt from a solution from a previously conducted asphalt mixture in accordance with Method A of Test Methods
extraction. The asphalt is recovered with properties substan- D 2172 (centrifuge method) as there is some experimental
tially the same as those it possessed in the bituminous mixture evidence that the recovered asphalt may have slightly lower
and in quantities sufficient for further testing. penetration values when recovered from solutions obtained
1.2 This standard does not purport to address all of the from hot extraction methods.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5. Apparatus
priate safety and health practices and determine the applica- 5.1 Centrifuge, batch unit capable of exerting a minimum
bility of regulatory limitations prior to use. centrifugal force of 770 times gravity,4 or continuous unit
capable of exerting a minimum force of 3000 times gravity.
2. Referenced Documents (The apparatus specified in Test Methods D 96 may also be
2.1 ASTM Standards: 2 used.)
C 670 Practice for Preparing Precision and Bias Statements 5.2 Centrifuge Tubes—A supply of wide-mouth bottles or
for Test Methods for Construction Materials centrifuge tubes as shown in Fig. 1 or Fig. 2 of Test Methods
D 96 Test Methods for Water and Sediment in Crude Oil by D 96.
Centrifuge Method (Field Procedure)3 5.3 Distillation Assembly, as shown in Fig. 1, and consisting
D 2172 Test Methods for Quantitative Extraction of Bitu- of the following items:
men from Bituminous Paving Mixtures 5.3.1 Extraction Flasks—Two 250-ml, wide-mouth, heat-
D 2939 Test Methods for Emulsified Bitumens Used as resistant flasks, one for distillation and the other for the
Protective Coatings receiver.
E 1 Specification for ASTM Liquid-in-Glass Thermometers 5.3.2 Glass Tubing—Heat-resistant glass tubing, having
10-mm inside diameter and gooseneck shaped (as shown in
3. Summary of Test Method Fig. 1) for connecting the flask to the condenser.
3.1 The solution of solvent and asphalt from a prior extrac- 5.3.3 Inlet Aeration Tube,5 at least 180 mm in length,
tion is distilled under prescribed conditions to a point where having a 6-mm outside diameter with a 10-mm bulb carrying
most of the solvent has been distilled, at which time carbon six staggered side holes approximately 1.5 mm in diameter.
dioxide gas is introduced into the distillation process to remove 5.3.4 Electric Heating Mantle, with variable transformer, oil
all traces of the extraction solvent. The recovered asphalt bath, or fluidized sand bath, to fit a 250-ml flask.
(distillation residue) can then be subjected to further testing as 5.3.5 Water-Jacketed Condenser, Allihn type, with 200-mm
required. minimum jacket length or equivalent.
5.3.6 Thermometer—An ASTM Low Distillation Ther-
mometer 7E or 7F, as specified, having a range from −2 to
1
This method is under the jurisdiction of ASTM Committee D04 on Road and 300°C or 30 to 580°F, respectively, and conforming to the
Paving Materials and is the direct responsibility of Subcommittee D04.25 on
Analysis of Bituminous Mixtures. requirements in Specification E 1.
Current edition approved Dec. 1, 2003. Published January 2004. Originally
approved in 1961. Last previous edition approved in 1995 as D 1852 – 95a.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or An “International” No. 2 centrifuge operating at 1900 rpm or an “SMM
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Continuous Centrifuge” exerting a force of 3000 times gravity at 9000 rpm, have
Standards volume information, refer to the standard’s Document Summary page on been found satisfactory for this purpose.
5
the ASTM website. Inlet Aeration Tube, Part No. 226, available from Wm. A. Sales, Ltd., 419
3
Withdrawn. Harvester Court, Wheeling, Ill. 60090; request Part No. 226.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 D 1856 – 95a (2003)

FIG. 1 Distillation Assembly for Bitumen Recovery

5.3.7 Gas Flowmeter,6 as shown in Fig. 1, or any flowmeter Cincinnati, OH 45211-4438. 1990/1991 values. The TLV is a time weighted
average for an exposure period of 8 h per day, 5 days per week.
capable of indicating a gas flow of up to 1000 ml/min. B
Short term exposure limit (STEL) as established by ACGIH. 1990/1991 values.
5.3.8 Corks, No. 20, drilled as shown in Fig. 1.
5.3.9 Flexible Elastomeric Tubing, resistant to chlorinated
8. Sample
solvents having sufficient length and size to connect the
aeration tube to flowmeter, and equipped with a pinch clamp or 8.1 The sample shall consist of the solution from a previous
stopcock to close aeration tube prior to introducing carbon extraction by Method A of Test Methods D 2172 of asphalt-
dioxide. aggregate mixture of sufficient quantity to result in 75 to 100 g
5.3.10 Separatory Funnel,7 (Alternative Procedure, see of recovered bitumen. More or less quantities of bitumen may
9.3.1) 125-ml capacity. be recovered; however, the properties of the recovered bitumen
may not be in agreement with those recovered of the afore-
6. Reagents and Materials mentioned quantities, and in case of a disagreement, 75 to 100
6.1 Carbon Dioxide Gas—A pressurized tank, with g should be recovered.
pressure-reducing valve or other convenient source. 8.2 During the extraction process, it is important that all of
6.2 The solvent for extracting the asphalt from mixtures the asphalt in the mixture be extracted as there could be some
should be reagent grade trichloroethylene.8 selective solvency of the asphalt and the harder, more viscous
components of the asphalt might be left in the mixture if
7. Precautions extraction is not carried to completion.
7.1 Caution—The solvent listed in 6.2 should be used only 8.3 Since heavy petroleum distillates such as mineral spirits
under a hood or with an effective surface exhaust system in a or kerosine will affect the properties of the recovered asphalt,
well-ventilated area, since it is toxic to some degree as it is important to avoid the use of such solvents in cleaning the
indicated below: extraction and recovery apparatus and use only trichloroethyl-
Solvent TLV, ppmA STEL, ppmB ene for cleaning. Residues of heavy petroleum solvents on the
Trichloroethylene 50 200 equipment may contaminate the recovered asphalt and affect its
_________
A
test properties. It is also necessary to use new filter rings, clean
Threshold limit value (TLV) as established by the American Conference of
Governmental Industrial Hygienists (ACGIH), Bldg. D-7, 6500 Glenway Ave.,
felt pads, or other uncontaminated filtering media in the
extraction process to avoid contamination from a previous
extraction.
6
The Monostat Corp. “Flowmeter” No. 9144 has been found satisfactory for this 8.4 Generally, the bitumen in mixtures will progressively
purpose. harden when exposed to air, particularly if the mixtures are in
7
Kimball separatory funnel No. 29028 has been found satisfactory for this a loose condition. Therefore, it is important to protect bitumi-
purpose.
8
Trichloroethylene, Technical Grade, Type I, Federal Specification O-T-634,
nous mixtures from exposure to air and preferably to store
latest revision may be used, but it is recommended that for each new supply of the them in airtight containers at a temperature below 0°C (32°F)
solvent a blank should be run on an asphalt of known properties. until they can be tested. When samples of bituminous mixture

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 D 1856 – 95a (2003)
are warmed for preparing representative proportions for extrac- contact with the bottom of the flask and introduce carbon
tion tests in accordance with Method A of Test Methods dioxide gas at a low rate (approximately 100 ml/min) to
D 2172, they should be placed in an oven in covered containers provide agitation and prevent foaming. If foaming or bumping
and heated to a maximum temperature of 110°C (230°F) for the occurs, introduce carbon dioxide intermittently at the begin-
minimum time to obtain workability, but no longer than 30 ning of the distillation at a rate of 100 ml/min to prevent this.
min. If the samples have been stored at a low temperature, they When the temperature reaches 157 to 160°C (315 to 320°F),
should be allowed to reach room temperature before placing increase the carbon dioxide gas flow to approximately 900
them in the oven. mL/min. Maintain this gas flow rate for 10 min while also
maintaining the temperature of the residue in the flask at 160 to
9. Procedure 166°C (320 to 330°F). If, after 10 min, dripping of condensed
9.1 The entire procedure, from the start of the extraction to solvent from the delivery tube is still occurring, maintain the
the final recovery, must be completed within 8 h. gas flow and temperature until 5 min after the dripping ceases
9.2 Centrifuge the solution from the previous extraction for in order to flush solvent vapors from the flask. In no case shall
a minimum of 30 min at 770 times gravity in either bottles or the time of flow of carbon dioxide gas be less than 15 min. At
centrifuge tubes in the specified batch apparatus. If a continu- the end of this period, discontinue the gas flow and heat.
ous centrifuge is used, the extract solution shall be charged at 9.4 If the residue in the flask is highly viscous at 163°C
a rate not to exceed 150 ml/min, while the unit is operating at (325°F), so that dispersion of the carbon dioxide in the residue
a speed calculated to produce a centrifugal force of not less is restricted and the recovered asphalt is expected to have a
than 3000 times gravity. penetration at 25°C (77°F) of less than 30, maintain the carbon
9.3 Concentrate the solution to about 200 ml by any primary dioxide gas flow and temperature for 20 to 22 min.
distillation operation using a flask large enough to hold all the 9.5 The recovered asphalt can be heated to reliquefy and
solution from the extraction. Transfer the residue from the portions taken for penetration, softening point, ductility, ash
primary distillation flask, using several washes of solvent to content, and kinematic and absolute viscosity determinations
rinse all of the residue into the 250-ml distillation flask. as required. Ash content determinations shall be conducted on
Assemble the apparatus as shown in Fig. 1, except position the all recovered bitumens in accordance with Test Methods
bottom of the aeration tube above the surface of the solution. D 2939 and reported with other test data on the recovered
Continue distillation until the temperature reaches 135°C asphalt. Ash contents of recovered asphalts greater than 1 %
(275°F), at which time lower the aeration tube so that the bulb may affect the accuracy of the penetration, ductility, softening
is in contact with the bottom of the flask, and introduce carbon point, or viscosity tests.
dioxide gas at a low rate (approximately 100 ml/min) to
NOTE 1—Determination of the weight of asphalt recovered serves as a
provide agitation and prevent foaming. If foaming or bumping
check to assure that all of the solvent has been removed when this weight
occurs, introduce carbon dioxide intermittently at the begin- is compared with the weight of asphalt extracted as determined by Test
ning of the distillation at a rate of 100 ml/min to prevent this. Methods D 2172. The weight of the recovered asphalt should be corrected
When the temperature reaches 157 to 160°C (315 to 320°F), for the ash content determined.
increase the carbon dioxide gas flow to approximately 900
mL/min. Maintain this gas flow rate for 10 min while also 10. Precision and Bias
maintaining the temperature of the residue in the flask at 160 to 10.1 Precision—Data from the AMRL9 proficiency sample
166°C (320 to 330°F). If, after 10 min, dripping of condensed database from 1974 to 1992 was analyzed to develop estimates
solvent from the delivery tube is still occurring, maintain the of test precision.10 The results of the analysis are summarized
gas flow and temperature until 5 min after the dripping ceases below. The grades of asphalt binders included in the analysis
in order to flush solvent vapors from the flask. In no case shall consisted of AC-5, AC-10, AC-15, AC-20, AC-30, AC-40,
the time of flow of carbon dioxide gas be less than 15 min. At AR-2000, and AR-4000. The precision estimates provided
the end of this period, discontinue gas flow and heat. apply to unaged asphalt binder having physical test properties
9.3.1 Alternative Procedure—Assemble the apparatus as within the following ranges:
shown in Fig. 1 with the separatory funnel in the thermometer Penetration at 25°C (77°F) 29 to 181
hole in the cork. (It may be advantageous to insert the Kinematic viscosity at 135°C (275°F), cSt 200 to 720
Viscosity at 60°C (140°F), P 520 to 5320
separatory funnel in a separate hole drilled in the cork stopper.)
Raise the aeration tube so that the bulb is above the surface of 10.1.1 Single-Operator Precision—The figures given in
the solution. Fill the separatory funnel with the centrifuged Column 2 are the coefficients of variation that have been found
solution and open the stopcock to fill the flask approximately to be appropriate for the tests and conditions described in
one half full of solvent mixture. Apply low heat to the flask and Column 1. When performed by the same operator on the same
start distillation. Adjust the funnel stopcock to introduce fresh sample in the same laboratory using the same apparatus, the
solvent at a rate that will keep the flask approximately one half difference in the results of two properly conducted tests,
full during distillation, adding additional solvent mixture to the
funnel until all solvent has been introduced into the distillation
flask. Wash the solvent mixture container and funnel with fresh 9
These numbers represent, respectively, the (1s %) and (d2s %) limits as
solvent to transfer all asphalt into the distillation flask. Con- described in ASTM Practice C 670.
tinue distillation until the temperature reaches 135°C (275°F), 10
The data is included in a research report available from ASTM Headquarters.
at which time lower the aeration tube so that the bulb is in Request RR: D04-1008.

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 D 1856 – 95a (2003)
expressed as a percent of their mean, shall not exceed the properly conducted tests, expressed as a percent of their mean,
figures given in Column 3. shall not exceed the figures given in Column 3.
Coefficient of Acceptable Range of Coefficient of Acceptable Range of
Test Index Variation Two Results Test Index Variation Two Results
(percent of mean)12 (percent of mean)12 (percent of mean)12 (percent of mean)12
Single-Operator Precision: Multilaboratory Precision:
Penetration at 25°C 11 30 Penetration at 25°C 21 58
(77°F) (77°F)
Kinematic viscosity at 9 26 Kinematic viscosity at 16 46
135°C (275°F), cSt 135°C (275°F), cSt
Viscosity at 60°C 18 51 Viscosity at 60°C 33 93
(140°F), P (140°F), P

10.1.2 Multilaboratory Precision—The figures given in 10.2 Bias—Since there is no data at this time to prepare a
Column 2 are the coefficients of variation that have been found bias statement, no statement on bias is made.
to be appropriate for the tests and conditions described in
Column 1. When performed by different operators in the 11. Keywords
different laboratories, the difference in the results of two 11.1 asphalt; bituminous mixture; distillation; solution

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