Designation: D2172/D2172M – 11

Standard Test Methods for

Quantitative Extraction of Bitumen From Bituminous Paving
Mixtures1
This standard is issued under the fixed designation D2172/D2172M; 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.
This standard has been approved for use by agencies of the Department of Defense.

1. Scope C670 Practice for Preparing Precision and Bias Statements

1.1 These test methods cover the quantitative determination for Test Methods for Construction Materials
of bitumen in hot-mixed paving mixtures and pavement D70 Test Method for Density of Semi-Solid Bituminous
samples. Aggregate extracted from a paving mixture may be Materials (Pycnometer Method)
used for sieve analysis using Test Method D5444. D604 Specification for Diatomaceous Silica Pigment3
1.2 The values stated in either SI units or inch-pound units D979 Practice for Sampling Bituminous Paving Mixtures
are to be regarded separately as standard. The values stated in D1461 Test Method for Moisture or Volatile Distillates in
each system may not be exact equivalents; therefore, each Bituminous Paving Mixtures
system shall be used independently of the other. Combining D1856 Test Method for Recovery of Asphalt From Solution
values from the two systems may result in non-conformance by Abson Method
with the standard. D2111 Test Methods for Specific Gravity and Density of
1.2.1 Measurements of volume and mass are only given in Halogenated Organic Solvents and Their Admixtures
SI units because they are the only units typically used in D3666 Specification for Minimum Requirements for Agen-
practice when performing this test method. cies Testing and Inspecting Road and Paving Materials
1.3 This standard does not purport to address all of the D5444 Test Method for Mechanical Size Analysis of Ex-
safety concerns, if any, associated with its use. It is the tracted Aggregate
responsibility of the user of this standard to establish appro- D6368 Specification for Vapor-Degreasing Solvents Based
priate safety and health practices and determine the applica- on normal-Propyl Bromide and Technical Grade normal-
bility of regulatory limitations prior to use. Specific hazards are Propyl Bromide
given in Section 7. 2.2 Federal Specifications:
O-T-634 (latest) normal Propyl Bromide, Technical4
NOTE 1—The results obtained by these test methods may be affected by
the age of the material tested, with older samples tending to yield slightly 3. Summary of Test Methods
lower bitumen content. Best quantitative results are obtained when the test
is made on mixtures and pavements shortly after their preparation. It is 3.1 The paving mixture is extracted with trichloroethylene,
difficult to remove all the asphalt when some aggregates are used and normal Propyl Bromide, or methylene chloride using the
some chlorides may remain within the mineral matter affecting the extraction equipment applicable to the particular method. The
measured asphalt content. bitumen content is calculated by difference from the mass of
the extracted aggregate, moisture content, and mineral matter
2. Referenced Documents in the extract. The bitumen content is expressed as mass
2.1 ASTM Standards:2 percent of moisture-free mixtures.
C128 Test Method for Density, Relative Density (Specific
Gravity), and Absorption of Fine Aggregate 4. Significance and Use
4.1 All of these test methods can be used for quantitative
determinations of bitumen in hot-mixed paving mixtures and
1
These test methods are under the jurisdiction of ASTM Committee D04 on
pavement samples for specification acceptance, service evalu-
Road and Paving Materials and are the direct responsibilities of Subcommittee ation, control, and research. Each method prescribes the
D04.25 on Analysis of Bituminous Mixtures. solvent or solvents and any other reagents that can be used in
Current edition approved Feb. 1, 2011. Published March 2011. Originally
approved in 1963. Last previous edition approved in 2005 as D2172 – 05. DOI:
10.1520/D2172-11.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Withdrawn. The last approved version of this historical standard is referenced
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM on www.astm.org.
4
Standards volume information, refer to the standard’s Document Summary page on Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700
the ASTM website. Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.

Copyright. © ASTM International, 100 Barr Harbor Drive P.O. box C-700, West Conshohocken, Pennsylvania 19428-2959, United States

1
 D2172/D2172M – 11
the test method. Test Method D1856 requires that Method A be Committee of the American Conference of Governmental
used when asphalt is recovered from solution. Industrial Hygienists6 for the current threshold limit values.
NOTE 2—The quality of the results produced by this standard are 8. Sampling
dependent on the competence of the personnel performing the procedure
and the capability, calibration, and maintenance of the equipment used. 8.1 Obtain samples in accordance with Practice D979.
Agencies that meet the criteria of Standard Practice D3666 are generally 8.2 Preparation of Test Specimens:
considered capable of competent and objective testing/sampling/ 8.2.1 If the mixture is not sufficiently soft to separate with a
inspection/etc. Users of this standard are cautioned that compliance with spatula or trowel, place it in a large, flat pan and warm to 110
Practice D3666 alone does not completely assure reliable results. Reliable 6 5°C [230 6 10°F] only until it can be handled or mixed.
results depend on many factors; following the suggestions of Practice
D3666 or some similar acceptable guideline provides a means of
Split or quarter the material until the mass of material required
evaluating and controlling some of those factors. for test is obtained.
8.2.2 The size of the test sample shall be governed by the
5. Apparatus nominal maximum aggregate size of the mixture and shall
5.1 Oven, capable of maintaining the temperature at 110 6 conform to the mass requirement shown in Table 1 (Note 3):
5°C [230 6 10°F]. NOTE 3—When the mass of the test specimen exceeds the capacity of
5.2 Pan, flat, at least 300 mm [12 in.] long, 200 mm [8 in.] the equipment used (for a particular method), the test specimen may be
wide, and 25 mm [1 in.] deep. divided into suitable increments, tested, and the results appropriately
5.3 Balance, or balances having an accuracy of at least combined for calculation of bitumen content (Section 12).
0.01 % of the sample mass. 8.2.3 In addition, a test specimen is required for the deter-
5.4 Hot Plate, electric, 700-W continuous or low, medium, mination of moisture (Section 9) in the mixtures. Take this test
and high settings. specimen from the remaining sample of the mixture immedi-
5.5 Small-Mouth Graduate, 1000 or 2000-mL capacity. ately after obtaining the extraction test specimen.
Optional small-mouth graduate, 100-mL capacity.
NOTE 4—If recovery of bitumen from the solution obtained from the
5.6 Ignition Dish, 125 mL capacity.
extraction test is not required, the entire test specimen may be dried to
5.7 Desiccator. constant mass in an oven at a temperature of 110 6 5°C [230 6 10°F]
5.8 Analytical Balance. prior to extraction instead of determining the moisture content (Section 9).

6. Reagents 9. Moisture Content

6.1 Purity of Reagents—Reagent grade chemicals shall be 9.1 Determine the moisture content of the mixture (see
used in all tests. Unless otherwise indicated, it is intended that 8.2.2) in accordance using the procedure described in Test
all reagents shall conform to the specifications of the Commit- Method D1461.
tee on Analytical Reagents of the American Chemical Society,5 9.2 Calculate the mass of water, W2, (12.1) in the extraction
where such specifications are available. Other grades may be test portion by multiplying mass percent water (9.1) by the
used, provided it is first ascertained that the reagent is of mass of the extraction test portion, W1, (12.1).
sufficiently high purity to permit its use without lessening the
accuracy of the determination. TEST METHOD A
6.2 Ammonium Carbonate Solution—Saturated solution of
10. Apparatus
reagent grade ammonium carbonate [(NH4)2CO3].
6.3 Methylene Chloride, technical grade. Caution—see 10.1 In addition to the apparatus listed in Section 5, the
Section 7. following apparatus is required for Test Method A:
6.4 normal-Propyl Bromide (nPB), conforming to Specifi- 10.1.1 Extraction Apparatus, consisting of a bowl approxi-
cation D6368. Caution—see Section 7. mating that shown in Fig. 1 and an apparatus in which the bowl
6.5 Trichloroethylene, technical grade, Type 1, Federal may be revolved at controlled variable speeds up to 3600
Specification O-T-634, latest revision. Caution—see Section r/min. The speed may be controlled manually or with a preset
7.
6
7. Hazards Available from American Conference of Governmental Industrial Hygienists,
1330 Kemper Meadow Drive, Cincinnati, OH 45240, (513) 742–2020, (www.acgi-
7.1 Caution—The solvents listed in Section 6 should be h.org).
used only under a hood or with an effective surface exhaust
system in a well-ventilated area, since they are toxic to various TABLE 1 Size of Sample
degrees. Consult the current Threshold Limit Concentration Nominal Maximum
Minimum Mass of Sample,
Aggregate Size Standard, Sieve Size
kg
mm
4.75 (No. 4) 0.5
5
Reagent Chemicals, American Chemical Society Specifications, American 9.5 3⁄8 in. 1
Chemical Society, Washington, DC. For suggestions on the testing of reagents not 12.5 1⁄2 in. 1.5
listed by the American Chemical Society, see Analar Standards for Laboratory 19.0 3⁄4 in. 2
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia 25.0 1 in. 3
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, 37.5 11⁄2 in. 4
MD.

2
 D2172/D2172M – 11

FIG. 1 Extraction Unit Bowl (Test Method A)

speed control. The apparatus should be provided with a 10.1.3 Low-ash paper filter rings may be used in place of the
container for catching the solvent thrown from the bowl and a felt filter ring (10.1.2). Such filter rings shall consist of low ash
drain for removing the solvent. The apparatus preferably shall filter paper stock approximately 1.3 mm [0.05 in.] thick. The
be provided with explosion-proof features and installed in a ash content of the paper shall not exceed 0.2 % (approximately
hood or an effective surface exhaust system to provide venti- 0.034 g per ring).
lation.
11. Procedure
NOTE 5—Similar apparatus of larger size may be used.
11.1 Determine the moisture content of the material in
10.1.2 Filter Rings, felt or paper, to fit the rim of the bowl. accordance with Section 9.

3
 D2172/D2172M – 11
11.2 Place a 650 to 2500-g test portion into a bowl. See W4 5 G[V1/~V 1 2 V2!# (1)
Annex A1 for alternative procedures to those prescribed herein
and in 11.5. where:
G = ash in aliquot, g,
11.3 Cover the test portion in the bowl with trichloroethyl-
V1 = total volume, mL, and
ene, normal Propyl Bromide, or methylene chloride and allow V2 = volume after removing aliquot, mL.
sufficient time for the solvent to disintegrate the test portion 11.6.2 Centrifuge Method:
(not over 1 h). Place the bowl containing the test portion and 11.6.2.1 For this test method use any suitable high-speed
the solvent in the extraction apparatus. Dry and determine the (3000 g or higher) centrifuge of the continuous-flow type.
mass of the filter ring and fit it around the edge of the bowl. 11.6.2.2 Determine the mass of a clean empty centrifuge
Clamp the cover on the bowl tightly and place a beaker under cup (or bowl) to 0.01 6 0.005 g and place in the centrifuge.
the drain to collect the extract. Position a container at the appropriate spout to catch the
11.4 Start the centrifuge revolving slowly and gradually effluent from the centrifuging operation. Transfer all of the
increase the speed to a maximum of 3600 r/min or until solvent extract (from Test Methods A, B, C, D, or E as appropriate) to
ceases to flow from the drain. Allow the machine to stop, add an appropriate (feed) container suitably equipped with a feed
200 mL of trichloroethylene, normal Propyl Bromide, or control (valve or clamp, etc.). To ensure quantitative transfer of
methylene chloride and repeat the procedure. Use sufficient the extract to the feed container, the receptacle containing the
200-mL solvent additions (not less than three) so that the extract should be washed several times with small amounts of
extract is not darker than a light straw color. Collect the extract clean solvent and the washings added to the feed container.
and the washings in a suitable graduate.

11.5 Remove the filter ring from the bowl and dry in air. If Start the centrifuge and allow to reach a constant operational
felt filter rings are used, brush off mineral matter adhering to speed (for example, 9000 r/min for the SMM type and
the surface of the ring and add to the extracted aggregate. Dry 20 000 + r/min for the Sharples type). Open the feed line and
the ring to constant mass in an oven at 110 6 5°C [230 6 feed the extract into the centrifuge at a rate of 100 to 150
10°F]. Carefully remove all the contents of the bowl into a mL/min. After all the extract has passed through the centrifuge,
metal pan and dry on a steam bath and then, dry to constant wash the feed mechanism (with centrifuge still running) with
mass in an oven or on a hot plate at 110 6 5°C [230 6 10°F]. several increments of clean solvent, allowing each increment to
If trichloroethylene or normal Propyl Bromide is used as the run through the centrifuge until the effluent is essentially
extraction solvent, the preliminary drying on a steam bath may colorless.
be omitted. The mass of the extracted aggregate, W 3, is equal 11.6.2.3 Allow the centrifuge to stop and remove the cup (or
to the mass of the aggregate in the pan plus the increase in mass bowl). Clean the outside with fresh solvent. Allow the residual
of the filter rings. solvent to evaporate in a funnel or steam hood and then dry the
11.5.1 Use the following alternative procedure when low- container in an oven controlled at 110 6 5°C [230 6 10°F].
ash filter rings are used: Place the aggregate and filter rings in Cool the container and redetermine the mass immediately. The
a clean metal pan. Dry as specified above. Carefully fold the increase in mass is the mass of mineral matter, W4, (12.1) in the
dried filter ring and stand it on the aggregate. Burn the filter extract.
ring by igniting with a bunsen burner or match. Determine the 11.6.3 Volumetric Method:
mass of the extracted aggregate in the pan, W3.
11.6.3.1 Place the extract in a previously tared and cali-
NOTE 6—Since dry aggregate absorbs moisture when exposed to air brated flask. Place the flask in a controlled-temperature bath
containing moisture, determine the mass of the extracted aggregate controlled to 60.1°C [0.2°F], and allow the contents to reach
immediately after cooling to a suitable temperature. the temperature at which the flask was calibrated. When the
11.6 Determine the amount of mineral matter in the extract desired temperature has been reached, fill the flask with solvent
by any of the following test methods: which has been kept at the same temperature. Bring the level of
11.6.1 Ashing Method: the liquid in the flask up to the neck, insert the stopper, making
11.6.1.1 Record the volume of the total extract in the sure the liquid overflows the capillary, and remove from the
graduate (11.4). Determine the mass of an ignition dish. Agitate bath. Wipe the flask dry, determine the mass to the nearest 0.1
the extract thoroughly and immediately measure approximately g, and record this mass as the mass of flask plus extract. See
100 mL into the ignition dish. Evaporate to dryness on a steam Annex A2 for a volumetric test method alternative procedure if
bath or hot plate, except use a steam bath when the solvent is a controlled-temperature bath is not used as prescribed herein.
benzene. Ash residue at a dull red heat 500 to 600°C [930 to 11.6.3.2 Calculate the volume of asphalt and fines in the
1110°F], cool, and add 5 mL of saturated ammonium carbonate extract as follows:
solution per gram of ash. Digest at room temperature for 1 h. ~ M1 2 M 2 !
Dry in an oven at 100°C to constant mass, cool in a desiccator, V1 5 V 2 2 (2)
~ G1 !
and determine the mass.
11.6.1.2 Calculate the mass of mineral matter in the total where:
volume of extract, W4, as follows: V 1 = volume of asphalt and fines in the extract,

4
 D2172/D2172M – 11

V2 = volume of the flask,

M1 = mass of the contents of the flask,
M 2 = mass of the asphalt and fines in the extract = mass of
the total samples minus the mass of the extracted
aggregate, and
G1 = specific gravity of the solvent determined to the
nearest 0.001 in accordance with Test Methods
D2111.
11.6.3.3 Calculate the mass of fines in the extract as follows:
M3 5 K ~M 2 2 G3V1! (3)

where:
M 3 = mass of fines in the extract,
G2 = specific gravity of fines as determined in accordance
with Test Method C128,
G3 = specific gravity of asphalts as determined in accor-
dance with Test Method D70,
K = G2 / G2 2 G3 ,
V1 = as given in 11.6.3.2, and
M2 = as given in 11.6.3.2.
12. Calculation of Bitumen Content
12.1 Calculate the percent bitumen in the test portion as
follows:

Bitumen content, % 5 F W1 2 W 2 G
~ W1 2 W 2 ! 2 ~ W 3 1 W 4 !
3 100 (4)

where:
W1 = mass of test portion,
W2 = mass of water in the test portion,
W3 = mass of the extracted mineral aggregate, and
W4 = mass of the mineral matter in the extract.
NOTE 7—When ashless filter rings are not used, add the increase in
mass of the felt filter ring to W4.
NOTE 8—For paving mixtures in which tar is used as the binder, a
modification of Test Method A is given in Annex A3.

TEST METHOD B
13. Apparatus
13.1 In addition to the apparatus listed in Section 5, the FIG. 2 Extraction Apparatus (Test Method B)
following apparatus is required for Test Method B:
13.1.1 Extraction Apparatus, similar to that shown in Fig. 2.
13.1.1.1 Glass Jar, cylindrical, plain, made of heat-resistant 13.1.1.3 Condenser, fabricated with a truncated hemispheri-
glass. The jar shall be free of cracks, scratches, or other cal condensing surface and a truncated conical top. Other
evidence of flaws that might cause breakage during heating. suitable geometric shapes may also be used provided they
13.1.1.2 Cylindrical Metal Frames, one or two. The lower accomplish the condensing and flow functions intended. The
frame shall have legs of sufficient length to support the frame, material used in fabricating the condenser shall be essentially
including the apex of the metal cone and paper cone liner unreactive to water and to the solvent used and shall be
above the solvent level. When two frames are used, the upper provided with suitable water inlet and outlet.
frame shall have legs of sufficient length to support the metal 13.1.1.4 Filter Paper, medium-grade, fast-filtering. The di-
cone and paper cone liner at or above the top rim of the lower ameter of the paper shall be such that when folded in
frame. The legs of the upper frame shall fit securely in the top accordance with the directions given below, it shall completely
rim of the lower frame. A bail handle may be provided on the line the metal cones in the frames.
inside of the top rim of each frame for convenient handling. 13.1.1.5 Heat Resistant-Coated Wire Mesh, approximately 3
The metal used in fabricating the frames shall be essentially mm [0.1 in.] thick for use as insulation between the glass jar
inactive to the solvents used in the test method. and hot plate.