ASTM D2172-95

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
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Designation: D 2172 – 95
Standard Test Methods for
Quantitative Extraction of Bitumen From Bituminous Paving
Mixtures
This standard is issued under the fixed designation D 2172; 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 D 604 Specification for Diatomaceous Silica Pigment
D 979 Practice for Sampling Bituminous Paving Mixtures
1.1 These test methods cover the quantitative determination
D 1461 Test Method for Moisture or Volatile Distillates in
of bitumen in hot-mixed paving mixtures and pavement
Bituminous Paving Mixtures
samples. Aggregate obtained by these test methods may be
D 1856 Test Method for Recovery of Asphalt from Solution
used for sieve analysis using Test Method C 117 and Test
by Abson Method
Method C 136.
D 2111 Test Methods for Specific Gravity of Halogenated
1.2 The values stated in inch-pound units are to be regarded
Organic Solvents and Their Admixtures
as the standard. The values given in parentheses are for
2.2 Federal Specifications:
information only.
O-T-620a (Int. Amd. 3) 1,1,1-Trichloroethane, Technical,
1.3 This standard does not purport to address all of the
Inhibited Methyl Chloroform)
safety concerns, if any, associated with its use. It is the
O-T-634 (latest) Trichloroethylene, Technical
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
3. Summary of Test Methods
bility of regulatory limitations prior to use. Specific hazards are
3.1 The paving mixture is extracted with trichloroethylene,
given in Section 7.
1,1,1-trichloroethane or methylene chloride using the extrac-
NOTE 1—The results obtained by these test methods may be affected by
tion equipment applicable to the particular method. The bitu-
the age of the material tested, with older samples tending to yield slightly
men content is calculated by difference from the mass of the
lower bitumen content. Best quantitative results are obtained when the test
extracted aggregate, moisture content, and mineral matter in
is made on mixtures and pavements shortly after their preparation. It is
the extract. The bitumen content is expressed as mass percent
difficult to remove all the asphalt when some aggregates are used and
of moisture-free mixtures.
some chlorides may remain within the mineral matter affecting the
measured asphalt content.
4. Significance and Use
2. Referenced Documents
4.1 All of these test methods can be used for quantitative
2.1 ASTM Standards:
determinations of bitumen in hot-mixed paving mixtures and
C 117 Test Method for Materials Finer Than 75-μm (No. pavement samples for specification acceptance, service evalu-
200) Sieve in Mineral Aggregates by Washing
ation, control, and research. Each method prescribes the
C 128 Test Method for Specific Gravity and Absorption of
solvent or solvents and any other reagents that can be used in
Fine Aggregate
the test method. Test Method D 1856 requires that Method A be
C 136 Test Method for Sieve Analysis of Fine and Coarse
used when asphalt is recovered from solution.
Aggregates
5. Apparatus
C 670 Practice for Preparing Precision and Bias Statements
for Test Methods for Construction Materials 5.1 Oven, capable of maintaining the temperature at 230 6
D 70 Test Method for Specific Gravity of Semi-Solid Bitu-
9°F (110 6 5°C).
minous Materials 5.2 Pan, flat, 12 in. (305 mm) long, 8 in. (203 mm) wide,
and 1 in. (25 mm) deep.
5.3 Balance, or balances having an accuracy of at least
These test methods are under the jurisdiction of ASTM Committee D-4 on
0.01 % of the sample mass.
Road and Paving Materials and are the direct responsibilities of Subcommittee
D04.25 on Analysis of Bituminous Mixtures.
Current edition approved Nov. 10, 1995. Published January 1996. Originally Annual Book of ASTM Standards, Vol 06.03.
published as D 2172 – 63 T. Last previous edition D 2172 – 93. Annual Book of ASTM Standards, Vol 15.05.
2 6
Annual Book of ASTM Standards, Vol 04.02. Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700
Annual Book of ASTM Standards, Vol 04.03. Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 2172
5.4 Hot Plate, electric, 700-W continuous or low, medium, 8.2.2 The size of the test sample shall be governed by the
and high settings. nominal maximum aggregate size of the mixture and shall
5.5 Small-Mouth Graduate, 1000 or 2000-mL capacity. conform to the mass requirement shown in Table 2 (Note 2):
Optional small-mouth graduate, 100-mL capacity.
NOTE 2—When the mass of the test specimen exceeds the capacity of
5.6 Ignition Dish, 125-mL capacity.
the equipment used (for a particular method), the test specimen may be
5.7 Desiccator.
divided into suitable increments, tested, and the results appropriately
5.8 Analytical Balance. combined for calculation of bitumen content (Section 12).
8.2.3 In addition, a test specimen is required for the deter-
6. Reagents
mination of moisture (Section 9) in the mixtures. Take this test
6.1 Purity of Reagents—Reagent grade chemicals shall be
specimen from the remaining sample of the mixture immedi-
used in all tests. Unless otherwise indicated, it is intended that
ately after obtaining the extraction test specimen.
all reagents shall conform to the specifications of the Commit-
7 NOTE 3—If recovery of bitumen from the solution obtained from the
tee on Analytical Reagents of the American Chemical Society,
extraction test is not required, the entire test specimen may be dried to
where such specifications are available. Other grades may be
constant mass in an oven at a temperature of 230 6 9°F (110 6 5°C) prior
used, provided it is first ascertained that the reagent is of
to extraction instead of determining the moisture content (Section 9).
sufficiently high purity to permit its use without lessening the
9. Moisture Content
accuracy of the determination.
6.2 Ammonium Carbonate Solution—Saturated solution of
9.1 Determine the moisture content of the mixture (see
reagent grade ammonium carbonate [(NH ) CO ].
4 2 3 8.2.2) in accordance using the procedure described in Test
6.3 Methylene Chloride, technical grade. Caution—see
Method D 1461.
Section 7.
9.2 Calculate the mass of water, W , (12.1) in the extraction
6.4 1,1,1-Trichloroethane, conforming to Federal Specifica-
test portion by multiplying mass percent water (9.1) by the
tion O-T-620a (Int. Amd. 3). Caution—see Section 7.
mass of the extraction test portion, W , (12.1).
6.5 Trichloroethylene, technical grade, Type 1, Federal
Specification O-T-634, latest revision. Caution—see Section
TEST METHOD A
7.
10. Apparatus
7. Hazards
10.1 In addition to the apparatus listed in Section 5, the
7.1 The solvents listed in Section 6 should be used only
following apparatus is required for Test Method A:
under a hood or with an effective surface exhaust system in a
10.1.1 Extraction Apparatus, consisting of a bowl approxi-
well-ventilated area, since they are all toxic to some degree as
mating that shown in Fig. 1 and an apparatus in which the bowl
indicated in Table 1:
may be revolved at controlled variable speeds up to 3600
r/min. The speed may be controlled manually or with a preset
speed control. The apparatus should be provided with a
TABLE 1 Solvent Toxicity
container for catching the solvent thrown from the bowl and a
Time-Weighted Average
drain for removing the solvent. The apparatus preferably shall
Solvent Concentration for 8-h exposure for
5-day week, ppm
be provided with explosion-proof features and installed in a
A
hood or an effective surface exhaust system to provide venti-
Methylene chloride 200
A
Trichloroethylene 100
lation.
A
1,1-Trichloroethane 350
NOTE 4—Similar apparatus of larger size may be used.
A
Threshold Limit Concentration Committee of the American Conference of
Governmental Hygienists, 1977 Values.
10.1.2 Filter Rings, felt or paper, to fit the rim of the bowl.
10.1.3 Low-ash paper filter rings may be used in place of the
felt filter ring (10.1.2). Such filter rings shall consist of low ash
8. Sampling
filter paper stock 0.05 6 0.005 in. thick. The nominal base
8.1 Obtain samples in accordance with Practice D 979.
weight of the paper shall be 330 6 30 lb for a ream (500
8.2 Preparation of Test Specimens:
sheets—25 by 38 in.). The ash content of the paper should not
8.2.1 If the mixture is not sufficiently soft to separate with a
exceed 0.2 % (approximately 0.034 g per ring).
spatula or trowel, place it in a large, flat pan and warm to 230
6 9°F (110 6 5°C) only until it can be handled or mixed. Split
TABLE 2 Size of Sample
or quarter the material until the mass of material required for
Nominal Maximum
test is obtained.
Minimum Mass of Sample,
Aggregate Size Standard, Sieve Size
kg
mm
4.75 (No. 4) 0.5
Reagent Chemicals, American Chemical Society Specifications, American 3
9.5 ⁄8 in. 1
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
12.5 ⁄2 in. 1.5
listed by the American Chemical Society, see Analar Standards for Laboratory
19.0 ⁄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. Pharmaceutical Convention, Inc. (USPC), Rockville, 37.5 1 ⁄2 in. 4
MD.
D 2172
11. Procedure and dry on a steam bath and then, dry to constant mass in an
oven or on a hot plate at 2306 9°F (110 6 5°C). If
11.1 Determine the moisture content of the material in
trichloroethylene or trichloroethane is used as the extraction
accordance with Section 9.
solvent, the preliminary drying on a steam bath may be
11.2 Place a 650 to 2500-g test portion into a bowl. See
omitted. The mass of the extracted aggregate, W , is equal to
Annex A1 for alternative procedures to those prescribed herein
the mass of the aggregate in the pan plus the increase in mass
and in 11.5.
of the filter rings.
11.3 Cover the test portion in the bowl with trichloroethyl-
11.5.1 Use the following alternative procedure when low-
ene, 1,1,1-trichloroethane or methylene chloride and allow
ash filter rings are used: Place the aggregate and filter rings in
sufficient time for the solvent to disintegrate the test portion
a clean metal pan. Dry as specified above. Carefully fold the
(not over 1 h). Place the bowl containing the test portion and
dried filter ring and stand it on the aggregate. Burn the filter
the solvent in the extraction apparatus. Dry and determine the
ring by igniting with a bunsen burner or match. Determine the
mass of the filter ring and fit it around the edge of the bowl.
mass of the extracted aggregate in the pan, W .
Clamp the cover on the bowl tightly and place a beaker under
the drain to collect the extract.
NOTE 5—Since dry aggregate absorbs moisture when exposed to air
11.4 Start the centrifuge revolving slowly and gradually containing moisture, determine the mass of the extracted aggregate
immediately after cooling to a suitable temperature.
increase the speed to a maximum of 3600 r/min or until solvent
ceases to flow from the drain. Allow the machine to stop, add
11.6 Determine the amount of mineral matter in the extract
200 mL of trichloroethylene, 1,1,1-trichloroethane or methyl-
by any of the following test methods:
ene chloride and repeat the procedure. Use sufficient 200-mL
11.6.1 Ashing Method:
solvent additions (not less than three) so that the extract is not
11.6.1.1 Record the volume of the total extract in the
darker than a light straw color. Collect the extract and the
graduate (11.4). Determine the mass of an ignition dish. Agitate
washings in a suitable graduate.
NOTE 1—See Table 3 for metric equivalents.
FIG. 1 Extraction Unit Bowl (Test Method A)
11.5 Remove the filter ring from the bowl and dry in air. If the extract thoroughly and immediately measure approximately
felt filter rings are used, brush off mineral matter adhering to 100 mL into the ignition dish. Evaporate to dryness on a steam
the surface of the ring and add to the extracted aggregate. Dry bath or hot plate, except use a steam bath when the solvent is
the ring to constant mass in an oven at 230 6 9°F (110 6 5°C). benzene. Ash residue at a dull red heat (500 to 600°C), cool,
Carefully remove all the contents of the bowl into a metal pan and add 5 mL of saturated ammonium carbonate solution per
D 2172
TABLE 3 Metric Equivalents for Figures
Inch-Pound Units, in. Metric Equivalent, cm Inch-Pound Units, in. Metric Equivalent, cm Inch-Pound Units, in. Metric Equivalent, cm
1 11 7
⁄8 0.32 1 ⁄16 4.3 5 ⁄8 14.9
3 3
⁄16 0.48 1 ⁄4 4.4 6 15.2
7 3 1
⁄32 0.56 2 ⁄16 5.5 6 ⁄8 15.5
1 7 3
⁄4 0.63 2 ⁄32 5.6 6 ⁄16 15.7
5 5 1
⁄16 0.79 2 ⁄16 5.9 6 ⁄4 15.9
3 1 1
⁄8 0.95 2 ⁄2 6.4 6 ⁄2 16.5
1 5 3
⁄2 1.27 2 ⁄8 6.9 7 ⁄8 18.7
5 13
⁄8 1.59 2 ⁄16 7.2 8 20.7
3 3
⁄4 1.9 3 7.6 9 ⁄4 24.7
1 2.5 3 ⁄4 9.6 10 25.4
1 1
1 ⁄8 2.86 4 10.2 10 ⁄8 25.7
3 1
1 ⁄16 3.02 4 ⁄4 10.8 12 30.5
1 ⁄32 3.57 5 12.7 14 35.5
1 7 1
1 ⁄2 3.8 5 ⁄16 13.8 14 ⁄2 37
1 ⁄8 4.1
gram of ash. Digest at room temperature for 1 h. Dry in an oven 11.6.3 Volumetric Method:
at 100°C to constant mass, cool in a desiccator, and determine 11.6.3.1 Place the extract in a previously tared and cali-
the mass. brated flask. Place the flask in a controlled-temperature bath
11.6.1.2 Calculate the mass of mineral matter in the total controlled to 0.2°F (60.1°C), and allow to come to the
volume of extract, W , as follows: temperature at which the flask was calibrated. When the
desired temperature has been reached, fill the flask with solvent
W 5 G@V /~V 2 V !# (1)
4 1 1 2
which has been kept at the same temperature. Bring the level of
where:
the liquid in the flask up to the neck, insert the stopper, making
G = ash in aliquot, g,
sure the liquid overflows the capillary, and remove from the
V = total volume, mL, and
1 bath. Wipe the flask dry, determine the mass to the nearest 0.1
V = volume after removing aliquot, mL.
g, and record this mass as the mass of flask plus extract. See
11.6.2 Centrifuge Method:
Annex A2 for a volumetric test method alternative procedure if
11.6.2.1 For this test method use any suitable high-speed
a controlled-temperature bath is not used as prescribed herein.
(3000 g or higher) centrifuge of the continuous-flow type.
11.6.3.2 Calculate the volume of asphalt and fines in the
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