T 170 METHODS OF SAMPLING AND TESTING

Standard Method of Test for

Recovery of Asphalt from Solution by Abson Method

AASHTO DESIGNATION: T 170-93

(ASTM DESIGNATION: D 1856-79)

1. SCOPE1 3. SUMMARY OF METHOD 5.3.1 Extraction Flasks-A 250 mL

wide-mouth heat resistant flask for
distillation and a suitable flask for the
1.1 This method covers the recovery by 3.1 The solution of solvent and asphalt receiver.
the Abson Method of asphalt from from a prior extraction is distilled under
solutions previously obtained by prescribed conditions to a point where 5.3.2 Glass Tubing-Heat-resistant glass
extracting asphalt mixtures with most of the solvent has been distilled, at tubing, having 10 mm inside diameter
reagentgrade trichlorethylene or reagent which time carbon dioxide gas is and a goose-neck shaped delivery tube
grade methylene chloride (NOTE 1). The introduced into the distillation process to (as shown in Figure 1) for connecting the
asphalt is recovered with properties remove all traces of the extraction flask to the condenser.
substantially the same as those it solvent. The recovered asphalt 5.3.3 Inlet Aeration Tube, at least 180
possessed in the asphaltic mixture and in (distillation residue) can then be mm in length having a 6 mm outside
quantity sufficient for further testing. subjected to further testing as required. diameter with a 10-mm bulb carrying six
1.2 The values stated in SI units are to be staggered holes approximately 1.5 mm in
regarded as the standard. diameter.3
4. SIGNIFICANCE AND USE
5.3.4 Electric Heating Mantle, with
NOTE 1-Trichloroethylene, Technical Grade. variable transformer, oil bath or fluidized
Type l. Federal Specification O-T634. latest 4.1 The asphalt should be extracted from sand bath, to fit a 250 mL flask.
revision or technical grade methylene may he the aggregate-asphalt mixture in
used but it is recommended that for each new 5.3.5 Water-Jacketed Condenser,
accordance with Method A or E (NOTE Allihan type, with 200 mm minimum
supply of the solvent a blank should be run on
an asphalt of known properties. In case of 2) of T 164 as there is some experimental jacket length, or equivalent.
dispute, reagent grade should be used. Blank evidence that the recovered asphalt may
Determinations-Introduce about 70 g of have slightly lower penetration values 5.3.6 Thermoineter-An ASTM Low
asphalt into a 2000-mL flask: add about 800 when recovered from solutions obtained Distillation Thermometer 7C (7F) as
mL of solvent to dissolve the asphalt. allow from hot extraction methods. specified, having a range of -2 to 300°C
the solution to stand for about 4 hours: (30 to 580°F), respectively, and
concentrate the solution by distillation to about NOTE 2-Equipment in Method E of T 164 can conforming to the requirements in ASTM
200 mL and then recover the asphalt. (Total be modified by a vacuum trap attached to the Specification E 1.
elapsed time, from when the solvent is added top of the "end-point" site tube to collect the
to the time the recovery test is completed is 5.3.7 Gas Flow Meter, as shown in
extract to allow its use for recoveries.
about 7 hours.) Figure 1, or any type capable of
indicating a gas flow of up to 1000 mL
5. APPARATUS per minute.4
2. REFERENCED DOCUMENTS
5.3.8 Corks, Nº 20, drilled as shown in
5.1 Centrifuge, batch unit capable of Figure 1.
2.1 AASHTO Standards: exerting a minimum centrifugal force of 5.3.9 Flexible Elastometric Tubing,
T 111 Inorganic Matter or Ash in 770 times gravity or a continuous unit resistant to chlorinated solvents, having
Bituminous Materials capable of exerting a minimum force of sufficient length and size to connect the
T 164 Quantitative Extraction of 3000 times gravity. The apparatus aeration tube to a flowmeter, and
Bitumen from Bituminous specified in ASTM D 96, Test for Water equipped with a pinch clamp or stopcock
Paving Mixtures and Sediment in Crude Oils by to close aeration tube prior to introducing
Centrifuge, may also be used.2 carbon dioxide.
2.2 ASTM Standards:
5.2 Centrifuge Tubes-A supply of 250 to 5.3.10 Separator- Funnel,5 125 ml -
D 96 Water and Sediment in Crude 500 mL wide mouth bottles, or centrifuge capacity or larger.
Oils tubes as shown in Figure 1 or 2 of ASTM
D 2939 Emulsified Bitumens Used as D 96. 3
Protective Coatings Kimball tube Nº 49055 has been found satisfactory
5.3 Distillation Assembly, as shown in for this purpose, also Inlet aeration Tube, Part Nº
D 4701 Technical Grade Methylene Figure 1 and consisting of the following 226, available from W m. A. Sales Ltd.. 419
Chloride items: Harvester Court, Wheeling, III., 60090. or equivalent
has been found suitable
E1 ASTM Thermometers 4
The Monostat Corp., "Flowmeter' Nº 9144 has been
2.3 Federal Specification: found satisfactory for this purpose. Also ColePalmer
Nº FM082-03ST.
O-T-634 Technical 5
Kimball separatory funnel Nº 29028 has been found
Trichloroethylene 2 satisfactory for this purpose.
An "International" Nº 2 Centrifuge operating at
1900 r/min or an “SMM Continuous Centrifuge”
exerting a force of 3000 times gravity at 9000 r/pm,
1
Similar but not technically identical to ASTM have been found satisfactory for this purpose
Method.

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6. REAGENTS AND MATERIALS mixture be extracted as there could be they should be allowed to reach room
some selective solvency of the asphalt temperature before placing in the oven.
and the harder, more viscous components
6.1 Carbon Dioxide Gas-A pressurized of the asphalt might be left in the mixture
tank, with pressure-reducing valve or NOTE 3-Recommendation that the time in the
if extraction is not carried to completion. oven at I10°C (230°F) should not exceed 30
other convenient source.
8.3 Since heavy petroleum distillates minutes if at all possible.
6.2 The solvent for extracting the asphalt such as mineral spirits or kerosene will
from the mixtures should be reagent affect the properties of the recovered
grade trichloroethylene or reagent grade 9. PROCEDURE
asphalt, it is important to avoid the use of
methylene chloride. Other solvents may such solvents in cleaning the extraction
affect the bitumen to change its and recovery apparatus and use only 9.1 The entire procedure, from the start
properties significantly from that as it trichloroethylene or methylene chloride of the extraction to the final recovery,
exists in the mixture (see NOTE 1). for cleaning. Residues of heavy must be completed within 8 hours.
petroleum solvents on the equipment may 9.2 Centrifuge the solution from the
7. PRECAUTIONS contaminate the recovered asphalt and previous extraction for a minimum of 30
affect its test properties. It is also minutes at 770 times gravity in either 250
necessary to use new filter rings, clean to 500 mL wide-mouth bottles or
7.1 Caution-The solvents listed in felt pads, or other uncontaminated
Section 6.2 should be used only under a centrifuge tubes in batch apparatus
filtering media in the extraction process specified. If a continuous centrifuge is
hood or with an effective surface exhaust to avoid contamination from a previous
system in a well-ventilated area, since used, the extract solution shall be charged
extraction. at a rate not to exceed 150 mljminute,
they are toxic to some degree as indicated
8.4 Generally, the bitumen in mixtures while the unit is operating at a speed
below:
will progressively harden when exposed calculated to produce a centrifugal force
to air, particularly if the mixtures are in a of not less than 3000 times gravity.
8. SAMPLE loose condition. Therefore, it is important 9.3 Concentrate the solution to about 200
to protect bituminous mixtures from mL by any primary distillation operation
exposure to air and preferably to store using a flask large enough to hold all the
8.1 The sample shall consist of the them in airtight containers at a
solution from previous extraction of a solution from the extraction. Transfer the
temperature below 0°C (32°F) until they residue from the primary distillation
sample of sufficient mass to result in can be tested. When samples of
approximately 75 to 100 g of recovered flask, using several washes of solvent to
bituminous mixture are warmed for rinse all of the residue into the 250 mL
bitumen. More or less quantities of preparing representative proportions for
bitumen may be recovered; however, the distillation flask. Assemble the apparatus
extraction tests in accordance with as shown in Figure 1 and introduce
properties of the recovered bitumen may Method A or E (NOTE 2) of Method T
not be in agreement with those recovered carbon dioxide gas at a low rate
164, they should be placed in an oven in (approximately 100 mL/minute) to
of the aforementioned quantities, and in covered containers and heated to a
case of a disagreement, 75 to 100 g provide agitation and prevent foaming.
maximum temperature of 110°C (230°F) Continue the distillation until the
should be recovered. for the minimum time to obtain temperature reaches 157 to 160°C (315 to
8.2 During the extraction process, it is workability (NOTE 3). If the samples 320°F), at that point increase the carbon
important that all of the asphalt in the have been stored at a low temperature, dioxide gas flow to approximately 900
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T 170 METHODS OF SAMPLING AND TESTING

mUminute. Maintain this gas flow rate flask approximately one-half full during penetration, ductility, softening point, or
for 10 minutes while also maintaining the distillation, adding additional solvent viscosity tests.
temperature of the residue in the flask at mixture to the funnel until all solvent has
160 to 166°C (320 to 330°F). The setting been introduced into the distillation flask.
NOTE 4-Determination of the mass of asphalt
of the variable transformer for obtaining When the temperature reaches 157 to recovered serves as a check to assure that all
this temperature can be established by a 160°C (315 to 320°F), increase the of the solvent has been removed when this
few trial runs; generally a higher setting carbon dioxide gas flow to approximately mass is compared with the mass of asphalt
can be used for the main distillation, 900 mL/minute. Maintain this gas flow extracted as determined by Method T 164. The
reducing the setting when most of the rate for 10 minutes while also mass of the recovered asphalt should be
solvent has been vaporized. In place of maintaining the temperature of the corrected for the ash content determined.
the electric heating mantle, an oil bath or residue in the flask at 160 to 166°C (320
a fluidized sand bath may be substituted to 330°F). If, after 10 minutes, dripping 10. PRECISION
in which the temperature during the of condensed solvent from the delivery
introduction of the COZ is maintained 8 tube is still occurring, maintain the gas
to 14°C (15 to 25°F) higher than the flow and temperature until 5 minutes 10.1 Repeatability and reproducibility
inside temperature. If after 10 minutes, after the dripping ceases in order to flush limits have not been established in
dripping of condensed solvent from the solvent vapors from the flask. In no case accordance with ASTM practice.
delivery tube is still occurring, maintain shall the time of flow of carbon dioxide However, a series of eight samples tested
the gas flow and temperature until 5 gas be less than 15 minutes. At the end of in duplicate by four laboratories in 1971
minutes after the dripping ceases in order this period, discontinue the gas flow and in a cooperative test program under the
to flush solvent vapors from the flask. In heat. direction of ASTM Subcommittee
no case shall the time of flow of carbon 9.4 If the residue in the flask is highly D04.256 provided the information given
dioxide gas be less than 15 minutes. At viscous at 163°C (325°F), so that in NOTE 5, on the accuracy of this
the end of this period, discontinue gas dispersion of the carbon dioxide in the method when applied to asphalt cement
flow and heat. residue is restricted and the recovered having physical test properties within the
9.3.1 Alternative Procedure-Assemble asphalt is expected to have a penetration following ranges:
the apparatus as shown in Figure 1 with at 25°C (77°F) of less than 30, maintain
the separatory funnel in the thermometer the carbon dioxide gas flow and Penetration 25°C (77°F) 23 to 73
hole in the cork. Raise the aeration tube temperature for 20 to 22 minutes. Kinematic viscosity at
380 to 660
so that the bulb is above the surface of 9.5 The recovered asphalt can be heated 135°C (275°F), mm2/s (cST)
the solution. Fill the separatory funnel Softening Point, ring-and- 48 to 59
to reliquefy and portions taken for ball, °C (°F) (118 to 138)
with the centrifuged solution and open penetration, softening point, ductility, ash
the stopcock to fill the flask content, and kinematic and absolute
approximately one-half full of solvent viscosity determinations as required. Ash NOTE 5-The task force data, on precision
mixture. Apply low heat to the flask and content determinations shall be tests on residues recovered by ASTM Method
start distillation. At this time lower the conducted on all recovered bitumens in D 1856. These data do not contain test data by
aeration tube so that the bulb is in contact Method E.
accordance with AASHTO T 111 and
with the bottom of the flask and reported with other test data on the
introduce carbon dioxide gas at a low rate recovered asphalt. Ash contents of
(approximately 100 mL/minute) to recovered asphalts greater than 1 percent 6
provide agitation and prevent foaming. ASTM, Subcommittee D-4 Road and Paving
may affect the accuracy of the Materials, Philadelphia. PA
Adjust the funnel stopcock to introduce
fresh solvent at a rate that will keep the

Number of samples 8 Softening point, ring-and- 0.83 (1.501)

Number of laboratories 4 ball, °C (°F)
Number of replicates, per 2
sample per laboratory Between-laboratory standard
Deviations
Within-laboratory standard Penetration, 25°C (77°F) 3.090
Deviations: Kinematic viscosity at 54.94
Penetration, 25°C (77°F) 1.836 135°C (275°F) mm/s (cSt)
Kinematic viscosity at 37.65 Softening point, ring-and- 2.11 (3.803)
135°C (275°F), mm2/s (cSt) ball, °C (°F)

OSHA Limits for Air Contaminants, ppm

29 CFR Ch. XVII (7-1-91 Edition)
a
Solvent TWA STELb CEILINGc PEAKd
Trichloroethylene 50 200 - -
a
8-hour time weighted average for 40-hour work week.
b
15-minute time weighted average per work day.
c
Maximum concentration except for peak.
d
5 minutes in any 2 hours for an 8-hour shift.

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