ASTM D244-00
(Test Method)Standard Test Methods for Emulsified Asphalts
Standard Test Methods for Emulsified Asphalts
SCOPE
1.1 These test methods and practices, given under the headings titled Composition, Consistency, Stability, and Examination of Residue, cover the examination of asphalt emulsions composed principally of a semisolid or liquid asphaltic base, water, and an emulsifying agent. The test methods cover the following tests:Test SectionsComposition:Water Content4-10Residue and Oil Distillate by Distillation11-15Residue by Evaporation16-22Particle Charge of Cationic Emulsified Asphalts23-28Consistency:Viscosity (Saybolt Furol)29-33Stability:Demulsibility34-39Settlement40-45Cement Mixing46-52Sieve Test53-58Coating59-62Miscibility with Water63-65Freezing66-68Coating Ability and Water Resistance69-76Storage Stability of Asphalt Emulsion77-83Examination of Residue84-91Identification Test for Rapid Setting Cationic Emulsified Asphalt92-99Identification of Cationic Slow Set Emulsions100-105Field Coating Test on Emulsified Asphalts106-111Emulsified Asphalt/Job Aggregate Coating Test112-117Weight per Gallon of Emulsified Asphalt118-124Residue by Low-Temperature Vacuum Distillation126-131
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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American Association State
Designation: D 244 – 00 Highway and Transportation Officials Standard
AASHTO No.: T59
Standard Test Methods and Practices for
Emulsified Asphalts
This standard is issued under the fixed designation D244; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 2. Referenced Documents
2.1 ASTM Standards:
1.1 These test methods and practices, given under the
headings titled Composition, Consistency, Stability, and Ex- C150 Specification for Portland Cement
amination of Residue, cover the examination of asphalt emul- C778 Specification for Standard Sand
sions composed principally of a semisolid or liquid asphaltic D5 Test Method for Penetration of Bituminous Materials
base, water, and an emulsifying agent. The test methods cover D70 Test Method for Specific Gravity and Density of
the following tests: Semi-Solid Bituminous Materials
D86 Test Method for Distillation of Petroleum Products
Test Sections
Composition:
D88 Test Method for Saybolt Viscosity
Water Content 4-10
D113 Test Method for Ductility of Bituminous Materials
Residue and Oil Distillate by Distillation 11-15
D128 Test Methods for Analysis of Lubricating Grease
Residue by Evaporation 16-22
Particle Charge of Cationic Emulsified Asphalts 23-28
D139 TestMethodforFloatTestforBituminousMaterials
Consistency:
D140 Practice for Sampling Bituminous Materials
Viscosity (Saybolt Furol) 29-33
D977 Specification for Emulsified Asphalt
Stability:
Demulsibility 34-39
D2042 Test Method for Solubility of Asphalt Materials in
Settlement 40-45
Trichloroethylene
Cement Mixing 46-52
Sieve Test 53-58 D2397 Specification for Cationic Emulsified Asphalt
Coating 59-62
D3289 Test Method for Specific Gravity or Density of
Miscibility with Water 63-65
Semi-Solid and Solid Bituminous Materials by Nickel
Freezing 66-68
Coating Ability and Water Resistance 69-76 Crucible
Storage Stability of Asphalt Emulsion 77-83
E1 Specification for ASTM Thermometers
Examination of Residue 84-91
E11 Specification for Wire-Cloth Sieves for Testing Pur-
Identification Test for Rapid Setting Cationic Emulsified 92-99
Asphalt poses
Identification of Cationic Slow Set Emulsions 100-105
E145 Specification for Gravity-Convection and Forced-
Field Coating Test on Emulsified Asphalts 106-111
Ventilation Ovens
Emulsified Asphalt/Job Aggregate Coating Test 112-117
Weight per Gallon of Emulsified Asphalt 118-124
Residue by Low-Temperature Vacuum Distillation 126-131 3. Sample Conditioning for Testing
3.1 All emulsions with viscosity requirements of 50°C
1.2 The values stated in SI units are to be regarded as the
should be heated to 50 6 3°C in the original sample container
standard. The values given in parentheses are for information
in a 71°C water bath or oven. The container should be vented
only.
torelievepressure.Afterthesamplereaches50 63°C,stirthe
1.3 This standard does not purport to address all of the
sample to achieve homogeneity.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
Annual Book of ASTM Standards, Vol 04.01.
1 3
These test methods are under the jurisdiction of ASTM Committee D04 on Annual Book of ASTM Standards, Vol 04.03.
Road and Paving Materials and are the direct responsibility of Subcommittee Annual Book of ASTM Standards, Vol 04.04.
D04.42 on Emulsified Asphalt Tests. Annual Book of ASTM Standards, Vol 05.01.
Current edition approved July 10, 2000. Published September 2000. Originally Annual Book of ASTM Standards, Vol 14.03.
published as D244–26T. Last previous edition D244–99. Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 244
COMPOSITION
WATER CONTENT The end of the condenser shall be ground to an angle of 30 6
5° from the vertical axis of the condenser.
4. Scope
6.5 Trap—The trap shall be made of annealed glass con-
structed in accordance with Fig. 1(c) and shall be graduated in
4.1 This test method covers the procedure for determining
0.10-mL divisions from 0 to 2 mL, and in 0.20-mL divisions
the water content of an emulsified asphalt by reflux distillation
from2to25mL.
using a water trap.
6.6 Solvent—Xylolorotherpetroleumdistillateconforming
to the following distillation requirements: 98% distills be-
5. Significance and Use
tween 120 and 250°C. This distillation shall be conducted in
5.1 This test method measures the amount of water present
accordance with Test Method D86.
in the emulsified asphalt, as distinguished from either bitumen
or petroleum solvent.
7. Sample
6. Apparatus and Materials
7.1 Obtain a representative sample of the material for test
using standard procedures as specified in Practice D140.
6.1 MetalStill—Themetalstill(Fig.1(a))shallbeavertical
cylindrical vessel, preferably of copper, having a faced flange
NOTE 1—The difficulties in obtaining representative samples for this
at the top to which the head is tightly attached by means of a
determination are unusually great, so that the importance of sampling
clamp. The head shall be made of metal, preferably brass or cannot be too strongly emphasized.
copper,andshallbeprovidedwithatubulation25.4mm(1in.)
8. Procedure
in inside diameter.
6.2 Glass Still—The glass still (Fig. 1(b)) shall be a short- 8.1 When the material to be tested contains less than 25%
neck, round-bottom flask, made of well-annealed glass, and water, place 100 6 0.1 g of sample in the still. When the
having an approximate capacity of 500 mL. material contains more than 25% water, use a 50 6 0.1-g
6.3 Heat Source—The heat source used with the metal still sample. Thoroughly mix the sample to be tested with 200 mL
shall be a ring gas burner of 100-mm (4-in.) inside diameter or of solvent by swirling, taking proper care to avoid any loss of
an electric mantle heater. The heat source for the glass still material.
shall be either an ordinary gas burner or an electric heater. 8.2 Connect the still, trap, and condenser by means of
6.4 Condenser—The condenser shall be a water-cooled tight-fitting corks as shown in Fig. 1(a) or (b). Adjust the end
reflux glass-tube type, having a jacket not less than 400 mm in of the condenser in the trap to a position which will allow the
length, with an inner tube 9.5 to 12.7 mm in outside diameter. end to be submerged to a depth of not more than 1 mm below
A=45to55mm E=25to38mm
B = 14 to 16 mm F = 186 to 194 mm
C=12to16mm H=18to19mm
D = 235 to 255 mm
FIG. 1 Apparatus for Determining Water Content
D 244
the surface of the liquid in the trap after distillation conditions 13. Apparatus
have been established. When using the metal still, insert a
13.1 Aluminum-Alloy Still, (see Fig. 2), approximately
heavy paper gasket, moistened with the solvent, between the
1 3
241.3 mm (9 ⁄2 in.) in height by 95.3 mm (3 ⁄4 in.) in inside
lid and flange before attaching the clamp. 3
diameter with one 121-mm (4 ⁄4-in.) inside diameter ring
8.3 When the ring burner is used with the metal still, place
burner, having holes on the inner periphery and having three
it about 76.2 mm above the bottom of the still at the beginning
spacers, to ensure centering of burner around the still (see Fig.
of the distillation, and gradually lower it as the distillation
3).
proceeds. Regulate the heat so that the condensate falls from
NOTE 2—Residue by distillation results obtained with iron stills in
the end of the condenser at a rate of from 2 to 5 drops per
accordance with Method D244–66 are acceptable. Similarly results
second. Continue the distillation at the specified rate until no
obtainedwitha127-mm(5-in.)ringburnerasinsubsequentissuesofTest
water is visible on any part of the apparatus and a constant
Methods D244 are acceptable.
volumeofwaterisobtainedinthetrap.Removeanypersistent
13.2 Connection Apparatus, consisting of a 12.5 6 0.5 mm
ringofcondensedwaterinthecondensertubebyincreasingthe
glassormetalconnectingtube.Themetalconnectingtubemay
rate of distillation for a few minutes.
be secured to the lid by a threaded compressing fitting. Other
condensers of 12.5 6 0.5 mm glass or metal tubing may be
9. Calculation and Report
used providing that the wetted length is 400 to 550 mm (15.5
9.1 Calculate the water content as follows:
to 218).
13.3 Graduated Cylinder, 100-mL, with graduation inter-
Watercontent,% 5 ~A/B!3100 (1)
vals of 1.0 mL.
where:
13.4 Thermometer—Two ASTM Low-Distillation Ther-
A = volume of water in trap, mL, and
mometers,graduatedeitherinFahrenheitorCelsiusdegreesas
B = original weight of sample, g.
specified, having a range from−2 to+300°C, (30 to 580°F)
9.2 Report the result as “. water weight percent, ASTM
respectively, and conforming to the requirements for Ther-
D244.”
mometer 7C or 7F as prescribed in Specification E1, or any
other thermometric device of equal accuracy or response.
10. Precision and Bias
NOTE 3—For details of the assembly of apparatus for the distillation
test, see Fig. 4.
10.1 The following criteria should be used for judging the
acceptability of results (95% probability):
13.5 Balance,capableofweighing3500gtowithin 60.1g.
10.1.1 Duplicate results by the same operator should not be
14. Procedure
considered suspect unless they differ by more than the follow-
ing amount:
14.1 Weigh 200 6 0.1 g of a representative sample of the
Water Content, weight % Repeatability, weight %
emulsion in the previously weighed aluminum-alloy still (in-
30 to 50 0.8
cludinglid,clamp,thermometersandgasket,ifgasketisused).
14.2 Use a gasket of oiled paper between the still and its
10.1.2 The results submitted by each of two laboratories
cover, or grind the joint to a tight fit. Securely clamp the cover
should not be considered suspect unless they differ by more
onthestill.Othergasketmaterialsmaybeusedprovidingthey
than the following amount:
withstand the maximum temperature reached during distilla-
Water Content, weight % Reproducibility, weight %
tion.
30 to 50 2.0
14.3 Insert a thermometer, or other thermometric device,
RESIDUE AND OIL DISTILLATE BY DISTILLATION throughacork,ineachofthesmallholesprovidedinthecover.
Adjustthesethermometerssothattheendofthebulbofoneis
11. Scope 6.4 mm from the bottom of the still and the bulb of the other
is approximately 165.1 mm from the bottom of the still.
11.1 This test method covers the quantitative determination
14.4 Place the ring burner around the still about 152.4 mm
of residue and oil distillate in asphalt emulsions composed
(6 in.) from the bottom of the still.Apply heat by lighting this
principally of a semisolid or liquid asphaltic base, water, and
burnerandadjustingtolowflame.Alsoapplyjustenoughheat
an emulsifying agent.
from a bunsen burner to the connecting tube to prevent
condensation of water in this tube.
12. Significance and Use
12.1 This test method can be used for quantitative determi-
Available from P & H Electronics, 442 Columbia St., Lafayette, IN 47901,
nation of residue and oil distillates in asphalt emulsions for
KoehlerInstruments,Inc.,168-56DouglasAve.,Jamaica,NY11433,andHumboldt
specification acceptance, service evaluation, control, and re-
Mfg. Co., 7300 W. Agatite Ave., Chicago, IL 60656.
search.Thistestmethodcanalsobeusedtoobtainresidueand 9
Available from Humboldt Manufacturing Co., Catalog No. H-1876, 7302 W.
oil distillate for further testing. Agatite Ave., Chicago, IL 60656.
D 244
NOTE 4—The location of the burner at the start of the test is flexible. It
may be raised to decrease chance of foam-over or lowered to middle of
still for emulsion containing no solvent.Asudden change in temperature
reading of upper thermometer indicates foam on bulb. Remove heat until
foaming ceases.
14.6 Immediately at the expiration of the heating period,
again weigh the still and accessories as described in 14.1.
Calculate and report the percentage residue by distillation.
Record the volume of oil distillate to the nearest ⁄2mL.
Calculateandreporttheoildistillateasavolumepercentageon
the total emulsion. Save this oil distillate if identification is
desired.
NOTE 5—The aluminum-alloy still at room temperature (9.1) weighs
1.5 g more than at 260°C. Correct for this error by adding 1.5 g to gross
weight obtained in 14.6 prior to calculating the percentage of residue by
distillation.
14.7 Remove the cover from the still, stir, and immediately
poursuitableportionsoftheresidueintoan8-oztinorsuitable
molds and containers for making the required tests. Handle or
condition molds and containers for desired examination of the
residueasdescribedinSections86-91,andproceedasrequired
by the appropriate ASTM test method from the points that
follow the pouring stage. If there is foreign matter in the
residue, the material shall be poured through a 300-µm sieve
prior to pouring into the test molds and containers.
15. Precision and Bias
15.1 The following criteria should be used for judging the
acceptability of results (95% probability):
15.1.1 Duplicate results by the same operator should not be
considered suspect unless they differ by more than the follow-
ing amount:
Metric Equivalents
Residue by Distillation, Repeatability,
weight % weight %
in. mm
50 to 70 1.0
⁄8 3.2
⁄16 4.8
15.1.2 The results submitted by each of two laboratories
⁄8 9.5
should not be considered suspect unless they differ by more
⁄2 12.7
than the following amount:
⁄16 14.3
⁄8 15.9
Residue by Distillation, Reproducibility,
⁄4 19.1
weight % weight %
1 25.4
50 to 70 2.0
1 ⁄8 41.3
1 ⁄4 44.5
15.2 The precision for penetration of residue from distilla-
2 ⁄4 57.2
tion by this method is the same as that shown in Section 79.
2 ⁄2 63.5
4 101.6
5 ⁄8 130.2
RESIDUE BY EVAPORATION
6 ⁄4 158.8
7 ⁄4 184.2
9 ⁄2 241.3
16. Scope
16.1 This test method covers procedures for a relatively
NOTE 1—The still cover may be machined from Rolled Aluminum
rapid determination of the percentage of emulsion residue.
Plate Alloy 3003-H14.
FIG. 2 Aluminum-Alloy Still
17. Significance and Use
14.5 Move the ring burner approximately level with the 17.1 The test may be used to indicate compositional char-
bottom when the temperature can be read on the lower acteristics of emulsified asphalt. Evaporation residue may also
thermometer, approxima
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