ASTM D244-09(2017)
(Test Method)Standard Test Methods and Practices for Emulsified Asphalts
Standard Test Methods and Practices for Emulsified Asphalts
SIGNIFICANCE AND USE
5.1 This test method measures the amount of water present in the emulsified asphalt, as distinguished from either bitumen or petroleum solvent.
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 and practices:
Test
Sections
Composition:
Water Content
4 – 10
Residue and Oil Distillate by Distillation
See Test Method
D6997
Residue by Evaporation
See Test Method
D6934
Particle Charge of Cationic Emulsified Asphalts
See Practice
D7402
Consistency:
Viscosity (Saybolt Furol)
See Test Method
D7496
Stability:
Demulsibility
See Test Method
D6936
Settlement
See Test Method
D6930
Cement Mixing
See Test Method
D6935
Sieve Test
See Test Method
D6933
Aggregate Coating
See Practice
D6998
Miscibility with Water
See Practice
D6999
Freezing
See Practice
D6929
Coating Ability and Water Resistance
11 – 18
Storage Stability of Asphalt Emulsion
See Test Method
D6930
Examination of Residue
19 – 26
Identification Test for Rapid Setting Cationic Emulsified Asphalt
27 – 34
Identification of Cationic Slow Set Emulsions
See Practice
D7402
Field Coating Test on Emulsified Asphalts
35 – 40
Emulsified Asphalt/Job Aggregate Coating Test
41 – 46
Density of Emulsified Asphalt
See Test Method
D6937
Residue by Low-Temperature Vacuum Distillation
See Test Method
D7403
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Buy Standard
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation:D244 −09 (Reapproved 2017) American Association State
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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope
Emulsified Asphalt/Job Aggregate Coating Test 41–46
Density of Emulsified Asphalt See Test Method
1.1 These test methods and practices, given under the
D6937
headings titled Composition, Consistency, Stability, and Ex- Residue by Low-Temperature Vacuum Distillation See Test Method
D7403
amination of Residue, cover the examination of asphalt emul-
1.2 The values stated in SI units are to be regarded as the
sions composed principally of a semisolid or liquid asphaltic
standard. The values given in parentheses are for information
base, water, and an emulsifying agent. The test methods cover
only.
the following tests and practices:
Test Sections 1.3 This standard does not purport to address all of the
Composition:
safety concerns, if any, associated with its use. It is the
Water Content 4–10
responsibility of the user of this standard to establish appro-
Residue and Oil Distillate by Distillation See Test Method
D6997
priate safety, health, and environmental practices and deter-
Residue by Evaporation See Test Method
mine the applicability of regulatory limitations prior to use.
D6934
1.4 This international standard was developed in accor-
Particle Charge of Cationic Emulsified Asphalts See Practice
D7402 dance with internationally recognized principles on standard-
Consistency:
ization established in the Decision on Principles for the
Viscosity (Saybolt Furol) See Test Method
Development of International Standards, Guides and Recom-
D7496
Stability: mendations issued by the World Trade Organization Technical
Demulsibility See Test Method
Barriers to Trade (TBT) Committee.
D6936
Settlement See Test Method
2. Referenced Documents
D6930
Cement Mixing See Test Method 2
2.1 ASTM Standards:
D6935
C778Specification for Standard Sand
Sieve Test See Test Method
D6933
D5Test Method for Penetration of Bituminous Materials
Aggregate Coating See Practice
D70Test Method for Density of Semi-Solid Bituminous
D6998
Materials (Pycnometer Method)
Miscibility with Water See Practice
D6999
D86Test Method for Distillation of Petroleum Products and
Freezing See Practice
Liquid Fuels at Atmospheric Pressure
D6929
D113Test Method for Ductility of Bituminous Materials
Coating Ability and Water Resistance 11–18
Storage Stability of Asphalt Emulsion See Test Method
(Withdrawn 2016)
D6930
D128Test Methods for Analysis of Lubricating Grease
Examination of Residue 19–26
D139Test Method for Float Test for Bituminous Materials
Identification Test for Rapid Setting Cationic Emulsi- 27–34
fied Asphalt
D140Practice for Sampling Bituminous Materials
Identification of Cationic Slow Set Emulsions See Practice
D977Specification for Emulsified Asphalt
D7402
Field Coating Test on Emulsified Asphalts 35–40 D2042Test Method for Solubility of Asphalt Materials in
Trichloroethylene
1 2
These test methods and practices are under the jurisdiction ofASTM Commit- For referenced ASTM standards, visit the ASTM website, www.astm.org, or
tee D04 on Road and Paving Materials and are the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee D04.42 on Emulsified Asphalt Test. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Oct. 1, 2017. Published October 2017. Originally the ASTM website.
approved in 1926. Last previous edition approved in 2009 as D244–09. DOI: The last approved version of this historical standard is referenced on
10.1520/D0244-09R17. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D244−09 (2017)
D2397Specification for Cationic Emulsified Asphalt D6999Practice for Miscibility of Emulsified Asphalts
D3289Test Method for Density of Semi-Solid and Solid D7402PracticeforIdentifyingCationicEmulsifiedAsphalts
Asphalt Materials (Nickel Crucible Method) D7403Test Method for Determination of Residue of Emul-
D6929Practice to Evaluate the Effect of Freezing on Emul- sified Asphalt by Low Temperature Vacuum Distillation
D7496Test Method for Viscosity of Emulsified Asphalt by
sified Asphalts
D6930Test Method for Settlement and Storage Stability of Saybolt Furol Viscometer
E1Specification for ASTM Liquid-in-Glass Thermometers
Emulsified Asphalts
D6933Test Method for Oversized Particles in Emulsified E11Specification forWovenWireTest Sieve Cloth andTest
Sieves
Asphalts (Sieve Test)
D6934Test Method for Residue by Evaporation of Emulsi- E145Specification for Gravity-Convection and Forced-
Ventilation Ovens
fied Asphalt
D6935Test Method for Determining Cement Mixing of
3. Sample Conditioning for Testing
Emulsified Asphalt
D6936TestMethodforDeterminingDemulsibilityofEmul- 3.1 All emulsions with viscosity requirements of 50°C
sified Asphalt should be heated to 50 6 3°C in the original sample container
D6937Test Method for Determining Density of Emulsified in a 71°C water bath or oven. The container should be vented
Asphalt torelievepressure.Afterthesamplereaches50 63°C,stirthe
D6997Test Method for Distillation of Emulsified Asphalt sample to achieve homogeneity.
D6998Practice for Evaluating Aggregate Coating using
Emulsified Asphalts
COMPOSITION
WATER CONTENT 6.6 Solvent—Xylol or other petroleum distillate conforming
to the following distillation requirements: 98% distills be-
4. Scope
tween 120 and 250°C. This distillation shall be conducted in
4.1 This test method covers the procedure for determining
accordance with Test Method D86.
the water content of an emulsified asphalt by reflux distillation
7. Sample
using a water trap.
7.1 Obtain a representative sample of the material for test
5. Significance and Use
using standard procedures as specified in Practice D140.
5.1 This test method measures the amount of water present
NOTE 1—The difficulties in obtaining representative samples for this
in the emulsified asphalt, as distinguished from either bitumen
determination are unusually great, so that the importance of sampling
or petroleum solvent.
cannot be too strongly emphasized.
6. Apparatus and Materials
8. Procedure
6.1 MetalStill—Themetalstill(Fig.1(a))shallbeavertical
8.1 When the material to be tested contains less than 25%
cylindrical vessel, preferably of copper, having a faced flange
water, place 100 6 0.1 g of sample in the still. When the
at the top to which the head is tightly attached by means of a
material contains more than 25% water, use a 50 6 0.1-g
clamp. The head shall be made of metal, preferably brass or
sample. Thoroughly mix the sample to be tested with 200 mL
copper,andshallbeprovidedwithatubulation25.4mm(1in.)
of solvent by swirling, taking proper care to avoid any loss of
in inside diameter.
material.
6.2 Glass Still—The glass still (Fig. 1(b)) shall be a short-
8.2 Connect the still, trap, and condenser by means of
neck, round-bottom flask, made of well-annealed glass, and
tight-fitting corks as shown in Fig. 1(a) or (b). Adjust the end
having an approximate capacity of 500 mL.
of the condenser in the trap to a position which will allow the
6.3 Heat Source—The heat source used with the metal still
end to be submerged to a depth of not more than 1 mm below
shall be a ring gas burner of 100-mm (4-in.) inside diameter or
the surface of the liquid in the trap after distillation conditions
an electric mantle heater. The heat source for the glass still
have been established. When using the metal still, insert a
shall be either an ordinary gas burner or an electric heater.
heavy paper gasket, moistened with the solvent, between the
lid and flange before attaching the clamp.
6.4 Condenser—The condenser shall be a water-cooled
reflux glass-tube type, having a jacket not less than 400 mm in
8.3 When the ring burner is used with the metal still, place
length, with an inner tube 9.5 to 12.7 mm in outside diameter.
it about 76.2 mm above the bottom of the still at the beginning
The end of the condenser shall be ground to an angle of 30 6
of the distillation, and gradually lower it as the distillation
5° from the vertical axis of the condenser.
proceeds. Regulate the heat so that the condensate falls from
6.5 Trap—The trap shall be made of annealed glass con- the end of the condenser at a rate of from 2 to 5 drops per
structed in accordance with Fig. 1(c) and shall be graduated in second. Continue the distillation at the specified rate until no
0.10-mL divisions from 0 to 2 mL, and in 0.20-mL divisions water is visible on any part of the apparatus and a constant
from2to25mL. volume of water is obtained in the trap. Remove any persistent
D244−09 (2017)
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
ringofcondensedwaterinthecondensertubebyincreasingthe COATING ABILITY AND WATER RESISTANCE
rate of distillation for a few minutes.
11. Scope
9. Calculation and Report
11.1 This test method is intended to aid in the identification
9.1 Calculate the water content as follows:
of asphalt emulsions suitable for mixing with coarse-graded
calcareous aggregates. It can be applied to other aggregates.
Watercontent,% 5 ~A/B! 3100 (1)
(See Note 2.)
where:
A = volume of water in trap, mL, and
12. Significance and Use
B = original weight of sample, g.
12.1 Thistestmethodcoversthedeterminationoftheability
9.2 Report the result as “. water weight percent, ASTM
of an asphalt emulsion to (1) coat an aggregate thoroughly, (2)
D244.”
withstand a mixing action while remaining as a film on the
aggregate, and (3) resist the washing action of water after
10. Precision and Bias
completion of the mixing.
10.1 The following criteria should be used for judging the
13. Apparatus
acceptability of results (95% probability):
10.1.1 Duplicate results by the same operator should not be
13.1 MixingPan—Awhite-enameledkitchensaucepanwith
considered suspect unless they differ by more than the follow-
handle, of approximately 3-L capacity.
ing amount:
13.2 Mixing Blade—A putty knife with a 31.8 by 88.9-mm
Water Content, weight % Repeatability, weight %
steel blade with rounded corners.A254.0-mm kitchen mixing
30 to 50 0.8
spoon may be used as an alternative.
10.1.2 The results submitted by each of two laboratories
13.3 Sieves—Standard 19.0-mm and 4.75-mm sieves con-
should not be considered suspect unless they differ by more
forming to Specification E11.
than the following amount:
Water Content, weight % Reproducibility, weight % 13.4 Constant-Head Water-Spraying Apparatus—An appa-
30 to 50 2.0
ratusforapplyingtapwaterinasprayunderaconstantheadof
D244−09 (2017)
1 in = 25.4 mm 8 in. = 230.2 mm
2 in. = 50.8 mm 1 ft = 304.8 mm
6 in. = 152.4 mm 1 ft 10 ⁄4 in. = 577.9 mm
3 1
7 ⁄4 in = 196.9 mm 2 ft 1 ⁄2 in. = 647.7 mm
2ft6 ⁄2 in. = 774.7 mm
NOTE 1—Use galvanized steel sheeting for the tank.All joints and fitting attachments shall be soldered and shall be watertight.All couplings shall be
standard brass garden hose fittings. The 19-mm pipe valve shall be placed as close as possible to the bottom of the tank, allowing space to shut off the
valve. The tank shall be placed on a suitable stand, so that the distance from the bottom of the spray head to the top of the test sample is 0.914 m 6
25.4 mm.
FIG. 2Constant-Head Flow Tank
774.7 mm (Figs. 2 and 3). The water shall issue from the 14.2 Calcium Carbonate—Chemically pure, precipitated
apparatus in a low-velocity spray. calciumcarbonate(CaCO )shallbeusedasadusttobemixed
with the standard reference aggregate.
13.5 Thermometer—An ASTM low softening point ther-
mometer 15F (or 15C), having a range from −2 to 80°C and 14.3 Water—Tap water of not over 250 ppm CaCO hard-
conforming to the requirements in Specification E1. ness for spraying over the sample.
13.6 Balance,capableofweighing1000gtowithin 60.1g.
15. Sample
13.7 Pipet, of 10-mL capacity.
15.1 The sample shall be representative of the asphalt
emulsion to be tested.
14. Materials
14.1 Aggregate—Standard reference aggregate shall be a
16. Procedure for Tests with Dry Aggregate
laboratory-washed and air-dried limestone aggregate graded to
16.1 Carry out the test at 23.9 6 5.5°C.
pass the 19.0-mm sieve and be retained on the 4.75-mm sieve.
16.2 Weigh 461 g of the air-dried, graded reference aggre-
NOTE 2—Aggregates other than limestone may be used, provided
gate in the mixing pan.
calcium carbonate is omitted throughout the test method. Laboratory
washing and air drying of such aggregates shall also be omitted.
16.3 Weigh 4.0 g of CaCO dust in the mixing pan and mix
with the 461 g of aggregate for approximately 1 min by means
of a mixing blade to obtain a uniform film of dust on the
Limestone from the Monon Stone Co. of Monon, IN, has been found suitable
as reference aggregate. aggregate particles.
D244−09 (2017)
NOTE 1—A Speakman, Model 235S, all brass, fixed shower head has been found acceptable.
NOTE 2—Existing 101.6-mm diameter shower heads may continue to be used.
NOTE 3—0.05 in. = 1.3 mm
6 in. = 152.4 mm
7 ⁄4 in. = 196.9 mm
FIG. 3Spray Nozzle Assembly
NOTE3—Thetotalweightofaggregateanddustshallequal465g.Ifno
overflow water runs clear. Carefully drain off the water in the
calcium carbonate is included, the weight of aggregate alone shall be
pan. Scoop the mixture from the mixing pan on to absorbent
465g.
paper for evaluation of coating retention in the washing test.
16.4 Weigh 35 g of the asphalt emulsion into the aggregate
16.7 Evaluate the mixture immediately by visual estimation
in the pan and mix vigorously with the mixing blade for 5 min
astothetotalaggregatesurfaceareathatiscoatedwithasphalt.
usingatossingactioncreatedbyaback-and-forthmotioninan
16.8 Repeat the evaluation by visual estimation of the
elliptical path of the mixing blade or spoon. At the end of the
coating of aggregate surface area by asphalt after the mixture
mixing period, tilt the pan and permit a
...
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D244 − 09 (Reapproved 2017) American Association State
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. 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 U.S. Department of Defense.
1. Scope
Emulsified Asphalt/Job Aggregate Coating Test 41 – 46
Density of Emulsified Asphalt See Test Method
1.1 These test methods and practices, given under the
D6937
headings titled Composition, Consistency, Stability, and Ex- Residue by Low-Temperature Vacuum Distillation See Test Method
D7403
amination of Residue, cover the examination of asphalt emul-
1.2 The values stated in SI units are to be regarded as the
sions composed principally of a semisolid or liquid asphaltic
standard. The values given in parentheses are for information
base, water, and an emulsifying agent. The test methods cover
only.
the following tests and practices:
Test Sections 1.3 This standard does not purport to address all of the
Composition:
safety concerns, if any, associated with its use. It is the
Water Content 4 – 10
responsibility of the user of this standard to establish appro-
Residue and Oil Distillate by Distillation See Test Method
D6997 priate safety, health, and environmental practices and deter-
Residue by Evaporation See Test Method
mine the applicability of regulatory limitations prior to use.
D6934
1.4 This international standard was developed in accor-
Particle Charge of Cationic Emulsified Asphalts See Practice
D7402
dance with internationally recognized principles on standard-
Consistency:
ization established in the Decision on Principles for the
Viscosity (Saybolt Furol) See Test Method
Development of International Standards, Guides and Recom-
D7496
Stability:
mendations issued by the World Trade Organization Technical
Demulsibility See Test Method
Barriers to Trade (TBT) Committee.
D6936
Settlement See Test Method
2. Referenced Documents
D6930
Cement Mixing See Test Method 2
2.1 ASTM Standards:
D6935
C778 Specification for Standard Sand
Sieve Test See Test Method
D6933
D5 Test Method for Penetration of Bituminous Materials
Aggregate Coating See Practice
D70 Test Method for Density of Semi-Solid Bituminous
D6998
Materials (Pycnometer Method)
Miscibility with Water See Practice
D6999
D86 Test Method for Distillation of Petroleum Products and
Freezing See Practice
Liquid Fuels at Atmospheric Pressure
D6929
D113 Test Method for Ductility of Bituminous Materials
Coating Ability and Water Resistance 11 – 18
Storage Stability of Asphalt Emulsion See Test Method
(Withdrawn 2016)
D6930
D128 Test Methods for Analysis of Lubricating Grease
Examination of Residue 19 – 26
Identification Test for Rapid Setting Cationic Emulsi- 27 – 34 D139 Test Method for Float Test for Bituminous Materials
fied Asphalt
D140 Practice for Sampling Bituminous Materials
Identification of Cationic Slow Set Emulsions See Practice
D977 Specification for Emulsified Asphalt
D7402
Field Coating Test on Emulsified Asphalts 35 – 40 D2042 Test Method for Solubility of Asphalt Materials in
Trichloroethylene
1 2
These test methods and practices are under the jurisdiction of ASTM Commit- For referenced ASTM standards, visit the ASTM website, www.astm.org, or
tee D04 on Road and Paving Materials and are the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee D04.42 on Emulsified Asphalt Test. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Oct. 1, 2017. Published October 2017. Originally the ASTM website.
approved in 1926. Last previous edition approved in 2009 as D244 – 09. DOI: The last approved version of this historical standard is referenced on
10.1520/D0244-09R17. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D244 − 09 (2017)
D2397 Specification for Cationic Emulsified Asphalt D6999 Practice for Miscibility of Emulsified Asphalts
D3289 Test Method for Density of Semi-Solid and Solid D7402 Practice for Identifying Cationic Emulsified Asphalts
Asphalt Materials (Nickel Crucible Method) D7403 Test Method for Determination of Residue of Emul-
sified Asphalt by Low Temperature Vacuum Distillation
D6929 Practice to Evaluate the Effect of Freezing on Emul-
sified Asphalts D7496 Test Method for Viscosity of Emulsified Asphalt by
Saybolt Furol Viscometer
D6930 Test Method for Settlement and Storage Stability of
Emulsified Asphalts E1 Specification for ASTM Liquid-in-Glass Thermometers
E11 Specification for Woven Wire Test Sieve Cloth and Test
D6933 Test Method for Oversized Particles in Emulsified
Asphalts (Sieve Test) Sieves
E145 Specification for Gravity-Convection and Forced-
D6934 Test Method for Residue by Evaporation of Emulsi-
fied Asphalt Ventilation Ovens
D6935 Test Method for Determining Cement Mixing of
3. Sample Conditioning for Testing
Emulsified Asphalt
D6936 Test Method for Determining Demulsibility of Emul- 3.1 All emulsions with viscosity requirements of 50 °C
sified Asphalt should be heated to 50 6 3 °C in the original sample container
D6937 Test Method for Determining Density of Emulsified in a 71 °C water bath or oven. The container should be vented
Asphalt to relieve pressure. After the sample reaches 50 6 3 °C, stir the
D6997 Test Method for Distillation of Emulsified Asphalt sample to achieve homogeneity.
D6998 Practice for Evaluating Aggregate Coating using
Emulsified Asphalts
COMPOSITION
WATER CONTENT 6.6 Solvent—Xylol or other petroleum distillate conforming
to the following distillation requirements: 98 % distills be-
4. Scope
tween 120 and 250 °C. This distillation shall be conducted in
4.1 This test method covers the procedure for determining
accordance with Test Method D86.
the water content of an emulsified asphalt by reflux distillation
7. Sample
using a water trap.
7.1 Obtain a representative sample of the material for test
5. Significance and Use
using standard procedures as specified in Practice D140.
5.1 This test method measures the amount of water present
NOTE 1—The difficulties in obtaining representative samples for this
in the emulsified asphalt, as distinguished from either bitumen
determination are unusually great, so that the importance of sampling
or petroleum solvent.
cannot be too strongly emphasized.
6. Apparatus and Materials
8. Procedure
6.1 Metal Still—The metal still (Fig. 1(a)) shall be a vertical
8.1 When the material to be tested contains less than 25 %
cylindrical vessel, preferably of copper, having a faced flange
water, place 100 6 0.1 g of sample in the still. When the
at the top to which the head is tightly attached by means of a
material contains more than 25 % water, use a 50 6 0.1-g
clamp. The head shall be made of metal, preferably brass or
sample. Thoroughly mix the sample to be tested with 200 mL
copper, and shall be provided with a tubulation 25.4 mm (1 in.)
of solvent by swirling, taking proper care to avoid any loss of
in inside diameter.
material.
6.2 Glass Still—The glass still (Fig. 1(b)) shall be a short-
8.2 Connect the still, trap, and condenser by means of
neck, round-bottom flask, made of well-annealed glass, and
tight-fitting corks as shown in Fig. 1(a) or (b). Adjust the end
having an approximate capacity of 500 mL.
of the condenser in the trap to a position which will allow the
6.3 Heat Source—The heat source used with the metal still
end to be submerged to a depth of not more than 1 mm below
shall be a ring gas burner of 100-mm (4-in.) inside diameter or
the surface of the liquid in the trap after distillation conditions
an electric mantle heater. The heat source for the glass still
have been established. When using the metal still, insert a
shall be either an ordinary gas burner or an electric heater.
heavy paper gasket, moistened with the solvent, between the
lid and flange before attaching the clamp.
6.4 Condenser—The condenser shall be a water-cooled
reflux glass-tube type, having a jacket not less than 400 mm in
8.3 When the ring burner is used with the metal still, place
length, with an inner tube 9.5 to 12.7 mm in outside diameter.
it about 76.2 mm above the bottom of the still at the beginning
The end of the condenser shall be ground to an angle of 30 6
of the distillation, and gradually lower it as the distillation
5° from the vertical axis of the condenser.
proceeds. Regulate the heat so that the condensate falls from
6.5 Trap—The trap shall be made of annealed glass con- the end of the condenser at a rate of from 2 to 5 drops per
structed in accordance with Fig. 1(c) and shall be graduated in second. Continue the distillation at the specified rate until no
0.10-mL divisions from 0 to 2 mL, and in 0.20-mL divisions water is visible on any part of the apparatus and a constant
from 2 to 25 mL. volume of water is obtained in the trap. Remove any persistent
D244 − 09 (2017)
A = 45 to 55 mm E = 25 to 38 mm
B = 14 to 16 mm F = 186 to 194 mm
C = 12 to 16 mm H = 18 to 19 mm
D = 235 to 255 mm
FIG. 1 Apparatus for Determining Water Content
ring of condensed water in the condenser tube by increasing the COATING ABILITY AND WATER RESISTANCE
rate of distillation for a few minutes.
11. Scope
9. Calculation and Report
11.1 This test method is intended to aid in the identification
9.1 Calculate the water content as follows:
of asphalt emulsions suitable for mixing with coarse-graded
calcareous aggregates. It can be applied to other aggregates.
Water content, % 5 A/B 3 100 (1)
~ !
(See Note 2.)
where:
A = volume of water in trap, mL, and 12. Significance and Use
B = original weight of sample, g.
12.1 This test method covers the determination of the ability
9.2 Report the result as “. water weight percent, ASTM
of an asphalt emulsion to (1) coat an aggregate thoroughly, (2)
D244.”
withstand a mixing action while remaining as a film on the
aggregate, and (3) resist the washing action of water after
10. Precision and Bias
completion of the mixing.
10.1 The following criteria should be used for judging the
13. Apparatus
acceptability of results (95 % probability):
10.1.1 Duplicate results by the same operator should not be
13.1 Mixing Pan—A white-enameled kitchen saucepan with
considered suspect unless they differ by more than the follow-
handle, of approximately 3-L capacity.
ing amount:
13.2 Mixing Blade—A putty knife with a 31.8 by 88.9-mm
Water Content, weight % Repeatability, weight %
steel blade with rounded corners. A 254.0-mm kitchen mixing
30 to 50 0.8
spoon may be used as an alternative.
10.1.2 The results submitted by each of two laboratories
13.3 Sieves—Standard 19.0-mm and 4.75-mm sieves con-
should not be considered suspect unless they differ by more
forming to Specification E11.
than the following amount:
Water Content, weight % Reproducibility, weight % 13.4 Constant-Head Water-Spraying Apparatus—An appa-
30 to 50 2.0
ratus for applying tap water in a spray under a constant head of
D244 − 09 (2017)
1 in = 25.4 mm 8 in. = 230.2 mm
2 in. = 50.8 mm 1 ft = 304.8 mm
6 in. = 152.4 mm 1 ft 10 ⁄4 in. = 577.9 mm
3 1
7 ⁄4 in = 196.9 mm 2 ft 1 ⁄2 in. = 647.7 mm
2 ft 6 ⁄2 in. = 774.7 mm
NOTE 1—Use galvanized steel sheeting for the tank. All joints and fitting attachments shall be soldered and shall be watertight. All couplings shall be
standard brass garden hose fittings. The 19-mm pipe valve shall be placed as close as possible to the bottom of the tank, allowing space to shut off the
valve. The tank shall be placed on a suitable stand, so that the distance from the bottom of the spray head to the top of the test sample is 0.914 m 6
25.4 mm.
FIG. 2 Constant-Head Flow Tank
774.7 mm (Figs. 2 and 3). The water shall issue from the 14.2 Calcium Carbonate—Chemically pure, precipitated
apparatus in a low-velocity spray. calcium carbonate (CaCO ) shall be used as a dust to be mixed
with the standard reference aggregate.
13.5 Thermometer—An ASTM low softening point ther-
mometer 15F (or 15C), having a range from −2 to 80 °C and 14.3 Water—Tap water of not over 250 ppm CaCO hard-
conforming to the requirements in Specification E1. ness for spraying over the sample.
13.6 Balance, capable of weighing 1000 g to within 60.1 g.
15. Sample
13.7 Pipet, of 10-mL capacity.
15.1 The sample shall be representative of the asphalt
emulsion to be tested.
14. Materials
14.1 Aggregate—Standard reference aggregate shall be a
16. Procedure for Tests with Dry Aggregate
laboratory-washed and air-dried limestone aggregate graded to
16.1 Carry out the test at 23.9 6 5.5 °C.
pass the 19.0-mm sieve and be retained on the 4.75-mm sieve.
16.2 Weigh 461 g of the air-dried, graded reference aggre-
NOTE 2—Aggregates other than limestone may be used, provided
gate in the mixing pan.
calcium carbonate is omitted throughout the test method. Laboratory
washing and air drying of such aggregates shall also be omitted.
16.3 Weigh 4.0 g of CaCO dust in the mixing pan and mix
with the 461 g of aggregate for approximately 1 min by means
4 of a mixing blade to obtain a uniform film of dust on the
Limestone from the Monon Stone Co. of Monon, IN, has been found suitable
as reference aggregate. aggregate particles.
D244 − 09 (2017)
NOTE 1—A Speakman, Model 235S, all brass, fixed shower head has been found acceptable.
NOTE 2—Existing 101.6-mm diameter shower heads may continue to be used.
NOTE 3—0.05 in. = 1.3 mm
6 in. = 152.4 mm
7 ⁄4 in. = 196.9 mm
FIG. 3 Spray Nozzle Assembly
NOTE 3—The total weight of aggregate and dust shall equal 465 g. If no
overflow water runs clear. Carefully drain off the water in the
calcium carbonate is included, the weight of aggregate alone shall be
pan. Scoop the mixture from the mixing pan on to absorbent
465 g.
paper for evaluation of coating retention in the washing test.
16.4 Weigh 35 g of the asphalt emulsion into the aggregate
16.7 Evaluate the mixture immediately by visual estimation
in the pan and mix vigorously with the mixing blade for 5 min
as to the total aggregate surface area that is coated with asphalt.
using a tossing action created by a back-and-forth motion in an
16.8 Repeat the evaluation by visual estimation of the
elliptical path of the mixing blad
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D244 − 09 D244 − 09 (Reapproved 2017) American Association State
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. 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 U.S. Department of Defense.
1. 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 and practices:
Test Sections
Composition:
Water Content 4 – 10
Residue and Oil Distillate by Distillation See Test Method
D6997
Residue by Evaporation See Test Method
D6934
Particle Charge of Cationic Emulsified Asphalts See Test Method
D7402
Particle Charge of Cationic Emulsified Asphalts See Practice
D7402
Consistency:
Viscosity (Saybolt Furol) See Test Method
D7496
Stability:
Demulsibility See Test Method
D6936
Settlement See Test Method
D6930
Cement Mixing See Test Method
D6935
Sieve Test See Test Method
D6933
Aggregate Coating See Practice
D6998
Miscibility with Water See Test Method
D6999
Miscibility with Water See Practice
D6999
Freezing See Practice
D6929
Coating Ability and Water Resistance 11 – 18
Storage Stability of Asphalt Emulsion See Test Method
D6930
Examination of Residue 19 – 26
Identification Test for Rapid Setting Cationic Emulsi- 27 – 34
fied Asphalt
Identification of Cationic Slow Set Emulsions See Test Method
D7402
Identification of Cationic Slow Set Emulsions See Practice
D7402
Field Coating Test on Emulsified Asphalts 35 – 40
Emulsified Asphalt/Job Aggregate Coating Test 41 – 46
These test methods and practices are under the jurisdiction of ASTM Committee D04 on Road and Paving Materials and are the direct responsibility of Subcommittee
D04.42 on Emulsified Asphalt Test.
Current edition approved June 1, 2009Oct. 1, 2017. Published July 2009October 2017. Originally approved in 1926. Last previous edition approved in 20042009 as
D244 – 04.D244 – 09. DOI: 10.1520/D0244-09.10.1520/D0244-09R17.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D244 − 09 (2017)
Density of Emulsified Asphalt See Test Method
D6937
Residue by Low-Temperature Vacuum Distillation See Test Method
D7403
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
C778 Specification for Standard Sand
D5 Test Method for Penetration of Bituminous Materials
D70 Test Method for Density of Semi-Solid Bituminous Materials (Pycnometer Method)
D86 Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure
D113 Test Method for Ductility of Bituminous Materials (Withdrawn 2016)
D128 Test Methods for Analysis of Lubricating Grease
D139 Test Method for Float Test for Bituminous Materials
D140 Practice for Sampling Bituminous Materials
D977 Specification for Emulsified Asphalt
D2042 Test Method for Solubility of Asphalt Materials in Trichloroethylene
D2397 Specification for Cationic Emulsified Asphalt
D3289 Test Method for Density of Semi-Solid and Solid Asphalt Materials (Nickel Crucible Method)
D6929 Practice to Evaluate the Effect of Freezing on Emulsified Asphalts
D6930 Test Method for Settlement and Storage Stability of Emulsified Asphalts
D6933 Test Method for Oversized Particles in Emulsified Asphalts (Sieve Test)
D6934 Test Method for Residue by Evaporation of Emulsified Asphalt
D6935 Test Method for Determining Cement Mixing of Emulsified Asphalt
D6936 Test Method for Determining Demulsibility of Emulsified Asphalt
D6937 Test Method for Determining Density of Emulsified Asphalt
D6997 Test Method for Distillation of Emulsified Asphalt
D6998 Practice for Evaluating Aggregate Coating using Emulsified Asphalts
D6999 Practice for Miscibility of Emulsified Asphalts
D7402 Practice for Identifying Cationic Emulsified Asphalts
D7403 Test Method for Determination of Residue of Emulsified Asphalt by Low Temperature Vacuum Distillation
D7496 Test Method for Viscosity of Emulsified Asphalt by Saybolt Furol Viscometer
E1 Specification for ASTM Liquid-in-Glass Thermometers
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
E145 Specification for Gravity-Convection and Forced-Ventilation Ovens
3. Sample Conditioning for Testing
3.1 All emulsions with viscosity requirements of 50°C50 °C should be heated to 50 6 3°C3 °C in the original sample container
in a 71°C71 °C water bath or oven. The container should be vented to relieve pressure. After the sample reaches 50 6 3°C,3 °C,
stir the sample to achieve homogeneity.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
COMPOSITION
D244 − 09 (2017)
WATER CONTENT
4. Scope
4.1 This test method covers the procedure for determining the water content of an emulsified asphalt by reflux distillation using
a water trap.
4.2 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
4. Scope
4.1 This test method covers the procedure for determining the water content of an emulsified asphalt by reflux distillation using
a water trap.
5. Significance and Use
5.1 This test method measures the amount of water present in the emulsified asphalt, as distinguished from either bitumen or
petroleum solvent.
6. Apparatus and Materials
6.1 Metal Still—The metal still (Fig. 1(a)) shall be a vertical cylindrical vessel, preferably of copper, having a faced flange at
A = 45 to 55 mm E = 25 to 38 mm
B = 14 to 16 mm F = 186 to 194 mm
C = 12 to 16 mm H = 18 to 19 mm
D = 235 to 255 mm
FIG. 1 Apparatus for Determining Water Content
the top to which the head is tightly attached by means of a clamp. The head shall be made of metal, preferably brass or copper,
and shall be provided with a tubulation 25.4 mm (1 in.) in inside diameter.
6.2 Glass Still—The glass still (Fig. 1(b)) shall be a short-neck, round-bottom flask, made of well-annealed glass, and having
an approximate capacity of 500 mL.
6.3 Heat Source—The heat source used with the metal still shall be a ring gas burner of 100-mm (4-in.) inside diameter or an
electric mantle heater. The heat source for the glass still shall be either an ordinary gas burner or an electric heater.
6.4 Condenser—The condenser shall be a water-cooled reflux glass-tube type, having a jacket not less than 400 mm in length,
with an inner tube 9.5 to 12.7 mm in outside diameter. The end of the condenser shall be ground to an angle of 30 6 5° from the
vertical axis of the condenser.
D244 − 09 (2017)
6.5 Trap—The trap shall be made of annealed glass constructed in accordance with Fig. 1(c) and shall be graduated in 0.10-mL
divisions from 0 to 2 mL, and in 0.20-mL divisions from 2 to 25 mL.
6.6 Solvent—Xylol or other petroleum distillate conforming to the following distillation requirements: 98 % distills between 120
and 250°C.250 °C. This distillation shall be conducted in accordance with Test Method D86.
7. Sample
7.1 Obtain a representative sample of the material for test using standard procedures as specified in Practice D140.
NOTE 1—The difficulties in obtaining representative samples for this determination are unusually great, so that the importance of sampling cannot be
too strongly emphasized.
8. Procedure
8.1 When the material to be tested contains less than 25 % water, place 100 6 0.1 g of sample in the still. When the material
contains more than 25 % water, use a 50 6 0.1-g sample. Thoroughly mix the sample to be tested with 200 mL of solvent by
swirling, taking proper care to avoid any loss of material.
8.2 Connect the still, trap, and condenser by means of tight-fitting corks as shown in Fig. 1(a) or (b). Adjust the end of the
condenser in the trap to a position which will allow the end to be submerged to a depth of not more than 1 mm below the surface
of the liquid in the trap after distillation conditions have been established. When using the metal still, insert a heavy paper gasket,
moistened with the solvent, between the lid and flange before attaching the clamp.
8.3 When the ring burner is used with the metal still, place it about 76.2 mm above the bottom of the still at the beginning of
the distillation, and gradually lower it as the distillation proceeds. Regulate the heat so that the condensate falls from the end of
the condenser at a rate of from 2 to 5 drops per second. Continue the distillation at the specified rate until no water is visible on
any part of the apparatus and a constant volume of water is obtained in the trap. Remove any persistent ring of condensed water
in the condenser tube by increasing the rate of distillation for a few minutes.
9. Calculation and Report
9.1 Calculate the water content as follows:
Water content,%5 A/B 3100 (1)
~ !
where:
A = volume of water in trap, mL, and
B = original weight of sample, g.
9.2 Report the result as “. water weight percent, ASTM D244.”
10. Precision and Bias
10.1 The following criteria should be used for judging the acceptability of results (95 % probability):
10.1.1 Duplicate results by the same operator should not be considered suspect unless they differ by more than the following
amount:
Water Content, weight % Repeatability, weight %
30 to 50 0.8
10.1.2 The results submitted by each of two laboratories should not be considered suspect unless they differ by more than the
following amount:
Water Content, weight % Reproducibility, weight %
30 to 50 2.0
COATING ABILITY AND WATER RESISTANCE
11. Scope
11.1 This test method is intended to aid in the identification of asphalt emulsions suitable for mixing with coarse graded
calcareous aggregates. It can be applied to other aggregates. (See Note 2).
11.2 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
11. Scope
11.1 This test method is intended to aid in the identification of asphalt emulsions suitable for mixing with coarse-graded
calcareous aggregates. It can be applied to other aggregates. (See Note 2.)
D244 − 09 (2017)
1 in = 25.4 mm 8 in. = 230.2 mm
2 in. = 50.8 mm 1 ft = 304.8 mm
6 in. = 152.4 mm 1 ft 10 ⁄4 in. = 577.9 mm
3 1
7 ⁄4 in = 196.9 mm 2 ft 1 ⁄2 in. = 647.7 mm
2 ft 6 ⁄2 in. = 774.7 mm
NOTE 1—Use galvanized steel sheeting for the tank. All joints and fitting attachments shall be soldered and shall be watertight. All couplings shall be
standard brass garden hose fittings. The 19-mm pipe valve shall be placed as close as possible to the bottom of the tank, allowing space to shut off the
valve. The tank shall be placed on a suitable stand, so that the distance from the bottom of the spray head to the top of the test sample is 0.914 m 6
25.4 mm.
FIG. 2 Constant-Head Flow Tank
12. Significance and Use
12.1 This test method covers the determination of the ability of an asphalt emulsion to (1) coat an aggregate thoroughly, (2)
withstand a mixing action while remaining as a film on the aggregate, and (3) resist the washing action of water after completion
of the mixing.
13. Apparatus
13.1 Mixing Pan—A white-enameled kitchen saucepan with handle, of approximately 3-L capacity.
13.2 Mixing Blade—A putty knife with a 31.8 by 88.9-mm steel blade with rounded corners. A 254.0-mm kitchen mixing spoon
may be used as an alternative.
13.3 Sieves—Standard 19.0-mm and 4.75-mm sieves conforming to Specification E11.
13.4 Constant-Head Water-Spraying Apparatus—An apparatus for applying tap water in a spray under a constant head of 774.7
mm (Figs. 2 and 3). The water shall issue from the apparatus in a low-velocity spray.
13.5 Thermometer—An ASTM Low Softening Point Thermometerlow softening point thermometer 15F (or 15C), having a
range from −2 to 80°C80 °C and conforming to the requirements in Specification E1.
13.6 Balance, capable of weighing 1000 g to within 60.1 g.
13.7 Pipet, of 10-mL capacity.
D244 − 09 (2017)
NOTE 1—A Speakman, Model 235S, all brass, fixed shower head has been found acceptable.
NOTE 2—Existing 101.6-mm diameter shower heads may continue to be used.
NOTE 3—0.05 in. = 1.3 mm
6 in. = 152.4 mm
7 ⁄4 in. = 196.9 mm
FIG. 3 Spray Nozzle Assembly
14. Materials
14.1 Aggregate—Standard reference aggregate shall be a laboratory-washed and air-dried limestone aggregate graded to pass
the 19.0-mm sieve and be retained on the 4.75-mm sieve.
NOTE 2—Aggregates other than limestone may be used, provided calcium carbonate is omitted throughout the test method. Laboratory washing and
air-
...
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