A.

WATER CONTENT

Standard Method: D244 and D86

Scope

This test method covers the procedure for determining the water content of an emulsified asphalt by reflux distillation
using a water trap.

Significance and Use

This test method measures the amount of water present in the emulsified asphalt, as distinguished from either bitumen or
petroleum solvent.

Apparatus and Materials

Quantity Apparatus
Components of Apparatus:
1 Metal still
-vertical cylindrical vessel (preferably copper having a faced flange
at the top to which the head is tightly attached by means of a
clamp.
1 Glass still
-short-neck, round-bottom flask, made if annealed glass with a
capacity of 500 mL
1 Heat source
-ring gas burner of 100-mm inside diameter
-or electric mantle heater
1 Condenser
-water-cooled reflux glass-tube type
-with jacket not less than 400 mm in length
1 Trap
-made of annealed glass structed in accordance to Figure 1.
200 mL Solvent (xylol or other petroleum distillate conforming to the
following distillation requirements: 98% distills between 120°C or
250°C)

Procedure

1. Weight 50 g of sample into the distillation flask.

2. Mix the sample thoroughly with 200 mL solvent by swirling carefully.
3. Connect the still, trap, condenser using a tight-fitting cork.
4. Adjust the end of the condenser in the trap to a position which will allow the end of the submerged to a depth not
more than 1 mm below the surface of the liquid in the trap after distillation conditions have been established.
5. Insert a heavy paper gasket, moistened with the solvent, between the lid and flange before attaching the lamp, if
using metal still.
6. When using the ring burner, place it with the metal still about 76.2 mm above the bottom of the still at the beginning
of the distillation, gradually lower it as the distillation proceeds.
7. Regulate the heat so that the condensate falls from the end of the condenser at a rate 2 to 5 drops per second.
8. 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.
9. Remove any persistent ring or condensed water in the condenser tube by increasing the rate of distillation for a few
minutes.
10. Carry out in duplicate.

CALCULATION

Calculate water content following the equation below, where A is the volume of water in trap, and B is the mass of sample
distilled.
 A
% water content= × 100 %
B

B. RESIDUE AND OIL DISTILLATE BY DISTILLATION

Scope

This test method covers the quantitative determination of residue and oil distillates in asphalt emulsions.

Significant and Use

This test method can be used for quantitative determination of residue and oil distillate in asphalt emulsions for
specification acceptance, service evaluation, control and research. This test method can also be used to obtain residue and
oil distillate for further testing.

Apparatus

Quantity Apparatus
Components of Apparatus:
1 Aluminum alloy still
-241.3 mm height
-95.3 mm inside diameter

1 Ring burner
-121-mm inside diameter
-have holes on the inner periphery
-have three spaces
1 Glass still
-short-neck, round-bottom flask, made if annealed glass with a
capacity of 500 mL
1 Heat source
-ring gas burner of 100-mm inside diameter
-or electric mantle heater
1 Connection Apparatus
-12.5 ± 0.5 mm glass or metal connecting tube
-other condensers may be used as long as wetted length is 400 mm
to 550 mm
1 100-mL graduated cylinder
1 Thermometer 7C or 7F
1 Balance (capacity: 3500 ± 0.1 g)
 (a) Aluminimum still (b) Ring burner

Procedure

1. Weight aluminum alloy still (including lid, clamp, thermometers and gasket).
2. Weigh 200 ± 0.1 grams of a representative sample of the emulsion in the previously weight aluminum still.
3. Use a gasket of oiled paper between the still and its covers, or grind the joint to a tight fit.
4. Clamp the cover securely on the still.
5. Insert the thermometer through a cork in each of the small hole provided in the cover.
6. Adjust these thermometers so that the end of the bulb of one is 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.
7. Place the ring burner around the still about 152.4 mm from the bottom of the still.
8. Apply heat by lighting this burner and adjust to low flame.
9. Apply heat from a Bunsen burner to the connecting tube to prevent condensation of water in this tube.
10. Move the ring burner approximately level with the bottom when the temperature can be read on the lower
thermometer, approximately 215°C.
11. Increase the temperature to 260 ± 5°C, maintaining it at this temperature for 15 minutes. Complete the total
distillation for in 60 ± 15 min from the first application of heat.
Note: 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. A sudden change in temperature reading of upper
thermometer indicates foam on bulb. Remove heat until foaming ceases.
12. Weigh the still and its accessories after heating.
Note: At room temperature, the aluminum still weights 1.5 grams more that at 260°C. Make necessary corrections by
adding 1.5 grams to the gross weight obtained at 260°C before any calculations.
13. Record the volume of oil distillate to the nearest 0.5 mL.
14. Remove the cover from the still, stir, and immediately pour suitable portions of the residue into an 8-oz tin or suitable
molds and containers for making the required tests.
15. Handle or condition molds and containers for desired examination of the residue.
16. Sieve the material through 300-microns mesh if there is foreign material present in the sample prior to pouring into
the test mold.
Calculations

Percentage residue is calculated as follows, where mf is the mass of still with its accessories containing the sample after
distillation, m i is the mass of still and its accessories, and m s is the mass of sample distilled.
mf −m i
% residue= × 100 %
ms

C. IDENTIFICATION OF OIL DISTILLATE BY MICRO-DISTILLATION

Scope

This test method outlines the test procedure for re-distillation of oil distillate obtained from previously distilled emulsified
asphalt sample.

Significant and Use

The results of this test method identify and characterize the oil distillate recovered from the emulsified asphalt.

Apparatus

Quantity Apparatus
Procedure

Calculations

Percentage residue is calculated as follows, where mf is the mass of still with its accessories containing the sample after
distillation, m i is the mass of still and its accessories, and m s is the mass of sample distilled.
m f −m i
% residue= × 100 %
ms
D. ASPHALT RESIDUE BY EVAPORATION

Standard Method: ASTM D244

Scope

This test method covers procedures for a relatively rapid determination of the percentage of emulsion residue. Note that
as the test method for residue by evaporation tends to give an asphaltic residue lower in penetration and ductility than the
distillation method, material may be accepted but shall not be rejected as failing to meet specifications containing
requirements for determination of residue by distillation, on data obtained by evaporation. If residue from evaporation fails
to meet the requirements for properties specified for residue from distillation, tests shall be rerun using the distillation
method.

Significance

This test may be used to indicate compositional characteristics of emulsified asphalt. Evaporation residue may also be
subjected to other characterization tests outlined under the examination of residue sections. However, properties of the
residue from the evaporation procedure may differ from those of the distillation residue.

Apparatus

Quantity Apparatus
3 1000 mL beaker (borosilicate glass or aluminum)
3 Stirring rod
1 Balance (500 g ± 0.1)
1 Oven
1 Sieve (300 microns mesh size)
Procedure

For residue non used for further analyses

1. Pre-heat oven to 163°C set point.

2. Weight clean, dry and empty 1000-L beaker with rod.
3. Weigh 50±0.1 g of thoroughly mixed emulsified asphalt into each of three beakers.
4. Place the beaker with rod containing the sample in the oven for two hours.
5. Remove each beaker and stir thoroughly the sample.
6. Replace to the oven for another hour of heating.
7. Remove the beakers from the oven.
8. Allow to cool to room temperature.
9. Weigh the beaker containing the sample with the rods.
10. If residue is to be analyzed further. Place the residue back to the oven and heat until sufficiently fluid.
11. Allow the sample to pass through a 300 microns sieve into a suitable container or molds for further analyses.

Raw Data Table

Sample from the Top Trial 1 Trial 2 Table 3

Weight of empty beaker + Rod (g)
Weight of sample (g)
Weight after 2 hours of heating
(beaker + rod + sample)
Weight after 3 hours of heating
(beaker + rod + sample) (g)
Calculations

Calculate the percentage of residue on each beaker as follows, where A is the weight of the beaker rod and residue, and B
is the tare weight of beaker and rod.

Residue , %=2(A−B)
Report the percentage residue as average of the three results.
E. ASPHALT RESIDUE BY DISTILLATION

Standard Method: ASTM D244

Scope

This test method covers the quantitative determination of residue and oil distillate in asphalt emulsions composed
principally of a semisolid or liquid asphaltic base, water and an emulsifying agent.

Significance

This test method can be used for quantitative determination of residue and oil distillates in asphalt emulsions for
specification acceptance, service evaluation, control, and research. This test method can also be used to obtain residue
and oil distillate for further testing.

Apparatus

Quantity Apparatus
1 Aluminum-Alloy Still
~241.3 mm height
~95.3 mm inside diameter
With one 121-mm inside diameter ring

Procedure

Raw Data Table

Trial 1 Trial 2 Table 3

Calculations

F. DETERMINATION OF VISCOSITY OF EMULSIFIED ASPHALT

Standard Method: ASTM D244

Scope

This test method employs the Saybolt Furol viscometer to measure the consistency of an asphalt emulsion. This is
applicable for all types of emulsions under the specifications stated in ASTM D 977 and D2397.

Significance

Viscosity is defined as the resistance of a fluid to flow. This property is important for emulsion asphalt as this determines
their applicability. When used in application types of construction, the material must be thin enough to be uniformly
applied through the spray bar of distributor, yet thick enough so that it will not flow from the crown or grade of the road.
For mixing grade emulsions, the viscosity may affect mixability and resulting thickness of film on the aggregate. The
viscosity of may emulsions is affected by shear. Therefore, strict adherence to test procedure is necessary to achieve
precision.

Apparatus

Quantity Apparatus
1 Saybolt Furol Viscometer (complies with specifications in ASTM D88)
1 Sieve (850 µm or No.20)
1 ASTM Thermometer No. 17C or 17F (for 25°C)
ASTM Thermometer No. 19F or 19C (for 50°C)
1 Water bath (capable of maintaining 25°C and 50°C)
Procedure

A. Preparation of Apparatus
1. Clean the viscometer thoroughly with an appropriate solvent of low toxicity.
2. Remove all solvent from the viscometer and its gallery.
3. Clean the receiving flask in the same manner.
4. Set-up the viscometer and bath in an area where they will not be exposed to drafts or rapid changes in air
temperature and dust or vapors that might contaminate the sample.
5. Place the receiving flask beneath the viscometer so that the graduation mark on the flask is from 100 to 130 mm
below the bottom of the viscometer tube, and so that the stream of oil will just strike the neck of the flask.
6. Fill the bath to at least 6 mm above the overflow rim of the viscometer with an appropriate bath medium.
7. Provide adequate stirring and thermal control for the bath so that the temperature of a test sample in the viscometer
will not vary more than ± 0.03°C (± 0.05°F) after reaching the selected test temperature.

Note:

 Do not make viscosity measurements at temperatures below the dewpoint of the room’s atmosphere.
 For calibration and referee tests. Keep the room temperature between 20 and 30°C and record the actual
temperature.
B. Calibration and Standardization
1. Calibrate the Saybolt Furol viscometer at periodic intervals by measuring efflux time at 37.8°C (100°F) using an
appropriate viscosity oil standard (See table below for reference).
2. Follow the procedure outlined in section C.
3. Efflux time of the viscosity oil standard shall equal the certified Saybolt viscosity value. If the efflux time differs from
the certified value by more than 0.2%, calculate a correction factor (F) for the viscometer as follows, where V is the
certified Saybolt viscosity of the standard, t is the measured efflux time.
V
F=
t

4. Repeat calibration procedure but at a temperature of 50.0°C using a viscosity oil standard having an efflux time of 90
s.
5. Viscometers or orifices requiring corrections greater than 1.0% shall not be used in referee testing.

C. Test at 25°C
1. Stir the sample thoroughly without incorporating bubbles and pour it into a 118-mL bottle.
2. Place the bottle in water bath at 25°C for 30 minutes.
3. Mix the sample in the bottle by inverting it several times slowly enough to prevent bubble formation.
4. Pour the sample into the viscometer through the 850-µm sieve or 20-mesh strainer, allowing a small portion to flow
through the outlet tube to waste.
5. Place the cork in position.
6. Fill the viscometer without stirring the sample.

D. Determination of Viscosity
1. Establish and control the bath temperature at the selected test temperature.
Note: standard temperature for Saybolt Furol are 25.0°C, 37.8°C, 50.0°C, and 98.9°C.
2. Insert a cork stopper, having a cord attached for its easy removal, into the air chamber at the bottom of the
viscometer.
Note: Ensure that the cork fit tightly enough to prevent the escape of air.
3. Heat sample in its original container to the selected test temperature.
4. Stir the sample well.
5. Strain the sample through Sieve No.20 in the filter funnel directly into the viscometer until the level is above the
overflow rim.
6. Stir the sample in the viscometer with the appropriate viscosity thermometer equipped with a thermometer support.
Use a circular motion at 30 to 50 rpm in a horizontal plane.
7. Remove thermometer when the sample temperature remains constant within 0.03°C (0.05°F) of the test
temperature during 1 min of continuous stirring.
8. Immediately place the tip of the withdrawal tube in the gallery at one point and apply suction to remove oil until its
level in the gallery is below the overflow rim.
Note: Do not touch the overflow rim with the withdrawal tube as it reduces the effective liquid head of the sample.
9. Check that the receiving flask is in proper position.
10. Snap the cork from the viscometer using the attached cord, and start the timer at the same instant.
11. Stop the time the instant the bottom of the oil meniscus reaches the graduation mark on the receiving flask.
12. Record the efflux time in seconds to the nearest 0.1 s.

Table A.1 Raw Data Table

Trial 1 Trial 2
A. Calibration
Standard Oil Used
Temperature
Saybolt Furol Viscosity (s)
Correction Factor
B. Determination of Viscosity
Temperature
Efflux time (s)
Calculations

 Multiply the efflux time (t exp) with the correction factor ( F ) calculated for the viscometer.

Efflux time=F ×t exp

 Report the corrected efflux time as the Saybolt Furol viscosity of the oil at the temperature at which the test was
made.
 Report values to the nearest whole seconds for values of 200 or higher, otherwise report to the nearest 0.1 s.

Additional Theoretical Background

Table A.4 Recommended Bath Media

Table A.3 Saybolt Viscosity Oil Standards

G. STORAGE STABILITY TEST (24 HOURS)

Standard Method: ASTM D244

Scope

This test method relates the ability of an asphalt emulsion to remain as a uniform dispersion during storage. It is
applicable to asphalt emulsions composed principally of a semisolid or liquid asphalt or liquid asphaltic base, water, and an
emulsifying agent. Moreover, this test is useful in determining, in a comparatively short time, the storage stability or
settlement of emulsified asphalt. It is a measure of the permanence of the dispersion as related to time, but it is not to be
construed to have significance as a measure of other stability aspects involved in use.

Summary of Test Method

This test determines the difference in percent residue of samples taken from the top and bottom of material placed in
undisturbed simulated storage for 24 hours. The result is expressed as the average of the two individual values obtained
by determining the difference between the percent residue of the top and bottom samples for each storage cylinder.

Significance

This method covers the ability of the emulsified asphalt to remain as a uniform dispersion during storage.

Apparatus

Quantity Apparatus
2 500 mL graduated cylinders
-with cork stopper
-outside diameter of 50 mm
-graduation is 5 mL
1 50 mL pipet
1 Balance (500 g to within +- 0.1)
4 1000 mL breaker
4 Stirring rod
1 Oven- capable of maintaining a temperature of 163 ± 3°C

Procedure

1. Bring the temperature of the emulsion to room temperature (21°C to 27°C).

2. Place a 500 mL representative sample in each of the two glass cylinders.
3. Stopper the cylinders and allow them to stand undisturbed at laboratory air temperature for 24 hours.
4. Weigh four 1000 mL beaker with stirring rod.
5. After standing the two cylinders for a period of 24 hours, remove 55 mL from the top of the emulsion by means of
the pipet without disturbing the mixture.
6. Take approximately 390 mL of from each cylinder.
7. Mix thoroughly each portion remaining in the cylinder.
8. Mix thoroughly each portion taken of the sample from the top and bottom of the cylinder.
9. Weight 50.0 g of each sample into separate beakers.
10. Adjust the temperature of the oven to 163°C ± 2.8°C.
11. Place the beakers containing the rods and sample in the oven for two hours.
12. Remove the beaker from the oven and thoroughly stir the residue. Record the weight.
13. Replace in the oven for another hour.
14. Then remove the beakers from the oven. Take the weight.
15. Allow to cool to room temperature.
16. Weigh the beaker containing the sample together with the rods.

Raw Data Table

Sample from the Top Trial 1 Trial 2

Weight of empty beaker + Rod (g)
Weight of sample (g)
Weight after 2 hours of heating
(beaker + rod + sample)
 Weight after 3 hours of heating
(beaker + rod + sample) (g)
Sample from the Bottom Trial 1 Trial 2
Weight of empty beaker + Rod (g)
Weight of sample (g)
Weight after 2 hours of heating
(beaker + rod + sample)
Weight after 3 hours of heating
(beaker + rod + sample) (g)

Calculations

Calculate the storage stability or settlement for the cylinder as follows:

% stability =B− A
Where A is the percentage of residue from the top of the sample, B is the percentage from the bottom of the sample.

Percentage residue for the top and bottom is calculated as follows, where mf is the mass of beaker and rod with the
sample after drying for 3 hours, m i is the mass of empty beaker with rod, and ms is the mass of sample.
mf −mi
Percentage residue ( A∨B )= ×100 %
ms
Additional Theoretical Background

 When storing and handling emulsions, particles may stick together making flocculation which is not desirable in
subsequent handling in the construction of highways.
 Reasons for flocculation may be due to a low chemical load, thermal shock, or prolonged storage.
 Flocculation leads to coalescence, that is particle stick together making larger particle. Then the heavier asphalt
particles settle to the bottom of the storage tank. This may be due to the prolonged storage, lack of mixing, problem with
asphalt compatibility or wrong chemical load.
 Knowing settlement and storage stability of emulsions, one can design proper storage facility for storing emulsions
for a short term or long term.
 The end users may decide whether the emulsion is in good quality meeting with highway specifications.
H. STORAGE STABILITY TEST (5 DAYS)

Standard Method: ASTM D244

Scope

This test method measures the settlement of an emulsified asphalt that occurs in a cylindrical container.

Significance

This method is a measure of the uniformity of an emulsified asphalt dispersion in a cylindrical container.

Apparatus

Quantity Apparatus
2 500 mL graduated cylinders
-with cork stopper
-outside diameter of 50 mm
-graduation is 5 mL
1 50 mL pipet
1 Balance (500 g to within +- 0.1)
4 1000 mL breaker
4 Stirring rod
1 Oven- capable of maintaining a temperature of 163 ± 3°C

Procedure

1. Bring the temperature of the emulsion to room temperature (21°C to 27°C).

2. Place a 500 mL representative sample in each of the two glass cylinders.
3. Stopper the cylinders and allow them to stand undisturbed at laboratory air temperature for 5 days.
4. Weigh four 1000 mL beaker with stirring rod.
5. After standing the two cylinders for a period of 24 hours, remove 55 mL from the top of the emulsion by means of
the pipet without disturbing the mixture.
6. Take approximately 390 mL of from each cylinder.
7. Mix thoroughly each portion remaining in the cylinder.
8. Mix thoroughly each portion taken of the sample from the top and bottom of the cylinder.
9. Weight 50.0 g of each sample into separate beakers.
10. Adjust the temperature of the oven to 163°C ± 2.8°C.
11. Place the beakers containing the rods and sample in the oven for two hours.
12. Remove the beaker from the oven and thoroughly stir the residue. Record the weight.
13. Replace in the oven for another hour.
14. Then remove the beakers from the oven. Take the weight.
15. Allow to cool to room temperature.
16. Weigh the beaker containing the sample together with the rods.

Raw Data Table

Sample from the Top Trial 1 Trial 2

Weight of empty beaker + Rod (g)
Weight of sample (g)
Weight after 2 hours of heating
(beaker + rod + sample)
Weight after 3 hours of heating
(beaker + rod + sample) (g)
Sample from the Bottom Trial 1 Trial 2
Weight of empty beaker + Rod (g)
Weight of sample (g)
Weight after 2 hours of heating
 (beaker + rod + sample)
Weight after 3 hours of heating
(beaker + rod + sample) (g)

Calculations

Calculate the storage stability or settlement for the cylinder as follows:

% stability =B− A
Where A is the percentage of residue from the top of the sample, B is the percentage from the bottom of the sample.

Percentage residue for the top and bottom is calculated as follows, where mf is the mass of beaker and rod with the
sample after drying for 3 hours, m i is the mass of empty beaker with rod, and ms is the mass of sample.
mf −mi
Percentage residue ( A∨B )= ×100 %
ms
Additional Theoretical Background

The 24 hours storage stability is dealt with shorter storage stability of emulsified asphalt, while 5-day settlement test
investigate what would happens when it is stored for long time, possible problems which may raise due to lack of proper
mixing, asphalt compatibility, effect of wrong chemicals, etc.