Improvement of Quality Management for Highway

and Bridge Construction and Maintenance

Appendix C-1

Laboratory Test on Asphalt Cement,

Emulsified Asphalt and Bituminous Mix

A. Laboratory Test on Asphalt Cement

DETERMINATION OF SPECIFIC GRAVITY

OF SEMI-SOLID BITUMINOUS MATERIALS

APPARATUS:

1. Pycnometer, glass, consisting of cylindrical or conical vessel carefully ground to receive an

accurately fitting glass stopper 22 to 26 mm. in diameter. The stopper shall be provided with a
hole 1.0 to 2.0 mm in diameter, centrally located in reference to the vertical axis. The top surface
of the stopper shall be smooth and substantially plane and the lower surface shall be concave in
order to allow all air to escape though the bore. The height of the concave section shall be 4.0 to
6.0 mm at the center. The stopper Pycnometer shall have the capacity of 24 to 30 ml. and shall
weight not more than 40 g.

2. Water bath, constant temperature, capable of maintaining the temperature within 0.1°C (0.2°F) of
the test temperature.

3. Thermometers, Calibrated liquid-in-glass, total immersion-type of suitable range with graduations

at least every 0.1 °C (0.2 °F) and a maximum scale error of 0.1 °C (0.2 °F).

Water Bath
Pycnometer with Stopper

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-1
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

DETERMINATION OF SPECIFIC GRAVITY

OF SEMI-SOLID BITUMINOUS MATERIALS

PROCEDURE:

1. Preparation of Equipment
1.1 Partially fill a 600 ml. or larger Griffin low-form beaker with freshly boiled and cooled distilled
water to a level that will allow the top of the pycnometer to be immersed to a depth of not
less than 40 mm.

1.2 Partially immersed the beaker in the water bath to a depth sufficient to allow the bottom of
the beaker to be immersed to a depth not less than 100 mm. while the top of the beaker is
above the water level of the bath. Clamp the beaker in place.

1.3 Maintain the temperature of the water bath within 0.1°C (0.2 °F) of the test temperature.

2. Calibration of Pycnometer:
2.1 Thoroughly clean, dry, and weight the pycnometer to the nearest 1mg. designate this mass
as A.

2.2 Remove the beaker from the water bath. Fill the pycnometer with fresh boiled distilled
water, placing the stopper loosely in the pycnometer. Place the pycnometer in the beaker
and press the stopper firmly in place. Return the beaker to the water bath.

2.3 Allow the pycnometer to remain in the water for a period of not less than 30 min. Remove
the pycnometer, immediately dry the top of the stopper with one stroke of a dry towel, (Note
1) then quickly dry the remaining outside area of the pycnometer and weight to the nearest
mg. Designate the mass of the pycnometer plus water as B.

NOTE 1: Do not re-dry the top of the stopper even if a small droplet of water forms due to expansion. If
the top is dried at the instant of removing the pycnometer from the water, the proper mass of the
contents at the test temperature will be recorded. If moisture condenses on the pycnometer during
weighing, quickly redry the outside of the pycnometer (excluding the top) before recording the mass.

PROPER TEST PROCEDURE:

1. Preparation of Sample – Heat the sample with care, stirring to prevent local overheating, until
the sample has become sufficiently fluid to pour. In no case should the temperature be raised to
more than 56°C (200°F) above the expected softening point for asphalt. Do not heat for more
than 30 mins. and avoid incorporating air bubbles into the sample.

2. Pour enough sample into the clean, dry, warmed pycnometer to fill it about three fourths of its
capacity. Take precautions to keep the material from touching the sides of the pycnometer above
the final level, and to prevent the inclusion of air bubbles (note 2).Allow the pycnometer and its
content to cool to ambient temperature for a period of not less than 40 mins. and weight of the
pycnometer plus sample as C.

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-2
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DETERMINATION OF SPECIFIC GRAVITY

OF SEMI-SOLID BITUMINOUS MATERIALS

3. Remove the beaker from the water bath. Fill the pycnometer containing the asphalt with freshly
boiled distilled or deionized water, placing the stopper loosely in the pycnometer. Do not allow
any air bubbles to remain in the pycnometer. Place the pycnometer in the beaker and press the
stopper firmly in place. Return the beaker to the water bath.

4. Allow the pycnometer to remain in the water bath for a period of not less than 30 min. Remove
the pycnometer from the bath. Dry and weigh using right technique and timing. Designate this
weight of Pycnometer plus sample plus water as D.

NOTE 2: if any air bubbles are in advertently included, remove by brushing the surface of the
asphalt in the pycnometer with high “soft” flame of the Bunsen burner. In order to avoid overheating,
do not allow the flame to remain in contact with asphalt more than few seconds at any one time.

CALCULATIONS:

1. Calculate the specific gravity to the nearest third decimal as follows :

Specific Gravity = (c-a)/ (b-a)-(d-c)

where:

a = mass of pycnometer (plus stopper)

b = mass of pycnometer filled w/ water

c = mass of pycnometer partially filled with asphalt

d= mass of pycnometer plus asphalt plus water

Page 3 of 3

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-3
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

A. Laboratory Test on Asphalt Cement

DETERMINATION OF LOSS ON HEATING

OF OIL AND ASPHALTIC COMPOUNDS

APPARATUS :

1. Oven - the oven shall be electrically heated and can be operated to temperatures up to 180 °C
(365 °F).

2. Rotating Shelf - the oven shall be provided with a circular metal having a minimum diameter of
250 mm (9.8 in.). The shelf shall be provided with a mechanical means of rotating it at the rated of
5 to 6 rpm.

3. Thermometer - An ASTM Loss on Heat Thermometer graduated in Celsius degrees, having a

range from 155 to 170 °C.

4. Container - The container in which the sample is to be tested shall be of metal or glass,
cylindrical in shape, and shall have a flat bottom. Its inside dimensions shall be substantially as
follows: diameter, 55 mm (2.17 in.), depth, 35 mm (1.38 in).

Rotary Oven

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-4
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

DETERMINATION OF LOSS ON HEATING

OF OIL AND ASHALTIC COMPOUNDS

PROCEDURE:

1. Preparation of sample - Heat the sample with care, stirring as necessary, to prevent local
overheating until it has become sufficiently fluid to pour. In no case should the temperature be
raised to more than 100°C or 180°F above the expected softening point. First test the material
under examination for water and, if water is present, remove it by suitable methods of
dehydration before subjecting the material to the loss on heating test, or obtain another sample
that is free of water.

2. Place 50.0 + 0.5 g. of sample of the water-free material to be tested in a tared container and
weight to the nearest 0.01 g. If the material has been heated to facilitate transfer, cool the
sample to room temperature before making the initial weighing. Set the oven to a temperature of
163°C (325°F), and place the container with the weighed sample on and near the circumference
of the circular shelf, in one of the recesses if the recommended shelf is used. Close the oven
and rotate the shelf during the entire test at a rate of 5 to 6 rpm. Maintain the temperature at
163 + 1°C (325 + 1°F) for 5 hours after the sample has been introduced and the oven has again
reached that temperature. The 5 hour period shall start when the temperature reaches 162°C
(324°F), and in no case shall the total time that sample in the oven be more then 5 hrs. and 15
mins. At the conclusion of the heating period, remove the sample from the oven, cool to room
temperature, weight to the nearest 0.01 g., calculate the loss due to heating.

3. Determine the temperatures by means of the specified thermometer, which shall be supported
from the shaft of the circular shelf in a vertical position approximately 19 mm (0.75 in.) inside the
periphery, and with the bottom of the thermometer bulb 6 mm (0.25 in.) above the shelf.

CALCULATION:

Please refer to the attached worksheet for the computation of the loss on heating of oil and asphaltic
compounds.

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-5
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

A. Laboratory Test on Asphalt Cement

DETERMINATION OF SOLUBILITY
OF ASPHALT MATERIALS IN TRICHLOROETHYLENE

APPARATUS AND MATERIALS

The assembly of the filtering apparatus is illustrated in Fig. 3. Details of the component parts are as
follows:

1. Gooch Crucible, glazed inside and outside with the exception of outside bottom surface. The
Approximate dimensions shall be a diameter of 44 mm. at the top, tapering to 36 mm. at the
bottom, and a depth of 2 mm.

2. Glass Fiber Pad, 3.2 cm, 3.5 or 3.7 cm. in diameter. (What man Grade 934 AH).

3. Filter Flask, heavy-wall, with side tube 250 or large capacity.

4. Filter Tube, 40 to 42 mm inside diameter.

5. Rubber Tubing or Adapter, for holding the Gooch crucible on the filter paper.

6. Erlenmeyer Flask - 125 ml. or other suitable container.

7. Oven - capable of maintaining a temperature of 110 + 5°c (230 + 10°F).

8. Desiccator - of suitable size, charged with an effective dessicant.

9. Analytical Balance

10. Reagent - Trichloroethylene, technical grade.

NOTE 1 - Other suitable assemblies permitting vacuum filtration with Gooch crucible may be used

Filtering Apparatus Assembly Oven

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-6
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

DETERMINATION OF SOLUBILITY
OF ASPHALT MATERIALS IN TRICHLOROETHYLENE

PROCEDURE:

1. Preparation of Sample - if the sample is not fluid, heat to any convenient temperature, but in any
o o
case not more than 100 C or 180 F above the softening point.

2. Transfer approximately 2 g. of the sample into the tared 125 ml Erlenmeyer Flask or other
suitable container. Weigh accurately to the nearest 1mg. Add 100 ml. of trichloroethylene to the
container in small portions with continous agitation until all lumps disappear and no undissolved
sample adheres to the container. Stopper the flask otherwise cover the container and set aside
for at least 15 mins.

3. Place the previously prepared and weighed crucible in the filtering tube. Wet the glass fiber pad
with the small portion of trichloroethylene and decant the solution through the glass fiber pad
of the crucible with or without light suction as maybe necessary. When the insoluble matter
is appreciable, retain as much of it as possible in the container until the solution has drained
through the mat. Wash the container with a small amount of solvent and, using a stream of
solvent from a wash bottle, transfer all insoluble matter to the crucible. Use a “policeman” if
necessary to remove any insoluble matter adhering to the container. Rinse the policeman and
container thoroughly. Wash the insoluble matter in the crucible with solvent until the filtrate is
substantially colorless, then apply strong suction to remove the remaining solvent. Remove the
crucible from the tube, wash the bottom free of any dissolved matter, and place the crucible on
top of an oven or on a steam bath until all odor of the trichloroethylene is removed. Place in an
oven at 110 + 5°C (230 + 10°F) for at least 20 mins. Cool in a desiccator for 30 + 5 min. and
weigh. Repeat the drying and weighing until constant weight (+ 0.3 mg) is obtained.

NOTE 2 - In order to obtain precise results, the cooling time in the Dessicator must be approximately
the same (within + 5 min.) after all heatings. For example if the empty crucible is weighed after a 30 +
5 minute cooling in the dessicator. Either empty crucibles or crucibles containing insoluble matter that
have remained in a desiccators overnight should be re heated in an oven for at least 30 min. then
allowed to cool for the prescribed period before weighing.

CALCULATION:

1. Calculate either the total percentage of insoluble matter or the percentage of sample soluble in
the solvent used as follows :
A

Insoluble, percent = x 100

B

Soluble, percent = 100 -

B

where :
A = total weight insoluble
B = total weight sample

2. For percentages of insoluble less than 1.0, report to the nearest 0.10%. For percentages of
insoluble 1.0 or more, report to the nearest 0.1 %.
Page 2 of 2

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-7
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

A. Laboratory Test on Asphalt Cement

SPOT TEST OF ASPHALTIC MATERIALS

APPARATUS

1. Flask, 50 ml capacity, either Florence Flask or wide mouth flat bottom Soxhlet flask
approximately 45 mm (1¾ in.) in diameter by 60 mm (2 3/8 in.) high.

2. Cork Stopper for Flask provided with a 200 (8 in.) length of 6.4 mm (1/4 in.) glass tubing.

3. Filter Paper Whatman No. 50, (the 70 mm size is sufficient).

4. Pipette or Buret with 0.1 ml graduations.

5. Thermometer - ASTM precision Thermometer 64°C or 64°F.

6. Balance - a balance conforming to the requirements of AASHTO M 231, Class C.

7. Materials:

a. Xylene - Chemically pure

b. Normal Heptane

Note 1: Xylene Equivalents - To determine the xylene equivalent two or more samples of the asphalt
to be examined shall be dispersed in the prescribe mixed solvent, the percentage of xylene being made
to vary by successive 5 percent (volume) increments until two asphalts solutions have been found, one
of which the solvent contains 5 percent more xylene shows a negative spot. The xylene equivalent
would then be reported by the xylene percentage in the two solvents used in these two solutions, for
example as 10-15 percent napthaxylene equivalent or 20-25 percent hepta-xylene equivalent” as the
case may be.

PROCEDURE

1. Preparation of sample - heat the sample with care, stirring to prevent local overheating, until the
sample has become sufficiently fluid to pour.

Spot Test on Asphaltic Materials

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-8
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

SPOT TEST OF ASPHALTIC MATERIALS

2. A sample weighing 2 + 0.02 g shall be placed in the flask. If it does not flow readily at room
temperature the flask shall be carefully heated until the sample can be spread in a thin film
covering the bottom of the lower portion of the flask which shall then be allowed to cool to room
temperature.

With the pipette or buret, place in the flask 10.2 ml of the specified solvent. Insert quickly into the
neck of the flask the cork stopper with its 200 mm (8 in.) length of tubing and swirl the flask with a
rapid circular motion for 5 sec. the flask shall then be immersed for 55 sec. and removed and
swirled for 5 sec.(unless the sample is a thin liquid in which case heating is necessary)

The Flask shall be removed from the bath and swirled for 5 sec, and each minute thereafter the
flask shall be alternately immersed for 55 sec. and removed and swirled for 5 sec until complete
dispersion has taken place.

3. After complete dispersion as judged by tilting the flask, the end of the glass tube shall be lowered
below the level of the solution and the flask allowed to cool for 30 min. at room temperature.

3.1 The asphalt solvent mixture shall then be warmed for 15 min. in a water bath maintained at
temperature of 32 + 0.5°C (89.6 + or 1.0°F). The asphalt solvent mixture shall be
thoroughly stirred and by means of a clean stirring rod a drop of the warm mixture shall be
placed on the Whatman No. 50 filter paper. After 5 min. the spot shall be examined by
holding the paper approximately at right angles to the line of vision with a good light source
(preferably diffused daylight) at the observers back. If the drop forms a brown or yellowish-
brown circular strain, with darker solid or annular nucleus in the center, the test shall be
reported as positive.

4. If, however the drop forms a uniform brown circular strain, judgment shall be set aside in its tightly
stoppered flask at room temperature in a subdued light, to be retest 24 h after the first
examination. The mixture warmed to 32 + 0.5°C (89.6 + 1.0°F) for 15 min. as before shall then
vigorously stirred until uniform and a drop from its shall again be placed on the filter paper. If the
drop 24 h old mixture still forms a uniformly brown circular strain, the test shall be reported as
“negative” but if a darker solid or annular nucleus, the test shall be reported as “positive”.

Page 2 of 2

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-9
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

A. Laboratory Test on Asphalt Cement

DETERMINATION OF PENETRATION OF BITUMINOUS MATERIALS

APPARATUS

1. Penetration Apparatus - any apparatus that permits the needle holder (spindle) to move
vertically without measurable friction and is capable of indicating the depth of penetration to the
nearest 0.1 mm. will be acceptable. The weight of the spindle shall be 47.50 + 0.05 g. The total
weight of the needle ad the spindle assembly shall be 50.0 + 0.05 g. Weight of 50 + 0.05 g and
100 + 0.05 g shall also be provided for total loads of 100 and 200 g, as required for some
conditions of the test. The surface on which the sample container rest shall be flat and the axis
of the plunger shall be at approximately 90o to this surface. The spindle shall be easily detached
for checking its weight.

2. Penetration Needle - The needle shall be made from fully hardened and tempered stainless
steel, grade 220-C or equal, HRC 54 to 60. It shall be approximately 50 mm (2 in.) in length and
1.00 to 1.02 mm (0.0394 to 0.0402 in.) in diameter. It shall be symmetrically tapered at
one end by grinding to cone having an angle between 8.7 and 9.7 over the entire cone length
and whose axis within 0.0127 mm, (0.005 in) maximum run out (total indicator reading). After
tapering, the point shall be ground off to a truncated cone, the smaller base of which shall be
from 0.14 to 0.16 mm (0.0055 to 0.0063 in.) in diameter. The truncation shall be square with the
needle axis within 2 deg, and the edge shall be sharp and free from burrs.

3. Sample Container - A metal or glass cylindrical, bottom container of essentially the following
dimension shall be used:

For penetration below 200:

Diameter, mm 55
Internal depth, mm 35

For penetration between 200 and 350:

Diameter, mm 70
Internal depth, mm 45

4. Water Bath - A bath having a capacity of at least liters and capable of maintaining a temperature
of 250.1 oC or any temperature of test within 0.1°C

5. Transfer Dish - When used, the transfer dish for the container shall be a cylinder with a flat
bottom made of glass, metal or plastic. It shall be provided with some means which will insure a
firm bearing and prevent rocking of the container. It shall have a minimum inside diameter of 90
mm (3.5 in.) and a minimum depth above the bottom bearing of 55 mm (2.17 in).

6. Timing Device - For hand-operated penetrometers any convenient timing device such as
electric timer, a stop watch, or other spring activated device may be used provided it is
graduated in 0.1 sec or less and is accurate to within + 0.1 sec for 60 second interval.

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-10
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DETERMINATION OF PENETRATION OF BITUMINOUS MATERIALS

7. Thermometers - Calibrated, liquid-in-glass thermometers of suitable range with subdivisions

and maximum scale error of 0.1°C (0.2°F) or any other thermometric device of equal accuracy,
precision and sensitivity shall be used.

8. Heater - An oven or hot plate, heated by electricity gas shall be provided for melting samples.

Standard Penetrometer

PROCEDURE:

1. Preparation of Sample

1.1 Heat the sample carefully to avoid local overheating until it has become fluid. Then with
constant stirring, raise the temperature of the asphalt sample not more than 100°C or 180°F
above its softening point or the tar-pitch sample not more than 56°C. Avoid the inclusion of
air-bubbles. Then pour it into the sample container to a depth such that, when cooled to the
temperature of test the depth of the sample is at least 10 mm greater than the depth to which
the needle is expected to penetrate. Pour separate samples for each variation in test
conditions.

1.2 Loosely cover each container and its contents as a protection against dust, and allow to cool
in an atmosphere at a temperature not higher than 30 °C or 86 °F and no lower than 20°C or
68°F for not less than 1½ h nor more than 2 h when the sample is in 175 ml (6 oz) container
for not less than 1 h nor more than 1½ h when the sample is in a 90 ml (3 oz) container.
Then place the sample in the water bath maintained at the prescribed temperature of test
along with the transfer dish if used, and allow it to remain for not less than 1 ½ h when the
sample is in a 175 ml (6 oz) container, and for not less than 1 nor more than 1½ h when the
sample is in a 90 ml (3 oz) container.

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-11
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

DETERMINATION OF PENETRATION OF BITUMINOUS MATERIALS

2. Test Conditions

2.1 Where the conditions of test are not specifically mentioned, the temperature, load and time
are understood to be 25°C, 100 g, 5 sec, respectively. Other conditions of temperature,
load and time maybe used for special testing, such as:

Temperature Load, g Time, sec

0°C (32°C) 200 60

4°C (39.2°F) 200 60

46.1°C (115°F) 50 5

In such cases, the specific conditions of test shall be reported.

3. Proper Test Procedure

3.1 Examine the needle holder and guide to establish the absence of water and other
extraneous matter. Clean the penetration needle with toluene or other suitable solvent, dry
with a clean cloth and insert the needle in the penetrometers. Unless otherwise specified,
place the 50 g. weight above the needle, making the total moving load 100 + 0.1 g. If test
are made with the penetrometer in the bath, place the sample container directly on the
submerged stand of the penetrometer. Keep the sample container completely covered with
the water in the bath. If the test are made with the penetrometer outside the bath, place the
sample container in the transfer dish, cover the container completely with water from the
constant temperature bath and place the transfer dish on the stand of the penetrometer. In
either case, position the needle by slowly lowering it until its tip just makes contact with
surface of the sample. This is accomplished by bringing the actual needle tip into contact
with its image reflected by the surface of the sample from a properly place source of light.
Either note the reading of the penetrometer dial or bring the pointer to zero. Quickly release
the needle holder for the specified period of time and adjust the instrument to measure the
distance penetrated in tenths of a millimeter. If the container moves, ignore the result.

3.2 Make at least three determinations at point on the surface of the sample not less than 10
mm from the side of the container and not less than 10 mm apart. If the transfer dish is
used, return the sample and transfer dish to the constant temperature bath between
determinations. Use a clean needle for each determination. If the penetration is greater
than 200, use at least 3 needles leaving them in the sample until the 3 determination have
been completed.

NOTE 1 - for referee test, penetration at temperatures other than 77°C (25°F) without
removing the sample from the bath.

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-12
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DETERMINATION OF PENETRATION OF BITUMINOUS MATERIALS

3.3 The needles, containers, and other conditions described in this method provide for
determination of penetration up to 350. However, the method maybe used for direct
determination up to 500 provided special containers and needles are used. The container
shall be at least 60 mm in depth. The over-all volume of material in the container should not
exceed 125 ml to permit proper temperature adjustment of the sample.

CALCULATION:

Report to the nearest whole unit the average of at least three penetrations whose values do not
differ by more than the amount shown below:

Penetration 0 50 150 150

to to to to

149 149 249 over

Maximum difference
between highest and
lowest determinations 2 4 6 8

Page 4 of 4

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-13
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

A. Laboratory Test on Asphalt Cement

DETERMINATION OF DUCTILITY OF BITUMINOUS MATERIALS

APPARATUS

1. Mold - the mold shall be made of brass, the ends b and b’ being known as clips, and the parts a
and a’ as sides of the mold. The dimensions of the assembled mold shall be show in Fig. 4 with
the permissible variations indicated.

2. Base Plate - the base plate shall be made of non-absorbent material, of sufficient thickness to
prevent deformation, and of a sufficient size to hold from one to three molds as desired. The
plate shall be flat so that the bottom surfaces of each mold will touch throughout.

3. Water Bath - the water Bath shall be maintained at the specified test temperature varying not
more than + 0.5°C (+ 1.0°F) from this temperature. The volume of water shall be not less than 50
mm and such that 10 l. the depth of the water shall not be less 50 mm and such that the mold
can be immersed to a depth of 25 mm. the water in the bath shall be free from oil and slime or
other organic growth.

4. Testing Machine - For pulling the briquette of bituminous material apart, any apparatus may be
used which is so constructed that the specimen will be continuously immersed in water, as
specified without undue vibration.

5. Thermometer - For test at 25°C (77°F) use ASTM Saybolt Viscosity Thermometer No. 17°C
(1°F) to measure the temperature of the water bath and the temperature of the water in the
testing machine. For test at other temperature, use ASTM thermometers of an appropriate range
and accuracy equal to that of the No. 17. Since the accuracy of the test results is dependent
upon closely controlled conditions of temperature, the thermometers should be calibrated by the
Method for Verification and Calibration of Liquid-in-Glass Thermometers (ASTM Designation :
E77).

6. Heater - an oven or hot plate, heated by electricity or gas, may be used to melt the bituminous
material.

7. Container - Any suitable container may be used to hold the bituminous material while being
melted.

8. Trimmer - Any convenient implement, such as putty knife, or spatula, maybe used provided that
the cutting edge is straight and at least 38 mm (1 ½ in) wide.

9. Materials - mercury or glycerin and talc.

Standard ductility machine

Mold for ductility

Page 1 of 3
test specimen

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-14
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

DETERMINATION OF DUCTILITY OF BITUMINOUS MATERIALS

PROCEDURE

1. Preparation of Apparatus - Assemble the mold on the base plate, and to prevent the material
under test from sticking, coat the surface of the plate and the interior surfaces of sides a and a’
with the suitable release agent (Note 1).

NOTE 1 - Mixtures of glycerine and dextrine or talc (3 grams glycerine to about 5 grams dextrine or
talc has been used satisfactorily), Dow-Corning Silicone Stop-Cock Grease, or castor oil-versamid
900 [100:1 mixture by weight heated to 204 to 232°C ( 400 to 450°F) and stirred until homogeneous]
have been proven suitable. Other release agents may be used provided results obtained are
comparable to those obtained when using one of the above.

2. Molding of Specimens - Heat the sample with care to prevent local overheating until it has
become sufficiently fluid to pour. After thorough stirring, taking care not to entrain any air bubbles,
pour the bituminous material into the mold. Pour the material in a thin stream back and forth from
end to end until the mold is more than level full. In filling the mold, take care not to disarrange the
parts of the mold and so distort the briquet. Let the mold and contents cool to room temperature
for a period of 30 to 40 mins. And then place the base plate and filled mold in the water bath, and
with a hot trimmer cut off the excess bituminous materials so that the mold is just level full. Take
care during the trimming operation that the specimen is not pulled away from the base plate or
from the side pieces of the mold.

3. Keeping Specimen at Standard Temperature - Place the base plate and mold, with briquette
specimen, in the water bath and keep at specified temperature for a period of 85 to 95 min. then
remove the briquet from the plate, detach the side pieces, and immediately test the briquet.

4. Testing - At the start of the test, the water in the tank of the testing machine shall cover the
specimen both above and below by 25 mm. Attach the clips to the pins or hooks of the testing
machine and pull the clips apart at the specified rate of spread until the briquet ruptures or the
limit of travel of the machine of the machined is reached. If necessary, by the use of solute
which does not interfere with the test, adjust the specific gravity of the liquid in the testing
machine so that the bituminous material neither comes to the surface nor touches the bottom of
the bath at any time during the test. Measure and record the distance through which the clips
have been pulled to produce rupture, or record the fact if the specimen failed to rupture within
the capacity of the machine.

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-15
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DETERMINATION OF DUCTILITY OF BITUMINOUS MATERIALS

CALCULATION:

1. A normal test is one in which the material between the two clips pull out to a point or thread until
rupture occurs at the point where the thread has practically no cross-sectional area. Report the
average of three normal test as the ductility of the sample.

2. If the bituminous material comes in contact with the surface of the water or the bottom of the
bottom of the bath, the test shall not be considered normal. Adjust the specific gravity of the
bath by the addition of either methyl alcohol or sodium chloride so that the bituminous material
neither comes to the surface of the water, not touches the bottom of the bath at any time during
the test.

3. If a normal test is not obtained on three tests, report the ductility as being unobtainable under the
conditions of the test.

Page 3 of 3

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-16
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

A. Laboratory Test on Asphalt Cement

DETERMINATION OF FLASH POINT BY CLEVELAND OPEN CUP

APPARATUS

1. Cleveland Open Cup Apparatus - this apparatus consist of the test cup, heating plate, test
flame, applicator, heater, and supports. The assembled apparatus, eating plate, and cup are
illustrated in Fig. 5, 6, 7 respectively.

2. Shield - a shield 460 mm (18 in) square and 610 mm (24 in) high and having an open front is
recommended.

3. Thermometer - A thermometer having a range as shown below :

Thermometer Number

Thermometer Range ASTM IP

20 to 760°F 11 F 28 F

- 6 to + 400°C 11 C 28 C

4. Pipet

NOTE 1 - There are automatic flash point testers available and in use which maybe advantageous in
the saving of testing time, permit the use of smaller samples, and have other factor which may merit
their use. If automatic testers are used, the user must be sure that all of the manufacturer’s instructions
for calibrating, adjusting, and operating the instruments are lowed. In any cases of dispute, the flash
point as determined manually shall be considered the referee test.

Cleveland Open Cup Apparatus

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-17
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

DETERMINATION OF FLASH POINT BY CLEVELAND OPEN CUP

PROCEDURE:

1. Preparation of Sample

Heat the sample with care, stirring to prevent local overheating, until it has become sufficiently
fluid to pour.

2. Proper Test Procedure

2.1 Fill the cup at any convenient temperature (Note 2) so that the top of the meniscus is
exactly at the filling line. If too much sample has been added to the cup, remove the excess,
using a pipet; however, if there is sample on the outside of the apparatus, empty, clean,
and refill it. Destroy any air bubbles on the surface of the sample.

NOTE 2 - Viscous samples should be heated until they are reasonably fluid before being poured into
the cup. For asphalt cement, the temperature during heating must not exceed 100°C or 180°F above
the expected softening point. Extra caution must be exercised with liquid asphalts which should be
heated only to the lowest temperature at which they can be poured.

2.2 Light the test flame and adjust it to a diameter of 3.8 to 5.4 mm. (0.15 to 0.2 in).

2.3 Apply heat initially so that the rate of temperature rise of the sample is 0.14 to 17 °C (25 to
30°F)/min. When the sample temperature is approximately 56 °C (100 °F) below the
anticipated flash point, decrees the heat so that the rate is 5 to 6 °C (9 to 11 °F)/min.

2.4 Starting at least 28°C (50°F) below the flash point, apply the test flame when the
temperature read on the thermometer reaches each successive 2°C (5°F) mark. Pass the
test flame across the center of the cup, at right angles to the diameter which passes
through the thermometer. With a smooth, continuous motion apply the flame either in a
straight line or along the circumference of a circle having a radius of at least 150 mm (6
in.) the center of the test flame must move in a plane not more than 2.5 mm (0.10 in.) above
the plane of the upper edge of the cup and passing in one direction only. At the time of the
next test flame application, pass the flame in the opposite direction. The time consumed in
passing the test flame across the cup in each case shall be about 1 s.

NOTE 3 - Meticulous attention to all details relating to the test flame applicator. Size the test flame,
rate the temperature increase, and rate of passing the test flame over the sample is necessary for
good results.

2.5 Record as the observed flash point the temperature read on the thermometer when a flash
appears at any point on the surface of the oil, but do not confuse the true flash with the
bluish halo that sometimes surround the test flame.

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-18
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DETERMINATION OF FLASH POINT BY CLEVELAND OPEN CUP

CALCULATION

1. Observe and record the barometric pressure at the time of the test. When the pressure differs
from 760 mm Hg, correct the flash or fire point, or both, by means of the following equations:

Corrected flash or fire point, or both = F + 0.06 (760 – P)

or Corrected flash on fire point, or both = C + 0.03 (760 – P)

where:
F = observed flash or fire point, or both to the nearest 5°F

C = observed flash or fire point , or both, to the nearest 2°F

P = Barometric Pressure, mm Hg

2. Record the corrected flash or fire point, or both, to the nearest 5°F or 2°C.

3. Report the recorded flash or fire point value, or both, as the COC flash or fire point or both T-48-
IP 36 of the sample tested.

Page 3 of 4

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-19
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and Bridge Construction and Maintenance

Laboratory Tests on Asphalt Cement (Sample)

Page 4 of 4

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-20
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

B. Laboratory Test on Emulsified Asphalt

DETERMINATION OF VISCOSITY OF EMULSIFIED ASPHALT

APPARATUS:

1. Saybolt Viscometer
2. Bath
3. 60 cc Receiving Flask
4. No. 100 Sieve
5. Thermometer

PROCEDURE:

1. Stir the sample thoroughly and pour into a 100 ml. flask. Place the flask in the water bath at 250C
for 30 mins.

2. Place the cork stopper in position and pour the sample into the viscometer through the No. 20
sieve

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-21
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B. Laboratory Test on Emulsified Asphalt

DETERMINATION OF VISCOSITY OF EMULSIFIED ASPHALT

3. Place a 60 cc receiving flask under the outlet tube. Snap the cork at the same time starting the
timer

4. Stop the timer the moment the lower meniscus on the flask reaches the 60 cc mark. Record the
effluent time in second.

Page 2 of 2

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-22
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

B. Laboratory Test on Emulsified Asphalt

SIEVE TEST OF EMULSIFIED ASPHALT

APPARATUS:

1. Sieve No. 20
2. Pan
3. Sodium Oleate Solution/Distilled Water
4. Balance

PROCEDURE:

1. Record the mass of the sieve + pan

2. Weigh 1000 gms of the emulsified asphalt into a suitable container

3. Pour the sample through sieve No. 20.

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-23
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SIEVE TEST OF EMULSIFIED ASPHALT

4. Wash the container and residue until the washwater is clear

5. Place the pan under the sieve and oven dry for two hours at 110 0C

6. Cool and weigh

CALCULATION:

Weight Residue
Sample Retained,% = ---------------------------- X 100
1000

Page 2 of 2

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-24
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

B. Laboratory Test on Emulsified Asphalt

DETERMINATION OF CEMENT MIXING OF EMULSIFIED ASPHALT

APPARATUS:

1. Sieves (No. 80 and No. 14)

2. Dish (watch glass)
3. Stirring Rod
4. Graduated Cylinder
5. Balance
6. Cement
7. Oven

PROCEDURE:

1. Dilute the emulsion with distilled water to a residue of 55%, as determined by the distillation test

CALCULATION:

Example: % residue = 58

55  58 x 100 = 95 ml of sample

For 100 ml solution:

100 - 95 = 5 ml of water for dilution

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-25
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DETERMINATION OF CEMENT MIXING OF EMULSIFIED ASPHALT

2. Sieve 50 grams of portland cement through No. 80 sieve

3. Measure a 100 ml solution with the computed proportion

4. Add the diluted solution to the 50 grams cement

Page 2 of 5

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-26
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DETERMINATION OF CEMENT MIXING OF EMULSIFIED ASPHALT

5. Stir the mixture at once with the steel rod using a circular motion at a rate of 60 rpm

6. At the end of the one minute mixing period, add 150 ml of distilled water and continue the stirring
for 3 minutes

7. Stir the mixture at once with the steel rod using a circular motion at a rate of 60 rpm

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-27
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DETERMINATION OF CEMENT MIXING OF EMULSIFIED ASPHALT

8. At the end of the one minute mixing period, add 150 ml of distilled water and continue the stirring
for 3 minutes

9. Weigh the No. 14 sieve with a pan or watch glass

10. Pour the mixture through a weighed No. 14 sieve. Use repeated washings to completely
remove material from the mixing bowl

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-28
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DETERMINATION OF CEMENT MIXING OF EMULSIFIED ASPHALT

11. Pour the washings over the sieve

12. Rinse the sieve using distilled water, held at a height approximately 6 inches until the water is
clear.

13. Place the sieve in the weighed watch glass/shallow pan and oven dry at 163 0C until constant
weight

Page 5 of 5

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-29
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

B. Laboratory Test on Emulsified Asphalt

DETERMINATION OF STORAGE STABILITY OF EMULSIFIED ASPHALT

APPARATUS:
1. Two (2) 500mL Cylinders
2. Glass Pipet
3. Balance
4. Beakers (1000 mL cap)
5. Oven

PROCEDURE:
1. Place a 500 ml sample to a glass cylinder

2. Stopper the cylinder and allow to stand undisturbed at laboratory air temperature for 24 hours.

3. Remove approximately 55 ml from the top of the emulsion by means of a pipet

4. Weigh 50 gms into the previously weighed beaker with a 7 inches glass rod inside and a watch
glass

5. Take the total weight of the beaker

6. Siphon off the next 390 ml from the cylinder without any disturbance to the bottom sample

7. Mix the emulsion remaining in the cylinder and weigh 50 grams into the previously weighed
beaker with glass rod and watch glass

8. Take the total weight of the beaker

9. Heat the two beakers containing the top and bottom sample in a stove for an hour to remove
0
water and then transfer in an oven at a temperature of 163 C for an hour. Cool and weigh

10. The numerical difference in the asphalt contents of the top and bottom samples represents the
storage stability of the emulsion

Page 1 of 1

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-30
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

B. Laboratory Test on Emulsified Asphalt

DETERMINATION OF RESIDUE BY EVAPORATION OF EMULSIFIED ASPHALT

APPARATUS:

1. Iron Still
2. Heat source
3. Thermometer

PROCEDURE:

1. Weigh iron still empty. Pour 200 gms sample in the iron still

2. Heat the iron still with sample until all water has evaporated, increase the temperature to 260 C
for 15 minutes. Extinguish the flame and weigh the iron still with residue

3. Immediately pour the contents of the iron still into a residue container

4. Calculate the percent residue

Formula:
Weight Residue
%, Residue = ------------------------------------ x 100
200

Page 1 of 1

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-31
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Laboratory Tests on Emulsified Asphalt (Sample)

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-32
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Laboratory Tests on Emulsified Asphalt (Sample)

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-33
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and Bridge Construction and Maintenance

C. Laboratory Test on Bituminous Mixes

EXTRACTION TEST ON BITUMINOUS MIXES

APPARATUS:

1. Extraction machine
2. Oven
3. Pans
4. Filter Rings
5. Graduated Cylinder
6. Solvent (gasoline)

PROCEDURE:

1. Place the sample in a pan and heat/warm until it can be handled or mixed

2. Mix the sample thoroughly, quartering first before sampling

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-34
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EXTRACTION TEST ON BITUMINOUS MIXES

3. Weigh an 850 grams sample

4. Place the sample in the bowl

5. Cover the sample with the solvent (gasoline)

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-35
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EXTRACTION TEST ON BITUMINOUS MIXES

6. Weigh the filter ring

7. Fit the filter ring around the edge of the bowl

8. Clamp the cover on the bowl tightly

Page 3 of 5

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-36
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EXTRACTION TEST ON BITUMINOUS MIXES

9. Place container under the drain to collect the solvent. Start the centrifuge revolving slowly and
gradually increase the speed to a maximum of 3600 RPm until the solvent ceases to flow from the
drains. Allow the machine to stop, add 200 ml (or more as appropriate for mass of sample) solvent
and repeat the procedure at least three (3) times.

10. After the completion of the process transfer the aggregates from the bowl to the pan

O
11. Dry to constant mass together with the filter ring in an oven at 110  50 C. Cool and weigh

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-37
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EXTRACTION TEST ON BITUMINOUS MIXES

12. Cool the aggregates and the filter ring and weigh

CALCULATION:

W1 - (W2 + W3)
Asphalt Content, % by mass of dry aggregates = ------------------------------- x 100
W2 + W3

where:
W1 = mass of sample, grams
W2 = mass of extracted aggregates, grams
W3 = increase in mass of filter ring, grams

Page 5 of 5

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-38
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

C. Laboratory Test on Bituminous Mixes

GRADING/MECHANICAL ANALYSIS OF EXTRACTED AGGREGATES

APPARATUS:

1. Set of Sieves
2. Pans
3. Heating Device
4. Balance
5. Disbursing Agent

PROCEDURE:

1. Pans The test sample (aggregate from extraction test) after being dried & weighed shall be
placed in a container & covered with water. Add a sufficient amount of wetting or disbursing agent
such as calgon or soap which will promote the separation of fine material.

2. The contents of the container shall be agitated vigorously.

3. The wash water shall be poured over a 0.075 mm wash sieve. The operation shall be repeated
until the wash water is clear.

4. The washed aggregates in the container shall be dried to constant mass at a temperature of 110
 50C and weighed.

5. The aggregate shall be sieved over sieves of the various sizes required by the specification
covering the mixture, including the 0.075 mm sieve.

6. The weight of material passing each sieve and retained on the next and the amount passing the
0.075 sieve shall be recorded. Compute & report percent (%) passing on each sieve.

Page 1 of 1

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-39
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

C. Laboratory Test on Bituminous Mixes

DETERMINATION OF BULK SPECIFIC GRAVITY OF BITUMINOUS MIXES

APPARATUS: Specific Gravity Balance

PROCEDURE:

1. Weigh the specimen in air

0
2. Immerse the specimen in water bath at 25 C for 3 to 5 minutes. Weigh.

3. Surface dry the specimen by blotting with a damp towel/cloth. Weigh

CALCULATION:

Formula:

Mass of the dry specimen in air, in grams

Bulk Specific Gravity, Mass of the specimen in
= -
Gmb Mass of the saturated-dry specimen in air, water, in grams
in grams

Page 1 of 1

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-40
 Improvement of Quality Management for Highway
and Bridge Construction and Maintenance

C. Laboratory Test on Bituminous Mixes

IMMERSION COMPRESSION TEST OF BITUMINOUS MIXES

APPARATUS:

1. Testing Machine

2. Balance

3. Molds

4. Supports

5. Heating Device

6. Oven

7. Water Bath

8. Spatula

PROCEDURE:

1. Weigh around 2000 grams of the sample. The weighed sample shall be brought to the molding
0
temperature which is 124  10 C.

2. Approximately one-half of the heated mixture shall be placed in the molding cylinder & spaded
vigorously 25 times with 15 of the blows being delivered around the inside of the mold & the
remaining 10 at random over the mixture.

Page 1 of 7

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-41
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C. Laboratory Test on Bituminous Mixes

IMMERSION COMPRESSION TEST OF BITUMINOUS MIXES

3. The sample shall be spaded vigorously 25 times with 15 of the blows being delivered around the
inside of the mold & the remaining 10 at random over the mixture. The remaining half of the
mixture shall be quickly transferred to the molding cylinder & the same spading action repeated.

4. The mixture shall be compressed between the top & bottom plungers under an initial load of 150
psi to set the mixture against the side of the mold. The support bars shall then be removed an the
entire molding load of 3000 psi shall be applied for 120 seconds.

5. The mixture shall be compressed between the top & bottom plungers under an initial load of 150
psi to set the mixture against the side of the mold. The support bars shall then be removed the
entire molding load of 3000 psi shall be applied for 120 seconds.

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-42
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IMMERSION COMPRESSION TEST OF BITUMINOUS MIXES

6. The specimen shall be removed from the mold with an ejection device. Make at least four
specimens.

0
7. After removal from the mold specimen shall be oven cured for 24 hours at 60 C

8. Allow the specimen to cool to room temperature for at least two hours then determine the bulk
specific gravity.

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-43
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IMMERSION COMPRESSION TEST OF BITUMINOUS MIXES

9. Air dry the two specimens for at least four hours prior to the determination of the dry stability.

0
10. Immerse the other two specimens in a water bath with a temperature of 50 C for four days.

11. Transfer the two specimens to another water bath with a temperature of 250C & store them there
for two hours.

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-44
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IMMERSION COMPRESSION TEST OF BITUMINOUS MIXES

12. Determine the wet stability.

CALCULATION:

Formula:
Wet Stability
Index of Retained Strength = x 100
Dry Stability

Page 5 of 7

Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-45
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Laboratory Tests on Bituminous Mix (Sample)

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-46
 Improvement of Quality Management for Highway
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Laboratory Tests on Bituminous Mix (sample)

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Quality Control Manual on Concrete and Steel Bridge Structures Appendix C1-47