Bituminous Materials and properties.pptx

BITUMINOUS
MATERIALS
Ms.Kanemozhe R K M.Tech
Department of Civil Engineering
National Institute of Technology, Tiruchirappalli – 620015.

PAVING BINDERS
 Bitumen
 Tar
 Cutback
 Emulsion
 Modified Binders

BITUMEN AND TAR - ORIGIN
 Naturally occurring deposits of bitumen are formed
from the remains of ancient, microscopic algae and other
once-living things.
 When these organisms died, their remains were
deposited in the mud on the bottom of the ocean or lake
where they lived.
 Under the heat and pressure of burial deep in the earth,
the remains were transformed into materials such as
bitumen, kerogen, or petroleum.
 Deposits at the La Brea Tar Pits are an example.
 There are structural similarities between bitumens and
the organic matter in carbonaceous meteorites.
However, detailed studies have shown these materials
to be distinct.

BITUMEN AND TAR - ORIGIN
 Asphalt or bitumen can sometimes be confused with "tar",
which is a similar black, thermoplastic material produced by
the destructive distillation of coal.
 During the early and mid 20th century when town gas was
produced, tar was a readily available product and extensively
used as the binder for road aggregates.
 The addition of tar to macadam roads led to the word tarmac,
which is now used in common parlance to refer to road-
making materials.
 However, since the 1970s, when natural gas succeeded town
gas, asphalt (bitumen) has completely overtaken the use of
tar in these applications.
 BITUMEN is a petroleum product obtained by the
distillation of petroleum crude. TAR is a thermoplastic
material obtained from the destructive distillation.

Sl.
No.
Bitumen Tar
1 Bitumen is found in black to brown
in colour
Tar is usually found in brown
colour
2 Bitumen is obtained from fractional
distillation of crude oil
Tar is obtained by destructive
distillation of coal or wood
3 Bitumen is soluble in carbon
disulphide and carbon tetra chloride
Tar is soluble in toluene
4 Molecular weight range for road
bitumen is 400 to 5000
Molecular weight range for road
tar is 150 to 3000
5 Bitumen consists of large amount of
aromatic hydrocarbon
Tar consist of large amount of
oily matter with lower molecular
weight
6 Bitumen show resistance to coating
road aggregate and also does not
retain in presence of water
Tar coats more easily and retain
it better in presence of water
7 Free carbon content is less Free carbon content is more
8 It shows more resistance to
weathering action
It shows less resistance to
weathering action
9 Less temperature susceptibility More temperature susceptibility

BITUMEN
 Bitumen is a complex material, its property
ranges from viscous liquid to brittle solid.
 While bitumen shows linear viscoelastic
behaviour at small strains, the nonlinear
behaviour becomes more prominent at large
strains (Monismith and Secor 1962, Pagen 1968,
Cheung and Cebon 1997).
 The deformation of bitumen is loading rate and
temperature dependent (Van der Poel, 1955,
Deshpande and Cebon 1997).

 Early uses of Bitumen in History
 Ancient uses in Road Construction
Water proofing
Mortars
Adhesives
1830s in Europe
1850s in USA

Known for its adhesive and cohesive assets, bitumen is mostly utilised in
the construction industry. Bitumen is applied on road paving because it is
viscous when hot, but solid once it cools down. Therefore Bitumen
operates as the binder/glue for pieces of the aggregate.
Bitumen is applied in construction and maintenance of:
 Highways  Reservoir and pool linings
 Airport runways  Soundproofing
 Footways / Pedestrian Ways  Pipe coatings
 Car parks  Cable Coatings
 Racetracks  Paints
 Tennis courts  Building Water Proofing
 Roofing  Tile underlying waterproofing
 Damp proofing  Newspaper Ink Production
 Dams  And many other applications
BITUMEN - APPLICATIONS

GLOBAL BITUMEN
 The global bitumen market size was USD 66.10
billion (around Rs.4.2 trillion) in 2015 and is
expected to witness significant growth over the
next eight years owing to increasing use in
various applications.

GLOBAL BITUMEN
 The Indian bitumen market that is currently
around 5 million tonnes is expected to grow in the
future due to the Government’s proposed construction
projects to upgrade the road network.
 In India, Bitumen is mostly used as a binder in road
construction and in roofing and waterproofing
applications.
 Nearly 90% of this demand is provided from domestic
production of bitumen, whilst the remaining 10% is
imported, mainly from the UAE and Iran.
 The bitumen currently used in India are either
penetration grades or the currently preferred viscosity
grades.

Bitumen Applications in India
Paving
Water
proofing and
Roofing

GLOBAL BITUMEN
 In the emerging global bitumen market, demand
is expected to reach 122 million tonnes by 2018.
Increasing road construction activities in the fast-
growing markets of India and China will be the
main growth drivers of the bitumen market in
Asia.
 During 2014–2015, total bitumen sales in India
were 4.8 million tonnes.
 VG 10 bitumen comprises 35% of demand in
India, VG 30 comprises 60% of demand and
VG 40 comprises 5% of demand.

BITUMEN - PROPERTIES
 Petroleum Bitumen, normally called “Bitumen” or “Asphalt”
is produced by refining crude oil.
 Natural or Refined, Blend of heavy Hydrocarbons
 Chemical constituents: Maltenes, Asphaltenes
 Bitumen is often defined as suspension of Asphaltene into a
Maltene matrix.
 Properties and qualities of bitumen depend on the crude oil
used for its manufacture.
Solid
Softens with temperature
Non volatile
Black
Adhesive
Cohesive
Water proof
Durable
Important
Properties

BITUMEN - MANUFACTURING
 It is produced to grade specification either by directly
refining or by blending. Polymers and additives are
sometimes used to modify the thermoplastic characteristics
of bitumen to enhance final product performance.
 The crude oil is pumped from storage tanks, where it is kept
at about 60°C, through a heat exchanger system where its
temperature is increased to typically 200°C by exchanging
heat gained from the cooling of newly produced products in
the refining process.
 The crude is then further heated in a furnace to typically
300° C where it is partly vaporized into an Atmospheric
Distillation Column. Here the physical separation of the
components occurs.

BITUMEN - MANUFACTURING
 The lighter components rise to the top and the heaviest
components (the atmospheric residue) fall to the bottom of the
column and pass through a second heat exchanger prior to
treatment in a vacuum distillation column.
 Finally, Bitumen is obtained by vacuum distillation or vacuum
flashing of atmospheric residue from the vacuum distillation
column. This is “straight run bitumen”.
 An alternative method of bitumen production is by precipitation
from residual fractions by propane or butane-solvent
deasphalting.
 The bitumen thus obtained has properties which derive from the
type of crude oil processed and from the mode of operation in the
vacuum unit or in the solvent deasphalting unit.
 The grade of the bitumen depends on the amount of volatile
material that remains in the product: the smaller the amount of
volatiles, the harder the residual bitumen.

Standard Bitumen Production Scheme

Typical Bitumen Production Scheme

CRUDE OIL ANALYSIS AND
SELECTION
 The crude oil or blends of crude oils can come from
several sources, those that would be naturally
occurring and those created or extracted from oil
sands or shale.
 Only a limited number of crude oils or blends are
considered are suitable for producing bitumen of the
required quality in commercial quantities.
 In general, heavy crude oils (G > 0.9) are used.
 These crude oils tend to contain higher sulphur
contents.
 Common practice – Blending crude oils
 Oil sand, shale oil and Oil shale

Venezuelan Nigerian Light
0
10
20
30
40
50
60
70
80
90
100
58
1
33
46
6
20
3
33
Gasoline
Kerosene
Gas oil
Residuum
CRUDE OIL VARIATIONS

DISTILLATION
 Most common refining process is straight reduction to
grade from petroleum crude oil or a crude blend, using
atmospheric and vacuum distillation.
 Atmospheric distillation is used for physically
separate light, lower boiling point, petrochemical and
fuel fractions from the non boiling component known as
Atmospheric Residuum.
 To remove the last traces of light of the lighter fractions
and avoid thermal transformation of the molecules, the
atmospheric residuum is introduced into a Vaccum
distillation unit.
 Depending on the specification grade requirements, the
vacuum residuum can be used either directly, further
processed, or used as a component of blended bitumens.

Schematic diagram of the Distillation Process

AIR RECTIFICATION
 A mild degree of air-blowing is commonly used to
make minor adjustments to the physical properties,
such as decreasing the penetration and/or
increasing the stiffness of the bitumen.
 Air rectified bitumens are predominantly used in
paving applications and the application
temperature is equal to paving application
temperatures using straight run bitumens.
 Air rectified bitumen materials are also used for the
production of polymer modified binder grades and
as the base bitumen for the production for the
production of bitumen emulsion.

SOLVENT DEASPHALTING
 The properties of vacuum residuum can be modified
by use of subsequent refining process steps.
 ROSE – Residual Oil Solvent Extraction
 Propane, Butane, Isobutene, pentane or super
critical solvent extraction
 To separate asphaltene type fractions from
residuums for producing lubricating oil base stocks.
 The hard bitumen remaining can be blended to
producing specification grade bitumen.

Schematic diagram of Propane Deasphalting Process

VACUUM DISTILLATION OF
THERMAL CRACKED RESIDUUM
 In a visbreaking unit, a residue stream is heated to
temperatures between 440-500°C.
 Long paraffinic side chains attached to aromatic rings are the
primary cause of the high pour point and viscosity seen with
residues. Visbreaking is carried out under conditions
optimised to break off these long side chains and
subsequently transform them to form shorter molecules with
lower viscosity and pour point.
 When used for bitumen production the thermally cracked
residuum is subjected to vacuum distillation to remove the
distillate fractions which are then further treated and used in
the fuel production.
 The product obtained after vacuum distillation is a hard
material which can be used as a blending component for
bitumen production.

Schematic diagram of the Thermal cracking Process

OXIDATION
 Oxidised or Blown bitumen
 85-140 cum/min of air through bitumen feedstock at
elevated temperatures  Change in Physical
properties
 Varying degrees of chemical reactions  Increase in
apparent molecular weight and polarity of bitumen 
Stiffening of Bitumen
 Catalysts (not true): Ferric chloride, Hydrochloric acid,
Phosphorous pentoxide, Phosphoric acid, Flux (Europe)
 Oxidation unit: Reactor vessel, Air blower, off-gas
treatment facility and temperature control equipment

OXIDATION
 The oxidation reaction is Exothermic.
 Reactor may be fitted with a water jacket and/or
water spray facility at the head of the reactor, or
internal addition of water, to control the bitumen
temperature.
 Injection of steam/water into the reactor head
space may also be used to reduce the oxygen
content of the off-gases to manage the risk of fire
or explosion.
 The rate of oxidation depends on feedstock
properties and operating parameters.

Schematic diagram of the Bitumen Oxidation Process

OTHER PROCESSES
 To produce small amounts of bitumen
 Further treatments or extraction processes applied
to residual materials, to remove or convert
constituents that are unsuitable for bitumen
performance.
 Hydrodesulphurisation, Hydrogenation

BITUMEN BLENDING
 To meet specifications
 Higher and Lower viscosity products or bitumen
are blended together.
 Blending at refinery, terminals or 3rd
party
facility where blend components and finished
products can be easily transported by truck, rail
or barge to their final locations.

BITUMEN – CHEMICAL
CHARACTERISTICS
 Complex chemical mixture of molecules that are
predominantly hydrocarbons.
 Predominantly soluble in Carbon disulphide
 Mostly in colloidal state
 Composition:
Carbon – 82 - 88%
Hydrogen – 8 - 11%
Sulphur – 0 - 6%
Oxygen – 0 - 1.5%
Nitrogen – 0 - 1%
Traces of metals – Vanadium, Nickel, Iron, Magnesium, Calcium
 Complete chemical analysis of bitumen is very
difficult
 Asphaltenes (5-25%) are responsible for viscosity

BITUMEN PROCESSING
 ASTM D4124-09 Standard Test Method for
Separation of Asphalt into Four Fractions
 ASTM D2007 – 11 Standard Test Method for
Characteristic Groups in Rubber Extender and
Processing Oils and Other Petroleum-Derived
Oils by the Clay-Gel Absorption
Chromatographic Method

STUDY OF BITUMEN
Bitumen is a visco-elastic material. Hence its properties are dependent
on temperature and rate of loading.
 Purity of material
 Safety in handling
 Cohesion
 Adhesion to aggregate
 Workability / Fluidity / Consistency for different operations
 Durability during service life of pavement
 Behaviour at high, low and average service temperature
 Behaviour at high temperature associated with construction activities

PURITY OF BITUMEN
 Pure bitumen completely dissolves in Carbon Disulphide.
Percentage insoluble material indicates the impurity of
bitumen.
 Bitumen should be free of water as it causes foaming at high
temperature.
 Test: Water content test
 ASTM D2042 – 15: Standard Test Method for Solubility of
Asphalt Materials in Trichloroethylene
 ASTM D1461 – 17: Standard Test Method for Moisture or
Volatile Distillates in Asphalt Mixtures

SOLUBILITY TEST – ASTM D2042
 Degree of solubility in Trichloroethylene of
Asphalt materials having no or less mineral
matter.
 The portion that is soluble in trichloroethylene
represents the active cementing constituents.
 This method is not applicable to tars and their
distillation residues or highly cracked petroleum
products.
 The sample is dissolved in trichloroethylene and
filtered through a glass fiber pad. The insoluble
material is washed, dried, and weighed.

 Bitumen or Gooch crucible – Glazed inside and outside; top dia-44
mm, tapered bottom dia-36 mm, depth-20 to 30 mm.
 Filter tube - 40 to 42 mm inside dia
 Filter flask – Heavy wall, 250, 500 or 1000 mL capacity
 Glass micro fiber filterpad – 30 – 32 mm dia, fine porosity, 1.5
micrometre particle retention
 Rubber Tubing or Adapter - for holding the crucible on the filter
tube.
 Erlenmeyer Flask, 125 mL.
 Oven, capable of maintaining a temperature of 110±5°C.
 Reagent - Trichloroethylene
APPARATUS REQUIRED

PROCEDURE
Crucible preparation:
 Place the crucible plus one thickness of the filter pad in an
oven at 110±5°C for 15 min.
 Allow to cool in a desiccator for 30±5 min, and then
determine the mass to the nearest 0.1 mg.
 Designate this mass as A. Store in the desiccator until ready
for use.
Sample preparation:
 If the sample is not fluid, heat to any convenient
temperature, but in any case not more than 100°C above the
softening point.
 Normally the temperature at which this test is run is not
critical, and it may be performed at the laboratory air
temperature.

PROCEDURE
 Transfer approximately 2 g of the sample into a tared 125-mL
Erlenmeyer flask or other suitable container. Smaller sample sizes
may be necessary if more than 0.5 % insoluble material is expected.
 Allow the sample to cool to ambient temperature and then
determine the mass to the nearest 1 mg. Designate this mass as B.
 Add 100 mL of the trichloroethylene to the container in small
portions with continuous agitation until all lumps disappear and
no undissolved sample adheres to the container.
 Stopper the flask or otherwise cover the container and set aside for
at least 15 min
 Place the previously prepared and weighed crucible in the filtering
tube. Wet the filter pad with a small portion of trichloroethylene
and decant the solution through the filter pad of the crucible with
or without light suction as may be necessary.

PROCEDURE
 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 colourless, 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 odour
of the trichloroethylene is removed.
 Place the crucible in an oven at 110±5°C for at least 20 min.
Cool the crucible in a desiccator for 30±5 min and determine its
mass to the nearest 0.1 mg. Repeat the drying and weighing
until constant mass is obtained. Designate this mass as C.

MOISTURE OR VOLATILE
DISTILLATES – ASTM D1461-17
 Determination of moisture or volatile petroleum fractions of the
asphalt in asphalt mixtures.
Apparatus:
 Metal Still - A vertical cylindrical still having a faced flange at
the top to which the head is tightly attached by means of a clamp.
The head shall be of metal, preferably of copper or brass, and
shall have a tube opening of 25.4 mm of inside diameter to
facilitate attachment of the specified trap/condenser assembly.
 Trap - Well-annealed glass. For determination of water in asphalt
mixtures, a glass trap of 10- or 25-mL capacity shall be used.
 Condenser -Water-cooled reﬂux glass-tube type, having a
condenser jacket not less than 400 mm long with an inner tube
9.5 to 12.7 mm in outside diameter. End of the condenser inserted
in the trap shall be ground off at an angle of 30° from the vertical
axis.

 Solvent – Aromatic solvent (High solvency and Dispersing power)
– Xylene or a blend of 20% toluene and 80% xylene. For asphalt
and similar petroleum products, a petroleum distillate, 5 % boiling
between 90 and 100°C and 90% distilling below 210°C may be
used.
 Heating Device— Any satisfactory source of heat that will be
capable of maintaining a rate of distillation of 85 to 95 drops⁄min.
Sampling:
 The sample shall be representative of the material and shall be of
such size as practical to ﬁll the container in which it is transported
to the laboratory. For duplicate tests, a 1.9-L friction-top tin pail
full of the material would be satisfactory.
Test Specimen and Sampling:
 Thoroughly mix the sample and weigh out an amount estimated to
show a percentage of moisture or diluent within the capacity of the
trap calibration. Keep the remainder of the sample in its tightly
covered container. The weighed sample should be preferably not
less than 500 g for normal mixtures. Thoroughly break up this
sample to avoid larger lumps, and place it in the still.

PROCEDURE FOR MOISTURE
DETERMINATION:
 After the sample has been placed in the still, add 200mL of the solvent and
quickly stir it into the sample.
 Assemble the components of the apparatus, choosing the trap in accordance
with the expected water content of the sample and making all connections
vapour and liquid tight.
 Insert a gasket of heavy paper, moistened with water between the still body
and cover. The condenser tube and trap must be chemically clean to ensure free
drainage of water into the bottom of the trap.
 Insert a loose cotton plug in the tip of the condenser to prevent condensation of
atmospheric moisture inside it. Circulate cold water through the jacket of the
condenser.
 Apply heat at such a rate that reﬂuxing will start within 5 to 10 min after the
heat has been applied and the condenser solvent will drip into the trap at a
rate of 85 to 95 drops/min.
 Continue the distillation until three successive readings of the trap at 15-min
intervals show no increase in the amount of water being condensed, except that
in no case shall distillation continue for more than 1.5 h.
 Allow the contents of the trap to reach room temperature and read the volume
of water in the trap to the nearest scale division. Record the volume of water
and calculate in weight percent.

PROCEDURE FOR VOLATILE
DISTILLATES DETERMINATION:
 After the sample has been placed in the still, add 350mL of water and
approximately 3 g of sodium carbonate (Na2CO3) and quickly stir into the
sample.
 Firmly attach the still cover and assemble the trap and condenser, except that
the gasket is moistened with solvent and the trap used shall be the dilution trap.
 Apply heat at such a rate that the water and solvent will begin to reﬂux in 5 to
10 min after the heat has been applied and will drip from the condenser at the
rate of 85 to 95 drops⁄min.
 In case the sample contains a large amount of very volatile solvent, it may be
necessary to add a second water-cooled condenser above the ﬁrst one or to reduce
the rate of distillation somewhat to prevent escape of the solvent.
 Continue distillation until three successive readings of the upper and lower
levels of the diluent at 15-min intervals show no increase in the quantity being
collected.
 Then remove the source of heat and allow the trap and contents to reach room
temperature. Allow the trap to stand a minimum of 30 min to permit the solvent
to separate.
 Record the volume of diluent in the trap to the nearest scale division and
calculate in weight percent.

SAFETY IN HANDLING
 Bitumen is heated to high temperatures and it should be
safe to handle at such temperatures.
 Test: Flash and Fire Point
 Flash point is used in shipping and safety regulations to
define flammable and combustible materials. It can indicate
the possible presence of highly volatile and flammable
materials in a relatively non-volatile or non-flammable
material.
 The fire point is one measure of the tendency of the test
specimen to support combustion.
 ASTM D92-16b: Standard Test Method for Flash and Fire
Points by Cleveland Open Cup Tester
 ASTM D93-16a: Standard Test Methods for Flash Point by
Pensky-Martens Closed Cup Tester

CONSISTENCY OF BITUMEN
 Degree of fluidity at a particular temperature
 Test: Penetration test, Softening point, Ductility, Fraass
Breaking point, Viscosity
 ASTM D5/D5M-13: Standard Test Method for
Penetration of Bituminous Materials
 ASTM D113-17: Standard Test Method for Ductility of
Asphalt Materials
 The Fraass Breaking Point is the temperature at which
bitumen first becomes brittle, as indicated by the
appearance of cracks when a thin film of the bitumen on
a metal plaque is cooled and flexed in accordance with
specified conditions.
 Viscosity – Fundamental Rheological property of bitumen

VISCOSITY
 It is the fundamental Rheological property of bitumen
 Rheology is the study of flow and deformation of materials.
 Sliding plate viscometer
 Rotational viscometer
 Efflux viscometers
 Capillary viscometer
 ASTM D2170/D2170M-10: Standard test method for Kinematic
Viscosity of Asphalts
 ASTM D2171: Standard test method for Viscosity of Asphalts by
Vacuum Capillary Viscometer
 ASTM D4402/D4402M-15: Standard test method for Viscosity
determination of Asphalt at elevated temperatures using a
Rotational Viscometer
 ASTM D7496-17: Standard test method of Emulsified Asphalt by
Saybolt Furol Viscometer

AGING OF BITUMEN
 Inevitable phenomena when bitumen is subjected to
environmental conditions in the presence of heat, light and
oxidation
 Causes: Loss of volatile matter and oxidation
 Short term and Long term aging
 Short term – Storage, transportation, mixing and placing
 Long term – Oxidation during service life
 Properties:
 Harder and stiffer bitumen
 Penetration and Ductility reduce.
 Viscosity and Softening point increase.

HARDENING MECHANISM
 Reversible
 Change in reorientation of microstructure
 Reversible with temperature, mechanical
energy
 Irreversible
 Permanent changes to microstructure
 Chemical changes and loss of material

REVERSIBLE HARDENING
 Steric hardening
 Change in Structure during application of tensile
load
 Extremely slow process occurring at room
temperature
 Takes days to weeks to reach equilibrium
conditions
 Application of constant tensile load on cylindrical
specimen and total deformation is measured at a
constant time interval.

 Strain Hardening
 Change in reorientation due to deformation
 Material attains original consistency after the load
is removed

 Physical Hardening:
 Thermo-reversible process
 Occurs at low temperature range of -15 to -35°C
 Takes one or two days
 Occurs in all glassy materials irrespective of their
chemical nature, crystallizable or wax fractions and
length of molecular chains
 Rate of hardening is more rapid at the beginning and
decreases with increasing isothermal storage

IRREVERSIBLE HARDENING
Short term aging
 Changes to the material from the refinery to the
end of mixing and compaction process.
 Repeated heating and cooling process during
transfers
 High temperatures over a short period of time

IRREVERSIBLE HARDENING
Long term Aging
 Changes over a period of time when it is laid on the
pavement.
 Heating and cooling during changes in pavement
service temperature
 Moderate temperatures over a long period of time

FACTORS AFFECTING AGEING
 Age hardening occurs as a result of compositional changes in the
bitumen.
 The changes that occur as a result of age hardening are as yet, not
well understood, primarily due to bitumen being a rather complex
mixture of organic molecules that vary widely in composition.
 Traxler identified 15 effects which may influence the chemical,
rheological and adhesion characteristics of bitumen.
 Petersen identified 3 composition related factors that govern the
changes that could cause hardening as follows:
 Loss of oily components of bitumen by volatility or absorption by porous
aggregate
 Changes in chemical constitution of bitumen molecules from
reaction with atmospheric oxygen
 Molecular structuring that produces thixotrophic effects
Ref: Performance and Durability of Bituminous materials – Edited by J.G.Cabrera and J.R.Dixon

TRAXLER’S 15 EFFECTS CAUSING
AGING
 Oxidation (in dark)
 Photooxidation under direct sunlight
 Volatilization
 Photooxidation under reflected light
 Photochemical action of direct light
 Photochemical action of reflected light
 Polymerization
 Age hardening
 Exudation of oil
 Changes by nuclear energy
 Action of water
 Absorption of oil by solid
 Absorption of asphaltic components at solid surface
 Chemical reactions or catalytic effects
 Microbiological deterioration

MEASUREMENT OF AGING
 Thin Film Oven test, Rolling Thin Film Oven Test
for short term aging.
 ASTM D1754-09: Standard Test Method for Effects
of Heat and Air on Asphaltic Materials (Thin-Film
Oven Test)
 ASTM D2872-12: Standard Test Method for Effect
of Heat and Air on a Moving Film of Asphalt
(Rolling Thin-Film Oven Test)
 Pressure Aging Vessel for Long term Aging.
 ASTM D6521-13: Standard Practice for Accelerated
Aging of Asphalt Binder Using a Pressurized Aging
Vessel (PAV)

THIN-FILM OVEN TEST-D1754
 Determination of the effects of heat and air on a ﬁlm of
semisolid asphaltic materials
 The effects of this treatment are determined from
measurements of selected asphalt properties before and
after the test.
 Indicates approximate change in properties of asphalt
during conventional hot-mixing at about 150°C [302°F]
as indicated by viscosity, penetration, or ductility
measurements.
 It yields a residue which approximates the asphalt
condition as incorporated in the pavement. If the
mixing temperature differs appreciably from the 150°C
[302°F] level, more or less effect on properties will
occur.

 TFOT
 A ﬁlm of asphaltic material is heated in an oven
for 5 h at 163°C [325°F]. The effects of heat and
air are determined from changes incurred in
physical properties measured before and after
the oven treatment. An optional procedure is
provided for determining the change in sample
mass.
 Precision values for the method have been
developed for viscosity, viscosity change,
penetration change, mass change, and ductility.

Apparatus:
 Oven - Rotating Shelf—The oven shall be provided with a single metal circular shelf
having a minimum diameter of 250 mm [9.8 in.] and a maximum diameter of 450 mm [18
in.].The shelf construction shall be such that it provides a flat surface for support of the
containers without blocking all air circulation through the shelf when the containers are
in place. The shelf shall be suspended by a vertical shaft and centered with respect to the
horizontal interior dimensions of the oven and shall be provided with a mechanical means
of rotating it at the rate of 5.5 ±1.0 r/min. The preferred vertical position for the shelf is
150 mm [6 in.] above the bottom of the oven (exclusive of space occupied by the heating
element). The shelf shall be constructed or marked in such a way that the sample
containers can be placed in the same position during each test. There shall be a minimum
of two and a maximum of six sample container positions. Each sample container position
shall be symmetrical with respect to the shaft and to any holes in the shelf. The number of
sample container positions shall be the maximum that will fit on the shelf without
violating the above requirements and without excessive overhang.
 Thermometric Device—An ASTM Loss on Heat Thermometer having a range from 155 to
170°C and conforming to the requirements for Thermometer 13C or a Grade A platinum
resistance thermometer, commonly known as a PRT or an RTD (or both), connected to a
meter readable to 0.1°, and verified accurate at 163°C [325°F], shall be used for
determining the test temperature. The 13C thermometer, if used, shall be supported from
the shaft of the circular shelf in a vertical position at a point equidistant from the center
and outer edge of the shelf. The bottom of the thermometer bulb shall be 40 mm [1.5 in.]
above the top of the shelf. The thermometer shall be radially centered over a sample
container position. If a PRTor RTD is used for determining the test temperature, it shall
be independent of the oven temperature control system and the tip of the measuring
sensor shall be positioned 40 mm [1.5 in.] above the top of the shelf and centered over the
arc of the rotating pans. Thermometric devices shall be calibrated when initially installed,
and their accuracy at 163°C [325°F] shall be verified at least annually thereafter.

 Container—Cylindrical pans, 140±1 mm [5.5±0.04 in.] in
inside diameter and 9.5±1.5 mm [3⁄8±1⁄16 in.] deep with a
ﬂat bottom. Fifty millilitres of the sample in this size
container give a ﬁlm thickness of approximately 3.2 mm [1⁄8
in.]. Pans shall be made of stainless steel and shall have a
metal thickness of approximately 0.64 mm [0.025 in.].
Preparation of Oven:
 Ensure that the thermometric device tip is positioned 40
mm [1.5 in.] above the top of the shelf and centered over the
arc of the rotating pans.
 Ensure the oven is level so that the shelf rotates in a
horizontal plane. The maximum tilt during rotation shall
not be more than 3° from the horizontal.
 Preheat oven for a minimum of two hours prior to testing,
with the control setting adjusted to the setting that will be
used during the test. The setting shall be selected such that
when the oven is fully loaded, the oven will equilibrate at
163.0±1°C [325±2°F].

Preparation of Samples
 Place sufficient material for the test in a suitable container
and heat to a ﬂuid condition. Extreme care should be taken so
that there is no local overheating of the sample and that the
highest temperature reached is not more than 163°C [325°F].
 Stir the sample during the heating period, but avoid
incorporating air bubbles in the sample. Transfer 50±0.5 g
into each of two or more tared containers.
 At the same time, pour a portion of the sample into the
containers speciﬁed for measurement of original asphalt
properties. Complete the tests by appropriate ASTM Test
Methods D5, D2170, orD2171.
 If the quantitative value of the mass change is desired, cool
the samples for the oven test to room temperature and
determine the mass of each sample separately to the nearest
0.001 g. If the mass change is not required, allow the samples
to cool to approximately room temperature before placing in
the oven

Procedure
 With the oven preheated and adjusted, quickly place the asphalt samples in the
predetermined sample container positions on the circular shelf. Fill any vacant
positions with empty sample containers, so that every sample container position is
occupied. Close the oven door and start rotating the shelf. Maintain the specified
temperature range for 5 h after the sample has been introduced and the oven has
again reached that temperature.
 The 5-h period shall start when the temperature reaches 162°C [323°F] and in no case
shall the total time that a sample is in the oven be more than 51⁄4 h. At the conclusion
of the heating period, remove the samples from the oven. If the mass change is being
determined, cool to room temperature, determine the mass to the nearest 0.001 g, and
calculate the mass change on the basis of the asphalt in each container (Note 6).
 After determining the mass of the samples, place them on a refractory-board and then
on the shelf of the oven maintained at 163°C [325°F]. Close the oven and rotate the
shelf for 15 min.
 Remove each pan individually and transfer the contents by pouring and scraping into
a seamless metal container of approximately 240-mL [8-oz] capacity. Remove
substantially all of the material from the pans by scraping with a suitable tool such as
a spatula or putty knife. While the residue is being removed from each pan, the oven
door shall remain closed, with the heater power on, and the remaining samples
rotating on the shelf. The final pan shall be removed from the oven within 5 min of
the removal of the initial pan. Stir the combined residues thoroughly, in a semi fluid
state, until homogenous. If needed, heat the combined residues in the covered metal
container in an oven at a temperature not exceeding 163°C [325°F]. Complete the
tests on residue by appropriate ASTM Test Methods D5, D2170, orD2171 within 72 h
of performing this test.

ROLLING THIN-FILM OVEN TEST-
D2872
The RTFO was developed as an improvement to the Thin-Film
Oven Test (TFOT) for short term asphalt binder aging. The
TFOT placed asphalt binder samples in shallow pans and
then heated them in an oven for an extended period of time to
accomplish simulated aging. The RTFO is an improvement
over the TFOT because:
 Fresh asphalt binder is continuously exposed to heat and air
flow due to the rolling action of the carousel.
 Asphalt binder modifiers, if used, usually remain dispersed
in the asphalt binder due to the rolling action of the
carousel.
 No surface skin, which inhibits aging, forms on the asphalt
binder because of the rolling action of the carousel.
 The test is reasonably short at 85 minutes.

 This test method indicates approximate change in properties of
asphalt during conventional hot-mixing at about 302°F (150°C) as
indicated by viscosity and other rheological measurements. It yields
a residue which approximates the asphalt condition as incorporated
in the pavement. If the mixing temperature differs appreciably from
the 302°F (150°C) level, more or less effect on properties will occur.
This test method also can be used to determine mass change, which
is a measure of asphalt volatility.
 A moving ﬁlm of asphaltic material is heated in an oven for 85 min
at 325°F (163°C). The effects of heat and air are determined from
changes in physical test values as measured before and after the
oven treatment.

Apparatus:
 Oven
 Flow meter – It may be any suitable type capable of accurately
measuring the airflow at a rate of 4000 mL/min. The flowmeter
shall be located downstream of all regulating devices and
upstream of the copper coil. The flowmeter shall be positioned
so it is maintained at approximately room temperature.
 Thermometer
 Container - The container in which the sample is to be tested
shall be of clear, transparent, heat-resistant glass.
 Cooling Rack - A wire or sheet metal rack, constructed of
stainless steel or aluminum, which allows the sample
containers to cool in a horizontal position, with each container
in the same horizontal plane. The rack shall be constructed in a
way that allows air to flow freely around each container with at
least 1 in. (2.5 cm) clearance between containers and at least 1
in. (2.5 cm) clearance between the containers and any solid
surface.

Determination of Oven Preheat Time
 Adjust the oven control thermostat to the setting that will
be used during the test. Select this setting so that when
the oven is fully loaded and the air is on, the oven will
equilibrate at 325±1°F (163±0.5°C), as indicated by the
test thermometer. Turn the oven on and simultaneously
record the start time to the nearest whole minute.
Determine and record the temperature of the oven at 15-
minute intervals. Continue this process until the oven
reaches thermal equilibrium. Thermal equilibrium is
considered to be the time when the oven temperature does
not vary by more than 1ºF (0.5ºC) between two consecutive
readings. The oven preheat time is the time that it takes to
reach thermal equilibrium plus an additional 30 minutes.
 In lieu of completing the steps described above, a
minimum preheat time of 4 hours may be used.

Preparation of Oven
 Position the air outlet oriﬁce so that it is 1⁄4in±1⁄8in. (6 mm±3
mm) from the opening of the glass container. The oriﬁce shall
also be so positioned that the jet blows horizontally into the
central arc of the opening of the circling glass container.
 Position the thermometer so that the end of the bulb of the
thermometer is within 1 in. (25.4 mm) of an imaginary line level
with the center of the shaft holding the revolving carriage.
 Level the oven so that the horizontal axes of the glass containers
when in position in the carriage are level to within ±1.0°.
 Start the fan. The fan shall remain on whenever the oven heater
is on and the oven door is closed.
 Preheat the oven for the preheat time or longer prior to testing
with the control thermostat adjusted to the setting that will be
used during the test. Select this setting so that when the oven is
fully loaded and the air is on, the oven will equilibrate at
325±1°F (163±0.5°C), as indicated by the test thermometer.

Procedure:
 Heat the sample in its container with a loosely fitted cover in an oven not to
exceed 302°F (150°C) for the minimum time necessary to ensure that the
sample is completely fluid. Manually stir the sample but avoid
incorporating air bubbles.
 Pour 35±0.5 g of the sample into each of the required glass containers,
providing sufficient material for characterizing tests which are to be run on
the residue.
 Immediately after pouring the sample into a glass container, turn the
container to a horizontal position. Rotate the container slowly for at least
one full rotation, and attempt to pre-coat its cylindrical surface. It is not
necessary to pre-coat the open end of the container, and care should be
taken to prevent the sample from flowing out of the container during this
step. Place the container horizontally in a clean cooling rack that is
maintained in a draft-free, room-temperature location away from ovens and
other sources of heat.
 Allow the glass sample containers to cool in the cooling rack for a minimum
of 60 min, and a maximum of 180 min.
 With the oven at operating temperature and the airflow set at 4000±200
mL/min, arrange the containers holding the asphalt in the carriage so that
the carriage is balanced. Fill any unused spaces in the carriage with empty
containers. Close the door and rotate the carriage assembly at a rate of
15±0.2 r/min.

 Maintain the samples in the oven with the air flowing and the carriage
rotating for 85 min. The test temperature of 325±l°F (163±0.5°C) shall be
reached within the first 10 min; otherwise, discontinue the test.
 At the conclusion of the testing period, remove any samples for mass
change determination and place them horizontally in the cooling rack.
Then, remove each remaining glass sample container, one at a time, and
transfer its contents to a collection container having a capacity at least 30
% greater than the total expected volume of residue. This transfer shall be
accomplished by first pouring out any residue that will flow freely from
the glass sample container and then scraping out as much of the
remaining residue as practical. While the residue is being removed from
each sample container, the oven door shall remain closed, with the heater
power on, the air on, and the remaining samples rotating in the carriage.
The final container shall be removed from the oven within 5 min of
removal of the initial container.
 Test the residue within 72 h of performing the RTFO test.
 If the mass change is being determined, allow the designated residue
sample containers to cool on the cooling rack for a minimum of 60 min and
a maximum of 180 min. After cooling, determine the mass of these
container. Separately place each container vertically on the balance, and
record the mass. Note whether any sample appears to have flowed out of
the bottle.

PRESSURIZED AGING VESSEL –
D6521
 Accelerated aging (oxidation) of asphalt binders by means of
pressurized air and elevated temperature. This is intended to
simulate the changes in rheology which occur in asphalt binders
during in-service oxidative aging but may not accurately simulate
the relative rates of aging.
 It is normally intended for use with residue from Test Method
D2872 (RTFOT), which is designed to simulate plant aging.
 The aging of asphalt binders during service is affected by ambient
temperature and by mixture-associated variables, such as the
volumetric proportions of the mix, the permeability of the
mix, properties of the aggregates, and possibly other
factors.
 This conditioning process is intended to provide an evaluation of
the relative resistance of different asphalt binders to oxidative
aging at selected elevated aging temperatures and pressures, but
cannot account for mixture variables or provide the relative
resistance to aging at in-service conditions.

 Asphalt binder is normally ﬁrst conditioned using RTFOT. Residue
from the RTFOT is then placed in standard stainless steel pans and
aged at the speciﬁed conditioning temperature for 20 h in a vessel
pressurized with air to 2.10 MPa. The conditioning temperature is
selected according to the grade of asphalt binder. The residue is
then vacuum degassed.
Temperature Simulation
194°F (90°C) cold climate
212°F (100°C) moderate climate
230°F (110°C) hot climate

Apparatus:
 An equipment system consisting of a pressure vessel, ovens, pressure-
controlling devices, temperature-controlling devices, pressure and
temperature measuring devices, and a temperature and pressure
recording system

 Pressure Vessel - A stainless steel pressure vessel
designed to operate at 2.1±0.1 MPa between 90 and
110°C with interior dimensions adequate to hold ten
PAV pans and a pan holder.

Pressure and Temperature Controlling Devices:
 A pressure relief valve
 A pressure regulator or regulating system
 A slow-release bleed valve or pressure controller
 Temperature Controlling Device—A digital temperature control
device for maintaining the temperature at the conditioning
temperature 60.5°C.
 A heating device (forced-draft oven or ﬂuid bath) capable of
maintaining the temperature within the pressure vessel.
 A pressure vessel with an integral temperature control system
that is capable of restoring the pre-conditioning temperature,
within the vessel after loading the pans and the pan holder, prior
to pressurizing the vessel within 2 hours of placing the loaded
vessel in the heating device, and maintaining the temperature
within the pressure vessel.
Stainless Steel Pans - Cylindrical pans, each 1401 mm (5.50.04 in.) in
inside diameter and 9.51.5 mm (3/81/16 in.) deep, with a ﬂat bottom.

Procedure
 Place the pan holder inside the pressure vessel.
 Combine the hot residue from the RTFOT bottles into a single
container, stir to blend, and then transfer to PAV pans for PAV
conditioning, or allow the hot residue in the container to cool to room
temperature and cover and store at room temperature for PAV
conditioning at a later date. If conditioned asphalt binder is allowed to
cool to room temperature, heat it until it is sufficiently fluid to pour
and stir it before pouring it into the PAV pans.
 Place each PAV pan on a balance and add 50±0.5 g mass of asphalt
binder to the pan. This will yield approximately a 3.2-mm thick film of
asphalt binder.
 Place the filled pans in the pan holder. Place the panholder with
filled pans inside the pressure vessel and close the pressure vessel.
Unused slots in the pan holder need not be filled with empty pans.
 If an oven is used, place the loaded and closed pressure vessel in the
oven. If the temperature inside the vessel has not reached the desired
temperature for applying pressure within 2 h of loading the pan
holder and pans, discontinue the procedure and discard the asphalt
samples.

 Maintain the temperature and air pressure inside the pressure
vessel for 20 h±10 min.
 At the end of the 20-h conditioning period, begin the slow reduction
of the internal pressure of the PAV, using the air pressure bleed
valve. The bleed valve should be preset to an opening that requires
8 to 15 min to equalize the internal and external pressures on the
PAV, thus avoiding excessive bubbling and foaming of the asphalt
binder.
 Vacuum degas the aged samples.
 Remove the pan holder and pans from the PAV, and place the pans
in an oven set to 168±5°C for 15±1 min.
 Preheat the vacuum oven to 170±5°C.
 Remove the pans from the oven and scrape the hot residue from all
pans containing the same sample into a single container. After the
last pan of a sample has been scraped, and if additional containers
are to be prepared, transfer the container to the 168°C warming
oven.
 After all of the containers have been prepared, transfer them to the
vacuum oven within one min. Once the last container has been
placed in the vacuum degassing oven, maintain the temperature.

TEMPERATURE SUSCEPTILITY OF
BINDERS
 Bitumen is thermoplastic.
 Variation in consistency with temperature is
known as Temperature susceptibility.
 Penetration index
A – Temperature
susceptibility
0.015-0.06 for
paving bitumen

 Penetration Index is correlated to A by
PI value ranges from -3 (for highly susceptible
bitumen) to +7 (for low susceptibility, highly blown
bitumen)

GRADATION OF BITUMEN
 Penetration Grading
 Viscosity Grading
 Performance Grading

CUTBACKS
 Low viscosity bitumen whose viscosity is reduced
by Volatile solvents
 After application, the volatile component
evaporates leaving behind the desired quantity of
binder
 Types of Cutbacks
 Rapid Curing (Naphtha/Gasoline - Solvent)
 RC70, RC250, RC800 and RC3000
 Medium Curing (Kerosene - Solvent)
 MC30, MC70, MC250, MC800, MC3000
 Slow Curing (Diesel/Lubricating oil - Solvent)
 SC70, SC250, SC800, SC3000

EMULSIONS
 Two-phase system consisting of bitumen(50-75%),
water, and one or more emulsifiers(0.1-2%)
 Bitumen is dispersed throughout the water phase in
the form of discrete globules
 Used in pavement applications from 1920
 In India, about 3% of bitumen is used in the form of
Emulsions.
 Applications:
 Surface Treatments (Sealing, Microsurfacing)
 Recycling (Cold-in-place)
 Other applications (Patching, Tack coat, Seal coat, Prime
coat, Crack filling, Surface dressing, dust palliative,
bituminous mixes, soil stabilization)

EMULSION - CLASSIFICATION
 Based on electric charge surrounding the globules,
 Anionic (suitable for Calcareous aggregates)
 Cationic (Mostly used, Siliceous aggregate)
 Non-ionic (Rarely used)
 Based on how quickly emulsion reverts back to
bitumen,
 Rapid Setting (Surface dressing, Patch repair)
 RS1 – Tack coat, RS2 – Surface dressing
 Medium Setting (Premix with lesser fines)
 MS – Open Graded Premix
 Slow Setting (Premix with larger % fines)
 SS1 – Priming, Fog seal, Crack seal, SS2 – Slurry sealing,
Seal coat

TESTS ON CUTBACKS AND
EMULSION
 ASTM D402/D402M–14:Standard Test Method for Distillation of Cutback
Asphalt
 ASTM D3143-13: Standard Test Method for Flash Point of Cutback
Asphalt with Tag Open-Cup Apparatus
 ASTM D3666-16: Standard Specification for Minimum Requirements for
Agencies Testing and Inspecting Road and Paving Materials.
 ASTM D3910-11: Standard Practices for Design, Testing, and
Construction of Slurry Seal.
 ASTM D6934-08: Standard Test Method for Residue by Evaporation of
Emulsified Asphalt
 ASTM D6930-10: Standard Test Method for Settlement and Storage
Stability of Emulsified Asphalts
 ASTM D6997-12: Standard Test Method for Distillation of Emulsified
Asphalt
 ASTM D7403-09: Standard Test Method for Determination of Residue of
Emulsified Asphalt by Low Temperature Vacuum Distillation
 ASTM D7497-09: Standard Practice for Recovering Residue from
Emulsified Asphalt Using Low Temperature Evaporative Technique

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