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©SCULPT{Lab}, IIT (BHU) Varanasi ([Link] Dr. Agnivesh Pani

Module 3, Lecture 26-28

Highway Materials and

Testing – Bitumen
Course Instructor
Indian Institute of
Department of
Technology (BHU)
Civil Engineering
Varanasi
CE251 Transportation Engineering - Dr.
I Agnivesh Pani

©SCULPT{Lab}, IIT (BHU) Varanasi ([Link] Dr. Agnivesh Pani

Coverage of Syllabus
1. Bitumen – Physical Properties References

2. Production of Bitumen
3. Chemical Properties of Bitumen
Chapter 2, 3, 4
4. Ageing of Bitumen
5. Grading of Bitumen
6. Modifiers of Bitumen

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Why are we interested in Bitumen properties?

• Any material’s functional properties, performance and behavior
at different conditions (e.g., temperature, age) can be traced
back to chemical composition
• Simple to say – but difficult to carry out in the case of bitumen!
• Bitumen is not a designed material – it is a complex mixture of
numerous types of hydrocarbon (as opposed to simple polymers
such as Polyethylene)
Easy to
Characterize

Bitumen
Complex and difficult
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©SCULPT{Lab}, IIT (BHU) Varanasi ([Link] Dr. Agnivesh Pani

Bitumen is a Visco-elastic material

Study of Bitumen
• Bitumen is a visco-elastic material – hence its properties are dependent
on temperature, rate of loading, and frequency of loading

• Temperature and loading time are very important for studying bitumen
properties
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BITUMEN- A BINDING AGENT

• Terminology: Bitumen (European/Asian countries); Asphalt/Asphalt

Binder (North American countries)
• Definition: “A tar like mixture of hydrocarbons derived from petroleum,
naturally or by distillation, and used for road surfacing and roofing”
(Oxford Press, 1996)
• Bitumen and Tar are two distinctly different materials, of different origins,
and have different chemical and physical characteristics
• Bitumen is a crude oil product: Most places where you find crude oil are
sea beds.
• Mankind’s one of the oldest engineering material

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BITUMEN- A BINDING AGENT

• Bitumen – Black to Dark Brown
in colour, naturally occurring or
produced by petroleum
distillation
• Tar – Manufactured from
destructive distillation of
bituminous coal
• Tar is highly temperature
susceptible compared to
bitumen and its use is more
health hazardous than bitumen

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BITUMEN- A BINDING AGENT

• Natural/Lake Bitumen: Trinidad lake asphalt; Gilsonite; Rock asphalt
• Very hard to be used directly: 54% binder, 36% mineral matter, 10%
organic matter).
• Used during the last two decades of 19th century.

Called pitch
lakes – occurs
across two
intersecting
fault lines in
earth crust

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BITUMEN- A BINDING AGENT

Terminology
1. Natural Bitumen – Occurring as natural deposit (e.g., lake asphalt in
Tridinad), Rock asphalt
2. Gilsonite – Hard Variety of Naturally occurring bitumen (black and brittle)
3. Petroleum Bitumen – Obtained by refining process of petroleum
4. Straight-Run Bitumen – Petroleum bitumen whose viscosity has not been
adjusted by blending or softening with cut-backs or other solvents
5. Blown Bitumen – Straight run bitumen further treated by blowing air
through it while it is in hot condition - The oxygen in the air reacts with the
hydrocarbons → causes oxidative polymerization → molecules link
together → bitumen becomes harder and more viscous. Results: Higher
softening point, lower temperature susceptibility, more rubber-like properties
6. Asphalt – Mixture of bitumen and inert matter – (British Usage)
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7. Bituminous Mix – Mixture of Bitumen and Inert matter – BC, DBM, BM 8

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BITUMEN- A BINDING AGENT

• Mixtures of Bitumen
• Cutback and Fluxed Bitumen – Viscosity of bitumen is reduced
by adding solvent, normally derived from petroleum, such as
Kerosene, Gas Oil, Naphtha, etc. – Typically used for spray
applications (tack and prime coat) – use of tack coat is largely by
emulsions today (Replaced cutbacks)
• Bitumen Emulsion – A multi-phase system where bitumen
particles are dispersed in an aqueous medium (and not allowed
to coagulate using emulsifiers)
• Modified Bitumen – To change the performance/properties of
straight run bitumen (e.g., polymer modified bitumen)

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Production of Bitumen
Bitumen from Petrolem Crude – Fractional Distillation
What is Bitumen Yield? Bitumen yield refers to how much bitumen you
can extract from a given crude oil during the refining process. It is not
constant - it depends entirely on the nature (composition) of the parent
crude oil.

API Gravity - API gravity is an industry-standard measure of how heavy or

light a crude oil is, relative to water.
The formula is: API = 141.5/SG − 131.5 where SG = Specific Gravity of the
crude oil (ratio of its density to water at 60°F).

Interpreting API Values (Reference: Shell Bitumen Handbook)

Short residue (vacuum

residue) is given as feeding
The Inverse Relationship: API ↓ → Bitumen Yield ↑This makes intuitive stock for bitumen
sense: Low API = Heavy crude → High density → More heavy production
hydrocarbon fractions → More bitumen residue after CE251 Transportation Engineering - I
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Production of Bitumen
Bitumen from Petrolem Crude
• Predominantly soluble in carbon
disulphide
• Mostly in colloidal state
• Chemical Composition
• Carbon 82-88%
• Hydrogen 8-11%
• Sulphur 0 – 6%
• Nitrogen 0 – 1%
• Traces of Metals – Vanadium, Nickel,
Iron, Magnesium Calcim

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Physical Properties of Bitumen

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PHYSICAL PROPERTIES OF BITUMEN

• Considering the pavement durability problems arising significantly due to
bitumen ---- physical properties of it needs to be studied in detail

• Physical properties of bitumen can be broadly quantified using the

following tests
• Consistency tests
• Durability tests
• Purity test
• Safety test
• Consistency: Degree of fluidity of asphalt binder at
any given temperature

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PHYSICAL PROPERTIES OF BITUMEN

How to test for consistency of bitumen? Temperature is key
• Behavior at very high construction temperature (135 to 180 degrees)
• Behaviour during laying temperature (100 degrees)
• Behavior at high service temperature (40 to 60 degree)
• Behavior at low service temperature (10 to -20 degrees)
• Behavior at average service temperature (20 to 30 degrees)

4 Key Testing Temperature

• 25 degree Celsius – Average temperature of pavement
• 60 degree Celsius – Maximum temperature of pavement
• 135 degree Celsius – Mixing/Pumping/Spraying temperature
• 4 degree Celsius – Low temperature during winter

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PHYSICAL PROPERTIES OF BITUMEN

• Penetration of needle under given load
• Consistency Tests (100 gm or 200 gm) after a fixed duration
• Penetration (5s or 60 s) is measured in units of 0.1 mm
• Softening point (dmm)
• Ductility
• Viscosity

• Penetration test: 4 mm penetration means value of

penetration test = 40
• Simple empirical test usually done at 25 °C
• Can also be done at lower temperature (for eg. 4 °C)
• Sample at the standard temperature is placed under a
needle of prescribed dimension.
200 gm weight is recommended for
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PHYSICAL PROPERTIES OF BITUMEN

• Penetration test:
• Empirical test with high shear and short
loading time
• Is assumed to represent overall Pavement life stages
where cracking has
performance initiated
• Penetration of bitumen from aged
pavement has been correlated with
performance
• Penetration < 20 :Serious cracking
• Penetration (20-30) :Some cracking
• Penetration > 30 :Good resistance to cracking
“Use Soft Binder Ensuring a Minimum Stability of Mix at High Pavement Temperature”

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PHYSICAL PROPERTIES OF BITUMEN

• Softening point test:
• Determines the ‘phase change’ temperature of bitumen
• Ring and ball method is used
• Temperature at which the asphalt binder cannot support the weight of
a steel ball and starts flowing.
• Brass ring filled with bitumen and loaded with a steel ball is
suspended in a water (or ethylene glycol) bath which is heated at a
constant rate (5 °C/min)

Mettler Toledo

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PHYSICAL PROPERTIES OF BITUMEN

• Softening point test:
• Bitumen softens and the ball penetrates the sample and touches the
bottom of the plate which is at a distance of 25 mm.
• Temperature at touchdown is reported as the softening point.

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PHYSICAL PROPERTIES OF BITUMEN

• Ductility test:

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PHYSICAL PROPERTIES OF BITUMEN

• Ductility test:
• Measures the distance (in cm) that a bitumen sample placed in a
standard briquette will stretch before failure when pulled at a
standard rate (usually 5 cm/min) and at a standard temperature
(usually 25 °C)
• SG of the water should be same as that of bitumen to prevent
floating/sinking of the stretched sample. (Increase SG of water using
salt or reduce using alcohol-based solutions)
• Running the test at lower temperature (16 °C and 4 °C) is better for
quantifying the cracking resistance of HMA.

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PHYSICAL PROPERTIES OF BITUMEN

• Ductility test:
• Significance of the test has been debated because of its empirical
nature and poor reproducibility
• Ductility values lower than a certain value (<5 cm or <3 cm) at lower
test temperatures (13 °C or 16 °C) can quantify occurrence of
cracking: Doyle; Vallerga and Halstead (2010)
• At similar penetration values, asphalt binder with lower ductility
shows more cracking than asphalt binder with higher ductility
• Can differentiate between the cracking
resistance of asphalt binders if the test run on
highly stiff binder: Lower the test temperature;
or, test the binder after ageing – IS-73

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PHYSICAL PROPERTIES OF BITUMEN

• Frass Breaking Point test:
• Indicates the stiffness of bitumen at low
temperature
• Relevant for locations where low temperature is
anticipated
• Bitumen should not be too brittle at low
temperature (or else they will crack easily when
flexed)
• Temperature at which a thin film of 0.5 mm
thickness cracks when flexed

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PHYSICAL PROPERTIES OF BITUMEN

• Frass Breaking Point test:
• Thin film on steel plaque
is subjected to flexural
stress
• Observe the temperature
at which it cracks

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PHYSICAL PROPERTIES OF BITUMEN

What is a fundamental consistency
measurement that is not affected by changes in
test configuration or geometry of the sample?
• Viscosity
• Fundamental rheological property of bitumen
• Rheology is the study of flow and deformation of materials
• Several applications in which deformation and shapes of materials
are important (e.g., polymeric materials such as plastics – automotive
applications – aerospace applications – biomedical applications)
• Viscosity is the resistance offered by the fluid to a shearing force
(opposite of fluidity or consistency)
• It is necessary to learn about the flow and deformation of bituminous
binders at different temperatures
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PHYSICAL PROPERTIES OF BITUMEN

• Viscosity
• Viscosity at high handling temperature (135 degree or 160 degree)
and high (60 degree) or low service temperatures are of interest to us

Dynamic or Absolute Viscosity (h)

F A
F v
F 1/d
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PHYSICAL PROPERTIES OF BITUMEN

• Viscosity
Measurement of Absolute Viscosity – Sliding Plate Viscometer
• Fundamental definition as principle
• Bitumen film of known thickness is
sandwiched between two parallel plates
V
• Test conducted at selected temperature
and selected rate of shear (v)
• Force required to move the plate at a
velocity of v is measured

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PHYSICAL PROPERTIES OF BITUMEN

• Viscosity
Measurement of Absolute Viscosity – Rotational Viscometer
• Torque offered by the fluid to the rotation
of a spindle at a given rotation velocity at
a given temperature is measured

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PHYSICAL PROPERTIES OF BITUMEN

• Viscosity
Common Rotational Viscometer
• Brookfield viscometer is the most
popular type of rotational viscometer

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PHYSICAL PROPERTIES OF BITUMEN

Kinematic Viscosity - ν
This is absolute viscosity normalized by the fluid's density:
• Viscosity
Measurement of Kinematic Viscosity – Efflux Viscometer
• Standard size of the orifice – Time for
standard volume to flow is measured –
at the given test temperature
• Unit – seconds (Instruments are
calibrated to obtain corresponding
kinematic viscosity)
•Longer time = higher kinematic viscosity =
thicker/slower-flowing bitumen

ν = μ / ρ Unit: m²/s or Stokes (St)

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PHYSICAL PROPERTIES OF BITUMEN

• Viscosity
Common Efflux Viscometers
Standard Tar Viscometer

Saybolt-Furol Viscometer

Engler Viscometer is another

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PHYSICAL PROPERTIES OF BITUMEN

• Viscosity test: Capillary Viscometers
• Kinematic viscosity obtained by observing the
time required for a fixed volume of fluid to flow
through a standard capillary tube
• Narrow glass tubes (having narrow and wide
sections) through which bitumen flows

• 2 or more marks on the tube to indicate a particular

volume of flow

• Viscometers are calibrated and the product of flow

time and calibration factors give kinematic viscosity

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PHYSICAL PROPERTIES OF BITUMEN

• Viscosity test: Capillary Viscometers
• Cannon-Manning vacuum viscometer is typically
used
• Bitumen is poured through the larger size
opening to attain a specified level within the tube
• Viscometer is kept in a water/oil bath at 60 °C for
a prescribed period.
• A partial vacuum is applied on the smaller side to
initiate the flow of bitumen.
• Time required to flow between the timing marks is
recorded

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PHYSICAL PROPERTIES OF BITUMEN

• Viscosity test: Capillary Viscometers
• Time is multiplied with the calibration factor of
the tube to calculate the viscosity (in Poises)

𝑢
𝑢 =𝑡 ×
𝑡

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PHYSICAL PROPERTIES OF BITUMEN

• Viscosity test: Using Viscosity to Determine Mixing and Compaction Temp
• Mixing and compaction temperature can be determined as follows
• Test the binder at one additional temperature (for eg. 165 °C)
• A linear relationship is assumed between viscosity and temperature,
and the temperature ranges corresponding to the viscosity values of
0.17±0.02 Pa.s and 0.28±0.03 Pa.s are taken as mixing and
compaction temperatures, respectively.

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PHYSICAL PROPERTIES OF BITUMEN

• Viscosity test: Connecting Viscosity to Performance
• Viscosity at 60 °C has been correlated with resistance to rutting at high
pavement temperature.
• At locations having high pavement temperature, higher viscosity of asphalt
binder is desirable. (Viscosity should be high at higher temperatures)
• Use of stiff binder at very low temperatures can cause non-load associated
transverse shrinkage cracks (Viscosity should be low at lower temperatures)

• Ageing index defined using viscosity ratio is an

Ageing index = Viscosity of
indication of ageing susceptibility and occurrence of aged bitumen / viscosity of
raveling. Ageing susceptibility is also correlated with unaged bitumen
occurrence of early cracks in the pavement.

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PHYSICAL PROPERTIES OF BITUMEN

• Purity Test: Used to see the quality of supplied bitumen
• Bitumen is entirely soluble in carbondisulphide/tricholoroethylene
• Binder of known weight is dissolved in the standard solvent and
filtered through a glass fibre pad.
• Insoluble material is washed, dried and weighed.
• As per specifications, impurity should not be more than 1%.
[Link]
m

C2HCl3
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PHYSICAL PROPERTIES OF BITUMEN

• Purity based on Specific Gravity of Bitumen
• Determined using Pycnometer method at 27 degree
• Specific gravity of bitumen ranges from 1.02 to 1.04
• Does not influence the behavior of the binder
• Normally used for quality control purposes
• Useful for volumetric conversion in bituminous mix design

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PHYSICAL PROPERTIES OF BITUMEN

• Safety Test: To ensure safe working condition while heating bitumen
• Flash and Fire point (s) are measured using a Cleveland open cup
apparatus
• Flash point is the temperature to which bitumen can be safely heated
without any danger of instantaneous flash in presence of open flame.
• At fire point, a little higher temperature than flash point, the material
combusts in presence of open flame.

• Brass cup filled with bitumen is continuously heated at a prescribed rate

and a small flame is passed over the surface of the cup periodically.
• Temperature at which the vapor flashes and combust are recorded

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[Link]

The constructor

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Chemical Properties of Bitumen

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Material Characterization of Bitumen (Chemical)

Scales of Characterization
1. Elemental Analysis
2. Molecular Structure
3. Compositional Groups - (SARA Fraction)
Other Characterization Aspects
4. Functional Groups
5. Molecular Arrangement
6. Morphology
Microstructural Models Chemical Composition and Physical
Properties

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CHEMISTRY OF BITUMEN
• An understanding of the chemical factors affecting physical properties of
bitumen is fundamental: Affects Performance
• Bitumen is one of the components of crude oil which is a mixture of several
hydro carbon molecular groups: Amount and nature are highly variable.
• Elemental Composition:
• Carbon: 82-88%
• Hydrogen: 8-11%
• Sulfur: 0-6%
• Oxygen: 0-1.5% Heteroatoms
• Nitrogen: 0-1%
Trace quantities of metals such as Vanadium, Nickel, Iron, Magnesium and Calcium which
occurs in form of inorganic salts and oxides.

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Bitumen Chemical Properties

• Diverse molecular structure
• Typical arrangements:
• Straight or branched chains (Aliphatic or Paraffinic type)
• Simple or complex saturated rings (Naphthenic type)
• One or more stable six-carbon condensed unsaturated ring structure
(Aromatic type)

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CHEMISTRY OF BITUMEN
• Functional/Polar Groups:
• Different molecular arrangements containing S, O and N
• Creates imbalance of electrochemical forces and thereby produces a
dipole
• They impart functionality to the bitumen and is responsible for
interactions within the bitumen and other surfaces
• Amount of non-polar group, which act as dispersing agents for polar
groups also play a major role in determining the effect of polar group

• For example, pyridines (C5H5N) tend to adhere to aggregate surfaces

• Carboxylic acid (R-COOH) group can make salts (since they are weak
acids which are highly reactive) and may be removed from the
aggregate interface easily in presence of water
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• FTIR Spectroscopy is Sulfur Compounds Polysulfides

used to identify Sulfides
functionalities in bitumen Thiols
Thiophenes
Different Nitrogen Compounds Pyridinic
compounds Pyrrole, indole, carbazole
Porphyrins
containing
Oxygen Compounds Carboxylic
functional groups in
acids/naphthenic acids
bitumen Phenols
Ketones
Esters
Ethers
Anhydrides
FTIR analyses
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CHEMISTRY OF BITUMEN
• Compositional Model:
• Complex chemical composition
• Complete analysis is extremely difficult and laborious, if not impossible
• Correlation with mechanical response is impractical

• The most simple and generally accepted model is to consider bitumen

composed of asphaltenes and maltenes. Maltenes comprises of
resins and oils (saturates and aromatics)
Asphaltenes

Bitumen Resins

Maltenes
Oils (Saturates,
Aromatics)

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CHEMISTRY OF BITUMEN
• Asphaltenes (Complex Aromatic Material):
• High molecular weight dark brown to black
friable solids
• 5-25% having average particle size of 2-5 nm
• Precipitated by non-polar solvents (n-pentane/
n-heptane)
• Complex molecule with highest polarity
• High tendency to associate and interact
• Viscosity-building component.
• Low asphaltene content may lead to tenderness
in the mix

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CHEMISTRY OF BITUMEN
• Resins (n-heptane soluble):
• Dark, semi-solid/solid
• Fluid when heated, brittle when cold
• Being polar they are very adhesive
• Peptizing (dispersing) agents for asphaltenes 15-
25% - They help asphaltenes to stay dispersed in
an oily medium
• On oxidation they yield asphaltenes like molecules
• Balance between resins and asphaltenes is
important for appropriate dispersion of
asphaltenes. The relative proportion strongly
affects the rheological properties

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CHEMISTRY OF BITUMEN
• Aromatics (Lowest molecular weight napthenic
aromatic compound):
• Represents majority portion of dispersing
medium
• Non-polar with high dissolving capability for
higher MW H-C.
• 40-60%

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CHEMISTRY OF BITUMEN
• Saturates (Straight or branched chain aliphatic
hydrocarbon together with alkyl napthenes and some
alkyl aromatics):
• They are non-polar viscous oils – NOT Desirable due to
Temperature Susceptibility
• Straw coloured or colourless
• 5-20%

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CHEMISTRY OF BITUMEN
• Asphalt as a colloidal system
• Bitumen is typically described as a colloidal system where
asphaltenes are the solid particles in the form of molecule
clusters or micelles dispersed in the oils with resins
forming an interface
• The different phases of bitumen act as a continuum with no
distinct boundaries between them. The asphaltene micelles,
surrounded by a layer of resin, are randomly distributed
throughout the oil phase

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CHEMISTRY OF BITUMEN
• Asphalt as a colloidal system
• Not a true solution but a colloidal or micellar system
• Relative amount and characteristics of each component govern
the ‘type’ of colloidal system
• Sol: Resins keep asphaltenes highly peptized: Nitrogen bases in
asphalt are typically responsible for such characteristic.
Essentially viscous with little or no elasticity

• Gel: Resins are not effective in peptizing. Excessive presence of

paraffins in relative to nitrogen bases. Exhibit non-Newtonian behavior.
Suggests separation of dispersed and dispersing medium. Exhibits
elastic, in-elastic, and permanent deformation behavior
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N. Nciri, N. Kim, N. Cho, Mater. Chem.

Phys. 193 (2017) 477‒495. DOI: 10.1016/j.
matchemphys.2017.03.014

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©SCULPT{Lab}, IIT (BHU) Varanasi ([Link] Dr. Agnivesh Pani

CHEMISTRY OF BITUMEN
• Separation Technique
• Corbett Chromatographic
technique are most widely used
• Asphaltenes are precipitated using
n-heptane
• Heptane solution containing
remaining maltene fraction is
introduced in a chromatographic
column (silica-gel/alumina)
• Adsorbed fraction are sequentially
desorbed (washed out) using different Fast SARA
solvents of increasing polarity to get the Method
remaining three fractions (2019)

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CHEMISTRY OF BITUMEN
• How Structure of Bitumen Changes?
• The structure and properties of bitumen are a function of its
temperature, as well as its chemical nature, and the relative
proportion of its constituents
• As the temperature increases, the asphaltenes flow more freely and
the material becomes less viscous
• As the temperature decreases, asphaltenes become less soluble and
the micelles are bound in an ordered structure and the material
becomes more viscous
• Eventually, as the temperature is decreased below the glass
transition temperature, the structure is frozen, and the material
behaves as a rigid and brittle solid

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Aging of Bitumen and Durability Tests

Aging of Bitumen
• Bituminous binders undergo aging due to loss of volatile matter and
oxidation
• Short-Term Aging –
• Long-Term Aging –

What is short-term and long-term?

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Aging of Bitumen and Durability Tests

Aging of Bitumen
• Bituminous binders undergo aging due to loss of volatile matter and
oxidation
• Short-Term Aging – During storage, transportation, mixing, and placing (at
high temperature, bulk or thin film)

• Long-Term Aging – Due to oxidation occurring during the service life

• Penetration decreases with aging

• Viscosity increases with aging
• Softening point increases
• Ductility decreases

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Traxler, 1963
Shell Bitumen Handbook,
Sixth Edition

15 factors
responsible for
ageing

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Aging of Bitumen and Durability Tests

• Durability Tests: Durability tests quantifies the effect of ageing on the
properties of asphalt binder
• Bitumen ages during hot storage, production and in-service
• Organic molecules are affected by the presence of oxygen, UV radiation
and changes in temperature
• Leads to increase in stiffness
• As many as 15 different factors are responsible: Shell Bitumen Handbook
• Important factors are:
• Oxidation
• Volatilization
• Steric or Physical Hardening
• Exudation of Oils
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Aging of Bitumen and Durability Tests

• Oxidation:
• Polar groups containing oxygen are formed and tends to associate into
micelles (increases viscosity)
• Formation of carbonyl groups increases the molecular weight
• Degree of oxidation: f (temperature, period of exposure, film thickness)
• Above 100 °C, 10 °C increase in temperature doubles the stiffness of
bitumen
• Loss of Volatiles:
• Lower weight oils gets evaporated
• Function of temperature and exposure conditions
• Dense graded mixtures with higher film thickness of bitumen are more
resistant to loss of volatiles
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Aging of Bitumen and Durability Tests

• Steric/Physical Hardening:
• Combination of reorientation/restructuring of molecules within the
bitumen and slow crystallization of waxes
• Application of heat will reverse the process

• Exudation of Oils:
• Movement of light oil fractions of bitumen into
aggregates
• Function of exudation tendency of bitumen and
porosity of aggregates

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Aging of Bitumen and Durability Tests

• Durability Tests:
• Short Term Ageing: Binder undergoes short term ageing when they
are mixed with the aggregates at elevated temperature.
• Long Term Ageing: The long term ageing continues during the service
life when the pavement is continuously exposed to environmental and
other factors Shell Bitumen Handbook

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Lower void
content – higher
penetration –
lower aging

• Temperature
• Type of plant
• Bitumen Film thickness
• Air-voids
• Extent of UV rays
• Position of the mix

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Aging of Bitumen and Durability Tests

• Durability Tests
• Short Term Ageing: Thin Film Oven (TFO) and Rolling Thin Film
Oven (RTFO) tests are used to approximate the short term hardening
which occurs in the HMA mixing plant.
Bituminous binder is
kept as a thin film at
high temperature
(163) for a specified
period

Matest Test properties before

Vertex
and after TFO

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Aging of Bitumen and Durability Tests

• Durability Tests
• Short Term Ageing

• TFO:
• 50 g sample is kept in a cylindrical flat bottom
• Sample is conditioned at 163 °C and revolving
shelf is rotated at 5-6 rev/min for 5 hours.
• Change in properties of material such as
penetration or viscosity is commonly used to
quantify the effect of ageing
• Loss in weight is also measured and reported
(should not be > 1%)
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Aging of Bitumen and Durability Tests

• Durability Tests
• Short Term Ageing

• RTFO:
• A specified amount of binder is placed in the
transparent glass bottle.
• Bottle is placed in the RTFO rack at 163 °C and
rotated around the horizontal axis.
• Orifice of the sample bottle passes in front of an
air-jet (4000 ml/min) which purges the vapor
accumulated inside the bottle.

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Aging of Bitumen and Durability Tests

• Durability Tests
• Long Term Ageing: Pressure Ageing Vessel (PAV) is used to
approximate the long term ageing which occurs in the service
condition.

Pavement Interactive

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Aging of Bitumen and Durability Tests

• Durability Tests
• Long Term Ageing

• PAV:
• RTFO aged samples are placed in stainless steel pans for 20 hours
in a heated pressurized vessel (2.1 MPa) at a standard temperature.
• 90 °C, 100 °C or 110 °C
• Sample is removed, pressure is gradually released, kept in oven at
163 °C for 15 minutes.
• Scrapped samples kept in a vacuum oven for 30 mins at 170 °C for
degassing to remove entrapped air (that may have come from PAV)

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Some practical calculations for Bitumen

• Temperature Susceptibility by Slope Calculation

A – Temperature Susceptibility

0.015 to 0.06 for paving binders

A = log (Pen at T1) – log (Pen at T2) / T1-T2

Log (Pen) = AT + K

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Some practical calculations for Bitumen

• Temperature Susceptibility
• an assumption that penetration at the softening point is 800 simplifies it all
• Graph between logarithmic of penetration and temperature is plotted. Slope A
of this line is calculated
A = log (Pen at T1) – log (Pen at T2) / T1-T2
Most Bitumens have a penetration value of about
800 when test temperature is equal to SP

Therefore
A = log (Pen at 250c at T1) – log (800) / T1-SP

• Higher the value of A higher is the susceptibility

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Thank You.
Quote of the week -
Focus on earning with your mind rather than your time, and seek ownership
(equity) to gain freedom. Cultivate specific knowledge by following curiosity,
not trends.
Prioritize long-term games, compound interest in relationships, and building
a reputation with oneself
- Naval Ravikant

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Module 2, Lecture 29-31

Highway Materials and

Testing – Bituminous Mix
Course Instructor
Indian Institute of
Department of
Technology (BHU)
Civil Engineering
Varanasi
CE251 Transportation Engineering - Dr.
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©SCULPT{Lab}, IIT (BHU) Varanasi ([Link] Dr. Agnivesh Pani

Gradation of Bitumen
1. Penetration Grading – On the basis of Penetration at 250C

2. Viscosity Grading – On the basis of Viscosity at 600C

3. Performance Grading – Graded by the conditions

(temperatures) at which the binder is expected to perform
satisfactorily – Varies site to site – For each pavement, we need
to evaluate the variation of service temperature, mixing
temperature, etc.

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Penetration Grading
S stands for straight run
bitumen (not blended
neither modified nor blown)

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Penetration Grading
• Simple but empirical (not fundamental)
• Cannot be used for grading polymer-modified bitumen
• Does not providing guidance regarding mixing and
compaction temperatures to be used for bituminous mixes
(viscosity at high temperatures is not available)
• Penetration grading specifications do not provide good idea
about the temperature susceptibility of the binder

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Viscosity Grading

• AC-2.5 is used in very cold climates

• AC stands for asphalt cement
• S60 and S90 roughly correspond to AC-30 and AC-10

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Viscosity Grading
• More fundamental than penetration grading
• Bitumen having similar viscosities normally give similar
rutting performance (not in the case of penetration grading)
• Better guidance available for mixing and compaction
temperatures since viscosities are measured

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Performance Grading
• Result of a 50-million dollar, 5-year Strategic Highway Research
Programme (SHRP) conducted in the USA
• Also called Superpave (Superior Performance Pavements)
performance gradation
• Binders are graded by the temperature range (high and low)
within which the binder has appropriate properties to perform
satisfactorily
• Against rutting mode of failure (high temperature)
• Against fatigue failure of bituminous mixes (Intermediate temperature)
• Against low temperature cracking (Low temperatures)

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©SCULPT{Lab}, IIT (BHU) Varanasi ([Link] Dr. Agnivesh Pani

Performance Grading
• Complete range of temperatures experienced at a given site
are considered for selecting an appropriate grade of bitumen

• For example, PG 58-12 represents a binder that is expected to

perform satisfactorily in a region having 7-day maximum
pavement temperature of 580C and minimum pavement
temperature of -120C

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Modified Bitumen

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Definition, Need and Role

• Modified bitumen are binders whose base properties are changed by use of a
chemical agent, which when added, alters the chemical/physical structure,
leading to change in its mechanical properties
• Why is modification required?
• Increase in rainfall and temperature variations
• Increase in vehicular loading, tyre pressures, new axle configurations
• To reduce frequency of maintenance
• Tendency to use thinner layers

• What do modifiers do?

• Improves high temperature performance without
affecting performance at other temperatures
• Stiffness and/or elastic component increases

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Types and Requirement

• Wide range of products have been researched for modification of bitumen
• Polymers are the most common modifying agents which enlarges the temperature
range of resistance to distresses such as rutting and thermal cracking
• Polymers consist of macro-molecules in which same group of atoms are repeated
many times (monomers)
• Requirement
• Easy availability at low cost
• Should blend easily with bitumen
• Should not degrade at high temperatures
• Should be stable during storage, transportation and laying
• Improve resistance of bitumen to distresses at
varying temperature range

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From Shell Bitumen Handbook

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From Shell Bitumen Handbook

Some common polymers

• SBS
• SBR
• EVA
• PE
• CRMB

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Factors affecting dispersion

• Addition of polymers disturbs the equilibrium of base bitumen: asphaltenes and
polymers competes for solvency of maltene phase
• Factors affecting dispersion
• Chemical structure of base bitumen
• Molecular weight of polymer
• Type and concentration of polymer
• Polymer structure
• Manufacturing process
• Presence of cross linking agents such as sulfur
• Critical concentration
• Is a function of type of polymer
• Shift from bitumen rich phase to polymer rich phase
Optical Techniques like Fluorescence Microscopy will
help us understand the dispersion characteristics
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Tests for PMBs

• Tested using traditional bitumen tests
• Special tests:
• Storage stability for phase separation
• Elastic recovery
• Storage Stability
• Simple hot storage test to judge the incompatibility between bitumen and
polymer
• PMB placed in a cylindrical tube and stored vertically (160-180 °C) for 2-3 days
• Softening point difference between top and bottom samples is used to quantify
phase separation
• Difference should not be more than 3 °C

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Tests for PMBs

• Elastic recovery
• Use to assess degree of modification
• Bitumen sample is pulled to a specific distance
(usually 10 cm) in a ductility machine and cut
immediately
• Rate of pull is 5 cm/min and the temperature is
typically 15 °C
• After 1 hr, elongated half is brought near the fixed
half and length is measured (X)
• Elastic recovery, % = (10-X)/X * 100

• A minimum recovery of 70% is expected in case of

elastomeric modification

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