Bitumen Production, Tests

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Bitumen production,

Properties, Types and


Tests
by:
Dr Shiva Prashanth Kumar Kodicherla
E-mail: skodicherla@nust.na
Tel: (+264) 61 207 2277
Introduction:
• Bitumen on the other hand, is produced by fractional
distillation of petroleum (called manufactured bitumen)
• Bitumen has also been found to exist as Natural Asphalt
(American ‘Native Asphalt’) in some deposits
Natural asphalt is available from:
• Trinidad Island – Most widely known supply of natural asphalt
used in pavement engineering
• Venezuela
• USA and Iran – Rock Asphalt is found (type of natural asphalt
that is found in the solid form)
• The term Asphalt in the UK (and in the European
specifications) refers to the mixture of bituminous binder and
mineral aggregates (like in Hot Mix Asphalt – HMA, used as a
road surfacing material)
Manufacturing of bitumen:
• Bitumen is colloidally dispersed hydrocarbons in crude
petroleum.

• During the fractional distillation process to refine petroleum


crudes, this material remains as residual.

• This process has produced bitumen that has become plentiful


and of good quality, making natural asphalt to be relatively
less desired.
Fractional distillation process of crude petroleum:
Bitumen properties:
Rheological properties of bitumen
• Viscous liquid
• Above softening point: nearly viscous performance
• Below breaking point: Elasticity
• Difference: plasticity index

Temperature Consistency
-20°C Pure elasticity
30°C Viscoelasticity
180°C Pure viscosity
Bitumen grading:
Different specifications (or agencies) use different approaches for grading and naming the
grades of bitumen. There are three general groups of bitumen that are graded in different
ways:
1. Paving grade bitumen
• Bitumen from this group has specification from European standards and US standards
as well
• The European specifications subdivide bitumen from this group into three subgroups
• Specifications of two subgroups are based on the penetration values and the last
subgroup of soft bitumen is based on the kinematic viscosity at 60º C
• The subgroup used in pavement engineering has penetration values ranging from 20 to
220 dmm
• This subgroup has eight grades designated by the penetration values at 25⁰ C
• 20/30 30/45 35/50 40/60 50/70 70/100 100/150 160/220
• With the US specifications paving bitumen is graded based either on the Penetration
or Viscosity value
• Six Viscosity grades by ASTM are designated by AC and a number denoting viscosity at
60⁰ C (0.1 of value)
• AC ‐ 2.5 AC ‐ 5 AC ‐ 10 AC ‐ 20 AC ‐ 30 AC ‐ 40
• ASTM has specified five bitumen grades based on penetration designated in
the same way as European (40/50 60/70 85/100 120/150 200/300)
• Current specifications of bitumen in South Africa (SANS 307) uses the
ASTM tests on Penetration values
• Four bitumen grades are currently available in South Africa (SANS 307)
specified with penetration values (40/50 60/70 80/100 150/200)
2. Hard paving grade bitumen
• This type have bitumen that have very high stiffness modulus values
• They are used in places where the daily traffic flow is very high when annual
temperatures are intermediate or high
• European standards have specifications for this group
3. Oxidised bitumen
• This type of bitumen is not used for pavement construction, but in
waterproofing, roofing, adhesives and insulations
• It is produced by blowing air through hot bitumen (at temperature ranging
between 240⁰ C and 320 ⁰ C)
• Changes to molecular weight when blown, makes it harder and less
susceptible to temperature changes
Tests on bitumen grading:

The suitability of bitumen as binder for road


construction is ensured by carrying out the
following tests:
• Penetration Test,
• Float Test Tests for bitumen consistency
• Viscosity Test,
• Softening Point Test (Ring and ball test),
• Flash and Fire Point Test, and
• Ductility Test
Penetration Test :

• Penetration test involves measuring the penetration of


a standard needle into a sample of bitumen under
standard temperature, time and load.

• The test is an empirical method and not fundamental


and so it does not tell the rheological behaviour of
bitumen.

• It is not a very good method for grading of bitumen.


Penetration Test:
• This test is aimed at assessing the hardness or softness of
the bitumen
• The depth of penetration of the needle is measured in the
units of 0.1 mm and is reported as penetration units
Example: If a needle penetrates 10mm, the bitumen
penetration is recorded as 100
• The test is done using a Penetrometer, which consists of a
needle assembly weighing 100g (standard load)
• The needle is made to penetrate the binder for five seconds
(standard time)
• The test is carried out at a temperature of 250C (standard
temperature)
• The binder whose penetration ranges between 8mm and
10mm has a penetration grade of 80/100
Float test:
• Coat the brass plate with an equal value of glycerin and dextrin.
• Put the collar from the small end on the brass plate.
• Heat the bitumen until it becomes completely liquid. Do not overheat the
specimen. Because its properties changed due to evaporation. The lowest
temperature at which the bitumen becomes liquid is suitable. 
• Pour the melted sample into the collar. Be sure there is a little extra material
on the collar.
• Place the tar bitumen immediately in the water bath at a temperature of 5
°C for 5 minutes. But for asphalt and asphalt products let them cool at room
temperature. Then placed in a water bath at a temperature of 5 ° C for 5
minutes.
• Cut the excess bitumen from the top of the collar. Then place the assembly
in the water bath again. It should remain there, about 15 to 30 minutes.
• Record the time until the moment that water breaks through the material.
This time is the float value.
Float test:
Viscosity test:
• Viscosity grading is more fundamental than penetration grading

• Bitumen with similar viscosities normally give similar rutting


performance, which is not the case with penetration grading

• Better guidance can be formulated for mixing and compaction


temperatures with viscosity grading as viscosities can be measured at
higher temperatures
• 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 (at high temperature)
• Fatigue failure of bituminous mixes (at intermediate temperature)
• Low temperature cracking (at low temperature)
Viscosity test:
• Viscosity, the opposite of fluidity, is the resistance given by the fluid to
a shearing force
• It is the basic rheological property (or behaviour) of bitumen
• Viscosity can be defined as Dynamic (or Absolute) viscosity μ, which
is given by
Following its definition, the absolute viscosity can be measured by a
Sliding Plate Viscometer
 In this case, a bitumen film of known thickness is placed between
two plates
 For a selected temperature and rate of shear (i.e., velocity v), the
force F needed to move the plate at velocity v is measured and μ
calculated
 The common approach is to use the rotational (Brookfield)
viscometer, where the resistance given by the bitumen to the rotation
of a spindle at a given rotational velocity at a given temperature is
measured from which the viscosity μ can be calculated
 The units used to measure dynamic viscosity are;
 In SI system N‐s/m2 = Pa‐s = kg/(m.s)
 In metric (cgs) system g/(cm.s) = dyne.s/cm2 = poise (p)
Softening point test (Ring and ball test:
• Bitumen being visco‐elastic material does not have a definite melting
point
• A softening point, a temperature at which bitumen attains a specified
consistency (bitumen changes from semi‐solid to liquid state), is then used
• The test gives an idea of the temperature susceptibility of bitumen
• It is carried out by placing a sample of bitumen in a ring with a steel ball
on top
• The whole assembly is placed in a water bath which is heated (at a
controlled rate of 50C per minute) while stirring
• As the bitumen softens, the ball and the soft bitumen will start sinking
• Softening point is the temperature at which the softened bitumen touches
a plate placed at a specified distance below the ring
• A soft grade bitumen has lower softening point
Softening point test (Ring ball test):
Flash and fire point test:
• This test is for assessing the safety when working with bitumen
since it is used at high temperatures
• The tests indicate the fire hazard posed by the binder (i.e.,
bitumen)
• Flash point is the temperature at which bitumen gives off
vapours, which ignite in the presence of a flame, but the vapours
do not burn
• By the definition, a flash point of a liquid is the lowest
temperature at which a liquid can form an ignitable mixture in air
near the surface of the liquid
• Fire point is a temperature beyond the flash point where the
vapours ignite in the presence of the flame and continue to burn
• The test is normally carried out using the Cleveland Open Cup
apparatus
Ductility test:
• This test provides a measure of tensile properties of bitumen (ability of
bitumen to deform under load)
• If the binder does not have sufficient ductility, it will be more likely to crack
when it is extended
• It is carried out by stretching bitumen briquette of standard shape at a
standard rate of pulling at a standard temperature
Chemical composition of bitumen:
• Bitumen is a material with a complex chemical mixture of
molecules, which are predominantly hydrocarbons
• It may contain some traces of compounds that may contain;
• Oxygen, Sulphur and Nitrogen
• Nickel, Magnesium, Calcium, Iron and Vanadium (in the
form of inorganic salts and oxides)
The exact proportions of different elements
depends on two aspects:
• The source of the crude oil
• Modifications during the fractional distillation process
Chemical composition of bitumen:
Sol and Gel Type of Bitumen:

• With sufficient quantities of resins and aromatics of adequate solvating capacity,


asphaltenes are fully dispersed and the resulting micelles have good mobility
within the bitumen.
• In such cases the bitumen is known as a "solution" type (SOL) bitumen
• Insufficient quantities of aromatic or resin fraction to disperse the micelles, or
has insufficient solvating capacity, the micelles can associate together
• This leads to structures of linked micelles, and these types of bitumen are
known as "gelatinous" types (GEL) bitumen.
Bitumen ageing:
• Bituminous binders undergo aging due to the loss of volatile matter and oxidation
• This process normally occurs in two phases;
Short term aging
• This normally occurs at high temperature (can be in bulk or in thin films that
coats aggregates)
• The process can take place during storage, transportation, mixing and placing
• The extent of aging depends on the surface area exposed to the air
Long term aging
• This occurs due to oxidation, which occurs during the service life
• As bituminous binders age, they become harder and stiffer resulting into;
• Decrease of penetration
• Decrease of ductility
• Increase of viscosity
• Increase of softening point
Measurements/testing of the aging characteristics:

SHORT TERM AGING


This is measured either by:
• Thin Film Oven – TFO
• Rolling Thin Film Oven – RTFO
• In the RTFO the binder is kept at high temperature (1630C) for a
specific period
• The properties of the aged binder are then compared with those
of un‐aged binder.
LONG TERM AGING
• A Pressure Aging Vessel is used to simulate the long-term aging
that occurs over a long time in pavements.
Temperature susceptibility of binders:

• Bitumen being a thermo‐plastic material (i.e., being soft when hot and hard
when it is cold), has a major concern in the variation of its consistency with
temperature.
• Such variation of properties with temperature is called temperature
susceptibility.
• Its evaluation is done by conducting either viscosity test or penetration test at
different temperatures
Example: Penetration tests carried out at different temperatures like 200C,
400C etc.,
Chemical changes of bitumen:
• Changes in the bitumen composition which leads to changes in its properties occur
from the time of production
• During fractional distillation process, removal of lighter fractions from the crude oil
causes an increase in the concentration of asphaltene
• This change makes bitumen harder and less susceptible to the temperature changes
• During the processing of bituminous mixes (mixing, laying and compaction), bitumen
also undergoes chemical changes (see the diagram in the next slide)
• It is therefore important to observe the recommended temperatures during the
processing
• Bituminous mixtures start to harden after compaction due to the temperature drop as
some volatile content evaporating
• This form of hardening is non‐reversible
• The hardening process of bitumen continues during the service life of the material
due to the oxidation of organic compounds as well as further volatilization (increasing
the proportion of asphaltenes)
• This process is called AGEING of the bitumen, which is affected by two factors
 The voids in the bituminous mixture
 Climatic conditions – Ambient temperatures and the periods of sunshine
Chemical changes of bitumen:

• High ambient temperatures and longer periods of


sunshine in a year increase the oxidation
The chemical changes that occur causes bitumen
to:
 Experience reduction of penetration
 Reduce its elasticity
 Reduce its adhesion ability
 Increase its softening point
• Oxidation and ageing processes in bitumen can
be reduced by using chemical additives
Chemical changes of
bitumen:
Bitumen behaviour under the application of loads
• When bitumen is subjected to a load, its behaviour will depend on two conditions
• Temperature
• Loading duration
The material displays a kind of behaviour called VISCOELASTICITY, which can be subdivided in
three forms:
 Elastic Behaviour – which is exhibited under certain conditions (i.e., not always)
 Bitumen behaves elastically at low temperatures and/or when the load is applied for short
durations
This behaviour is characterized by two effects
 Deformation that does not depend on the time duration (not time dependent deformation)
 Deformation that is fully recovered when the load is removed (material does not suffer
permanent deformation under the action of the load)
• Viscous Behaviour – which is also exhibited under certain different conditions (i.e., not always).
This behaviour occurs at high temperatures and/or when the load is applied for prolonged
durations the material in this case behaves like fluid and the behaviour is characterized by one
main effect
• Material undergoes plastic deformation (deformation that is not recoverable on removing the
load)
Rut formation on pavements that have bituminous binders is a typical
plastic deformation that is caused
by repeated wheel loads at elevated temperatures
 Both, Elastic and Viscous Behaviour
 This happens at intermediate temperatures and/or where the material
exhibits both behaviours
 The diagram below shows the strain – time relationship for the bitumen
behaviour
Cutback and fluxed bituminous binders:
• Cutback bitumen is obtained by reducing viscosity of penetration
grade bitumen using volatile solvents
The volatile solvents (also called fluxes or cutters) that have been used
are divided into two groups:
Petroleum solvents
 These are lighter fractions of petroleum (commonly used are white
spirit and kerosene)
 These are the most common types and are simply referred to as
CUTBACK BITUMENS (ASPHALTS)
Flux oil
 Flux oil are less volatile compared to petroleum solvents
The resulting bitumen is called FLUXED BITUMEN
The flux oil can be from petroleum origin or from a plant‐based
products
 Cutbacks and fluxed bitumen become fluid enough (low viscosity) at normal
temperatures and so they need much less heating during the application
(compared to the bitumen)
 Once the flux evaporates, bitumen returns to its original state of being viscous
and binds the mineral aggregates
 The use of cutbacks (and the less frequently used fluxed) bitumen is faced by
three shortcomings:
 The flux materials are costly non‐renewable products, and their
evaporation amounts to loosing them away
 Evaporation of the flux also contributes to air pollution
 High energy demand for their production
 As a result, the use these products these days is limited to:
 Use for prime coating
 Production of ready‐mixed bituminous mix for repair work (potholes, utility
cuts etc.)
 In situ production of cold to semi‐warm bituminous mixtures especially in
the remote areas far from the hot mix plant
 American (and South African) standards, recognize cutbacks derived from
petroleum solvents only
• According to these standards, cutbacks grades are grouped according to the rate of
curing (i.e., rate of solvent evaporation) into:
 Slow Curing Cutbacks – SC
 Medium Curing Cutbacks – MC
 Rapid Curing Cutbacks – RC
• The medium curing (MC) cutbacks is the group that is mainly used in pavement work
• Grading of MC cutbacks is based on kinematic viscosity at 60o C and designated
using the minimum viscosity
• ASTM D 2027 and AASHTO M 82 identify five grades MC cutbacks
 MC‐30 – Min viscosity =30 mm2/s Max viscosity = 60 mm2/s Available in SA
specifications
 MC‐70 – Min viscosity = 0 070 mm2/s Max viscosity = 0 140 mm2/s
 MC‐250 – Min viscosity = 0 250 mm2/s Max viscosity = 0 500 mm2/s
 MC‐800 – Min viscosity = 0 800 mm2/s Max viscosity = 1 600 mm2/s
 MC‐3000 – Min viscosity = 3000 mm2/s Max viscosity = 6000 mm2/s Available in
SA specifications
 South African specifications specifies MC‐10 and the other two shown above (MC ‐30
and MC‐3000)
 For the SC and RC cutbacks, each one has four grades starting with MR‐70 and MS‐
70 (no MR‐30 and MS‐30)
Bituminous emulsions:
• Emulsion is a mixture of immiscible liquids, which forms two main components called PHASES
 Continuous phase
 The liquid forms a continuous medium in which the other liquid is dispersed
 Dispersed or discontinuous phase
 The liquid that is finely divided into very small droplets, which are dispersed in the continuous
phase
Bitumen emulsion is made with the following components:
 Bitumen forms the dispersed phase
 Water forms the continuous phase
 Emulsifier (or emulsifying agent) is added during the emulsification process to help in the
formation of the emulsion (modifying its properties and making it stable)
 An emulsifier carries a charge (+ve or ‐ve) that it introduces to the surface of the bitumen
particles
 The surplus emulsifier cause the water environment to either be acidic or alkaline
 Modifier is a polymer added to the emulsion if a modified bitumen emulsion is desired
 Other additives may be added in very small quantities to improve certain qualities of the
emulsion
• Examples of the additives, which can be used include;
 Coating improvers
 Anti‐stripping agents
 Stabilisers
 Acidity regulators
 Break control agents
• The charge introduced on the surface of the bitumen particles distinguishes the emulsions
into two classes
 Cationic or acidic emulsions – The particles are charged positively
•  This is the type that is mainly used these days, replacing the previously common anionic
type in the past
 Anionic or alkaline emulsions – The particles are negatively charged
 Bitumen emulsions have the following advantages
 Less amount of energy is used during their production and application
 As the evaporating medium is only water their use reduces atmospheric pollution
 As no heating is needed at all, bitumen emulsions provide a safe working environment
Temperature susceptibility of binders:

• Bitumen being a thermo‐plastic material (i.e., being soft when hot


and hard when it is cold), has a major concern in the variation of
its consistency with temperature
 Such variation of properties with temperature is called
temperature susceptibility
 Its evaluation is done by conducting either viscosity test or
penetration test at different temperatures
Example: Penetration tests carried out at different temperatures
like 200C, 400C etc.,
• A plot on a semi‐log scale of such a test yields a straight line graph
whose slope A is termed the TEMPERATURE SUSCEPTIBILITY
Temperature susceptibility of binders:

For paving binders, the value of A ranges between 0.015 and 0.06
 A more suitable parameter used to describe the temperature susceptibility of
bituminous binder is the PENETRATION INDEX (PI)
 This value is correlated to A by the following formula;
Thank you for your kind attention

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