Laboratory Testing of Bituminous

Material For Road Works

 Scope of Presentation
1. Penetration Test

2. Ductility Test

3. Softening Point Test

4. Specific Gravity Test

5. Flash & Fire Point Test

6. Solubility Test

7. Elastic Recovery Test on Modified Bitumen

8. Separation Difference Test on Modified Bitumen

08/10/22 2
 Penetration Test

08/10/22 3
 Significance
 The penetration test determine the
hardness or softness of bitumen

 The bitumen grade is specified in terms of

the penetration value

 30/40 and 80/100 grade bitumen are

commonly used

 In hot climates a lower penetration grade

bitumen is preferred and vise versa

08/10/22 4
 Significance
 Consistency of bitumen varies with temperature, constituents,
refining process, etc.

 Viscosity is an absolute property, but could not be determined

easily

 Viscosity of cutback bitumen by indirect method (orifice

viscometer)

 Too soft for penetration, too hard for orifice then perform float
test

08/10/22 5
 Significance
 Basic principle of penetration test:
measurement of penetration in units of 1/10th of a mm
of a standard needle of 100 gm in a bitumen sample
kept at 25°C for 5 seconds

 Higher penetration implies softer grade

 Purpose is classification

08/10/22 6
 Figure
Penetrometere Water Bath

Dial

Temperature Controller

Weight
Needle
Mould

08/10/22 7
 Procedure
 Heat the bitumen to softening point +900 C
 Pour the bitumen into the container at least 10 mm above the
expected penetration

 Place all the sample containers to cool in atmospheric temperature

for 1 hour 

 Place the sample containers in temperature controlled water bath at

a temperature of 250 C ± 1o C for a period of 1 hour
 Fill the transfer dish with water from the water bath to cover the
container completely

08/10/22 8
08/10/22 9
Continue. . . .

 Take off the sample container from the water bath,

place in transfer dish and place under the middle of
penetrometer
 Adjust the needle to make a contact with surface of
the sample
 See the dial reading and release the needle exactly
for 5 seconds
 Note the final reading
 Difference between the initial and final readings is
taken as the penetration value in 1/10th of mm
08/10/22 10
 Observation Sheet
(i) Pouring temperature = 100 oC

(ii) Period of cooling in atmosphere, minutes = 60 mts

(iii) Room temperature = 27 oC
(iv) Period of cooling in water bath, minutes = 60 mts
(v) Actual test temperature = 25 oC
Sample No 1 Sample No 2
Penetro-
meter dial Test Test Test Mean Test Test Test Mean
readings 1 2 3 value 1 2 3 value

Initial 0 0 0
Final 85 85 75
Average Value = 82 (Grade is 80/100)
08/10/22 11
 IS Specifications

Bitumen A35 & A45 & A65 & A90 & A200 &
A25
Grade S35 S45 S65 S90 S200

Penetration
20-30 30-40 40-50 60-70 80-100 175-225
Value

08/10/22 12
 Discussion
 Test is highly influenced by the pouring temperature, size of
needle, weight of needle, test temperature, duration of release
of needle

 IRC suggests 30/40, 60/70, 80/100 for BM

 High penetration grade is desirable in colder regions

 Penetration below 20 will result in cracking

 For lower penetration, bonding is difficult, but once achieved

will remain for a long time
08/10/22 13
 Ductility Test

08/10/22 14
 Ductility Machine
08/10/22 15
 Significance
 The ductility of bitumen improves the physical interlocking of
the aggregate bitumen mixes

 Under traffic loads the pavement layer is subjected to repeated

deformation. The binder material of low ductility would crack
and thus provide pervious pavement surface

 The test is believed to measure the adhesive property of

bitumen and its ability to stretch

08/10/22 16
 Significance
 Ductility and penetration go together, in general, but exception
can happen

 Ductility is the distance in cm to which a standard briquette of

bitumen can be stretched before the thread breaks

 Ductile materials is one which elongates when held in tension

08/10/22 17
 Procedure
 The bitumen sample is melted to temperature of 75oC to
100oC above the approx. softening point until it is fluid
 It is strained through IS sieve 30, poured in mould
assembly and placed on a brass plate, after a solution of
glycerine or dextrine is applied over all surfaces of the
mould exposed to bitumen
 Thirty to forty minutes after the sample is poured into the
moulds, the plate assembly along with the sample is
placed in water bath maintained at 27oC for 30 minutes
08/10/22 18
08/10/22
Briquette Moulds 19
Continue. . . .
 The sample and mould assembly are removed
from water bath and excess bitumen material is
cut off by leveling the surface using hot knife
 After trimming the specimen, the mould assembly
containing sample is replaced in water bath
maintained at 27oC for 85 to 95 minutes
 The slides of the mould are then removed and the
clips are carefully hooked on the machine without
causing any initial strain
 The pointer is set to read zero
08/10/22 20
 Ductilometer In Operation
08/10/22 21
Continue. . . .

 The machine is started and the two clips are thus

pulled apart horizontally
 While the test is in operation, it is checked whether
the sample is immersed in water up to a depth of at
least 10mm
 The distance at which the bitumen thread breaks is
recorded (in cm) and reported as ductility value

08/10/22 22
 Breaking of Thread

08/10/22 23
 Observation sheet
(i) Grade of bitumen = 60/70
(ii) Pouring temperature °C = 100 oC
(iii) Test temperature = 27 oC
(iv) Period of cooling (minutes) in Air = 40 min
In water bath before trimming = 30 min
In water bath after trimming = 90 min

Briquette Number
Mean
Test Property
a b c Value

Ductility (cm) 74 76 75

08/10/22 24
 IS Specification

Source of Paving Bitumen Minimum Ductility

& Penetration Grade (cm)
S 35 50
S 45,S 65 & S 90 75
Note: S denotes sources other than Assam
petroleum

08/10/22 25
 Discussion

 Ductility of bitumen is affected by the pouring temperature,

briquette size, placement of briquette, test temperature, rate of
pulling

 Ductility value ranges from 5-100. Low value implies cracking.

Some minimum ductility is needed for flexural strength

 The lack of ductility does not necessarily indicate poor quality.

08/10/22 26
 Softening Point

08/10/22 27
 Significance

 Bitumen does not melt, but change gradually from

solid to liquid

 Softening point is the temperature at which the

bitumen attains particular degree of softening under
specified test conditions

 Ring and ball apparatus is used for the test

08/10/22 28
 Ring & Ball Test Set-up

Mechanical Stirrer

Thermometer
Temp Controlled
Heating Plate
Glass Beaker

Metallic Support

Brass Rings
08/10/22 Steel Balls ø = 9.5 mm (2.5g) 29
(In Ø=15.9 Mm & Out Ø=17.5mm
 Procedure
 Heat the bitumen to a temperature between 125oC to
150oC
 Heat the rings at the same temperature on a hot plate
& place on glass plate coated with glycerin
 Fill up the rings with bitumen

 Cool for 30 minutes in air and level the surface with

a hot knife
 Set the rings in the assembly and place in the bath
containing distilled water at 5oC and maintain that
temperature for 15 minutes
08/10/22 30
Continue….

 Place the balls on the rings

 Raise the temperature uniformly at 5oC per minute till

the ball passes trough the rings
 Note the temperature at which each of the ball and
sample touches the bottom plate of the support
 Temperature shall be recorded as the softening point
of the bitumen

08/10/22 31
 Observation table
(i) Grade of bitumen = 60/70
(ii) Approximate softening point = 40 oC
(iii) Liquid used in water bath(water/Glycerin) = water
(iv) Period of air cooling (minutes) = 30 min
(v) Period of cooling in water bath(minutes) = 15 min

Sample
Test Property
a b mean
Temperature at each sample
42 42 42
touches bottom plate

08/10/22 32
 IS Specifications
Softening Point Repeatability (oC) Reproducibility (oC)
<30oC 2 4
30oC- 80oC 1 2
>80oC 2 4

Bitumen Grades Softening Point (oc)

S 35 55-65
A 45, S 45 & A 65 45-60
S 65 40-55
A 90 & S 90 35-50
A 200 & S 200 30-45
Note: S denotes sources other than Assam petroleum
08/10/22 33
 Discussion
 Test is affected by quality of liquid, weight of ball, rate of
heating etc

 It gives an idea of the temperature at which the bituminous

material attains a certain viscosity

 Bitumen with higher softening point is used in warmer places

 Softening point is very critical for thick films like joint and crack
fillers, to ensure they will not flow

08/10/22 34
 Specific Gravity

08/10/22 35
 Significance
 The specific gravity of bitumen is useful in bituminous
mix design

 Used to convert the specified bitumen content by

weight to volume basis when the binder is measured
by volume

 The specific gravity is useful to identify the source of

a bituminous binder

 Specific gravity of pure bitumen is in range of 0.97 to

1.07

 Specific gravity of cutback ranging from 1.10 to 1.25

08/10/22 36
 Procedure
 Clean and dry the specific gravity bottle and weigh along with the
stopper(W1)
 Fill the bottle with distilled water, place the stopper and keep in
water at a temperature of 27 ± 1oC for at least 30 minutes
 Remove the bottle from water, clean outside and weigh(W2)

 Empty the bottle, clean and dry

 Heat the bituminous material to pouring temperature and pour it

into the empty bottle unto half level without causing the entry of air
bubbles

08/10/22 37
 Specific Gravity Bottle Being
Weighed

08/10/22 38
Continue….

 Cool the bottle to 27oC and weigh along with

stopper(W3)
 Fill the remaining space of the bottle with distilled
water at 27oC, place the stopper and keep in water at
27oC for 30 minutes
 Take the bottle out, clean outside and weigh(W4)

Specific Gravity = W3-W1

(W2-W1)-(W4-W3)
08/10/22 39
 Observation table
Sl Wt of Wt of bottle Wt of bottle Wt of bottle +half Specific gravity
No. bottle + distilled +half filled filled material + (gm/cc)
(gm) water material distilled water g=(W3-W1)/
(gm) (gm) (gm) ((W2-W1)-(W4-
W3))
W1 W2 W3 W4

1 10 25 22.2 26.3 1.12

2 10 25 20.7 25.9 1.09

3 10 25 20.9 25.3 1.03

Average 1.08
Note: Permissible limit ………….Not less than 0.99 gm/cc.

08/10/22 40
 IS Specifications

Specific
Bitumen Grades Gravity
( IS:1202)

A 25, A 35, A 45, A 65, S 35, S 45 & S

0.99
65
A 90 & S 90 0.98
A 200 & S 200 0.97

Note: Specific Gravity of Pure Bitumen = 0.97-1.02

08/10/22 41
 Discussion
 Strict adherence to procedure, explicit temperature for
reproducible results

 Specific gravity is used in mix design and identifying the source

of bitumen

 High specific gravity indicates high mineral content

08/10/22 42
 Flash & Fire Point Test

08/10/22 43
 Significance
 Bitumen materials leave out volatiles at high
temperatures

 These volatiles catch fire causing flash

 This conditions is very hazardous and

therefore is essential to qualify this
temperature for each bitumen grade

 The minimum specified flash point of bitumen

used in pavement construction in Pensky
Martens open cup test is 175oC

08/10/22 44
 Significance
 Flash point : the lowest temperature at which flash occurs due
to the ignition of the volatile vapours when a small flame is
brought in contact with the vapours of the bitumen product
when gradually heated at standard conditions

 Fire point : occurs after flash point , the material catches fire
and continues to burn, and the lowest temperature is fire point

08/10/22 45
 Pensky-Martens Open Cup Method

Volatiles Getting Burnt

Spark Cable

Tripod Stand
Burner

08/10/22 46
 Procedure
 Fill bitumen into the cup up to the indicated mark

 Place the lid and set in the stove to heat the bitumen

 Insert the thermometer

 Apply heat at 5oC to 6oC per minute

 Stir at the rate of 60 rpm

 First apply the test flame at a temperature at least

17oC below the expected flash point and then at
intervals of 1oC to 3oC

08/10/22 47
Continue. . . .

 Discontinue the stirring during the application of test

flame
 Record the temperature reading on the thermometer
at the time of the flame application which causes a
bright flash to give the flash point of bitumen
 At fire point the material continues to burn for 5
Seconds

08/10/22 48
 Observation table

Sample No Flash point °C Fire point°C

1 270 300
2 280 306
Mean 275 303

Note: Permissible limit ………….min 220 0 C

08/10/22 49
 IS Specifications

IS
Temperature Repeatability Min
Specifica
o
C o
C Values
tions

Flash Point 3 175  73 & 1209

Fire Point 6 210 73 & 1209

08/10/22 50
 Discussion
 Closed cup system is more accurate

 Minimum value of flash point is 175°C

 Higher flash and fire point are desirable and safer at

construction site

08/10/22 51
 Solubility test

08/10/22 52
 Significance of Test

 Impurity in bitumen in form of inert minerals, carbon, salts, etc.

could be quantitatively analyzed by dissolving in solvent

 If black carbonaceous residue is over 0.5 %, the bitumen is

considered to be cracked

 The minimum proportion of bitumen soluble in carbon

disulphide is specified as 99 %

08/10/22 53
 Procedure
 Weigh 2 ml of bituminous material in a conical flask

 Add 100 ml of carbon disulphide and dissolve bitumen by

continuous stirring
 Allow the contents to stand for one hour and then filter through
pre-weighed gooch crucible
 Wash the material in gooch crucible by small amount of
trichloroethylene till filtrate is free from colour
 Dry the crucible in oven at 110 C for one hour

08/10/22 54
 Continue. . . .
Calculate the solubility in TCE as under

Matter soluble in TCE = W1-W2 x 100

W1

Where W1= Weight of bitumen sample

W2= Weight pf insoluble material

08/10/22 55
 Observation table

Sample Weight of Weight of Percentage of

No. bitumen insoluble soluble
sample material material
(W1) (W2) (W1-W2) / W1
1 10 0.12 98.8

2 10 0.08 99.2

Mean 99.0

08/10/22 56
 Discussion
 Carbon disulphide (CS2) is the most accepted solvent,
but is highly inflamable

 Alternate solvents include Carbon tetrachloride (CCl4),

methylene chloride, trichloro ethylene. They are
inflamable, but less accurate

 Insoluble materials are dust, salts, minerals,

 Indication of quality of refining petroleum and in

shipment
08/10/22 57
 Other tests
 Loss on heating

 Penetration after loss on heating

 Water content test

 Ash content test

 Viscosity test

08/10/22 58
 Elastic Recovery Test
(Modified Bitumen)

08/10/22 59
 Tests on modified bitumen
 Separation test

 Elastic recovery test

 Viscosity

 Loss in weight (TFOT Residue)

 Increasing softening point (TFOT Residue)

 Reduction in penetration (TFOT Residue)

 Elastic recovery (TFOT Residue)

08/10/22 60
 Elastic recovery
 Prepare three test specimens and condition it at temperature of
15o C
 Elongate the test specimen to 10 cm in the ductility machine at
the rate of 5 ± 0.25 cm per minute
 Immediately cut the test specimen into two halves at the mid
point using scissors
 Keep the test specimen in water bath in an undisturbed
condition for one hour

08/10/22 61
 After one hour, move the elongated half of the test specimen
back into position near the fixed half of the test specimen so
that the two pieces of modified bitumen just touch
 Record the length of the recombined specimen as X

 Calculate the percent elastic recovery as

Elastic Recovery (%) = 10-X x 100

10

08/10/22 62
 Observation table

Sample Length of
No. recombined Elastic recovery
specimen after (10-x)/10x100
one hour (X)
1 5 50

2 4 60

Mean 55

08/10/22 63
 Discussion
 To assess the degree of bitumen modification and quality of
modification

 A simple test used to optimize the doze of polymeric or rubber

additive
 Specification
 PMB (elastomeric) 50 % min
 PMB (plastomeric) 35 % min
 CRMB 35 % min
 NRMB 25-35 % min

08/10/22 64
 Separation Difference Test
(Modified Bitumen)

08/10/22 65
 Procedure
 Place the empty tube, with sealed end down the rack

 Heat the sample until sufficiently to pour. Care should be taken

to prevent localized over heating
 Pass the molten sample trough IS:600 micron sieve

 After thorough stirring, pour 50 gm into the vertically held tube

 Fold the excess tube over two times and crimp and seal

 Place the rack containing the sealed tubes in a 163 ± 5°C oven.

 Allow to tubes stand for 48 ± 4 hours

08/10/22 66
Continue….

 Remove the rack from the oven and place immediately in the
freezer at 6.7 ± 5 oC.
 Leave the tubes in the freezer to solidify the sample completely.

 Upon removing the tube from the freezer, place it on a flat

surface.
 Cut the tube into three equal portions with the knife.

 Discard the center portion and place the top and bottom
portions of the tube into separate beakers.
 After thoroughly stirring, pour the top and bottom samples into
marked rings for the Ring and Ball softening point test.
08/10/22 67
 Pouring Into the Vertically Held Tube
08/10/22 68
 Placing of Tube in Oven
08/10/22 69
 Cutting the Tube Into Three Equal Portions
08/10/22 70
 Observation table

Sample Softening point Softening point Separation

No. of top sample of bottom difference
sample
A B A-B

1 42 40 2
2 43 40 3
3 44 41 3
Average 2.67

08/10/22 71
 Discussion
 Separation of modifier and bitumen occur during hot storage

 Separation test evaluate this Ring and Ball softening point on

the top and bottom portion

 High separation value indicate poor modification

 Specification:
 PMB Max: 3 oC
 CRMB Max: 4 oC

08/10/22 72
08/10/22 73
 Significance
 Softening point, thus gives idea of the temperature at which the
bituminous material attains a certain viscosity

 Softening point is also sometimes used to specify hard bitumen and

pitches

 Higher softening point indicates lower temperature susceptibility

and is preferred in warmer climates

 Softening point is essentially the temperature at which the

bituminous binders have an equal viscosity

 The softening point of tar is therefore related to the equiviscous

temperature (e. v. t.)

08/10/22 74