EFFECT OF AGEING IN VARIOUS BITUMINOUS MIXES

Hapson Errol D,souza,Shreyansh.m.chougule

Under Graduate Students in Civil Engineering, Dayananda Sagar College of Engineering,

S.M. Hills, K.S. Layout, Bangalore-560 078.

([email protected]).

1.0 INTRODUCTION
Bitumen is a complex mixture of chemical compounds. It can be characterised by
fractionation into groups based on polarity. This is sometimes broken down into
asphaltenes- the structuring higher molecular weight highly polar portion, the resins the
”flexibilising “polar portion and the oils , that may be aromatic or aliphatic- these are
dispersing components. What can differentiate rheology is the balance and nature of these
materials.

All aging changes this basic balance in the bitumen .There are several
mechanisms of aging in bitumen and they depend on the bitumen composition as well as
climate and the aggregate in the system. . The main mechanisms of aging of bitumen are
oxidation and the loss of volatiles. When bitumen ages it becomes higher in viscosity (
stiffer) and the composition changes noticeably. These changes can lead to brittleness and
loss of adhesion, especially in the presence of water. (Oxidation products are acidic and
can be hydrolysed).

1.1 NEED OF STUDY

Bitumen is a complex mixture of molecules of a predominantly hydrocarbon

nature, which widely vary in their composition. They contain amongst others minor
amounts of heteroatoms containing sulphur, nitrogen and oxygen and trace quantities of
metals such as vandium, nickel, iron, magnesium and calcium, which occur in the form of
inorganic salts and oxides. The chemical composition of bitumen depends on the origin
of the crude oil and the processes used during bitumen manufacture. Since the chemical
composition of bitumen is extremely complex with the number of molecules with
different chemical structures being astronomically large, it is not feasible to attempt a
complete analysis of bitumen. The characteristics of this ageing process are critical for
understanding the performance of the pavement and have major implications for
pavement design. As the bitumen and the mix become stiffer , the stresses on the
underlying layers of pavement are reduced. This is confirmed by regular deflection
surveys which show that deflections on heavily trafficked motorways remain relatively
constant or, more often, decrease steadily with time. On the other hand, the fatigue
properties of the materials deteriorate with ageing making the material more susceptible
to cracking . Hence to overcome this problem of comparing the field data with the
laboratory results we have tried to analyse the field data

1.2 OBJECTIVES
A) To verify how well the specimens do fabricate using laboratory methods and
to the OBC of various binders.
B) To find changes in properties of bitumen due to ageing..
 

1.3 Problem statement

In developing countries like India, there is a dramatic growth in vehicular traffic .
The properties of bituminous mix vary from production site to field site due to time
required to transport these hot mix asphalt production plant to field. These properties in
turn affect pavement performance indicators, such as rutting and fatigue cracking.
 

2.0 Ageing mechanism

The rheological properties of bitumen change with time (i.e. bitumen becomes harder and
more elastic). This phenomen is called ageing. The amount and rate of ageing depend on
many factors like for example temperature, exposure to oxygen, chemical composition
and structure of the bitumen, etc. Basically, there are four mechanisms of bitumen
hardening: oxidation, loss of volatiles, physical hardening and exudative hardening
Oxidation

Oxidation is considered to be the main cause of bitumen ageing. Like many organic
substances, bitumen slowly oxidises when in contact with air. Polar groups are formed
which tend to associate into micelles of higher molecular weight. The increased and
stronger interactions make the bitumen more viscous. However, results from studies
show that not all bitumens harden (age) to the same extend.

Loss of volatiles
Evaporation of volatile components depends mainly on temperature and the conditions
of exposure. Penetration grade bitumens are relatively involatile and therefore the amount
of hardening resulting from loss of volatiles is usually fairly small.

Physical hardening

Physical hardening occurs during cooling and continues at service temperature. It is

attributed to reorientation of bitumen molecules and crystallization of waxes. Slow
cooling speeds up the process, while instant cooling to low temperature slows the process
down (especially relevant for laboratory testing of bitumen). Physical hardening is
strongly influenced by aggregate-bitumen interactions. Directly after cooling asphalt
sometimes appears to be soft as if it was still warm, while a few days later the asphalt
seems to have matured. This phenomen is called setting and is caused by slow physical
hardening. Reheating can reverse physical hardening.

Exudative hardening

If the constitution of a bitumen is unbalanced it may, when in contact with a porous

aggregate, exude an oily component into the surface pores of the aggregate, resulting in a
hardening of the bitumen film remaining on the aggregate surface. Exudation is primarily
a function of the ratio between the amount of low molecular weight paraffinic
components and the amount and type of asphaltenes. Hardening as a result of exudation
can be substantional when both the exudation tendency of the bitumen and the porosity of
the aggregate are high. Otherwise, exudative hardening will be negligible.
3.0 BINDER TESTS
Laboratory test on binders were conducted at Dayananda Sagar College of
Engineering (DSCE), Bangalore, using CPMB 40, OPMB 70, WPMB modified bitumen.
All the four binders were tested for viscosity, determined by using Rotational
Viscometer, in addition to this the flash point, penetration, softening point, ductility and
elastic recovery of binders were determined.

3.1 Rotational Viscosity Test

Viscosity tests were conducted on all the four binder using a rotational
viscometer. The Rotational Viscometer determines the asphalt viscosity by measuring the
torque necessary to maintain a constant rotational speed of a cylindrical spindle
submerged in an asphalt specimen held at a constant temperature, as per the ASTM 4402
standard test method. Unlike the capillary viscometers used with the viscosity-graded
method, the rotational viscometer can evaluate modified asphalt binders. The viscosity of
asphalt binders can be measured within the range of 0.01 Pa·s (0.1 poise) to 200 Pa-s
(2000 poise) [7]. All the four binders when measured for viscosity qualify the superpave
specifications of maximum value 3 Pa-s at 1350 C. The table 1.0 shows the viscosity test
results. Figure 1.0 show the rotational viscometer used to measure the viscosity.

Table 1.0: Showing Viscosity Test Result using Rotational Viscosity.

Test BCRMB- WPMB OPMB 70 CPMB 40 Test

Specifications 60 Criteria

Viscosity @ 0.68 0.59 0.55 0.61 ASTM 4402

1350 C in Pa-s,
Max 3.0 Pa-s

Figure 1.0: Rotational Viscosity.

Preparation of Aged Samples:

Place the empty tube, with sealed end down in the rack. Heat the sample carefully until
sufficiently fluid to pour, care should be taken to prevent localized over-heating. Pass the
molten sample through a NO. 50 ( IS 300 micron) sieve. After through stirring, pour 50g
into vertically held tube. Fold the excess tube over two times and crimp and seal.

Place the rack containing sealed tube in 163+- 5 C oven. Allow the tubes to stand
undisturbed in the oven for a period of 24+- 4 hours. At the end of the period, remove the
rack from the oven, and place immediately in the freezer at -6.7+- 5 C, taking care to
keep the tubes in vertical position at all times. Leave the tubes in the freezer for a
minimum period of 4 hours to solidify completely.

Upon removing the tube from the freezer, place it on a flat surface. Cut the tube
into 3 equal length portion with the
spatula and hammer. Place top,
middle and bottom portions of the
tube into separate beakers. Place the
beakers into a 163+- 5 C oven until
the bitumen is sufficiently fluid to
remove the pieces of aluminium tube.

Fig 1: showing separation specimen in the oven

3.2 Conventional Test Results

As we all know that bitumen is a viscio-elastic material, the conventional test

does not really measure the visco-elastic nature of the bitumen. The binders were
subjected to conventional tests like penetration, ductility, softening point, flash and fire
point and elastic recovery; the results are given in the table 2.0. These tests proved to pass
all the criteria given by IS specifications.

Table 2.0: Shows the Test Results of the Binders at various Temperatures

Test Description BCRMB-60 WPMB CRMB-40 OPMB 70

andCriteria

Penetration (mm) at 25 deg c IS: 1203-1 25  38  33  42 

Softening Point in deg C IS:1205- 63  61  61  59 

1978

Ductility (cm) IS: 1208-1978 >75  40  >75  >75 

3.3  1.8  5.3  5 

Elastic Recovery in % (Min 50%) at
15 deg c IRC SP :53-2002

Flash Point in deg C Min 230 deg C 250  205  210   

IS: 1209-1978

Fire Point in deg C IS: 1209-1978 310  248  260   

Specific gravity IS: 1202-1978 0.967  0.978  0.982  1.005 

Test Results for aged bitumen

1. OPMB-70

24 HOURS 48 HOURS 72 HOURS

ELASTIC TOP 50% 46% 38%

RECOVERY
MID 37% 42% 48%
IN PER.
BOT 50% 46% 41%

TOP 2.380 2.660 1.880

VISCOSITY MID 2.330 2.250 2.330

IN
BOT 2.550 1.780 2.300
PASCAL-S

2.3.1 ELASTIC RECOVERY V/S TIME 2.3.2 VISCOSITY V/S TIME

E L AS T IC RE CO V E RY IN P E R.

60% 3
V IS CO S IT Y IN P AS CAL -S

50% 2.5
40% TOP 2 TOP
30% MIDDLE 1.5 MIDDLE

20% BOTTOM 1 BOTTOM

10% 0.5

0% 0
24 48 72 24 48 72
TIME IN HOURS TIME IN HOURS
 2. WPMB

24 HOURS 48 HOURS 72 HOURS

ELASTIC TOP 16% 21% 24%

RECOVERY IN
MID 15% 24% 27%
PER.
BOT 17% 29% 24%

TOP .730 1.230 1.630

VISCOSITY IN MID .710 1.350 1.780

PASCAL-S
BOT .750 1.280 1.680

2.3.5 ELASTIC RECOVERY V/S TIME 2.3.4 VISCOSITY V/S TIME

E L A S T IC R E C O V E R Y IN P E R .

35% 4
V I S C O S I T Y I N P A S C A L -S

30% 3.5
25% 3
TOP 2.5 TOP
20%
MIDDLE 2 MIDDLE
15%
BOTTOM 1.5 BOTTOM
10%
1
5% 0.5
0% 0
24 48 72 24 48 72
TIME IN HOURS TIME IN HOURS
 

 
  

3. CPMB 

24 HOURS 48 HOURS 72 HOURS

ELASTIC TOP 6% 19% 23%

RECOVERY
MID 12% 21% 26%
IN PER.
BOT 16% 24% 22%

TOP 1.290 2.450 1.950

VISCOSITY MID 1.080 1.550 1.450

IN PASCAL-S BOT 1.000 1.230 1.480

                                                                                

2.3.7 ELASTIC RECOVERY V/S TIME 2.3.8 VISCOSITY V/S TIME

E L A S T IC R E C O V E R Y IN P E R .

30% 3
V I S C O S I T Y I N P A S C A L -S

25% 2.5
20% TOP 2 TOP
15% MIDDLE 1.5 MIDDLE

10% BOTTOM 1 BOTTOM

5% 0.5

0% 0
24 48 72 24 48 72
TIME IN HOURS TIME IN HOURS
 

 
4.0 PREPARATION OF DENSE BITUMINOUS MACADAM MIX
(DBM)
Tests on aggregate were conducted and physical properties are show in Table 4.0
below. Combined F & E index test for stone dust is not conducted. Aggregate gradation
adopted for the current study was superpave specifications for BC Grade-2. A gradation
curve was plotted, Figure 4.0 shows combined aggregate structure. The Optimum Binder
Content (OBC) of three binder’s viz., BCRMB-60, WPMB, OPMB 70 and CPMB 40
were 4.65, 4.6, 4.75 and 4.55% respectively by weight of aggregate this was found from
the Marshall test, this test also gave us the stability value for various binders.

Sl. No. Test Description Test Method Result

1. Combined F&E IS:2386 (Pt I-1963) 31.80

Index (%)

2. Specific Gravity IS: 2386 (Pt IV- 20mm 10mm

1963)

2.67 2.66

3. Impact Value (%) IS: 2386 (Pt IV- 21.46

1963)

4. L.A. Abrasion Value IS: 2386 (Pt IV- 11.44

(%) 1963)
 Figure 4.0: Gradation Curve for Dense Bituminous

4.1 Laboratory compaction or Marshall Method

The Marshall stability and flow test provides the performance prediction measure
for the Marshall mix design method. The stability portion of the test measures the
maximum load supported by the test specimen at a loading rate of 50.8 mm/minute. Load
is applied to the specimen till failure, and the maximum load is designated as stability.
During the loading, an attached dial gauge measures the specimen's plastic flow
(deformation) due to the loading. The flow value is recorded in 0.25 mm (0.01 inch)
increments at the same time when the maximum load is recorded. The important steps
involved in marshal mix design are summarized next.

4.1.1 Specimen preparation

Approximately 1200gm of aggregates and filler is heated to a temperature of 175-
190 deg C. Bitumen is heated to a temperature of 121-125 deg C with the first trial
percentage of bitumen (say 3.5 or 4% by weight of the mineral aggregates). The heated
aggregates and bitumen are thoroughly mixed at a temperature of 154-160 deg C. The
mix is placed in a preheated mould and compacted by a rammer with 50 blows on either
side at temperature of 138 deg C to 149 deg C. The weight of mixed aggregates taken for
the preparation of the specimen may be suitably altered to obtain a compacted thickness
of 63.5+/-3 mm. Vary the bitumen content in the next trial by +0:5% and repeat the
above procedure. Number of trials is predetermined.

4.12 Determine Marshall Stability and flow

Marshall Stability of a test specimen is the maximum load required to produce
failure when the specimen is preheated to a prescribed temperature placed in a special test
head and the load is applied at a constant strain (5 cm per minute). While the stability test
is in progress dial gauge is used to measure the vertical deformation of the specimen. The
deformation at the failure point expressed in units of 0.25 mm is called the Marshall flow
value of the specimen.
4.12 Determine Marshall Stability Value Of Aged Binder
After determining the marshall stability value and flow value the OBC’s of
various binder are kept in oven for 24, 48 and 72 hours at the temperature of 45degrees.
Now these samples are again tested for marshal stability value and a comparision is
made with the stability values of unaged determined through graph. Now for the
obtained OBC’s 9 marshal samples are prepared for each bitumen. These 9 samples are
equally determined into 3 samples and are binder. The values obtained are tabulated
below
 COMPARISIONS

800
700
FLOW VALUE
600
CPMB-40
500
400
 
WPMB
300
OPMB-70
200
100
0 
1  2 3
TIME(IN DAYS)

COMPARISIONS OF BITUMEN

6000
STABILITY VALUE 
5000

4000 CPMB-40

3000
 
WPMB
2000 OPMB-70
1000

0 
1  2 3
TIME(IN DAYS)
5. CONCLUSION

• In case of OPMB-70, the elastic recovery test gave a satisfactory results for top
and bottom portion at 24 hours and failed at 48 and 72 hours, while the middle
portion has failed to give satisfactory results at 24, 48, 72 hours. all portions of the
bitumen qualified at the 24, 48, and 72 hours in which the max. Value is taken as
3 p-s. The top and middle portion of the bitumen has increased its viscosity values
but the bottom portion initially increased and then decreased considerably.
Stability value decreases with time where as flow value decreases with time.
• In case of WPMB, the elastic recovery test failed to give a satisfactory results for
all the portion at 24, 48, 72 hours, even though the percentage of recovery has
increased. All the viscosity value has qualified for all the portions at 24, 48, 72
hours, but the viscosity value has increased considerably for all the portions.
Stability value increases with time where as flow value increases considerably
with time.
• In case of CPMB, the elastic recovery test has given very unsatisfactory results
for all the portions at 24, 48, 72 hours, but over a period of time the percentage of
recovery as increased considerably. In case of viscosity test all portions of the
bitumen at 24, 48, 72 hours gave a satisfactory results, but there was considerable
variation in the viscosity values of the bitumen. Stability value decreases with
time where as flow value decreases with time.
• WPMB gave better results when compare to other bitumen.
AKNOWLEDGEMENT

The work reported herein was conducted as a research studies at Dayananda Sagar
College of Engineering, Bangalore. Under the guidance of B.V. Kiran Kumar, assistant
professor, Dept. of Civil Engineering, DSCE. The authors acknowledge the valuble
guidance and support extended by our guide prof. B.V. Kiran Kumar. The authors would
also like to acknowledge M/s Tinna Overseas Ltd., Newdelhi and M/s K.K. Waste Plastic
management Pvt. Ltd., Bangalore. M/s Osnar Chemicals Ltd., Mumbai, Novophalt
Chemicals Ltd., Kolkata for providing with the samples.