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25th ARRB Conference Shaping the future: Linking policy, research and outcomes, Perth, Australia 2012
LABORATORY STUDY ON BITUMEN MODIFICATION FOR IMPROVED PHYSICAL, RHEOLOGICAL PROPERTIES AND THE EFFECT OF SHORT TERM AGEING
Maninder Singh, Indian Institute of Technology Roorkee, India Praveen Kumar, Indian Institute of Technology Roorkee, India ABSTRACT
Bitumen ageing is one of the principal factors causing the deterioration of bitumen pavements. It is responsible for deterioration of physical and chemical properties of the bitumen binder. The influence of vehicle traffic on road pavements causes natural aging processes and gradual loss of viscoelastic properties of bitumen binders. In the present study Ethylene Vinyl Acetate (EVA), a plastomer; Linear Styrene Butadiene Styrene (SBS), an elastomer and Crumb Rubber (CR) were used in various percentages (2 to 8%) as modifiers in 60/70 grade bitumen. The effect on physical properties in terms of penetration, softening point, weight loss and rheological properties of the bituminous binders in terms of their complex modulus (G*) and G*/Sin before and after ageing were measured. Testing was performed at temperatures ranging from 40 C to 70 C in increments of 6 C at a frequency of 10 rad/sec using dynamic shear rheometer (DSR). The results show that after ageing softening point increases and penetration decreases with increasing percentage of modifier. The G*/Sin is found to increase with increase in percentage of modifier after ageing indicating higher rutting resistance. Index Terms-- Modified bitumen, DSR, Complex modulus, Ageing, SBS.
INTRODUCTION
Environmental factors such as temperature, air and water can have a profound effect on the durability of asphalt concrete mixes. India is a very vast country, having widely varying climates, terrains, construction materials and mixed traffic conditions both in terms of loads and volumes. The flexible roads constitute about 98 percent of the total roads network.The use of quality binder is one of the requirements for the satisfactory pavement performance. The aim of binder modification is to produce new binders with better rheological and mechanical characteristics which allow the manufacturing and application of road bituminous mixes with improved performance. Increased traffic factors such as heavier loads, higher traffic volume and higher tyre pressure demand higher performance pavements.The purpose of bitumen modification using polymers and rubbers is to achieve desired engineering properties such as increased G*/Sin and reduced plastic flow at high temperatures and increased resistance to thermal fracture at low temperatures. Dynamic rheological properties refer to responses of a material to periodically varying strains or stresses and dynamic shear rheometer is used to measure these properties. The primary parameters for characterization of the bitumen are complex modulus (G*) and phase angle ().Phase angle measures the viscoelastic character of the bitumen. A purely viscous liquid and an ideal elastic solid demonstrate of 90 and 0 , respectively. The viscoelastic parameters of bitumen are functions of temperature and frequency, which may be modified by the addition of polymers. Polymer modification are known to improve binder performance as reported in number of studies [3,6,7,10,12,14].
ARRB Group Ltd and Authors 2012
Ageing or hardening of bituminous binder occurs during mixing and lay down process and during service. The complex process of ageing has been studied by several authors [4],[8],[9] and it was established that bitumen ageing is one of the principal factors causing negative change of physical structures and chemical compositions, and results in the deterioration of its physical behaviours [5].Under extreme aging conditions, even conventional binder is prone to lose its binding capacity [11].The oxidation of binder further contributes to change in the structural and functional grouping that is responsible for chemical and physical aging [2].After the short-term aging, the proportion of bitumen compounds such as asphaltenes and resins were increased [15].Subsequently it becomes less adhesive but more cohesive, and make it increasingly brittle and it was established that the complexity increases when the polymer is present [13].In phases of PMB dispersions processing as well as in phases in use, the rheological properties of PMB are very important.
EXPERIMENTAL PROGRAMME Materials

VG 30 bitumen was used for the present study. Crumb rubber (CR) and two types of polymers, ethylene vinyl acetate (EVA) and styrene butadiene styrene (SBS) with varying percentage of 2%, 5% and 8% were used in this study.CR is material locally available and material passing through 1.18 mm IS sieve and retained on 200 micron IS sieve was used (IRC: SP: 53-2002).Ethylene vinyl acetate (EVA) copolymer, available as pellets 4 to 5 mm in diameter supplied by KLJ Polymers, New Delhi was used. Styrene butadiene styrene (SBS) polymer used was powdered Finaprene 503 supplied by ATOFINA.Finaprene 503, a linear SBS polymer contains 31% styrene.
Preparation of modified bitumen

In preparing the modified binders, about 500 g of the bitumen was heated to fluid condition in a 1.5 litre capacity metal container. The mixing was performed in the laboratory using an oven fitted with a mechanical stirrer and rotated at 1550 rpm for mixing the bitumen and modifiers. For blending of crumb rubber with bitumen, bitumen was heated to a temperature of 160 C and then crumb rubber was added. The blend was mixed manually for about 3-4 minutes. The mixture was then heated to 170 C and the whole mass was stirred using a mechanical stirrer for about 50 minutes. Care was taken to maintain the temperature between 160 C to 170 C. For preparation of EVA blends, bitumen was heated to a temperature of 170 C. As the bitumen attained a temperature of 170 C, the different EVA polymer contents by mass (2 to 8%) were added to the bitumen and vigorously agitated. The temperature was maintained between 175 C to 180 C and mixing was then continued for 80-90 minutes. For SBS blends, bitumen was heated to a temperature of 170 C and the appropriate quantity of SBS copolymer was added. The temperature was maintained between 175 C to 180 C. The contents were gradually stirred for about 55 minutes. The modified bitumen was cooled to room temperature and suitably stored for testing.
Testing
Rotational Viscometer (ASTM D4402) was used for determining the kinematic viscosities of the samples at 135 C for 5 min at 20 rpm. SR 5 Asphalt Rheometer was used for measuring the dynamic rheological properties, as per guidelines prescribed in AASTHO TP5-1994.Ageing of the binders was performed by Thin Film Oven Test TFOT, ASTM D 1754) as specified by IRC: SP 53-2002 For the DSR measurements, the 25 mm plates with 1 mm gap were used for testing of neat and TFOT samples and measurements were taken in temperature range from 40 C to 70 C in an increment of 6 C. All the binders were tested at a frequency of 10 rad/sec to determine the performance grade as per SHRP specifications.
RESULTS AND DISCUSSION Before ageing

Table 1: Physical properties of unaged bitumen Binder type Penetration at 25 C, (dmm) (IS:12031978) 65 45 40 34 50 43 36 59 56 50 Softening point, (C) (IS:12051978) 48.5 63 70 74 65 75 83 52.5 57 59 Elastic recovery at 15 C, (%) (ASTM D5976-1996) 20 47 54 50 62 74 84 55 61 72 Specific gravity (IS:12021978) 1.037 1.033 1.031 1.026 1.029 1.022 1.013 1.031 1.025 1.02 Viscosity cP (IS 12061978) 554 919 1382 3133 1093 2715 4466 654 805 1205
60/70 2%EVA 5%EVA 8%EVA 2%SBS 5%SBS 8%SBS 2%CR 5%CR 8%CR
Physical properties
Penetration Test
The penetration values of bitumen modified with different percentage of Crumb rubber (CR), Ethylene vinyl acetate (EVA) and Styrene butadiene styrene (SBS) are shown in Table 1. The penetration values are decreasing significantly for 60/70 bitumen mixed with CR, EVA and SBS. It is observed that the penetration value decreases as the concentration of modifier increases. Further, the bitumen modified with EVA seems to be more effective in the penetration values as compared to CR and SBS modifiers.
Softening point test

As shown in Table1 the softening point increases with increase in percentage of modifiers as the bitumen becomes increasingly viscous. The effect of SBS on softening point is much more than that of EVA and CR. The softening point for 60/70 bitumen increased to more than 70 C by addition of 8% EVA and 5% and 8% SBS and should not be used in road construction, but may be used as a roofing material [1].
Elastic recovery results

The elastic recovery test was performed as per ASTM D5976-1996 and was found to increase with increase in percentage of modifiers. However, in case of bitumen modified with EVA, it slightly increases after 5%. It is clearly shown in Table 1 that the bitumen modified with SBS gives the maximum elastic recovery than that of bitumen modified with CR and EVA.
Specific gravity test results

Table 1 show that the specific gravity values decreases significantly by modifying the bitumen. The values for neat 60/70 bitumen are 1.037 which decreases to 1.02, 1.026 and 1.013 respectively for 8% CR, EVA and SBS.
Viscosity results
The viscosity increases on introduction of CR, EVA and SBS, but the change is more pronounced in case of SBS as compared to CR and EVA (Table 1).
Rheological properties
Effect on G*
Figure1: Relationship between G*and with temperature for bitumen modified with CR
Figure 2: Relationship between G*and with temperature for bitumen modified with EVA The complex modulus (G*) and phase angle () versus temperature at 10 rad/s, and variation in G*/Sin with temperature for 60/70 grade bitumen modified with CR, EVA and SBS are shown in Figure 13. It may be seen that the complex modulus G*of the modified binders is higher as compared to neat bitumen. It is observed that complex modulus increases significantly at lower temperatures compared to higher temperatures for all percentage of modified bitumen i.e. the variation in complex modulus decreases with increase in temperature. The complex modulus increases with increase in percentage of modifier. The improved elasticity is also different for the same percentage of various modifiers. However, in general, a binder with high values of G* at high temperature is expected to provide an improved deformation resistance.
Figure 3: Relationship between G*and with temperature for bitumen modified with SBS
Figure 4: G*/sin as a function of temperature for CR
Figure 5: G*/sin as a function of temperature for EVA
Effect on G*/Sin
Rutting of bituminous pavements is the most prevalent problem in India. It is useful to determine the stiffness of the bitumen at 60 C so that it can specify its minimum stiffness to ensure adequate resistance to rutting during summer. The parameter G*/sin is a measure of stiffness of the binder which is also used as an indicator for rutting resistance in the current US superpave specifications. The rutting resistance of the binder increases with increase in the percentage of modifier. The rutting resistance increases by nearly three times with addition of 2% SBS in 60/70 bitumen at 58 C Figure 6. By addition of 2% EVA, the rutting resistance is
increased by more than four times Figure 5. However, the increment in rutting resistance is less than two times in case of CR even with 5% CR Figure 4. EVA modified binder has shown higher rutting resistance value than SBS and CR modified binders at the same percentage of modifier. Therefore, EVA binder is suggested to use in the area of heavy traffic and at high temperatures. As per the specifications, to assure adequate performance at the hot-mix plant and during laying, the value for G*/sin , of the original unaged binder must be greater than 1.0 kPa at an assigned temperature which depends on the high temperature service environment of the binder. This reduces the potential of having a tender mix if at all the plant conditions are not as severe as those simulated by the TFOT. From Figure 4-6, it can be clearly seen that the values of G*/Sin are as per the specification values for all temperatures of 60/70 bitumen except higher temperatures (i.e.> 64 C) fails to meet the criterion.
Figure 6: G*/sin as a function of temperature for SBS Table 2: Physical properties after TFOT ageing Binder type 60/70 2%EVA 5%EVA 8%EVA 2%SBS 5%SBS 8%SBS 2%CR 5%CR 8%CR Penetration at 25 C, (dmm) 58 33.5 32 26 42 37.5 30 39 38 36.5 Softening point, (C) 51 67.5 74 77.5 68 79 85.5 56 60 62.5 % Wt. loss after TFOT 0.03 0.07 0.10 0.15 0.05 0.08 0.12 0.09 0.13 0.18
After ageing
Physical properties after ageing
Penetration test Due to evaporation of volatile material the bitumen after ageing hardens and thus penetration value decreases and the value decreases as the percentage of modifier increases (Table 2). Softening point test The softening point value increases after ageing and the value increases with increasing modifier content (Table 2).
Loss in weight
The loss of volatile fractions contributes to the difference in weights between original and aged sample. The maximum loss in weight should be 1% as per IRC: SP: 53:2002. From Table 1, it is observed that there are greater variations in the values after the modification is 5% or more (Table 2).
Rheological properties after ageing
Figure 7: Variation of G* with temperature for bitumen modified with CR after ageing
Figure 8: Variation of G* with temperature for bitumen modified with EVA after ageing
Figure 9: Variation of G* with temperature for bitumen modified with SBS after ageing
Effect on G* after ageing

Ageing of bitumen occurs by chemical and/or physical changes during the construction stage and throughout its service life. The process is usually accompanied by loss of volatiles and hardening of the binder, which in turn influences the deterioration of the asphalt pavement ageing of the binders was performed using TFOT in the present study. The complex modulus after short term ageing of bitumen at different temperatures is graphically represented in Figure
7-8. As can be seen, there is a constant increase in complex modulus, G*, with increase in percentage modification after Ageing the unmodified and modified bitumen. The result of ageing is an increase in complex modulus G*, which indicates the hardening of the bitumen.
Figure 10: Variation of G*/sin with temperature for bitumen modified with CR after ageing
Effect on G*/Sin after ageing

The rutting resistance as expected is found to increase with increase in the percentage of modifier after TFOT Ageing (Figure 10-12). Also, G*/sin varied almost linearly with temperature. Therefore, 60/70 binder can beneficially be used in the areas of heavy traffic and at high temperatures, if modified. To evaluate asphalts ability to resist rutting, the binder is aged using the thin film oven test (TFOT, ASTM D 1754). The residue must have a value of G*/sin , greater than 2.2 kPa at the service environment's highest temperature. From the values of G*/sin represented in Figure 10-12, it is observed 60/70 bitumen just meet the specifications at lower percentage of modification and higher temperatures.
Figure 11: Variation of G*/sin with temperature for bitumen modified with EVA after ageing
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Figure 12: Variation of G*/sin with temperature for bitumen modified with SBS after ageing
CONCLUSIONS
1. The physical properties of bitumen such as penetration, softening point and elastic recovery are improved with addition of the polymers and crumb rubber. There is a significant decrease in penetration values for modified blends, indicating the improvement in temperature susceptibility resistant characteristics. EVA modified binder gives lower penetration value.SBS modified binder gives higher softening point and better elastic recovery than EVA and CR modified binders. The softening point increases with increase in percentage of modifier as the bitumen becomes increasingly viscous. 2. Elastic recovery increases with increase in percentage of modifier for CR and SBS modified binders. Maximum elastic recovery was observed at 5% polymer for EVA modified binder. Higher value of elastic recovery indicates more flexibility to the binder and will increase the life of pavement at low temperature. 3. Following the ageing process, higher softening points as well as lower penetration values are found. The loss of volatile fractions contributes to the difference in weights between original and aged sample. 4. There is a constant increase in complex modulus, G*, with increase in percentage modification after ageing. The increase in complex modulus and decrease in phase angle of the modified binder indicate higher resistance to deformation as compared to neat bitumen. 5. The parameter G*/sin is a measure of stiffness of the binder. The rutting resistance as expected is found to increase with increase in the percentage of modifier after TFOT ageing. G*/sin varies almost linearly at higher temperature of 58 C. EVA modified binders were found to have higher rutting resistance to deformation under loading as compared to CR and SBS modified binders at high temperature. 6. In the present study, the value of G*(complex modulus) and G*/sin for EVA binders are found to be higher than SBS and CR modified binders. So EVA modified binders can be used in very high temperature and heavy traffic areas but it cannot be used at lower temperature as its ductility value is less.SBS modified binders can be used in all climatic conditions of low as well as high temperature (all places of India). CR modified binders will be suitable for moderately high temperature zone and low cost roads.
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Lots of previous studies on CR, SBS and EVA were conducted, but none of them compared the results amongst them. The present study compares the effect of binder modification with SBS, EVA and CR and states the climatic conditions in which each one should be used beneficially.
REFERENCES
Brown, E.R., Kandhal, P.S., Lee, D.Y. and Lee, K.W. (1996), Significance of Tests for Highway Materials, Journal of Materials in Civil Engineering, Vol.8, No.1, pp.26-40. Lamontagne, J., Dumas, P., Mouillet, V. and Kister, J. (2001), Comparison by Fourier transform infrared (FTIR) spectroscopy of different ageing techniques: application to road bitumen, Fuel, 80: 483-488, Lepe, A.P., Boza, F.J.M., Gallegos, C., Gonzalez, O., Muzoz, M.E. and Santamari, A. (2003), Influence of the Processing Conditions on the Rheological Behaviour of Polymer Modified Bitumen, Fuel 82, pp1339-1348. Lu, X.H. and Isacsson, U. (1998), Fuel 77 9-10: 961. Lu, X.H. and Isacsson, U. (2002), Construction and Building Materials 16:15, Mehndiratta, H.C. and Chandra, S. (2000), Investigation on Bituminous Mixes with Blended Modifiers, Journal of Institution of Engineers, India, Vol. 81, pp 115-119. Panda, M. and Mazumdar, M. (1997), Development and Evaluation of a Bituminous Paving Binder Containing Reclaimed Polyethylene, Indian Highways, IRC, Vol. 25, pp 11-21. Rek, V. and Barjaktarovi, M.Z. (2002), Mat Res Innov 6 2:39. Rek, V., Barjaktarovi, M.Z. and Holjevac Grguri, T. (2004), The rheological properties of aged polymer bitumen, In: Reichert T, eds. (2004) Natural and Artifical Ageing of Polymers, Gesellschaft frUmweltsimulatione eV GUS, Pfinztal. Singh, K.L. (2006), Rheological Behaviour of Bituminous Binders for Indian Conditions, Ph.D. Thesis, Transportation Engineering Section, Department of Civil Engineering, IIT Roorkee, pp 21-230. Valcke, E., Rorif, F. and Smets, S. (2009), Ageing of EUROBITUM bituminised radioactive waste: An ATRFTIR spectroscopy study, Journal of Nuclear Materials, 39: 175-185. Wahhab, H.A.A. and Amri, G.A. (1991), Laboratory Evaluation of Reclaimed Rubber Asphaltic Concrete Mixes, Journal of Materials in Civil Engineering, ASCE, Vol. 3, No. 3, pp 189-203. Whiteoak, C.D. (1991), Shell Symposium, Bucharest, Romania. Yousefi, A.A. (2002), Rubber Modified Bitumen, Iranian Polymer Journal, Vol11, No.5, pp 303309. Zhang, F., Yu, J. and Han, J. (2011), Effect of thermal oxidative ageing on dynamic viscosity, TG/DTG, DTA and FTIR of SBS and SBS/sulphur-modified asphalt, Construction and Building Materials, 25: 129-137.
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25th ARRB Conference Shaping the future: Linking policy, research and outcomes, Perth, Australia 2012

ARRB Group Ltd and Authors 2012

EXPERIMENTAL PROGRAMME Materials

Preparation of modified bitumen

ARRB Group Ltd and Authors 2012

RESULTS AND DISCUSSION Before ageing

Softening point test

Elastic recovery results

ARRB Group Ltd and Authors 2012

Specific gravity test results

ARRB Group Ltd and Authors 2012

ARRB Group Ltd and Authors 2012

Figure 4: G*/sin as a function of temperature for CR

Figure 5: G*/sin as a function of temperature for EVA

ARRB Group Ltd and Authors 2012

ARRB Group Ltd and Authors 2012

Rheological properties after ageing

ARRB Group Ltd and Authors 2012

Effect on G* after ageing

ARRB Group Ltd and Authors 2012

Effect on G*/Sin after ageing

ARRB Group Ltd and Authors 2012

ARRB Group Ltd and Authors 2012

ARRB Group Ltd and Authors 2012

ARRB Group Ltd and Authors 2012

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