Modification of Hot Mix Asphalt Using Polyethylene Therephthalate (Pet) Waste Bottles

SUST Journal of Engineering and Computer Sciences (JECS), Vol. 18, No.1, 2017

MODIFICATION OF HOT MIX ASPHALT USING POLYETHYLENE THEREPHTHALATE (PET) WASTE BOTTLES

Ahmed Mancy Mosa Civil Engineering Department, Al-Mansour University College, Baghdad, Iraq

Received: 27/04/2017 Accepted: 22/05/2017

ABSTRACT- This study covers usage of Polyethylene Therephthalate (PET) waste bottles to modify the properties of hot mix asphalt (HMA) mixtures. The study adopted usage of ground PET waste bottles with maximum particle size of 2.36 mm with different contents (0.1%, 0.3%, 0.5%, 0.7%, 0.9%, and 1.1% by the weight) to replace an equivalent portion of fine aggregate. The study involved a number of laboratory tests to investigate the effects of the mentioned PET content on the engineering properties of HMA. In addition to tests implemented to specify the properties of materials used and to determine mixing and compaction temperatures, the testing program included Marshall tests, rutting susceptibility tests, and indirect tensile strength tests applied on a number of control (unmodified) and modified samples. The results exhibited significant improvement in engineering properties of mixtures modified with optimum PET content (which was found to be 0.5%) in terms of increase in stability, stiffness, and indirect tensile strength and decrease in rutting susceptibility without adverse effects on the other desirable properties of the mixture.

اﻟﻣﺳﺗﺧﻠص- ﺗﻐطﻲ ﻫذﻩ اﻟدراﺳﺔ اﺳﺗﺧدام ﻣﺧﻠﻔﺎت اﻟﻘﻧﺎﻧﻲ اﻟﺑﻼﺳﺗﻛﯾﺔ ﻟﺗﺣﺳﯾن ﺧواص اﻟﺧﻠطﺎت اﻷﺳﻔﻠﺗﯾﺔ اﻟﺳﺎﺧﻧﺔ. ﺗﺑﻧت اﻟدراﺳﺔ اﺳﺗﺧدام اﻟﺑﻼﺳﺗك اﻟﻣﺳﺣوق ﺑﻣﻘﺎس ﺣﺑﯾﺑﻲ ﻻ ﯾﺗﺟﺎوز 2.36 ﻣﻠم و ﺑﻧﺳب اﺿﺎﻓﺔ ﻣﺧﺗﻠﻔﺔ ﯾﺷﻣل (0.1%؛ 0.3%؛ 0.5%؛0.7%؛ 0.9%؛ و 1.1% ﻣن وزن اﻟرﻛﺎم) ﻻﺳﺗﺑدال ﻛﻣﯾﺔ ﻣﻛﺎﻓﺋﺔ ﻣن اﻟرﻛﺎم اﻟﻧﺎﻋم ﺑﺎﻟﻣﺿﺎف اﻟﻣﻘﺗرح. ﺷﻣﻠت اﻟدراﺳﺔ ﻋدد ﻣن اﻟﻔﺣوص اﻟﻣﺧﺗﺑرﯾﺔ ﻟﺗﺑﯾن ﺗﺎﺛﯾر اﻟﻣﺿﺎف اﻟﻣﺷﺎر اﻟﯾﻪ و ﺑﺎﻟﻧﺳب اﻟﻣﺑﯾﻧﻪ اﻋﻼﻩ ﻋﻠﻰ اﻟﺧواص اﻟﻬﻧدﺳﯾﺔ ﻟﻠﺧطﺎت اﻻﺳﻔﻠﺗﯾﺔ اﻟﺳﺎﺧﻧﺔ. ﺑﺎﻻﺿﺎﻓﺔ اﻟﻰ اﻟﻔﺣوص اﻟﺗﻲ ﺗم ﺗﺑﻧﯾﻬﺎ ﻟﺗﺣدﯾد ﺧواص اﻟﻣواد اﻟﻣﺳﺗﺧدﻣﺔ و ﻟﺗﺣدﯾد درﺟﺎت ﺣرارة اﻟﻣزج و اﻟرص؛ ﺷﻣل ﺑرﻧﺎﻣﺞ اﻟﻔﺣوص ﻓﺣص ﻣﺎرﺷﺎل و ﻓﺣص اﻟﺗﺧدد و ﻓﺣص اﻟﺷد ﻏﯾر اﻟﻣﺑﺎﺷر. ﺗم اﺟراء ﻫذﻩ اﻟﻔﺣوص ﻋﻠﻰ ﻋدد ﻣن اﻟﻧﻣﺎذج ﻏﯾر اﻟﻣﺣﺳﻧﺔ و ﺗﻠك اﻟﻣﺣﺳﻧﺔ ﺑﺎﻟﻧﺳب اﻟﻣﺷﺎر اﻟﯾﻬﺎ. ﺑﯾﻧت اﻟﻧﺗﺎﺋﺞ ﺗﺣﺳﻧﺎ ﻣؤﺛرا ﻓﻲ اﻟﺧواص اﻟﻬﻧدﺳﯾﺔ ﻟﻠﺧﻠطﺎت اﻟﻣﺣﺳﻧﺔ ﺑﺎﻟﻧﺳﺑﺔ اﻟﻣﺛﻠﻰ (0.5%) ﻣن اﻟﻣﺿﺎف اﻟﻣﻘﺗرح. ﯾﻼﺣظ زﯾﺎدة اﻟﺛﺑﺎت و اﻟﺻﻼﺑﺔ و ﻣﻘﺎوﻣﺔ اﻟﺷد ﻏﯾر اﻟﻣﺑﺎﺷر و اﻧﺧﻔﺎض ﻗﺎﺑﻠﯾﺔ اﻟﺧﻠطﺔ ﻟﻠﺗﺧدد دون ﺗﺎﺛﯾر ﺳﻠﺑﻲ ﻋﻠﻰ ﺧواص اﻟﺧﻠﯾط.

Keywords: PET, Marshall Properties, Rutting Susceptibility, ITS

INTRODUCTION objective [9] as it increases its performance and Highway networks cover hundreds millions of service life and decreases its maintenance cost. lane-kilometers and supporting millions of Several traditional additives are used in vehicle-kilometers each year in the world [1]. modification of HMA [10-21]. However, using these Highways represent the main infrastructures in traditional additives adds supplementary cost. transportation [2] which controls the growth of Recently, there is a revolution in employment of economy [3-5] especially in developing countries [6]. waste materials in modification of HMA [22-31]. Asphaltic pavements can be considered as one of PET waste material is widely used to improve the the most important elements in highways properties of construction materials [32-46]. engineering [7]. Generally, most of the highways Therefore, using this waste material (PET) in are paved with HMA pavements [8]. Therefore, modification of HMA can promotes sustainable modification of HMA pavements is an essential construction especially when refer to the fact that HMA is one of the most used construction

62 SUST Journal of Engineering and Computer Sciences (JECS), Vol. 18, No.1, 2017 materials due to the huge volumes of highways prepared samples. The testing procedure includes projects. A number of researches were performed a number of tests to specify the properties of in this domain [47-62]. Ahmadinia et al. (2011, 2012) materials used and viscosity tests to determine and Baghaee et al. (2012) studied the performance mixing and compaction temperatures related to of PET on stone mastic asphalt [47-49]. The project predetermined asphalt viscosities. In addition, the includes a series of researches, majorly, focused testing program applied on unmodified and on resistance of mastic asphalt to permanent modified samples includes Marshall tests, rutting deformations. Vasudevan et al. (2012) proposed a susceptibility tests, and indirect tensile strength technique to use PET in flexible pavements [62]; tests (ITS) for unconditioned and conditioned similar approach was adopted by Gürü et al. samples. The results exhibited significant (2014) [56]. Rahman and Wahab (2013) studied the improvement in engineering properties of possibility of using recycled PET in HMA based modified samples compared to those of control on Malaysian standards and conditions [60]. (unmodified) samples. Baghaee et al. (2014, 2015) studied the effects of PET on permanent deformations in asphalt MATERIALS AND METHODS mixtures under dynamic and static loads [50-54]. In a. Aggregate addition to laboratory approach, the researches The aggregate used in this investigation was adopted theoretical approaches including statistical obtained from Al-Nibaee in Salah Aldine analysis and neuro-fuzzy methodology to achieve Governorate. Generally, the aggregate used in this the objectives of the researches. Modarres and study is angular, and free from clay, organics, and Hamedi (2014) and Dehghan and Modarres (2017) foreign materials. It has uniform quality, adopted PET fibers to study the fatigue composed of sound, tough, and durable particles. characteristics of HMA [55, 57,58]. Soltani et al. To investigate the properties of aggregate, a (2015) adopted response surface methodology to number of tests were performed. All properties analyze fatigue properties of HMA mixed with comply with the requirements of Iraqi standard PET. Moghaddam et al. (2016) adopted a specifications for roads and bridges where theoretical approach involving genetic algorithm, applicable as shown in Table 1. The gradation of the aggregate is illustrated in Figure 1. neural network and fuzzy logic to estimate the [59] fatigue life of MHA modified with PET waste . b. Asphalt cement However, the research in this domain must be The asphalt cement used in this investigation was extended to cover more effects of PET on the obtained from Al-Dora refinery in Baghdad city in properties of asphalt mixtures. Therefore, this Iraq. The properties of asphalt cement used in this study aims to fill the gaps left in the other study were investigated based on extensive researches through adopting additional tests, laboratory testing. The results of the tests were different asphalt grade, different PET contents and compared with Iraqi requirements where specified. particles’ size, and different aggregate origin and All properties comply the requirements of Iraqi gradation. In addition, the present study aims to standard specifications for roads and bridges as study the long term effects of using PET as a shown in Table 2. HMA modifier under different conditions such as saturation and freezing and thawing cycles. This c. PET study selected PET waste bottles due to its great PET is a semi-crystalline polymer has high tensile strength, high chemical resistance, and melting availability everywhere. This paper covers a o [63] laboratory-oriented study to investigate the effects point of 260±10 C . PET waste bottles, in this of using different PET contents (0.1%, 0.3%, study, were collected from local trash and, 0.5%, 0.7%, 0.9%, and 1.1% by the weight of mechanically, grinded into fine particles (not more aggregate) on the engineering properties of HMA. than 2.36 mm) to replace an equivalent portion of The PET content was considered to replace fine aggregate of HMA mixtures. The main equivalent amount of fine aggregates as the properties of PET used in this study are presented particle size of PET used in this study is within the in Table 3. range of fine aggregate. This action (equivalent This work, carried out in Khartoum North Power replacement) ensures constant asphalt contents in Station. The power station included two

63 SUST Journal of Engineering and Computer Sciences (JECS), Vol. 18, No.1, 2017 generators: unit 1 and unit 2. The implementation of the work involves two main steps: formulation d. Indirect Tensile Strength Test of economic dispatch problem and developing of Based on the predetermined optimum asphalt genetic algorithm solution. content (5.5% by weight of total mix) and the TESTING PROGRAM predetermined temperatures, a number of In addition to the tests performed to study the specimens were prepared for indirect tensile properties of materials used, a number of tests strength testing. The prepared specimens were of were implemented to determine the mixing and 100mm in diameter and 63.5±2.5mm in thickness. compaction temperatures and the optimum asphalt The prepared specimens had 7±0.5% air voids as content and to investigate the effects of PET on required by AASHTO T283. To achieve the the properties of HMA as described in the targeted air voids, a number of trials were following subsections. implemented using Marshall compaction hammer to specify the suitable number of blows. a. Viscosity Tests Afterward, seven sets each involved two samples The viscosity of asphalt was determined with (one for unconditioned testing and the other for different temperatures (120°C, 135°C, 150°C, and conditioned testing) were prepared to represent 165°C) in accordance with ASTM D 2170 to control mixture and mixtures modified with specify suitable mixing and compaction different PET contents. Conditioned specimens temperatures. These temperatures were adopted to were subjected to vacuum saturation in accordance prepare Marshall specimens. with AASHTO T283. In addition, the conditioned samples were subjected to freezing at -18±3oC; b. Marshall Test afterward, they were immersed in a water bath This part of testing program involved preparation with temperature of 60±1ºC for 24 hours. of a number of control asphalt mixture samples Unconditioned and conditioned specimens were (each involved three specimens) at the determined tested at 25oC to determine the ITS values. The mixing and compaction temperatures using tensile strength ratio values were calculated by Marshall method. The prepared samples were dividing the conditioned ITS values by tested using Marshall method to specify the unconditioned ITS values. optimum asphalt content and to investigate the properties of control mixture. The investigation RESULTS AND DISCUSSION covered bulk specific gravity, stability, flow, air a. Results of Viscosity Tests voids, total voids in mineral aggregate, and From viscosity test for asphalt cement, the stiffness. Based on optimum asphalt content, temperature ranges of mixing and compaction Marshall method was repeated for samples were determined to be (158-166: average=162) °C modified with the predetermined contents of PET and (140-147: average=143.5) °C respectively; to investigate their effects on the properties of these temperatures are related to predetermined HMA. viscosities required for mixing (150-190 c. Rutting Susceptibility Test centistokes) and compaction (250-310 To evaluate the rutting susceptibility of the centistokes). These temperatures were adopted for mixtures under this study, unmodified samples and preparation of Marshall Specimens. samples modified by PET with different contents were prepared and tested according to AASHTO T b. Marshall Test Results 324; each sample involved two specimens with Table 4 presents the properties of the control dimensions of (600mm x 200mm x 75mm). The mixture according to Marshall testing method. prepared samples were tested using wheel tracking Based on these results the optimum asphalt apparatus under full immersion conditions with content was determined to be 5.5% by weight of temperature of 50°C. The applied pressure was the mix. This percent was adopted to produce the about 730 kPa which simulates the contact tire modified mixtures. The results of Marshall tests pressure. The rut depth was recorded up to 20000 exhibited that all properties of control and selected wheel passes. modified mixture conform the requirements of the standards. Figure 2 illustrates the effects of

64 SUST Journal of Engineering and Computer Sciences (JECS), Vol. 18, No.1, 2017 different PET contents on the properties of the contents are slighter than those of air void ones. mixture. The justification of this trend is similar to that The results exhibited that the bulk specific stated in case of air voids trend. gravity(Gmb) values of modified samples decrease c. Results of Rutting Tests with increase of PET content as shown in Figure Figure 4-a illustrates the results of this test for 2-a. This behavior can be attributed to the decrease unmodified samples and those modified with in overall specific gravity of aggregate (Figure 2- different PET contents. The results exhibited that b) as a result to decrease in overall specific gravity the rutting susceptibility of modified samples is of fine aggregate (Figure 2-c) with increase of less than that of control samples. Figure 4-b PET content as the specific gravity of PET is less abstracts the values of rut depth after 20000 wheel than that of fine aggregates; a portion of fine passes for unmodified and modified samples. aggregate was replaced with equivalent amount of However, rut depth values decrease with increase PET as, previously, mentioned. In addition, of PET content up to 0.5% then increases with decrease in Gmb values with increase of PET increase of PET content. This behavior can be content can be a result of decrease in mixture attributed to the generation of stiffer mixture using compatibility. Decrease in mixture compatibility moderate PET content [47]. However, using can be justified by two reasons: inconsistence excessive PET contents decreases the stability and structure of PET and reduction in lubrication by increases the air voids which increase the rutting hot asphalt during compaction due to absorption of susceptibility. Unfortunately, mixtures with low an amount of asphalt by PET. Figure 2-d show that rutting susceptibility are, normally, exhibit low Stability values increase with increase of PET resistance to cracking [64] which make them content up to 0.5% then decease with increase of suitable for hot regions but not suitable for cold PET content. Moderate content of PET produces regions where cracking is more probable [65]. stiffer mixtures which make them more stable [48] Although that, the modified mixtures (especially compared to unmodified ones . However, those modified with optimum PET content) have excessive PET content, possibly, absorbs high properties suitable even for cold regions as the amount of asphalt, increases the heterogeneity of flow values are within the acceptable range. In mixture, and reduces compatibility leading to addition, the modified mixtures can be applied in decrease in stability. Figure 2-e exhibited that cold regions with some adjustments including Marshall flow values decrease with increase of increasing the asphalt content and using softer PET contents up to 0.3% then increase with asphalt cement initially. Precautions must be increase in PET content. As mentioned, adding adopted when applying these adjustments to cover PET produces stiffer mixtures which decrease the all engineering properties required in the mixture. flow. However, as excessive PET content Fortunately, the rut depth values in all samples are decreases the stability, it increases the flow less than 20% of the samples’ thickness which is consequently. The values of Marshall stiffness acceptable in pavement technology [66]. follow a trend similar to that obtained for Marshall stability as shown in Figure 2-f. However, the d. Results of ITS Tests highest stiffness value was attained using 0.3% The results of this tests of unconditioned samples PET content. These results are expected as (control and modified) exhibited that the ITS stiffness value is the stability divided by the flow. values of modified samples are higher than those Figure 2-g exhibited that the air void values of control samples as shown in Figure 5-a. This increase with increase in PET content. Three behavior is, probably, related to the reinforcing possible reasons may justify this trend: PET role of PET in the mixtures. ITS values obtained absorbs an amount of asphalt, decrease the mixture from testing of conditioned samples were similar homogeneity, and decrease compatibility; these to those obtained from unconditioned samples as factors increases the air voids. Figure 2-h shows modified samples exhibited higher ITS values than that VMA values changed by increase in PET that attained by control samples as shown in contents with a trend similar to that for air voids Figure 5-a. These results differ from results stated (Figure 2-g). However, the differences among by one literature [47]. This difference may be VMA values related to addition of different PET attributed to the differences in the properties of

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materials used. Figure 5-b presents the values of [6] A. M. Mosa, R. Atiq, M. Raihantaha and A. Ismail, TSR; all were more than 80% which satisfies the (2011), A knowledge base system to control requirements [66]. construction problems in rigid highway pavements, Australian Journal of Basic and Applied Sciences CONCLUSIONS 5, no. 6, 1126-1136. This study is a laboratory-oriented approach to [7] M. S. Ranadive and A. B. Tapase, (2016), investigate the effects of different contents of PET Parameter sensitive analysis of flexible pavement, on the engineering properties of HMA. From the International Journal of Pavement Research and Technology 9, no. 6, 466-472. results of the tests stated in the previous [8] A. S. M. A. Rahman and R. A. Tarefder, (2016), subsections, addition of PET to the HAM Dynamic modulus and phase angle of warm-mix improves its engineering properties. PET content versus hot-mix asphalt concrete, Construction and of 0.5% can be considered as the optimum content Building Materials 126, 434-441. as it produces highest stability, lowest rutting [9] D. Arslan, M. Gürü and M. Kürşat Çubuk, (2012), susceptibility and fulfills the requirements of the Performance assessment of organic-based synthetic other parameters. However, 0.3% can be calcium and boric acid modified bitumens, Fuel considered as alternative optimum content (local 102, 766-772. optimum) as it produces higher stiffness, lower air [10] S. Tapkın, (2008), The effect of polypropylene voids (nearest to the most desirable value which is fibers on asphalt performance, Building and Environment 43, no. 6, 1065-1071. 4%), and lower flow compared to those attained [11] P. Cong, J. Yu, S. Wu and X. Luo, (2008), using 0.5% of PET. This content (0.3%) can be Laboratory investigation of the properties of adopted in hot regions to prevent pavement asphalt and its mixtures modified with flame distortions (due to low flow and high stiffness) and retardant, Construction and Building Materials 22, asphalt bleeding (due to sufficient air voids) no. 6, 1037-1042. without adverse effects on durability (as air voids [12] A. Aksoy, K. Şamlioglu, S. Tayfur and H. Özen, value is less than 5%). Therefore, this study (2005), Effects of various additives on the moisture recommends using PET as waste material as an damage sensitivity of asphalt mixtures, effective additive in HMA technology. Construction and Building Materials 19, no. 1, 11- 18. REFERENCES: [13] N. Su and J. S. Chen, (2002), Engineering [1] M. Mazumder, V. Sriraman, H. H. Kim and S.-J. properties of asphalt concrete made with recycled Lee, (2016), Quantifying the environmental glass, Resources, Conservation and Recycling 35, burdens of the hot mix asphalt (HMA) pavements no. 4, 259-274. and the production of warm mix asphalt (WMA), [14] K. L. Magadi, N. Anirudh and K. M. Mallesh, International Journal of Pavement Research and (2016), Evaluation of bituminous concrete mixture Technology 9, no. 3, 190-201. properties with steel slag, Transportation Research [2] A. Gomes Correia, M. G. Winter and A. J. Procedia 17, 174-183. Puppala, (2016), A review of sustainable [15] F. Cheriet, K. Soudani and S. Haddadi, (2015), approaches in transport infrastructure geotechnics, Influence of natural rubber on creep behavior of Transportation Geotechnics 7, 21-28. bituminous concrete, Procedia - Social and [3] A. M. Mosa, M. R. Taha, A. Ismail and R. A. O. K. Behavioral Sciences 195, 2769-2776. Rahmat, (2013), A diagnostic expert system to [16] S. Tapkın, (2013), Optimal polypropylene fiber overcome construction problems in rigid highway amount determination by using gyratory pavement, Journal of Civil Engineering and compaction, static creep and Marshall stability and Management 19, no. 6, 846-861. flow analyses, Construction and Building Materials [4] E. A. Oluwasola, M. R. Hainin and M. M. A. Aziz, 44, 399-410. (2015), Evaluation of asphalt mixtures [17] M. Panda, A. (2013), Suchismita and J. Giri, incorporating electric arc furnace steel slag and Utilization of ripe coconut fiber in stone matrix copper mine tailings for road construction, asphalt mixes, International Journal of Transportation Geotechnics 2, 47-55. Transportation Science and Technology 2, no. 4, [5] M. Mazumder, H. Kim and S.-J. Lee, (2016), 289-302. Performance properties of polymer modified [18] C. E. Sengul, A. Aksoy, E. Iskender and H. Ozen, asphalt binders containing wax additives, (2012), Hydrated lime treatment of asphalt International Journal of Pavement Research and concrete to increase permanent deformation Technology 9, no. 2, 128-139.

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Table 1: The properties of aggregate Test Unit Test Specifications Compliance Result Los Angeles AASHTO T % <30 14 Comply Abrasion Value 96 AASHTO T Plasticity Index - <3 0 Comply 89 Gypsum Content % BS 1377 <1 0 Comply

Flakiness % BS 812 <20 3 Comply AASHTO T Soundness % <12* 2.1 Comply 104 Gsbca** - - 2.650 NA Gsbfa** - AASHTO T - 2.748 NA Gsbmf** - 84 - 2.700 NA Gsbagg** - - 2.716 NA

*American specifications were applied where Iraqi specifications are unspecified ** Gsbca, Gsbfa , Gsbmf, Gsbagg =Bulk Specific Gravity of coarse aggregate, fine aggregate, mineral filler, and overall aggregate respectively

Table 2: The properties of asphalt Asphalt Property Conditions Test Specifications Used 25 °C , 100g, 5 Penetration, 0.1 mm AASHTO T-49 40-50 47 Sec Flash Point, °C Open Cup AASHTO T-78 >240 267 Loss on Heating, % 5hrs., 163 °C AASHTO T-47 <0.75 0.50 Penetration After Based on AASHTO T-49 >52 61 Heating, % Original 25 °C, 50 Ductility, cm AASHTO T-51 >100 >100 mm/min Softening Point, °C Ring and Ball AASHTO T-53 54-60 54 Increase of Softening Ring and Ball AASHTO T-53 <10 8 Point, °C 5hrs., 163 °C Solubility, % Organic Solvent AASHTO T-44 >99 99.99 Pycnometer, 25 ASTM Specific Gravity NA 1.02 °C D-70

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Table 3: Properties of PET 2.36 mm 100% Particle Finer than 1.18 mm AASHTO T 127 50% 0.425 mm 0% Specific Gravity ASTM D 792 1.385 Melting Point - 255oC

Table 4: Properties of control mixture based on Marshall method Asphalt content Specific Marshall Flow VMA Air Voids Stiffness (% by total Gravity Stability (0.25 mm) (%) (AV) (%) (kN/mm) weight of mix) (Gmb) (kN) 4.5 2.407 12 6.2 15.4 5.2 15.52 5 2.441 14.49 8.1 14.6 4.6 14.32 5.5 2.470 15.61 11.5 14.1 4.2 10.88 6 2.462 11.88 13 14.8 3.5 7.28 6.5 2.451 8.81 15.1 15.6 3 4.64 7 2.443 7.73 18.9 16.3 2.7 3.28 7.5 2.420 6.04 21.2 17.6 2.1 2.24

Values related to optimum asphalt content 5.5 2.464 14.7 11.7 14.1 4.1 10.05

Figure 1: Aggregate gradation

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Figure 2: Results of Marshall tests

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Figure 4 Results of wheel track rut depth

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Figure 5 Indirect Tensile Strength tests results of unconditioned and conditioned samples