Materials and Structures

, Volume 47, Issue 7, pp 1205–1220 | Cite as

Laboratory investigation of bitumen based on round robin DSC and AFM tests

  • Hilde Soenen
  • Jeroen Besamusca
  • Hartmut R. Fischer
  • Lily D. Poulikakos
  • Jean-Pascal Planche
  • Prabir K. Das
  • Niki Kringos
  • James R. A. Grenfell
  • Xiaohu Lu
  • Emmanuel Chailleux
Original Article


In the past years a wide discussion has been held among asphalt researchers regarding the existence and interpretation of observed microstructures on bitumen surfaces. To investigate this, the RILEM technical committee on nano bituminous materials 231-NBM has conducted a round robin study combining differential scanning calorimetry (DSC) and Atomic Force Microscopy (AFM). From this, methods for performing DSC and AFM tests on bitumen samples and determination of the influence of wax on the observed phases, taking into account thermal history, sample preparation and annealing procedure, are presented and critically discussed. DSC is used to measure various properties and phenomena that indicate physical changes such as glass transition temperature (T g) and phase transition such as melting and crystallization. In the case of existence of wax, either natural or synthetic, it can further indicate the melting point of wax, that could be used to determine wax content. The results from seven laboratories show that T g temperatures obtained from the heating scans are more repeatable and easier to obtain in comparison to the cooling scans. No significant difference was noted for T g’s obtained from the first and second heating scans. AFM is an imaging tool used to characterize the microstructures on a bituminous surface. Using AFM three phases in the materials with wax could be distinguished. The changes in the phases observed with AFM for increases in temperature were correlated with the DSC curve, and it could be established that the so called “Bee” structure disappeared around the melting peak in the DSC curve. Thus, this research has confirmed the relation between the microstructures on a bitumen surface and the wax content.


Bitumen Asphalt DSC AFM Wax Multiphase material 



The authors would like to thank the members of RILEM technical committee 231-NBM for their cooperation and input and Nynas and Q8 for supplying the materials. The contribution of W. Grimes, T. Pauly, F. Turner and J. Forney at WRI, P. Izdebski and B. Fischer and C. Walder from Empa, P. Wedin from Nynas, C. Nijssen-Wester from KPR&T and C. Petiteau from IFSTTAR is greatly appreciated.


  1. 1.
    ISO 11357-1 Plastics-Differential scanning calorimetry, DSC (2009)Google Scholar
  2. 2.
    ASTM 1356-08 Standard Test Method for Assignment of the Glass Transition Temperatures by Differential Scanning CalorimetryGoogle Scholar
  3. 3.
    ASTM D 3418-12 Standard Test Method for Transition Temperatures and Enthalpies of Fusion and Crystallization of Polymers by Differential Scanning CalorimetryGoogle Scholar
  4. 4.
    Loeber L, Sutton O, Morel J, Valleton J-M, Muller G (1996) New direct observations of asphalts and asphalt binders by scanning electron microscopy and atomic force microscopy. J Microsc 182(1):32–39CrossRefGoogle Scholar
  5. 5.
    Pauli AT, Grimes RW, Beemer AG, Turner TF, Branthaver JF (2011) Morphology of asphalts, asphalt fractions and model wax-doped asphalts studied by atomic force microscopy. Int J Pavement Eng 12(4):291–309CrossRefGoogle Scholar
  6. 6.
    Schmets A, Kringos N, Pauli T, Redelius P, Scarpas T (2010) On the existence of wax-induced phase separation in bitumen. Int J Pavement Eng 11(6):555–563CrossRefGoogle Scholar
  7. 7.
    Fischer H, Poulikakos LD, Planche J-P, Das P, Grenfell J (2013) Challenges while performing AFM on Bitumen Proceedings International RILEM Symposium on Multi-Scale Modeling and Characterization of Infrastructure Materials Stockholm 2013Google Scholar
  8. 8.
    Masson J-F, Leblond V, Margeson J (2006) Bitumen morphologies by phase-detection atomic force microscopy. J Microsc 221(1):17–29CrossRefMathSciNetGoogle Scholar
  9. 9.
    Masson J-F, Leblond V, Margeson J, Bundalo-Perc S (2007) Low-temperature bitumen stiffness and viscous paraffinic nano- and micro-domains by cryogenic AFM and PDM. J Microsc 227(Part 3):191–202Google Scholar
  10. 10.
    Jäger A, Lackner R, Eisenmenger-Sittner Ch, And Blab R (2004) Identification of four material phases in bitumen by atomic force microscopy. Road Mater Pavement Des (EATA) 5:9–24CrossRefGoogle Scholar
  11. 11.
    Das PK, Kringos N, Wallqvist V, Birgisson B (2013) Micromechanical investigation of phase separation in bitumen by combining AFM with DSC results. Road Mater Pavement Des 14(S1):25–37Google Scholar
  12. 12.
    Lu X, Langton M, Olofsson P, Redelius P (2005) Wax morphology in bitumen. J Mater Sci 40(8):1893–1900CrossRefGoogle Scholar
  13. 13.
    Lu X, Redelius P (2007) Effect of bitumen wax on asphalt mixture performance. Constr Build Mater 21(11):1961–1970CrossRefGoogle Scholar
  14. 14.
    Planche JP, Claudy PM, Létoffé JM, Martin D (1998) Using thermal analysis methods to better understand asphalt rheology. Thermochim Acta 324(1–2):223–227CrossRefGoogle Scholar
  15. 15.
    Lu X, Redelius P (2006) Compositional and structural characterization of waxes isolated from bitumens. Energy Fuels 20(2):653–660CrossRefGoogle Scholar
  16. 16.
    Michon LC, Netzel DA, Turner TF, Martin D, Planche J-P (1999) A 13C NMR and DSC study of the amorphous and crystalline phases in asphalts. Energy Fuels 13(3):602–610CrossRefGoogle Scholar
  17. 17.
    Musser BJ, Kilpatrick PK (1998) Molecular characterization of wax isolated from a variety of crude oils. Energy Fuels 12:715–725CrossRefGoogle Scholar
  18. 18.
    European Standard EN 12606-1. Bitumen and bituminous binders-determination of the paraffin wax content-part 1:method by distillationGoogle Scholar
  19. 19.
    ASTM D3418-12 Standard Test Method for Transition Temperatures and Enthalpies of Fusion and Crystallization of Polymers by Differential Scanning CalorimetryGoogle Scholar
  20. 20.
    Fischer HR, Dillingh EC, Hermse CGM (2012) On the interfacial interaction between bituminous binders and mineral surfaces as present in asphalt mixtures, Appl Surf Sci. ISSN 0169-4332,  10.1016/j.apsusc.2012.11.034
  21. 21.
    Soenen H, Besamusca J, Poulikakos LD, Planche, J-P, Das P, Grenfell J, Chailleux E (2013) Differential Scanning Calorimetry applied to bitumen: Results of the RILEM NBM TG1 Round Robin test. Proceedings International RILEM Symposium on Multi-Scale Modeling and Characterization of Infrastructure Materials Stockholm 2013Google Scholar
  22. 22.
    Claudy P, Letoffe JM, Rondelez F, Germanaud L, King GN, Planche JP. A new interpretation of time-dependent physical hardening in asphalt based on DSC and Optical thermo-analysis. ACS Fuel preprints, Washington DC, 1992_pp 1408–1426Google Scholar

Copyright information

© RILEM 2013

Authors and Affiliations

  • Hilde Soenen
    • 1
  • Jeroen Besamusca
    • 2
  • Hartmut R. Fischer
    • 3
  • Lily D. Poulikakos
    • 4
  • Jean-Pascal Planche
    • 5
  • Prabir K. Das
    • 6
  • Niki Kringos
    • 6
  • James R. A. Grenfell
    • 7
  • Xiaohu Lu
    • 8
  • Emmanuel Chailleux
    • 9
  1. 1.Nynas NVAntwerpenBelgium
  2. 2.Kuwait Petroleum Research and TechnologyEuropoort (Rt)The Netherlands
  3. 3.TNO, Technical SciencesEindhovenThe Netherlands
  4. 4.Empa, Swiss Federal Laboratories for Materials Science and TechnologyDübendorfSwitzerland
  5. 5.Western Research InstituteLaramieUSA
  6. 6.Division of Highway and Railway EngineeringKTH Royal Institute of TechnologyStockholmSweden
  7. 7.Nottingham Transportation Engineering CentreUniversity of NottinghamNottinghamUK
  8. 8.NynasNynäshamnSweden
  9. 9.IFSTTARVersaillesFrance

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