This recommendation is an output of a small-scale round-robin test involving three different laboratories from TG2 of the RILEM TC 295-FBB: “Fingerprinting bituminous binders using physico-chemical analysis” concerning the use of ¹H-NMR for fingerprinting of bituminous binders. It demonstrates the full capabilities of ¹H-NMR as a robust characterisation tool for complex organic materials, like bituminous binders, to examine their molecular composition in a reproducible way and with the best possible detail. This recommendation documents the key factors in sample preparation and the sensitivity of data post-processing steps. It concludes with best practices and a case study examining the effect of laboratory ageing on two bituminous binders. Overall, it highlights the potential, to the broader scientific community, of another efficient chemometric tool for bituminous binders.

Attenuated Total Reflection Fourier Transform Infrared spectroscopy has become a popular spectroscopic technique in bituminous binder analysis. However, comparable results are not obtainable yet due to differences in devices, measurement routines, sample preparation procedures, and spectral evaluation. Thus, the Task Group 1 of the RILEM TC 295-FBB: “Fingerprinting bituminous binders using physicochemical analysis” focuses on bringing this method towards pre-standardization. This study evaluates the reproducibility and consistency from round robin test, where 21 participating laboratories performed six different preparation techniques on three different binders in an unaged, short-term, and long-term aged state. A total of 6461 spectra were recorded and evaluated for their mean, standard deviation and coefficient of variation (CV) in the spectral region between 1800 and 600 cm⁻¹. The results show that the solid sample preparation methods provide excellent reproducibility, with a coefficient of variation below 2%. Only the solvent method showed a higher coefficient of variation at 7.18%. Outliers with a high CV were detected and categorized into two groups: one where only one of the four samples differed and the other where all 16 spectra showed slight scattering in the overall absorption. The consistency of the method is significantly influenced by the accuracy of sample preparation, which is crucial for minimizing differences in slope, baseline, and noise in the spectra. These findings show the excellent reproducibility of these sample preparation methods and will be further examined to establish universal indices for evaluating effects such as ageing, bringing the method closer towards standardization.

The chemical irreversible hardening of epoxy modified bitumen is affected by various physical factors and the successful application of this technology is directly linked with full understanding of chemo-rheological material characteristics. This study proposes a model to describe the material viscosity evolution during hardening of epoxy modified bitumen. The findings from numerical analyses performed to assess the mechanical response of epoxy modified bituminous binders are presented. Information of the chemical interaction of epoxy within a bituminous matrix was collected and all the influential factors have been determined. The proposed chemo-rheological model accounting for the polymerization of the epoxy in the bitumen was formulated and the sensitivity of material parameters, such as activation energy, reaction order and extent of hardening reaction until the gel point of epoxy modified binders, was demonstrated. Results of the analyses suggest that lower levels of activation energy increase the degree of hardening and the rate of viscosity development. By decreasing the hardening reaction until the gel point the achieved viscosity of epoxy modified bitumen was increased showing the importance of gel reaction extent on material viscosity evolution. The numerical studies have shown also that the polymerization rate in the epoxy modified bitumen is highly dependent on the temperature under various (non-) isothermal conditions. Also, the polymerization rate should be considered through all the material curing processes to avoid unwanted variations in the mechanical properties.

Epoxy modified bitumen (EMB) is a promising technology for long lasting paving materials ensuring higher resistance to rutting, oxygen- and moisture-induced damage. In this paper, an analysis of the chemical reactions that take place during the chemical hardening process (curing) of epoxy modified bitumen
was conducted by means of Fourier Transform Infrared (FT-IR) spectrometer. For various amount of epoxy resin modification in bitumen, the hardening process was evaluated under various conditions. The fluctuation of the most crucial chemical groups occurring during the hardening process was identified and discussed. After the interpretation of chemical hardening, the critical hardening conditions were determined and fatigue tests were performed by Dynamic Shear Rheometer (DSR). Comparison with the unmodified bitumen shows that the fatigue resistance of epoxy modified binders improved significantly with increasing the amount of the epoxy resin in bitumen.