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.

Understanding aging across material scales is critical for predicting the long-term performance of bituminous materials. This study investigates the aging of binder, mastic, and asphalt mixture samples under various temperature, pressure, reactive oxygen species (ROS), and humidity. Chemical aging processes were analysed using attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR), principal component analysis (PCA), and Euclidean distance. Normalisation, baseline correction, and advanced ATR correction were used to enhance the accuracy of FTIR results. Hydrated lime in mastics enhanced the resistance to oxidative aging, particularly under hygrothermal conditions. PCA identified key spectral regions for understanding aging processes of bituminous materials. Porous asphalt (PA) mixtures aged more than stone mastic asphalt under field-like conditions. PCA identified distinct aging clusters at low and high pressure. Euclidean distance analysis indicated that binder-level aging can approximate mastic and mixture aging under certain conditions. The findings confirm that FTIR indices are effective for multi-scale aging studies.

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.

Bitumen, a crucial constituent in the composition of asphalt pavements, plays a vital role in the performance and durability of pavements. Bitumen undergoes aging over time due to complex interactions between its chemical components and various environmental factors. In this investigation, the study focuses on examining the aging process of bitumen under the combined influence of moisture and reactive oxygen species (ROS). The findings highlight the importance of considering ROS and moisture as critical factors contributing to accelerated aging. Results obtained from Fourier-transform infrared (FTIR) spectroscopy, SARA fractionation, and optical inverse microscope (OIM), as well as dynamic shear rheometer (DSR) examination, indicate that the concurrent influence of these factors induces significant aging in bitumen, with the extent of this impact being modulated by the bitumen's inherent aging susceptibility. The insights obtained from this study enhance strategies to justify the destructive impacts of aging, extending the operational lifespan of asphalt pavements.

Oxidative aging induces significant stiffening of asphalt binders that leads to a pronounced reduction in the overall durability of asphalt pavements. The strategic implementation of antioxidant additives provides a potential solution to alleviate this issue. This work presents results from the second phase of the global consortium for antioxidants research aimed at investigating the effectiveness of potential antioxidants in increasing the durability of asphalt binders. Sixteen laboratories around the world participated in this effort and a total of 28 binders from diverse geographical regions were tested. Two promising antioxidants, namely zinc diethyldithiocarbamate (ZDC) and kraft lignin were evaluated in this phase and blended with the binders at specific proportions. Subsequently, a comprehensive investigation was conducted to assess rheological characteristics and chemical properties of the various blends, utilising Dynamic Shear Rheometer (DSR) measurements and Fourier Transform Infrared (FTIR) Spectroscopy. The findings indicate that additives such as ZDC hold considerable promise as an effective antioxidant, particularly when considering a wide diversity of binders. In general, its incorporation does not compromise the rutting performance of the binders and significantly improves fatigue performance. Therefore, research efforts should be focused on exploring additional facets to assess its practical applicability in field.

The design and use of antioxidant additives to reduce or slow down the aging of asphalt binders can bring about tremendous benefits to the asphalt industry. Despite many isolated and scattered research efforts showing mixed results, the application of this science to engineering-based solutions has been limited due to variability in results and conflicting data available. This work presents the results from a global interlaboratory study to test the effectiveness of promising antioxidant additives, namely kraft lignin, calcium hydroxide, zinc diethyldithiocarbamate and phenothiazine to increase the resilience of asphalt binders and provide insights towards understanding the complex intricacies between chemistry and rheology. Specifically, seven different binders from various geographical regions in the world i.e., Texas (USA), Vienna (Austria), Illinois (USA), Antwerp (Belgium), and Delft (Netherlands) were blended with the antioxidants at two proportions. Subsequently, the chemical and rheological properties of the blends were evaluated using Fourier transform infrared (FTIR) spectroscopy and dynamic shear rheometer (DSR). The results indicate that although some antioxidants may reduce oxidation based chemical indices, their effect on rheology is more complicated and possibly related to unique physicochemical interactions in each binder. From a macro-perspective, zinc diethyldithiocarbamate showed promising results with a good correlation between rheology and chemistry for the majority of the binders. These additives or other additives with the same working principles should be investigated further. Additionally, significant research efforts must also be directed towards approaches aimed at understanding mechanisms of interaction and relating results with specific binder compositions.