Evaluating the reproducibility and consistency of different sample preparation techniques used for ATR-FTIR spectroscopy from the RILEM 295-FBB TG1 round robin test
Johannes Mirwald (Technische Universität Wien)
Sadaf Khalighi (TU Delft - Pavement Engineering)
Aikaterini Varveri (TU Delft - Pavement Engineering)
Bernhard Hofko (Technische Universität Wien)
Dheeraj Adwani (The University of Texas at Austin)
Augusto Cannone-Falchetto (Aalto University)
Michael Elwardany (FAMU-FSU College of Engineering)
Rita Kleiziené (Vilnius Gediminas Technical University)
Katarzyna Konieczna (Warsaw University of Technology)
Maciej Maliszewski (Road and Bridge Research Institute)
Virginie Mouillet (Université Paris Cité)
Sayeda Nahar (TNO)
Nathalie Piérard (Belgian Road Research Centre)
Georgios Pipintakos (Universiteit Antwerpen)
Laurent Porot (Kraton Chemical B.V.)
Kristina Primerano (Swiss Federal Laboratories for Materials Science and Technology (Empa))
Aditi Sharma (University of Waterloo)
Pejoohan Tavassoti (University of Waterloo)
Sandra Weigel (Federal Institute for Materials Research and Testing Berlin)
Jens Wetekam (University of Kassel)
Jiqing Zhu (Swedish National Road and Transport Research Institute)
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Abstract
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.
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