Evaluating the reproducibility and consistency of different sample preparation techniques used for ATR-FTIR spectroscopy from the RILEM 295-FBB TG1 round robin test

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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Publication Details

Journal
Materials and Structures
Published
2025-09-19
DOI
https://doi.org/10.1617/s11527-025-02755-1
Citations
2
Primary Topic
Fault Detection and Control Systems
Type
article
Field-Weighted Citation Impact
2.43
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article

Evaluating the reproducibility and consistency of different sample preparation techniques used for ATR-FTIR spectroscopy from the RILEM 295-FBB TG1 round robin test

Bernhard Hofko, Dheeraj Adwani, Sayeda Nahar, Kristina Primerano et al.
2 citations
Materials and Structures
Fault Detection and Control Systems
2.43
article

Evaluating the reproducibility and consistency of different sample preparation techniques used for ATR-FTIR spectroscopy from the RILEM 295-FBB TG1 round robin test

Bernhard Hofko, Dheeraj Adwani, Sayeda Nahar, Kristina Primerano, Sandra Weigel, Virginie Mouillet, Sadaf Khalighi, Augusto Cannone Falchetto, Jens Wetekam, Rita Kleizienė, Nathalie Piérard, Jiqing Zhu, Laurent Porot, Maciej Maliszewski, Johannes Mirwald, Pejoohan Tavassoti, Michael Elwardany, Aikaterini Varveri, Γεώργιος Πιπιντάκος, Aditi Sharma, Katarzyna Konieczna
article en
2 citations

Abstract

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.

Materials and StructuresVol. 58(8)
University of Kassel (DE), Warsaw University of Technology (PL), Florida A&M University - Florida State University College of Engineering (US), Federal Institute For Materials Research and Testing (DE), TU Wien (AT), Netherlands Organisation for Applied Scientific Research (NL), University of Antwerp (BE), University of Waterloo (CA), Vilnius Gediminas Technical University (LT), Road and Bridge Research Institute (PL), Institute of Polymers (BG), Belgian Road Research Centre (BE), Université Gustave Eiffel (FR), Swedish National Road and Transport Research Institute (SE), Swiss Federal Laboratories for Materials Science and Technology (CH), The University of Texas at Austin (US), Delft University of Technology (NL), Aalto University (FI)
Openalex Percentile: Top 10%
Fault Detection and Control Systems
2.43
DOIOpen Access PDFOpenAlex
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