Differential Scanning Calorimetry Applied to Bitumen: Results of the RILEM NBM TG1 Round Robin Test

Abstract

The application of Differential Scanning Calorimetry (DSC) has been proven useful in characterizing bituminous binders, distillates and crude oils. In this paper, results of the round robin test, organized by the Rilem TC 231 Nanotechnology-based Bituminous Materials (NBM) TG1 group are reported. The purpose is to investigate the repeatability and reproducibility of standard DSC measurements when applied to bituminous binders. In the full test program of the Rilem NBM group, DSC measurements are further compared to observations made in atomic force microscopy (AFM), AFM measurements are reported in a separate paper. Seven laboratories have participated in this round robin test. Four bituminous binders were investigated, containing various amounts of natural or added wax. The test program consisted of a well-defined isothermal annealing procedure, followed by a first heating and cooling scan, and afterwards followed by a second heating scan. At this stage, the data, as they were reported by the different participants, were compared. For the glass transition (Tg), mid temperatures, can be defined with a reasonable reproducibility, which improves if natural wax is not present. Regarding melting and crystallization, the shape of the melting curve is highly dependent on the thermal history of the samples. Peak temperatures of melting and crystallization phenomena were reported with a good reproducibility, while the reproducibility of melting enthalpies (or surface area’s under the melting and crystallization signals) was not satisfactory. Different reasons for this and recommendations for improving the results are discussed in the paper.