“…Among the characterization methods, the analysis of CaCO 3 in cementitious materials can be performed in the following way: (i) qualitative, by means of phenolphthalein, TEM and SEM methods, (ii) semi-quantitative, using the IR, MicroCT, XRD and XRF instruments and (iii) quantitative, through TGA analysis [11,[35][36][39][40]. In addition, XRD, SEM, IR and TGA can be applied, with their respective limitations, to identify the presence of different CaCO 3 polymorphs (amorphous carbonate, vaterite, aragonite and calcite) [31,[41][42]. Otherwise, NMR is applied only to analyze the siliceous ( 29 Si NMR) and aluminate ( 27 Al NMR) cement phases; however, it is not usually applied to analyze CaCO 3 from 13 C NMR [11,39,43].…”