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Several methods have been made to characterize the concrete during solidification and for this we proceed as way that we can collect non-overlapping ultrasonic signal that is when we choose vessels with well defined walls. Our work highlights the changes of the signals transmitted through the solidification of cement paste according to incidence angles. The work in question demonstrates the existence of a critical angle in this way the transmitted waves are strongly attenuated. This method is based on the determination of the FFT of signals collected during solidification cement and juxtaposed to form graphs being treated. Our method showed the presence of strong attenuations around well-defined angles.