Two sizes of test samples were selected to investigate the effect of size on the level of degradation. The smaller test specimens had dimensions of 40 × 40 × 160 mm, and the larger ones had dimensions of 100 × 100 × 400 mm. Both sizes of test specimens were always made of the same mortar. In one case, Blast Furnace Cement was chosen as the binder. In the other case, it was an alkali-activated material as a possibly more environmentally economical substitute. Both types of material were deposited in three degrading solutions: magnesium sulphate, ammonium nitrate and acetic acid. The reference set was stored in a water bath. After six months in the degradation solutions, a static elastic modulus was determined for the specimens during this test, and the acoustic emission was measured. Acoustic emission parameters were evaluated: the number of hits, the amplitude magnitude and a slope from the amplitude magnitude versus time (this slope should correspond to the Kaiser effect). For most of the parameters studied, the size effect was more evident for the more degraded specimens, i.e., those placed in aggressive solutions. The approximate location of emerging defects was also determined using linear localisation for smaller specimens where the degradation effect was more significant. In more aggressive environments (acetic acid, ammonium nitrate), the higher resistance of materials based on alkaline-activated slag was more evident, even in the case of larger test bodies. The experiments show that the acoustic emission results agree with the results of the static modulus of elasticity.