Spherical agglomeration (SA) of four products was observed by the focused beam reflectance measurement (FBRM), conclusions, similarities, differences were summarized and the agglomeration mechanism was revealed. The same was performed in the case of cooling crystallization with an alternating temperature profile (ATP) as well. Crystallization types were compared in case of using a double-walled glass reactor of 250 ml with a total solvent volume of 80 ml and, as a scale-up, a jacketed reactor of 750 ml with a total solvent volume of 500 ml, while applying different types of agitation. The effect of the addition of more cycles to the ATP methods was investigated. Light microscopic exposures prove significant differences between the SA and the ATP products.