This work is devoted to the scientific and technical aspects of individual stages of active optical fibers preforms’ optical-geometric parameters metrological control. The concept of a system presented makes it possible to carry out a study of a rare earth element distribution in the preform of an active optical fiber to monitor geometric parameters, and also to study the evolution of the refractive index profile along the length of the sample at a qualitative level. As far as it is known, it is the first description of the preform optical, geometric, and luminescent properties measurement within a single automated laboratory bench. Also, the novelty of the approach lies in the fact that the study of the refractive index profile variation along the length of the preform is, for the first time, conducted using the “dry” method, that is, without immersing the sample in synthetic oil, which makes the process less labor-intensive and safer.