The identification of raw materials and an effective maturation process for the development of peloids is essential to ensure consistent comparisons between commonly used peloids in ‘thermal centers’ (places that offer a variety of health and wellness treatments, also known as spas) and their therapeutic and well-being effects. The present study supports the need for scientific research which examines the variations in physicochemical, technological, and biological properties of peloids resulting from varying maturation conditions. These studies are necessary for establishing quality and safety standards and expanding our understanding of the therapeutic significance of peloids. The objective of the present study was to characterize an experimental maturation procedure using a specific Portuguese clay (bentonite) sourced from Benavila—Avis, which has particular physico-chemical characteristics, in conjunction with two distinct Portuguese mineral-medicinal waters (Hotel Cró and Thermal Spa, and Caldas da Rainha Thermal Hospital) as raw materials. The main aim of the study was to assess and characterize the resulting peloids by evaluating their physicochemical, technological, and biological properties. The experiment was conducted over a period of 90 days under carefully controlled lighting and agitation conditions. The rheological, mineralogical, and chemical properties relevant to a peloid intended for topical application and its potential transdermal delivery of elements were characterized. Additionally, the study investigated the biological activity within the maturation habitat, including chlorophyll, microalgae, and microorganisms. Eight samples, representing the four maturation conditions (stirring with light; stirring without light; no stirring with light, and no stirring and no light), were examined for 30, 60, and 90 days. The study showcased the influence of different mineral-medicinal waters on maturation conditions and on the final bentonite characteristics. Furthermore, it reinforced the importance of establishing quality-control procedures throughout the maturation cycle for bentonitic peloids, as well as the importance of monitoring their usage, reutilization, and disposal.