Today, magnetic nanoparticles are present in multiple medical and industrial applications. We take a closer look at the synthesis of magnetic iron oxide nanoparticles through the co-precipitation of iron salts in an alkaline environment. The variation of the synthesis parameters (ion concentration, temperature, stirring rate, reaction time and dosing rate) change the structure and diameter of the nanoparticles. Magnetic iron oxide nanoparticles are characterized by X-ray diffraction (XRD), Raman spectroscopy and transmission electron microscopy (TEM). Magnetic nanoparticles ranging from 5 to 16 nm in diameter were synthesized and their chemical structure was identified. Due to the evaluation of Raman spectra, TEM and XRD, the magnetite and maghemite nanoparticles can be observed and the proportion of phases and the particle size can be related to the synthesis conditions. We want to highlight the use of Raman active modes A 1g of spinel structured iron oxides to determine the content of magnetite and maghemite in our samples. Magnetite nanoparticles can be derived from highly alkaline conditions even without establishing an inert atmosphere during the synthesis. The correlation between the particle properties and the various parameters of the synthesis was modelled with linear mixture models. The two models can predict the particle size and the oxidation state of the synthesized nanoparticles, respectively. The modeling of synthesis parameters not only helps to improve synthesis conditions for iron oxide nanoparticles but to understand crystallization of nanomaterials.Crystals 2020, 10, 214 2 of 12 For these applications, an understanding and development of effective and low-cost synthesis routes are necessary. The size, stability and composition of magnetic nanoparticles need to be controlled in order to affect magnetic, optic and surface properties [5,14]. Since these physical and chemical properties are often related to the dimension of nanomaterials, the most simple approach is to investigate the size of nanoparticles for distinct synthesis conditions [2,[15][16][17]. Forge et al. and Roth et al. investigated the influence of several parameters on the particle size of iron oxide nanoparticles based on the alkaline co-precipitation synthesis [17][18][19]. Other studies focus on the formation pathways of iron oxide nanoparticles depending on the synthesis conditions and especially on the reaction time [20]. Such studies include the formation, which can be quite versatile for multiple synthesis routes [2,14,[20][21][22][23][24][25][26]. Although some works approach parameter studies by design of experiments, multiple questions concerning the co-precipitation are not understood [17,18]. For these nanoscale particles, it is quite challenging to characterize and predict their structure, especially at the surface [14,27]. Multiple approaches exist on classifying magnetic iron oxide nanoparticles and describing them according to their properties, which are strongly dependent on their environment, synthesis conditions...