Gold nanoparticles represent an important class of functional nanomaterials for optoelectronics, biomedical applications, and catalysis. Therefore, controllable synthesis of nanoparticles with specified size and shape is important. Though reduction of gold ions is quite a simple process and may be performed with many different protocols, the reproducibility of the results and transfer of protocols between independent research groups remains a challenging task. Machine learning analysis based on statistical approaches is hardly applicable to the published data, since most of the researchers report only successful syntheses. In this work, we apply uniform sampling of the reaction parameter space. The concentrations of gold precursor, reducing agent, and surfactant were varied via an improved Latin hypercube sampling, and each run was performed under in situ UV−vis control. Based on the resulting set of optical spectra, we address the relevant chemical questions about nanoparticle formation, their shape, and period of growth. Our work demonstrates a data driven approach applied to the space of reaction parameters in a limited available set of experiments.