Earth surficial environments are highly dynamic throughout time. Major changes occurred between the Neoarchean and Paleoproterozoic, including the earliest rise in atmospheric oxygen and widespread glaciations. An interesting aspect is that evidence of such events are preserved in similarly aged sedimentary rocks across the world, rising the question whether there is a temporal relationship between them. The Transvaal Supergroup, preserved in southern Africa, serves as an excellent case to study these topics. In the present thesis, high-precision U-Pb geochronology from various units are presented. This permitted to solve preexisting and discrepant datasets for specific units from the Transvaal Supergroup, significantly improving the chronostratigraphic framework of this iconic sedimentary sequence. Further, the stable isotope dataset in the Asbestos Hills Subgroup is dramatically enlarged, allowing for the paleoenvironmental reconstruction at time of deposition. Results support a highly-stable oxygen oasis that persisted for at least 20 millions of years. Also, the dominant redox settings were an intrinsic property of the atmosphere and hydrosphere, implying that both may have coexisted with different redox conditions. While fluctuations in atmospheric oxygen levels preceded the Paleoproterozoic glaciations by tenths of millions of years, significant changes in the redox settings of the hydrosphere are associated with the glaciation. Finally, our interpretation supports the hypothesis that the Great Oxidation occurred in a multi-step manner, spanning hundreds of millions of years.