This dataset contains hydrochemical and soil data collected along the first 1.3 km downstream of the White Main spring in northern Bavaria, Germany, from March 2023 to November 2024. Stream water samples were analyzed for in situ parameters, including discharge, water temperature [°C], pH [-], redox potential [mV], and electrical conductivity [µS/cm], as well as laboratory-measured parameters, including major ions and trace metals [mmol/l], alkalinity [mmol/l], dissolved inorganic and organic carbon concentrations (DIC, DOC [mmol/l]), and their stable isotope ratios (δ13CDIC/DOC [‰ VPDB]). In addition, calculated partial pressure of CO2 (pCO2 [µatm]) and carbon dioxide fluxes (FCO2 [mmol m⁻² d⁻¹]) are provided for the stream water samples. The dataset also contains laboratory measurements related to soil-derived natural organic matter from acid and base extracts of soil samples, including zeta potential [mV], particle size distribution [%], ultraviolet-visible absorbance (UV-VIS), and fluorescence measurements. UV-VIS absorbance and fluorescence measurements were additionally performed on stream water samples. The datasets were collected to characterize hydrochemistry, carbon concentrations, carbon dioxide dynamics, and soil-derived organic matter properties in a granitic headwater stream and to provide a basis for reuse in studies of headwater biogeochemistry, carbon cycling, and soil-water interactions.