Over a period of 30 years (1993–2022), headwater catchments in the Slavkov Forest (Czech Republic) exhibited a robust increase in stream water DOC (dissolved organic carbon) concentrations following a significant reduction in acidic atmospheric deposition. Sulfur deposition decreased from 34 kg ha−1 yr−1 in 1993 to 2.6 kg ha−1 yr−1 in 2022. Three Norway-spruce-dominated research sites—Černý Potok (CEP), a 15.2 ha peatbog catchment, Lysina (LYS), a 27.3 ha granitic catchment, and Pluhův Bor (PLB), a 21.6 ha serpentinite catchment, were investigated. The three–year average DOC concentration increased from 48.2 mg L−1 (1993–1995) to 68.3 mg L−1 (2020–2022) at CEP (0.69 mg L−1 yr−1). LYS showed an increase from 16.9 mg L−1 to 25.4 mg L−1 (0.30 mg L−1 yr−1 annually). The largest increase was recorded at PLB, with an increase from 15.7 mg L−1 to 36.7 mg L−1 (0.89 mg L−1 yr−1). A decline in ionic strength was identified as the main driver of the DOC increase. The annual runoff declined significantly at CEP and LYS from 465 mm to 331 mm as a result of rising air temperatures and reduced precipitation between 2014 and 2022. PLB (average of 266 mm) did not show a statistically significant decline. Recently, PLB experienced significant deforestation that likely lowered transpiration and thus increased catchment runoff. As a result, DOC fluxes did not change significantly at CEP (average 210 kg ha−1 yr−1) and LYS (90 kg ha −1 yr−1). However, PLB’s DOC flux more than doubled, increasing from 44 to 106 kg ha−1 yr−1. Drivers connected with global change, such as increasing temperatures, or potential chemical drivers, such as reductions in Al concentrations and pH changes, were not able to explain the observed changes in DOC concentra tions and fluxes.