Data for total surfactant activity (SA) and chromophoric dissolved organic matter (CDOM) during laboratory controlled irradiation experiments (solar simulator), using natural surface microlayer (SML) and subsurface water (SSW) from the Tyne estuary (UK); SA was measured using phase sensitive alternating-current voltammetry and CDOM was measured using spectrophotometry. Three sample treatments were used: irradiated samples (IS), dark controls (DC) and temperature controls (TC).