Biosorption with macroalgae is a promising technology for the bioremediation of industrial effluents. However, the vast majority of research has been conducted on simple mock effluents with little data available on the performance of biosorbents in complex effluents. Here we evaluate the efficacy of dried biomass, biochar, and Fe-treated biomass and biochar to remediate 21 elements from a real-world industrial effluent from a coal-fired power station. The biosorbents were produced from the freshwater macroalga Oedogonium sp. (Chlorophyta) that is native to the industrial site from which the effluent was sourced, and which has been intensively cultivated to provide a feed stock for biosorbents. The effect of pH and exposure time on sorption was also assessed. These biosorbents showed specificity for different suites of elements, primarily differentiated by ionic charge. Overall, biochar and Fe-biochar were more successful biosorbents than their biomass counterparts. Fe-biochar adsorbed metalloids (As, Mo, and Se) at rates independent of effluent pH, while untreated biochar removed metals (Al, Cd, Ni and Zn) at rates dependent on pH. This study demonstrates that the biomass of Oedogonium is an effective substrate for the production of biosorbents to remediate both metals and metalloids from a complex industrial effluent.