The removal of heavy metals such as Ni(II), Zn(II), Al(III), and Sb(III) from aqueous metal solutions was investigated using novel, cost effective, seaweed derived sorbents. Studies with a laboratory scale fixed-bed sorption column, using a seaweed waste material (referred to as waste Ascophyllum product (WAP)) from the processing of Ascophyllum nodosum as biosorbent, demonstrated high removal efficiencies (RE) for a variety of heavy metals including Ni(II), Zn(II) and Al(III), with 90, 90 and 74% RE achieved from initial 10 mg/L metal solutions, respectively. The presence of Sb(III) in multi component metal solutions suppressed the removal of Ni(II), Zn(II) and Al(III), reducing the RE to 28, 17 and 24%, respectively. The use of Polysiphonia lanosa as a biosorbent showed a 67% RE for Sb(III), both alone and in combination with other metals. Potentiometric and conductometric titrations, X-ray photoelectron and mid-infrared spectroscopic analysis demonstrated that carboxyl, alcohol, sulfonate and ether groups were heavily involved in Sb(III) binding by P. lanosa. Only carboxyl and sulfonate groups were involved in Sb(III) binding by WAP. Furthermore, a greater amount of weak acidic groups (mainly carboxylic functions) were involved in Sb(III) binding by P. lanosa, compared to WAP which involved a greater concentration of strong acidic groups (mainly sulfonates).