Display omitted •Co, Ni, Cu and Zn are successfully used in the preparation of activated carbons by microwave radiation.•The metal atoms have an impact on physicochemical and adsorptive properties.•SBET and pore volumes increase with atomic number and decrease with melting point.•Cu-MC, Co-MC and Ni-MC exhibit high hydrophobic properties compared to Zn-MC.•O-nitro phenol is the most adsorbed molecule from aqueous solution. First-row transition metals (Co, Ni, Cu and Zn) were successfully used in the preparation of activated carbons from wood biomass via microwave-assisted irradiation. Physical-chemical properties of the produced materials (MWAC) were studied by nitrogen adsorption–desorption curves, SEM, FTIR, UV–vis DRS and synchronous fluorescence spectroscopy, CHN elemental analysis, TGA/DTG, pHzpc, hydrophobic properties, and total acidity and basicity groups. Results showed that the metals were bound successfully in different amounts with surface functional groups of the wood biomass through ion exchange and surface complexation interaction during the impregnation step. Zn2+ and Cu2+ formed the most complexes. MWAC impregnated with Zn2+ showed higher pore volumes and surface areas, followed by Cu2+, Co2+ and Ni2+, independently of the ratio used. As the metal : biomass ratio was increased from 0.5 to 2, the surface area of MWAC increased from 300 to 620m2g−1 for Co-MC, 260 to 381m2g−1 for Ni-MC, 449 to 765m2g−1 for Cu-MC and from 572 to 1780m2g−1 for Zn-MC. The samples showed high values of carbon contents and oxygen-containing groups. An adsorption experiment revealed that samples prepared using ZnCl2 showed the highest sorption capacities (qe) for the tested adsorbates, followed by CuCl2, CoCl2 and NiCl2. These results matched with the surface areas and pore volumes trends, which were found to follow atomic number and melting point trends–Ni(II)<Co(II)<Cu(II)<Zn(II), rather than the Irving-Williams Series. The sorption capacities (qe) of molecules followed this order: 2-nitro phenol>bisphenol A>hydroquinone>4-nitro phenol>2-naphtol>paracetamol>caffeine>resorcinol.