© 2020 Informa UK Limited, trading as Taylor & Francis Group.In this investigation, a solid-phase extraction (SPE) process was improved for selective separation of Cr, Cu, Fe, Mn, Pb and Zn ions on novel ternary composite. These heavy metals were analyzed by flame atomic absorption spectrometry (Flame-AAS). To prepare the novel ternary composite, FeCl3was used as an oxidant agent in the chemical polymerization technique by formating polystyrene/polyglycidylmethacrylate/polyindole(PSt/PGMA/PIN) [25:25:50]. The structure of novel ternary composite was characterized by FTIR, TGA, X-RD and BET analysis technique. Themorphological surface analysis has been carried out by using SEM and AFM technique. Morphological studies have been show that composite has a smooth surface. To maximum recoveries of heavy metals, the optimum experimental conditions and analytical parameters were searched. These quantitative recoveries of analytes ions were determined at pH7. The detection limits (DL) were found as minimum of 0.9 μg/L and maximum 1.4 μg/L for Cr, Cu, Fe, Mn, Pb and Zn ions. Relative standard deviation (RSD) of the developed SPE process is below 3.3%. This improved SPE process is simple and selective. By the improved extraction method in which PSt/PGMA/PIN ternary composite used as solid phase, analyte ions were determined in certified reference material (CRM), various cosmetic and food products by flame AAS.