In this study, a series of Titanium to Zirconium ZSM-5 framework was prepared. Elucidations of the structure were performed using XRD, IR, DR, and SEM images. The results showed that Ti and/or Zr could exist in either tetrahedral or octahedral sites. Simultaneous dye photodegradation with the removal of heavy metal was performed and completely studied with four-dimensional curves. The analysis of the data showed that the metal ions could play an important role in the photodegradation mechanism of organic dye. Photodegradation mechanism is elucidated and kinetic studies showed that the degradation followed up pseudo-first-order kinetics. For the first time deconvolution of IR spectra could be assigned for the elucidation of the structure of prepared materials. The prepared materials are found to be efficient in multiple removals of organic/inorganic pollutants which raise its economic impact.