Dialdehyde starches with different aldehyde content from native corn starch were prepared by sodium periodate oxidation to be used as a tanning agent in leather making. For this purpose, native corn starch was oxidized with sodium metaperiodate in different molar ratios. After oxidation processes, the yields, solubility in water and aldehyde contents of the obtained dialdehyde starches were determined as well as structure characterizations by Proton Nuclear Magnetic Resonance Spectroscopy, Fourier Transform Infrared Spectroscopy and Gel Permeation Chromatography. Evaluating the gel permeation chromatography data, the dialdehyde starch samples which were thought to be in appropriate molecular weight/size to penetrate into skin fibers were selected to be used in the tanning process. Their tanning abilities were evaluated by investigating hydrothermal stabilities, filling and fiber isolation characteristics and physical properties determined by mechanical tests and organoleptically. From the evaluation of the results, it was revealed that sodium metaperiodate oxidized starches which have appropriate molecular weight and adequate aldehyde content has a remarkable tanning effect and can be utilized as a tanning agent with the advantages of not necessitating pickling process which means saving time and simplifying the production but more importantly offering an important advantage from an environmental point of view.