In the present study, after an investigation and study of organic di- and trisulfide characters, a method for the identification of S–S and S–S–S bonds using some common spectroscopy techniques,including ultraviolet (UV) spectroscopy, Raman, mass spectrometry (MS) and thin-layer chromatography (TLC), has been introduced and developed. It is worth mentioning that only the reported literature data and our own results have been used.