Sodium metaborate tetrahydrate (NaB(OH) 4 ·2H 2 O) was synthesized by reaction of anhydrous borax (Na 2 O· 2B 2 O 3 ) with sodium hydroxide (NaOH) under conditions at 90 o C for 150 min. The structure was characterized by Xray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM) and Thermogravimetric (TG) analyses. Moreover, dehydration kinetics of NaB(OH) 4 ·2H 2 O was carried out under non-isothermal conditions and the Coats-Redfern method was applied to analyze the TG data for calculation of activation energies (E a ) and pre-exponential factors (k o ) for different heating rates. It was determined that dehydration of sodium metaborate tetrahydrate occurred in five steps. According to the Coats-Redfern non-isothermal model, E a and k o were calculated as 50.89 kJ/mol and 26×10 4 min −1 for region I, 18.51 kJ/mol and 0.87×10 3 min −1 for region II, 15.72 kJ/mol and 0.52× 10 3 min −1 for region III, 4.37 kJ/mol and 0.04×10 3 min −1 for region IV and 37.42 kJ/mol and 8.56×10 3 min −1 for region V, respectively.