In situ FTIR study on the dehydration of natural goethite

Fourier Transform Infrared (FTIR) spectroscopy, thermal analysis -Differential Scanning Calorimetry (DSC) and Thermo-Gravimetry (TG-DTG) were used to study the dehydration behavior of synthetic goethite and two naturally occurring goethite samples (Natural 1 and Natural 2) from Banded Iron Formation (BIF), at C.S. Halli, Chitradurg district, Karnataka, India. Goethites and its dehydration products were also identified by powder X-ray Diffraction (XRD) method. The dehydration temperatures were at 538, 567 and 578 K for synthetic, Natural 1 and 2 goethite, respectively. On approaching the dehydration temperature, infrared active modes of the hydroxyl groups have shown distinct variations. The peak position for the stretching mode around 3150 cm−1 was shifted upwards, while that for in-plane- deformation mode around 890 cm−1 was down shifted indicating weakening of strength of the hydrogen bonding. No intermediate phase, so called hydro-hematite, was observed in these studies. The total absorbance (area under the peak) of these modes have shown the Arrehenius type behavior in the temperature range 500–600 K, using which the activation energy for the dehydration process was estimated as 71, 103 and 85 kJ/mol for synthetic, Natural 1 and 2 goethites respectively.