Low temperature synthesis and characterisation of lecontite, (NH₄)Na(SO₄)·2H₂0

Abstract

Lecontite, (NH₄)Na(SO₄).2H₂O, was synthesised at room temperature in high purity compared to earlier work with a minor impurity of mascagnite, (NH₄)₂SO₄. Rietveld refinement of the XRD results confirmed the crystal structure and unit cell dimensions as published earlier. Raman and Infrared spectroscopy, in conjunction with factor group analysis, resulted in a complex pattern of overlapping sulphate, NH and OH modes. The NH modes υ₁ was observed around 2880 cm⁻¹, υ₂ around 1700 cm⁻¹ overlapping with water OH-bending modes, υ₃ around 3300 cm⁻¹ overlapping with water OH-stretching modes around 3023, 3185 and 3422 cm⁻¹, and υ₄ around 1432, 1447 and 1462 cm⁻¹. The sulphate group in the crystal structure displays a decrease in symmetry from T _d as evidenced by the activation of the ν₁ mode at 982 cm⁻¹ and the ν₂ mode around 452 cm⁻¹ in the Infrared spectrum. The υ₃ mode shows clear splitting in the infrared spectra with a strong band at 1064 cm⁻¹ accompanied by two shoulders at 1107 and 1139 cm⁻¹. The Raman spectra show three weak bands at 1068, 1109 and 1135 cm⁻¹ with a shoulder at 1155 cm⁻¹. Similar splitting was observed for the υ₄ mode around 611 and 632 cm⁻¹ in the Infrared and Raman spectra, respectively.