A uranopilite from The South Alligator River, Northern Territory, Australia has been studied using X-ray diffraction, scanning electron microscopy with EDAX attachment and thermogravimetry in conjunction with evolved gas mass spectrometry. X-ray diffraction shows the mineral is a pure uranopilite with little or no impurities. SEM images show the uranopilite to consist of long elongated crystals up to 50 μm in length and 5 μm in width. Thermogravimetry combined with mass spectrometry shows that dehydration occurs around 31 °C resulting in the formation of metauranopilite. The first dehydration step over 20 -71 °C corresponds to the decrease of 5.4 wt %, equivalent to 6.076 H 2 O. The second dehydration step over 71-162.4 °C corresponds to a decrease of 4.7 wt % equivalent to 5.288 H 2 O making a total of 11.364 moles of H 2 O, close to 12 H 2 O for uranopilite. Dehydroxylation takes place over the temperature range 80 to 160 °C. The loss of sulphate occurs at higher temperatures in two steps at 622 and 636 °C. A mass loss also occurs at 755 °C accounted for by evolved oxygen.