Coal ash is known to contain a noticeable amount of valuable elements, including transition metals and lanthanides. Therefore it is quite actual problem to extract them for metallurgy and other applications. This paper presents the results of high gradient magnetic and mechanical separation, microscopy, element analyses and optical spectroscopy of brown coal ash taken from the combustion camera and chimney-stalk of Angren thermal power station. The separated magnetic fraction was 3.4 wt.%, where the content of Fe in ferrospheres increased to 58 wt.%. The highest contents of Fe and rare earth elements were found in the fine fractions of 50-100 µm. Optical absorption spectroscopy of water solutions of the magnetic fractions revealed Fe 2+ and Fe 3+ions in the ratio of ~1:1. The separated coal ash could be used for cleaning of technological liquid waste by means of the high gradient magnetic field.