After shutting down a cell for re-lining, we deal with the Spent Pot Lining (SPL), consisting of carbon and refractory materials. Most of SPL, which contains a lot of valuable components, remains un-used due to the difficulties associated with the extraction of such components and is transported to a landfill for industrial waste. The paper describes some efficient analytical methods used to analyze the chemical composition of SPL, including obtaining data on the qualitative composition and (or) the proportion of components in the part of the lining that is being researched, including information on the local distribution and structure of substances. The information obtained in the course of research on the impurity profile of SPL samples is necessary and important for the purpose of forecasting the service life of the cell and developing further technology for disposing or re-cycling this type of waste. The paper discusses the results obtained by different research methods: X-ray diffraction (XRD) analysis, approximate quantitative X-ray fluorescence analysis, thermogravimetric analysis (TGA), electron microscopy, which, together, provide more information on the object of researching.