Perovskites are investigated as potential working materials in new technologies, such as solid oxide fuel cells, thermochemical energy storage, and magnetic refrigerators. They are interesting due to their application properties, such as electrical conductivity, ferromagnetic properties, and reducibility. Properties of perovskites can be improved by doping and the formation of structural defects. The aim of this work was to investigate the possibility of preparing Sr-doped lanthanum manganite with the chemical formula La0.5Sr0.5MnO3 by coprecipitation procedure, and to analyse the observed phase separation. The material was prepared by coprecipitation procedure in which sources of metal cations (La3+, Sr2+, Mn2+) were dissolved in 0.5 M HNO3. The nitrate solution was added dropwise in 10 wt% NH4HCO3 solution, both solutions being heated to 65 °C. To achieve coprecipitation of all present metal cations, the pH value was maintained at 8 by the addition of aqueous ammonia. The obtained precipitate was filtered and dried to obtain the precursor powder. One part of the prepared powder was calcined at 1200 °C/2 h (sample CL_Sr0.5_p), while the other part was pressed into a tablet and sintered in the same conditions (sample CL_Sr0.5_tab). Even though FTIR and PXRD analyses of the sample CL_Sr0.5_p (Figs. 1A-C) showed the formation of the pure phase, light and dark spots were observed during the SEM analysis of the tablet (CL_Sr0.5_tab) fracture surface (Fig. 2). These spots were analysed by energy-dispersive spectroscopy (EDS). EDS analysis (Table 1) showed that the light spots were SrMnO3 phase, while the dark spots were La0.76Sr0.24MnO3 phase. The tablet was then ground and FTIR and PXRD analyses were conducted. The obtained FTIR results (Figs. 1A and 1B) showed some bands characteristic for the SrMnO3 phase, and low-intensity maxima originating from the SrMnO3 phase were observed on the diffractogram (Fig. 1C) of CL_Sr0.5_tab sample, confirming the existence of separated phase. This was additionally investigated by the Rietveld refinement analysis (Table 1), and it was determined that Sr concentration was 0.24 instead of the targeted 0.5. Therefore, the La0.76Sr0.24MnO3 phase was formed, while the rest of added strontium during the synthesis crystallised in the SrMnO3 phase. Since successful preparation of La0.5Sr0.5MnO3 by hydrothermal synthesis was reported by multiple authors, it can be concluded that the coprecipitation procedure is not suitable for high concentration doping of LaMnO3 due to the separation of Sr into the secondary phase, especially when in tablet form. Perovskiti su tema brojnih znanstvenih istraživanja zbog svojih primjenskih svojstava, kao što su električna vodljivost, feromagnetičnost i reduktivnost. Svojstva perovskita dodatno se mogu poboljšati dopiranjem te formiranjem strukturnih defekata. Cilj ovog rada bio je istražiti mogućnost pripreme stroncijem dopiranog lantanova manganita kemijske formule La0,5Sr0,5MnO3 postupkom koprecipitacije. Dio materijala žaren je na 1200 °C/2h, a dio je prešan u tabletu i sinteriran na istim uvjetima. Iako je rendgenska difrakcijska (PXRD) analiza žarenog praha ukazivala na nastanak čiste faze, morfološkom analizom lomne površine tablete uočene su dvije faze. Energijski razlučujuća rendgenska spektrometrija pokazala je da je svjetlija faza SrMnO3, dok je tamnija La0,76Sr0,24MnO3. Tableta je usitnjena te analizirana PXRD-om. Iako su se maksimumi poklapali sa standardnom rendgenskom karticom faze La0,5Sr0,5MnO3, Rietveldovom metodom utočnjavanja potvrđen je udio Sr od 0,24 i nastanak faze La0,76Sr0,24MnO3. Ostatak stroncija dodanog tijekom sinteze kristalizirao je u SrMnO3 fazu. Time je potvrđeno da je supstitucija moguća do određene mjere nakon koje postoji opasnost od izdvajanje nove faze, pogotovo ako je uzorak pripremljen u obliku tablete.