| Sažetak | U ovom je radu provedena validacija metode detekcije teških metala tehnikom masene spektrometrije povezane s induktivno spregnutom plazmom (engl. Inductively coupled plasma mass spectrometry, ICP-MS). Za postupak validacije korištene su temeljne standardne otopine (TSO) 19 elemenata (Ag, Al, As, Ba, Cd, Cr, Fe, Hg, K, Mn, Na, Ni, P, Pb, S, Sb, Se, V i Zn). Određeni parametri validacije su linearnost, preciznost, radno područje, granica detekcije (GD), granica kvantifikacije (GK) i istinitost. Validirana metoda je zatim primijenjena za određivanje elemenata u realnim uzorcima: voda sa ulaza i izlaza uređaja za pročišćavanje voda akumulacijskog jezera hidroelektrane (HE) s područja vapnenačkih stijena i na morski sediment iz područja srednjeg i južnog Jadrana. Uzorak sedimenta podvrgnut je kiseloj digestiji u zatvorenim teflonskim posudama u mikrovalnoj pećnici koristeći HNO3, HCl i HF. Optimalni uvjeti razgradnje uzorka sedimenta postignuti su u trećoj digestiji nakon 10 minuta, pri snazi od 400 W i volumenima kiselina; 1 mL HCl, 3 mL HNO3 i 1 mL HF. Rezultati analize pokazuju kako su u uzorku sedimenta prisutni Al, Fe, P i V. Rezultati dobiveni za uzorke vode na ulazu i izlazu iz uređaja za pročišćavanje vode akumulacijskog jezera HE pokazuju da su na ulazu povišene koncentracije S i Zn. Bitno je da su na izlazu iz uređaja za pročišćavanje vode svi elementi uspješno uklonjeni. |
| Sažetak (engleski) | In this study, the validation of the method for detecting heavy metals using inductively coupled plasma mass spectrometry (ICP-MS) was carried out. Fundamental standard solutions (FSS) of 19 elements (Ag, Al, As, Ba, Cd, Cr, Fe, Hg, K, Mn, Na, Ni, P, Pb, S, Sb, Se, V, and Zn) were used for the validation process. The specific validation parameters were linearity, precision, working range, limit of detection (LOD), limit of quantification (LOQ), and accuracy. The validated method was then applied to determine the elements in real samples: water from the inlet and outlet of a water treatment device of a hydroelectric reservoir (HE) in an area of limestone rocks, and in marine sediment from the central and southern Adriatic Sea. The sediment sample was subjected to acid digestion in closed Teflon vessels in a microwave oven using HNO3, HCl, and HF. The optimal conditions for sediment sample decomposition were achieved in the third digestion after 10 minutes and with the following acid volumes: 1 mL of HCl, 3 mL of HNO3, and 1 mL of HF. The analysis results show that Al, Fe, P, and V are present in the sediment sample. The results obtained for the water samples at the inlet and outlet of the hydroelectric reservoir water treatment device show elevated concentrations of S and Zn at the inlet. Importantly, all elements were successfully removed at the outlet of the water treatment device. |
