| Abstract | Maseni udjeli metala u sedimentu i tlu određeni su tehnikama spektrometrije masa uz
induktivno spregnutu plazmu (ICP‒MS) i rendgenske fluorescencije (XRF). Istraživanje je
provedeno na certificiranim referentnim materijalima i realnim uzorcima s područja
Novigradskog mora, a analizirani su maseni udjeli 27 elemenata (Ag, Al, As, Ba, Bi, Ca, Cd,
Co, Cr, Cs, Cu, Fe, K, Mg, Mn, Mo, Ni, Pb, Rb, Sb, Sc, Sn, Sr, Ti, U, V i Zn). Priprema
uzoraka za tehniku ICP‒MS temeljila se na razaranju uzorka u prisutnosti dušične,
klorovodične, fluorovodične i borne kiseline pomoću sustava za mikrovalnu razgradnju, dok
je priprema uzoraka za analizu tehnikom XRF uključivala prešanje uzoraka u pelete. Kontrola
točnosti analitičkih postupaka provedena je uz pomoć certificiranih referentnih materijala
potočnog, morskog i riječnog sedimenta, a određena je na temelju analitičkog povrata.
Analiza certificiranih referentnih materijala dokazala je da su tehnike usporedive za
određivanje masenih udjela As, Ca, Cu, Fe, K, Mn, Mo, Pb, Rb, Sr, Ti, V i Zn, dok je analiza
realnih uzoraka dokazala da su tehnike usporedive za određivanje masenih udjela As, Fe, Mn,
Pb, Rb, Sr i V. |
| Abstract (english) | Determination of metal concentration in sediment and soil samples was performed by
high‒resolution inductively coupled plasma mass spectrometry (ICP‒MS) and X‒ray
fluorescence (XRF). The study included certified reference materials and samples from the
Novigrad Sea area. In all samples, total concentrations of 27 elements (Ag, Al, As, Ba, Bi, Ca,
Cd, Co, Cr, Cs, Cu, Fe, K, Mg, Mn, Mo, Ni, Pb, Rb, Sb, Sc, Sn, Sr, Ti, U, V and Zn) were
analyzed. Sample preparation for ICP‒MS analysis was performed by digestion of samples in
the presence of nitric, hydrochloric, hydrofluoric and boric acids using a microwave digestion
system, while preparation of samples for XRF analysis involved pressing the samples into
pellets. Accuracy of analytical procedures was controled by the certified reference materials
(CRM) of stream, offshore marine and river sediments, and was determined based on
analytical recovery. The analysis of CRM proved that the techniques are comparable for
determining the concentrations of As, Ca, Cu, Fe, K, Mn, Mo, Pb, Rb, Sr, Ti, V and Zn, while
the analysis of real samples proved that the techniques are comparable for determining the
concentrations of As, Fe, Mn, Pb, Rb, Sr and V. |
