20.500.12556/DKUM-67929 Validation of electroanalytical method with antimony electrode for trace metal analysis Validacija elektroanalizne metode z antimonovo elektrodo za analizo težkih kovin v sledovih The purpose of this thesis is to validate the electroanalytical method with an antimony electrode for trace metal analysis. The validation began with the determination of the limit of detection (LOD) and the limit of quantification (LOQ), proceeded with determining the method’s linearity and concluded with determination of accuracy and precision. The trace metal analysis was conducted via square-wave anodic stripping voltammetry (SWASV). Cyclic voltammetry (CV) was used to test the reversibility of the [Fe(CN)6] 3/[Fe(CN)6] 4 system. All the analyses were conducted in a 0.01 M HCl solution. The LOD and LOQ were not possible to report with certainty, since the method has such a low LOD that the contamination with heavy metals, even in ultrapure acid, was too high. The method had a linear response at deposition potentials of 1.2 V, 1.1 V and 1.0 V vs. Ag/AgCl for Pb(II) and Cd(II) from 14.6 µg L 1 to 100.0 µg L 1. It has further been proven that the method is accurate and precise for all three deposition potentials at 15 µg L 1, 25 µg L 1, 30 µg L 1, 40 µg L 1 concentrations of analytes. The results have shown that the method is best used at a deposition potential of 1.1 V vs. Ag/AgCl. Namen diplomskega dela je validacija elektroanalizne metode z antimonovo elektrodo za analizo težkih kovin v sledovih. Validacija se je pričela z določevanjem meje zaznavnosti (LOD) in meje kvantifikacije (LOQ), nadaljevala z določanjem linearnosti in končala z določanjem točnosti in natančnosti. Analiza težkih kovin je bila izvedena s square-wave anodno striping voltametrijo (SWASV), za testiranje reverzibilnosti sistema [Fe(CN)6] 3/[Fe(CN)6] 4 pa smo uporabili metodo ciklične voltametrije (CV). Vse analize so bile izvedene v 0,01 M raztopini HCl. Meje LOD in LOQ ni mogoče določiti z dovolj veliko gotovostjo, saj ima metoda tako nizko LOD, da je bila kontaminacija s težkimi kovinami, tudi v ultra čisti kislini, prevelika. Metoda ima linearen odziv pri potencialih depozicije 1,2 V, 1,1 V in 1,0 V vs. Ag/AgCl za Pb(II) in Cd(II) v območju od 14,6 µg L 1 do 100,0 µg L 1. Dokazano je tudi, da je metoda natančna in točna za vse tri potenciale depozicije pri koncentraciji analitov 15 µg L 1, 25 µg L 1, 30 µg L 1, 40 µg L 1. Ugotovljeno je bilo, da je metoda najbolj uporabna pri potencialu depozicije 1,1 V vs. Ag/AgCl. heavy metal analysis trace analysis antimony electrode SWASV voltammetry Analiza težkih kovin analitika sledov antimonova elektroda SWASV voltametrija. true true false [A. Ramot] Angleški jezik Slovenski jezik Diplomsko delo/naloga 2017-09-04 10:11:09 2017-09-28 12:52:30 2022-08-01 14:38:02 2019-07-11 16:35:55 2017 0 Maribor 0 0000-00-00 NiDoloceno NiDoloceno NiDoloceno 0000-00-00 0000-00-00 0000-00-00 543.55:549.25(043.2) 21059094 URN:SI:UM:DK:RFFS88X0 VS_Ramot_Aljaz_2017.pdf VS_Ramot_Aljaz_2017.pdf 1 E56BEBEDB7ED9123B4CECA7302E9DFCD 8f4f2bf77bb773afebacfd9f068efb2428fd970bf512d568c7dba8a5ffb99c58 5d951b02-7c0f-11eb-bb7a-00155d0001ca 20.500.12556/dkum/c0d3a5fc-9bd9-4823-84e6-f1092515e2f5 https://dk.um.si/Dokument.php?lang=slv&id=118965 Fakulteta za kemijo in kemijsko tehnologijo 0 0 0