Validation of electroanalytical method with antimony electrode for trace metal analysis

diplomsko delo visokošolskega strokovnega študijskega programa I. stopnje

Aljaž Ramot (Author), Matjaž Finšgar (Mentor), Barbara Petovar (Co-mentor)

Abstract

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.

Keywords

heavy metal analysis;trace analysis;antimony electrode;voltammetry;SWASV;

Data

Language:	English
Year of publishing:	2017
Typology:	2.11 - Undergraduate Thesis
Organization:	UM FKKT - Faculty of Chemistry and Chemical Engineering
Publisher:	[A. Ramot]
UDC:	543.55:549.25(043.2)
COBISS:	21059094
Views:	1213
Downloads:	189
Average score:	0 (0 votes)
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Other data

Secondary language:	Slovenian
Secondary title:	Validacija elektroanalizne metode z antimonovo elektrodo za analizo težkih kovin v sledovih
Secondary abstract:	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.
Secondary keywords:	analiza težkih kovin;analitika sledov;antimonova elektroda;voltametrija;diplomske naloge;
URN:	URN:SI:UM:
Type (COBISS):	Bachelor thesis/paper
Thesis comment:	Univ. v Mariboru, Fak. za kemijo in kemijsko tehnologijo
Pages:	IX, 36 str.
ID:	10862132