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Študije in uporaba bakrovih elektrod v sodobni elektroanalizi
ID Obrez, Domen (Author), ID Kolar, Mitja (Mentor) More about this mentor... This link opens in a new window, ID Hočevar, Samo (Comentor)

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Abstract
Elektrokemijske tehnike so v primerjavi s spektroskopskimi in kromatografskimi metodami manj zapletene za uporabo in zanje običajno ni potrebna kompleksnejša obdelava vzorca pred meritvijo. Številne celo omogočajo in situ meritve – torej brez vzorčenja, kar je pri okoljski analizi zelo priročno za kontinuirni monitoring onesnažil v pretočnem sistemu kot je reka, morje ipd. Ena od elektrokemijskih tehnik, ki je primerna za določanje sledov kovin, je anodna inverzna (stripping) voltametrija, ki se je razvila v prejšnjem stoletju. V zadnjih 60 letih so se za takšne meritve najpogosteje uporabljale različne oblike živosrebrovih elektrod (kapljajoča, viseča, tankoplastna elektroda itd.), ki so okolju in živim organizmom škodljive, težavo pa predstavlja tudi rokovanje z živim srebrom, njegova hramba, itd. V mnogih državah je uporaba živega srebra močno omejena ali celo prepovedana. Kot nadomestek za živo srebro kot elektrodni material so bili preizkušeni mnogi prevodni materiali, kot so različne oblike prevodnega ogljika (pirolitski grafit, polikristalinični grafit, elektroda iz ogljikove paste, steklasti ogljik, ogljikova vlakna), zlato, platina, srebro, iridij, itd., toda nobeden od naštetih ni dosegel izjemnih elektroanaliznih karakteristik živosrebrovih elektrod. Leta 2000 je skupina iz Odseka za analizno kemijo (Kemijski Inštitut) v sodelovanju z ameriškim partnerjem (Department of Chemistry and Biochemistry, New Mexico State University, Las Cruces) vpeljala uporabo bizmuta za stripping voltametrično detekcijo izbranih sledov ionov težkih kovin. Temu je v letu 2006 sledila predstavitev tankoslojne antimonove elektrode, nedavno pa so na Odseku za analizno kemijo študirali tudi zanimivo uporabo tankoslojne bakrove elektrode za detekcijo nekaterih ionov težkih kovin v sledovih. V pričujočem magistrskem delu je predstavljena raziskava elektrokemijskih lastnosti in uporabe različnih bakrovih elektrod za določitev nizkih koncentracij Pb2+ in Cd2+ v vodnih medijih z anodno inverzno (stripping) voltametrijo. Pri svojem delu sem obravnaval tako tankoslojne bakrove elektrode, pripravljene na osnovni elektrodi iz steklastega ogljika in tiskani ogljikovi elektrodi, kot tudi trdne bakrove elektrode (trdna bakrova (disk) elektroda, tiskana bakrova elektroda in bakrova žica). Preučeval sem vplive različnih parametrov, kot so sestava medija, koncentracija bakrovih(II) ionov, čas depozicije bakra in analitov ter napetost depozicije, na stabilnost in občutljivost elektrode ter jih skušal optimizirati. Preučeval sem tudi območje linearnosti, ponovljivost meritev, spodnjo mejo zaznave (LOD) ter spodnjo mejo kvantifikacije (LOQ) za posamezno obravnavano elektrodo. Izkazalo se je, da imajo bakrove elektrode precej podobne lastnosti nekaterim že uveljavljenim in razširjenim kovinskim elektrodam, kot sta na primer antimonova in bizmutova elektroda. Odlikuje jih relativno visoka občutljivost in zato ugodno nizek LOD, dobra ponovljivost ter široko linearno koncentracijsko območje delovanja. Baker je kot elektrodni material poceni in zaradi svojih lastnosti (večina njegovih spojin je relativno nestrupenih za organizme – uporablja se celo za pospeševanje rasti pri reji prašičev) neproblematičen za uporabo.

Language:Slovenian
Keywords:baker, bakrova elektroda, težke kovine, svinec, kadmij, anodna inverzna voltametrija, stripping voltametrija, analiza sledov.
Work type:Master's thesis/paper
Typology:2.09 - Master's Thesis
Organization:FKKT - Faculty of Chemistry and Chemical Technology
Year:2022
PID:20.500.12556/RUL-134999 This link opens in a new window
COBISS.SI-ID:98727427 This link opens in a new window
Publication date in RUL:16.02.2022
Views:1388
Downloads:150
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Secondary language

Language:English
Title:Studies and uses of copper electrodes in modern electroanalysis
Abstract:
Electrochemical techniques are much less complicated for use compared to spectroscopic and chromatographic methods – sample preparation is usually not required. Many of them allow in situ determination, which is important in environmental analysis for continuous monitoring of contaminant concentrations in flow systems such as rivers and oceans. Anodic stripping voltammetry is one of the electrochemical techniques that developed in the late 20th century for the analysis of trace metals. In the last 60 years, different mercury electrodes (dropping mercury electrode – DME, hanging mercury dropping electrode – HDME, mercury film electrode – MFE) have been used for this kind of measurements, which are dangerous for the environment and living organisms. There is also a problem with handling and storage of mercury. Today, the use of mercury is restricted or even banned. Many electrically conductive materials such as various forms of electrically conductive carbon (pyrolytic graphite – PG, polycrystalline graphite, carbon paste electrode – CPE, glassy carbon electrode – GCE, carbon fibres, etc.), gold, platinum, silver, iridium, etc. have been used to replace mercury as electrode materials, but none of them exhibited excellent electroanalytical properties of mercury electrodes. In 2000, a group of scientists from the Department of Analytical Chemistry (National Institute of Chemistry, Ljubljana) in collaboration with an American partner institution (Department of Chemistry and Biochemistry, New Mexico State University, Las Cruces) introduced bismuth in stripping voltammetry measurements for the detection of heavy metal traces. Then, in 2006, the antimony film electrode was introduced. Recently, the use of copper film electrodes for the detection of selected heavy metal ion traces was investigated by the Department of Analytical Chemistry. This master’s thesis represents an investigation of properties and applications of various copper electrodes for determination of lead(II) and cadmium(II) ions in low concentrations in water solutions using anodic stripping voltammetry. In my work, copper-film electrodes based on glassy carbon electrodes and screen-printed electrodes (SPE) with carbon working electrode as well as bulk copper electrodes (copper disc electrode, SPE with copper working electrode, copper wire) were investigated. I investigated the influences of various parameters such as medium, copper(II) concentration, time of deposition of copper and analytes and deposition potential on the stability and sensitivity of the electrodes. In the next phase, the parameters were optimised to obtain the best performance of the electrodes, and then their range with linear response, repeatability and limits of detection and quantification (LOD, LOQ) were determined. The experiments have shown that copper electrodes are very similar to some other already established metal electrodes, for example, antimony and bismuth electrodes. They have good sensitivity and therefore a low detection limit, as well as good repeatability and a broad linear response. Copper as an electrode material is inexpensive and, due to its qualities (the toxicity of most its compounds to organisms is relatively low – it is even used as growth promoter in breeding pigs), it is not problematic to use.

Keywords:copper, copper electrode, heavy metals, lead, cadmium, anodic stripping voltammetry, trace analysis

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