Uporaba različnih spektroskopskih tehnik (ICP-MS, ICP-OES in AAS) pri določevanju kovin v bezgu

Marjanovič, Dejan (author), Kolar, Mitja (mentor)

Uporaba različnih spektroskopskih tehnik (ICP-MS, ICP-OES in AAS) pri določevanju kovin v bezgu Namen magistrskega dela je določiti vsebnosti kovin v vzorcih bezga. V prvem delu magistrske naloge smo analizirali vsebnost kovin v različnih delih bezga: Testne korenine, D 103 C Jagode, 3/8 Socvetja, Testni listi, Snigra BB Peclji, Testni poganjki in 4/16 Lubje. Zaradi največjih odstopanj v vsebnosti kovin smo se z nadaljnjim raziskovanjem usmerili na analize vsebnosti kovin v lubju in mladih poganjkih. Lubje in mladi poganjki zajemajo tretje in četrte generacije medvrstnih križancev bezga, ki obsegajo kombinacije dveh, treh ali štirih speciesov: črni (Sambucus nigra), modri (S. cerulea), rdeči (S. racemosa) in javanski (S. javanica). Skupaj s svojimi podvrstami smo v raziskavo vključili tudi samostojno vrsto S. nigra. Nekatere vzorčene rastline imajo enak zapis (enako starševsko strukturo), vendar zaradi genetske segregacije predstavljajo različne genotipe. V analizo smo vključili tudi nekatere klone (C1). Vzorce smo pripravili s klasičnim kislinskim in mikrovalovnim razklopom in določili vsebnosti kovin z uporabo različnih spektroskopskih tehnik (ICP-OES, AAS in ICP-MS). Pred začetkom analize smo vzorce ustrezno pripravili s kislinskim razklopom s segrevanjem nad gorilnikom (uporaba H2SO4, HNO3 in H2O2) in uporabo MW razklopa. Primerjali smo rezultate vsebnosti kovin pridobljenih z različnimi spektroskopskimi tehnikami. V okviru magistrskega dela smo ugotavljali tudi linearnost, LOD, LOQ, ponovljivost, interval zaupanja in iskanje ubežnika s pomočjo Dixonov in Grubbsov testa za izračun ubežnikov. S statističnimi testi: Spearmanov koeficient in Kruskal – Wallis-ov test smo preučevali povezave med posameznimi elementi in ničelno hipotezo, da so populacije mediane enake. Ugotavljali smo vpliv valovne dolžine na koncentracije kovin. S pomočjo razklopa z dušikovo(V) kislino, različnih ekstrakcij kovin, pri katerih smo uporabljali različne reagente smo želeli ugotoviti katere kovin so prisotne in vsebnosti le-teh v vzorcih križancev bezga. Za nadaljnjo analizo smo izbrali metodo ICP-OES zaradi ustrezno nizke meje zaznavnosti, širokega linearnega koncentracijskega območja in točnosti. Izvedli sem tudi delno validacijo metode. Vsebnost kovin v vzorcih smo določili s pomočjo metode umeritvene krivulje.

• Language: Slovenian
• Keywords: Induktivno sklopljena plazma z atomsko emisijsko spektroskopijo (ICP-AES), mikrovalovni razklop, kislinski razklop, bezeg
• Work type: Master's thesis/paper
• Typology: 2.09 - Master's Thesis
• Organization: FKKT - Faculty of Chemistry and Chemical Technology
• Year: 2019
• PID: 20.500.12556/RUL-110526
• COBISS.SI-ID: 1538432451
• Publication date in RUL: 16.09.2019

Secondary language

• Language: English
• Title: Use of various spectroscopic techniques (ICP-MS, ICP-OES and AAS) in determination of metals in Elderberry

Abstract

Use of various spectroscopic techniques (ICP-MS, ICP-OES and AAS) in determination of metals in Elderberry The purpose of the masterˈs degree is to determine the assay of metals in samples of elderberry. In the first part we analyzed the content of metals in different parts of plant in two parallels: Test roots, D 103 Strawberries, 3/8 Inflorescence, Leaves, Snigra BB stips, Test shoots and 4/16 Bark. Due to the highest differences in metal assay we continued to explore content of metals in bark and young shoots. Bark and young shoots cover the third and fourth generations of elderberry crosses, comprising combinations of two, three or four species: black (Samucus nigra), blue (S. cerulea), red (S. racemosa) and Javanese (S. javanica). Together with its subspecies, we also included an independent type of S. nigra in the study. Some of sampled plants have the same genetic record (same parental structure), but due to genetic segregation, they represent different genotypes. In analysis, we also included some clones (C1). Samples were prepared with classical acid and microwave digestion. We have determined the content of metals using various spectroscopic techniques (ICP-OES, AAAS and ICP-MS). Prior to start of the analysis samples were prepared by acid digestion by heating over the burner (use of H2SO4, HNO3 and H2O2) and the use of MW digestion. We compared the results of the metal content obtained with various spectroscopic techniques. In scope of masterˈs degree, we also determined linearity, LOD, LOQ, repeatability, interval of confidence and search for an outliner with Dixon and Grubbs test. With the statistical tests: Spearmanˈs coefficient and Kruskal-Wallis test we studied connections between individual elements and the zero hypothesis that the median populations are the same. We also investigated effect of wavelengths on metal concentrations. With digestion with nitrogen(V) acid, various extractions of metals in which different reagents were used, we wanted to determine which metals are present and their assay in samples. For further analysis, ICP-OES method was chosen due to low detection limit, wide linear concentration range and accuracy. We also performed partial validation of method. Assay of metals in samples was determined with method using calibration curve.

• Keywords: Inductively coupled plasma atomic emission spectroscopy (ICP-AES), microwave digestion, acid digestion, elderberry