Metoda spektrometrije masa uz induktivno spregnutu plazmu s laserskim otparavanjem u analizi nanočestica željeza

master's thesis

• Title (english): Laser ablation-inductively coupled plasma-mass spectrometry method in iron nanoparticles analysis
• Author: Natko Krajina
• Mentor: Sanda Rončević (mentor)
• Mentor: Ivan Nemet (komentor)
• Committee member: Sanda Rončević (predsjednik povjerenstva)
• Committee member: Tomica Hrenar (član povjerenstva)
• Committee member: Ivan Kodrin (član povjerenstva)
• Committee member: Ivan Nemet (član povjerenstva)
• Granter: University of Zagreb; Faculty of Science; (Department of Chemistry); Zagreb
• Defense date and country: 2023-09-28, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

U ovom radu sintetizirane su nanočestice neutralnog željeza (nZVI) za analizu sorpcije iona neodimija, europija, gadolinija, erbija i uranija iz vodene otopine na njihovu površinu. Sadržaj iona zaostao u vodenoj otopini određen je metodom spektrometrije masa uz induktivno spregnutu plazmu (ICP-MS), a sadržaj vezan na nanočestice željeza metodom spektrometrije masa uz induktivno spregnutu plazmu s laserskim otparavanjem (LA-ICP-MS). Ispitana je mogućnost uporabe polimliječne kiseline kao nosača čvrste faze za analizu metodom LA-ICP-MS. Zamijećena je loša reproducibilnost mjerenja te velika standardna odstupanja mjerenih signala. Za potrebe analize učinkovitosti sorpcije odabranih iona na nanočestice željeza metodom LA-ICP-MS načinjene su pastile uzoraka s mikrokristalnom celulozom. Pripravljena su tri kalibracijska standarda s mikrokristalnom celulozom i kalibracija je provedena uz željezo kao unutarnji standard. Pri analizi opažen je izvrstan linearni odziv te relativno nisko standardno odstupanje pri određivanju odabranih elemenata u tragovima. Analizom vodenih otopina lantanoida metodom ICP-MS nakon sorpcije, utvrđeno je da nZVI uklanjaju ione odabranih elemenata s vrlo visokom učinkovitošću.

Abstract (english)

In this experiment nanoparticles of zero-valent iron (nZVI) were synthesized and a sorption of neodymium, europium, gadolinium, erbium and uranium ions from aqueous solution onto their surface was analyzed. Amount of ions that had remained in aqueous solution after the sorption was determined by inductively coupled plasma-mass spectrometry (ICP-MS), and amount of ions adsorbed onto the surface of nZVI by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS). Applicability of polylactic acid as a solid carrier for LA-ICP-MS analysis was investigated, but poor measurement reproducibility and large standard deviation in measured signals were observed. Sample preparation for LA-ICP-MS analysis of bare nZVI included drying and homogenization by pressing nZVI with microcrystalline cellulose into pellets. Three calibration standards were prepared, and calibration was accomplished with iron as an internal standard. Highly linear response, and reasonably low standard deviations were observed during the analysis of the elements in ppm range. ICP-MS analysis of aqueous solutions after the sorption experiment showed very high sorption efficiency for all elements.

• Keywords: ioni lantanoida; lasersko otparavanje; nanočestice željeza; spektrometrija masa uz induktivno spregnutu plazmu
• Keywords (english): iron nanoparticles; LA-ICP-MS; lanthanide analysis; nanomaterial analysis
• Language: croatian
• URN:NBN: urn:nbn:hr:217:671476
• Study programme: Title: Graduate university studies in chemistry; specializations in: Research programme; Course: Research programme; Study programme type: university; Study level: graduate; Academic / professional title: magistar/magistra kemije (magistar/magistra kemije)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Embargoed access; Embargo expiration date: 2025-09-28
• Created on: 2023-10-18 11:49:20