Identifikacija kompleksnih spojeva lantanoida spektrometrijom masa

master's thesis

• Title (english): Identification of lanthanide complexes by mass spectrometry
• Author: David Klarić
• Mentor: Nives Galić (mentor)
• Committee member: Nives Galić (predsjednik povjerenstva)
• Committee member: Željka Soldin (član povjerenstva)
• Committee member: Morana Dulić (član povjerenstva)
• Committee member: Snežana Miljanić (član povjerenstva)
• Granter: University of Zagreb; Faculty of Science; (Department of Chemistry); Zagreb
• Defense date and country: 2018-09-28, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

Tehnikom spektrometrije masa uz ionizaciju elektroraspršenjem analizirana su vezna
svojstva sedam različitih kaliks[4]arenskih te kaliks[6]arenskih derivata s odabranim
kationima lantanoida (La3+, Eu3+, Yb3+). Kompleksiranje izostaje u slučaju esterskih derivata
kaliksarena bez obzira na veličinu kaliksarenske šupljine, dok amidni derivati sa svim
kationima lantanoida grade stabilne 1:1 komplekse.
Provedena je tandemna spektrometrija masa na odabranim ionima kaliksarena i
kompleksnih spojeva, predložene su odgovarajuće sheme fragmentiranja te je procijenjena
stabilnosti derivata kaliksarena i njihovih kompleksnih spojeva u plinskoj fazi. Pri
fragmentiranju izoliranih iona kaliksarenskih derivata i njihovih kompleksnih spojeva uočeno
je heterolitičko (induktivno) i homolitičko cijepanje veza. Disocijacija kompleksnih spojeva
nije uočena. Analize su provedene na dva različita instrumenta, trostrukom kvadrupolu i
ionskoj stupici te su uspoređeni rezultati dobiveni uz različite analizatore masa.

Abstract (english)

Binding properties of seven different calix[4]arenes and calix[6]arenes with selected
lanthanide cations (La3+, Eu3+, Yb3+) were investigated by electrospray ionization mass
spectrometry. Complexation was not observed in the case of ester calixarene derivatives,
regardless of the size of the calixarene cavity, while amide derivatives formed stable 1:1
complexes with all lanthanide cations.
Tandem mass spectrometry analysis of the selected calixarene and complex ions was
performed, corresponding fragmentation schemes and stability estimation of calixarene
derivatives and their complex compounds in the gas phase were suggested. During the
fragmentation of the isolated ions of the calixarenes and their complex compounds,
heterolytic (inductive) bond cleavage and homolytic bond cleavage were observed.
Dissociation of the complex compounds was not observed. The analyses were performed by
using two different instruments, triple quadrupole and quadrupole ion trap, and comparisons
of the results obtained with different mass analyzers were made.

• Keywords: lantanoidi; kaliksareni; kompleksni spojevi; spektrometrija masa
• Keywords (english): calixarenes; complex compounds; lanthanides; mass spectrometry
• Language: croatian
• URN:NBN: urn:nbn:hr:217:024735
• 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: Open access; Embargo expiration date: 2020-09-28
• Created on: 2018-11-19 13:22:57