Preconcentration and speciation of some metals with cloud point extraction

In this thesis study, two diffirent methods is developed in order to enrich some heavy metal ions (Cu+2 Zn+2, Ni+2, Cd+2, Co+2, Pb+2) at water samples and speciation of antimony water and juice samples via cloud point extraction and detection in Ultrasonic Nebulizer ICP-OES Inductively Coupled Plasma - Optical Emission Spectrometry. During this process firstly, the metal ions which are complexed with 5,7-diiodo-8-hydroxyquinoline in Triton X-114 surfactant environment have been imprisoned in the micelles, after phase separation via centrifuge, rich in surfactant phase has been diluted with 2 mol.L-1 HNO3 and measured in USN-ICP-OES device. In order to reduce noise and errors In has been used as internal standard. pH, surfactant concentration, ligand concentration, equilibration time, temperature and foreign ion effects have been researched for optimum conditions operation. LOD rates of the metals (Cu+2, Zn+2, Ni+2, Cd+2, Co+2, Pb+2) at optimum conditions (pH=7, 0.1 mmol.L-1 5,7-di-iodo-8-hydroxyquinoline, 0.06 % (w/v) Triton X-114) have occurred as 0.076, 0.30, 0.081, 0.022, 0.033 ve 0.049 µg.L-1. RSD % has formed between 2.08 % and 6.28 % (n=10). Developed method has been successfully applied on certified reference material and real water samples. Secondly, Sb(III) complexes which were complexed with Dithizone by using Triton X-114 surfactant, confined into micelle from aqueous phase via cloud point extraction procedure, after phase separation with centrifuge, surfactant rich phase has been solved with 2 mol.L-1 HNO3 and measured on USN-ICP-OES. In order to decrease noise and failures, In was used as internal standard. The effects of the rates of foreign ion and the species to each other, pH, surfactant concentration, ligand concentration, heating time and temperature has been researched for the optimum conditions of the procedure. L-Cystein and Sb(V) species have been reduced to Sb(III) species. LOD value of (pH=4, 0.04 mmol.L-1 dithizone, 0.06 % (w/v) Triton X-114) Sb(III) was performed as 0.038 µg.L-1 and RSD % has been performed as 2.59 % (n=12). The developed method was applied on certified reference material with water and fruit juices samples.