2-aminotiyofenol ile dialdehitlerden schiff bazlarının sentezi ve geçiş metalleri ile komplekslerinin eldesi, karakterizasyonu ve ekstraksiyonunda uygulamaları
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Tarih
2017
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info:eu-repo/semantics/openAccess
Özet
Bu çalışmada, yeni tiyo Schiff bazları, N,N’-bis(2-aminotiyofenol)-1,4- bis(karboksaldehit fenoksi)bütan (L1 ) ve N,N’-bis(2-aminotiyofenol)-1,7-bis(formilfenil)- 1,4,7-trioksaheptan (L2 ) sentezlenmiştir. Sentezlenen bu Schiff bazı ligandlarının Cu(II), Ni(II), Zn(II), Co(II) ve La(III) kompleksleri hazırlandı. Ligandların ve komplekslerin yapıları FTIR, Elemental Analiz, Magnetik Süssebtibilite, UV-vis, Kondüktometrik ölçümleri, 1H-NMR, 13C-NMR ve siklik voltametri verilerinden yararlanılarak karakterize edildi. Sentezlenen ligandlar ile bakır(II) ve nikel(II) iyonlarının sulu çözeltilerinden organik çözücüye ekstraksiyonu yapıldı. I. Aşamada sentezlenen ligandlar ile metal iyonlarının ekstraksiyonu üzerine sürenin etkisi incelenmiştir. Ekstraksiyon üzerine süresinin etkisini çalışmak için, 15, 30, 45, 60 ve 120 dakikalar seçildi. Ekstraksiyondan sonra sulu fazda kalan metal iyonlarının derişimleri AAS ile ölçüldü ve ekstrakte edilen metal yüzdeleri hesaplandı. II. Aşamada L1 ve L2 ligandları ile metal iyonlarının ekstraksiyonu üzerine pH’ının etkisini incelemek için sulu fazın pH’ı 3-10 aralığında değiştirilmiştir. Ortamın pH’ını ekstraksiyon süresince sabit tutmak için asetik asit-sodyum asetat ve sodyum karbonatsodyum bikarbonat tampon çözeltileri kullanıldı. Ekstraksiyon sonrası sulu fazda kalan metal iyonlarının derişimi AAS ile ölçülmüş ve ekstrakte edilen metal yüzdeleri hesaplanmıştır. Ekstraksiyon deneyleri sonucunda sayfa 45’ deki denklemden yararlanılarak, log H2L ye karşı log D nin grafiğe geçirilmesiyle elde edilen doğrunun eğiminden birleşme oranı ve kayma değerlerinden de log Kext sabitleri elde edildi. Anahtar Kelimeler: 2-aminotiyofenol, tiyo Schiff bazları, tiyo Schiff bazı kompleksleri, çözücü ekstraksiyonu, elektronik geçişler, siklik voltametri.
In this study, new thio Schiff bases, N,N’-bis(2-aminothiophenol)-1,4- bis(carboxylidene phenoxy)butane (L1 ) and N,N’-bis(2-aminothiophenol)-1,7- bis(formylphenyl)-1,4,7-trioksaheptane (L2 ) were synthesized. Cu(II), Ni(II), Zn(II), Co(II) and La(III) complexes with Schiff bases were prepared. The structure of the ligand and their complexes were determined by FTIR, elemental analyses, magnetic susseptibility, conductance measurements, 1H-NMR, 13C-NMR and cyclic voltammetry. There were investigated the extraction of copper(II) and nikel(II) ions from aqueous phase to organic phase with the synthesized ligands. In the first step, the effect of time on ligand and metal ions extractions were investigated. 15, 30, 45, 60 and 120 minutes were chosen in order to study the effect of time on extraction. After the extraction process the concentrations of metal ions left in aqueous phase were measured by AAS and the percentages of metal was calculated. In the second step, in order to investigate the effect of pH on the extraction of metal ions with L1 and L2 ligand, the aqueous phase of pH was changed between 3-10. To keep the medium pH constant during the extraction time acetic acid-sodium acetate and sodium carbonate-sodium bicarbonate buffer solutions were used. After the extraction process the concentrations of metal ions left in aqueous phase were measured by AAS the percentages of extracted Cu(II) and Ni(II) were calculated. By using equation (page 45) which was obtained from the extraction experiments the log H2L value was plotted against log D and linear line was obtained. The combination ratio was calculated from slope. The log Kext constant was obtained from the shift value. Key words : 2-aminothiophenol, thio Schiff bases, thio Schiff base complexes, solvent extraction, electronic transitions, cyclic voltammetry.
In this study, new thio Schiff bases, N,N’-bis(2-aminothiophenol)-1,4- bis(carboxylidene phenoxy)butane (L1 ) and N,N’-bis(2-aminothiophenol)-1,7- bis(formylphenyl)-1,4,7-trioksaheptane (L2 ) were synthesized. Cu(II), Ni(II), Zn(II), Co(II) and La(III) complexes with Schiff bases were prepared. The structure of the ligand and their complexes were determined by FTIR, elemental analyses, magnetic susseptibility, conductance measurements, 1H-NMR, 13C-NMR and cyclic voltammetry. There were investigated the extraction of copper(II) and nikel(II) ions from aqueous phase to organic phase with the synthesized ligands. In the first step, the effect of time on ligand and metal ions extractions were investigated. 15, 30, 45, 60 and 120 minutes were chosen in order to study the effect of time on extraction. After the extraction process the concentrations of metal ions left in aqueous phase were measured by AAS and the percentages of metal was calculated. In the second step, in order to investigate the effect of pH on the extraction of metal ions with L1 and L2 ligand, the aqueous phase of pH was changed between 3-10. To keep the medium pH constant during the extraction time acetic acid-sodium acetate and sodium carbonate-sodium bicarbonate buffer solutions were used. After the extraction process the concentrations of metal ions left in aqueous phase were measured by AAS the percentages of extracted Cu(II) and Ni(II) were calculated. By using equation (page 45) which was obtained from the extraction experiments the log H2L value was plotted against log D and linear line was obtained. The combination ratio was calculated from slope. The log Kext constant was obtained from the shift value. Key words : 2-aminothiophenol, thio Schiff bases, thio Schiff base complexes, solvent extraction, electronic transitions, cyclic voltammetry.
Açıklama
Anahtar Kelimeler
2-aminotiyofenol, Tiyo Schiff bazları, Tiyo Schiff bazı kompleksleri, Çözücü ekstraksiyonu, Elektronik geçişler, Siklik voltametri, 2-aminothiophenol, Thio Schiff bases, Thio Schiff base complexes, Solvent extraction, Electronic transitions, Cyclic voltammetry
