Yeni bir glioksim sentezi ve Nikel (II), Bakır (II), Kobalt (II) ile komplekslerinin hazırlanması
Başlık çevirisi mevcut değil.
- Tez No: 29370
- Danışmanlar: PROF. DR. HAMİT BOZTEPE
- Tez Türü: Yüksek Lisans
- Konular: Kimya, Chemistry
- Anahtar Kelimeler: Belirtilmemiş.
- Yıl: 1993
- Dil: Türkçe
- Üniversite: Çukurova Üniversitesi
- Enstitü: Fen Bilimleri Enstitüsü
- Ana Bilim Dalı: Kimya Ana Bilim Dalı
- Bilim Dalı: Belirtilmemiş.
- Sayfa Sayısı: 81
Özet
65 SUMMARY. In this study, a new glyoxime compound was synthesized and its metal complexes with Cu2+,Ni2+ and Co2+ were prepared. Structural characteristics of which were established by means of 1H-n.m.r., İr, UV and elementel analyses technics. A glyoxime derivative which is named as 2,4-bis(amino amfi- glyoxime)-6-phenyl-s-triazine (TG) was synthesized by addition of mono chloro amphi glyoxime to 2,6-diamino-4-phenyl-s-triazine in absolute alcohol. Elemental analysis of showed that TG has a C13H13N9O4 formula. G.C. analysis of ligand established its purity. The fact that OH protons peaks shifted(weak zone) (12,3 ppm) disappeared with D2O in 1H-n.m.r. spectrum, OH strecthing peaks which is specific for oximes appeared at 3200 cm"1. and the spectroscopic technics and elemental analysis proved that resulted compound is a glyoxime derivative. In addition, two singlet at 8.3-7.6 ppm represents aromatic protons and a singlet N-H peak at 6.8 ppm represents amidoxime and a singlet at 3.3 ppm represents C-H proton at aldoxime. A few characteristic absorptions for glyoxime group, OH, C=N, N-O, vibration bonds were observed at 3200, 1680, 980 cm- 1 respectively, by Ir. IR spectrum also showed that N-H strecthing and deformation bonds located at 3310 and 1595 cm-1 respectively. These results agree with the values given by previous publications. In order to transform amphi form of TG to anti form, ligand was treated with concentrated HCI for prolong time. However, a tansformation cold not be determined. Therefore the compound also was treated with a dry HCI in ether. But this attempt also66 When amphi TG ligand dissolved with concentrated HCI first then alcohol added for the mixture as precipitation started. However amphi TG transformed to anti TG by the method that consist of dissolving amphi TG with concentrated HCI then adding alcohol into the mixture as soon as precipitation started. This transformation was observed by the fact that Ni2 + complex had a red color. Spectroscopic analyses revealed that phenyl-s-triazin ring was cleaved during the transformation. Ni(ll), Co(ll), Cu(ll) transition metal complexes of TG were isolated from their alcohol-water solutions. Ir, 1H-n.m.r. In visible analyses and magnetic susseptibility measurements of these complexes revealed them to be amino glyoxime complexes. By utilizing a comlex which prepared via the reaction of amino anti-glyoxim ligand with nickel the investigation of qualitative and quantitative determination of Ni(ll) ion in aqua medium was performed When alcohol solution of dimethylglyoxim added into amonia solution of nickel accurance of specific red color of dimethylglyoxim solition can be observed. TG ligand converted to its antiform red color of (AG)2Ni solution was obtained by addition of alcohol solution of which ligand into amonia solution of nickel. These results reveals that AG gives spesific color for Ni(ll) as in case of DMG in addition determination Ni2+ remained in solution offer (AG)2Ni complex had been formed was carried out by means of Aqualytic M p-f o to meter AL.25 instrument.Results showed that in term of analytic point, AG could be used as an qualitative and quantitative indicator like dimethylglyoxim.
Özet (Çeviri)
65 SUMMARY. In this study, a new glyoxime compound was synthesized and its metal complexes with Cu2+,Ni2+ and Co2+ were prepared. Structural characteristics of which were established by means of 1H-n.m.r., İr, UV and elementel analyses technics. A glyoxime derivative which is named as 2,4-bis(amino amfi- glyoxime)-6-phenyl-s-triazine (TG) was synthesized by addition of mono chloro amphi glyoxime to 2,6-diamino-4-phenyl-s-triazine in absolute alcohol. Elemental analysis of showed that TG has a C13H13N9O4 formula. G.C. analysis of ligand established its purity. The fact that OH protons peaks shifted(weak zone) (12,3 ppm) disappeared with D2O in 1H-n.m.r. spectrum, OH strecthing peaks which is specific for oximes appeared at 3200 cm"1. and the spectroscopic technics and elemental analysis proved that resulted compound is a glyoxime derivative. In addition, two singlet at 8.3-7.6 ppm represents aromatic protons and a singlet N-H peak at 6.8 ppm represents amidoxime and a singlet at 3.3 ppm represents C-H proton at aldoxime. A few characteristic absorptions for glyoxime group, OH, C=N, N-O, vibration bonds were observed at 3200, 1680, 980 cm- 1 respectively, by Ir. IR spectrum also showed that N-H strecthing and deformation bonds located at 3310 and 1595 cm-1 respectively. These results agree with the values given by previous publications. In order to transform amphi form of TG to anti form, ligand was treated with concentrated HCI for prolong time. However, a tansformation cold not be determined. Therefore the compound also was treated with a dry HCI in ether. But this attempt also66 When amphi TG ligand dissolved with concentrated HCI first then alcohol added for the mixture as precipitation started. However amphi TG transformed to anti TG by the method that consist of dissolving amphi TG with concentrated HCI then adding alcohol into the mixture as soon as precipitation started. This transformation was observed by the fact that Ni2 + complex had a red color. Spectroscopic analyses revealed that phenyl-s-triazin ring was cleaved during the transformation. Ni(ll), Co(ll), Cu(ll) transition metal complexes of TG were isolated from their alcohol-water solutions. Ir, 1H-n.m.r. In visible analyses and magnetic susseptibility measurements of these complexes revealed them to be amino glyoxime complexes. By utilizing a comlex which prepared via the reaction of amino anti-glyoxim ligand with nickel the investigation of qualitative and quantitative determination of Ni(ll) ion in aqua medium was performed When alcohol solution of dimethylglyoxim added into amonia solution of nickel accurance of specific red color of dimethylglyoxim solition can be observed. TG ligand converted to its antiform red color of (AG)2Ni solution was obtained by addition of alcohol solution of which ligand into amonia solution of nickel. These results reveals that AG gives spesific color for Ni(ll) as in case of DMG in addition determination Ni2+ remained in solution offer (AG)2Ni complex had been formed was carried out by means of Aqualytic M p-f o to meter AL.25 instrument.Results showed that in term of analytic point, AG could be used as an qualitative and quantitative indicator like dimethylglyoxim.
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Doktora
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Kimya MühendisliğiSelçuk ÜniversitesiKimya Ana Bilim Dalı
PROF. DR. RAMAZAN MİRZAOĞLU