Investigation of thermal decomposition kinetics of Cr, Mo and W hexacarbonyl complexes of the schiff base salicylidene-3-amino-1, 2, 4-triazole using thermogravimetric methods
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Tarih
2006
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Cilt Başlığı
Yayıncı
Ege Üniversitesi
Erişim Hakkı
info:eu-repo/semantics/closedAccess
Özet
ÖZET SALİSİLİDEN-3-AMİNO-l,2,4-TRİAZOL SCHIFF BAZININ Cr, Mo ve W HEKZAKARBONİLLERİ İLE VERDİĞİ KOMPLEKSLERİN ISISAL BOZUNMA KİNETİĞİNİN TERMOGRAVİMETRİK OLARAK İNCELENMESİ Gülden GÜNSEVER Yüksek Lisans Tezi, Kimya Bölümü Tez Yöneticisi : Prof. Dr. Mehmet YÜREKLİ Şubat 2006, 77 sayfa Bu çalışmada Cr, Mo ve W hekzakarbonillerinin salisiliden-3-amino- 1,2,4-triazol (SAT) Schiff bazı ile yaptığı komplekslerin ısısal bozunma kinetiği, izotermal olmayan (dinamik) termogravimetri yöntemleriyle araştılmıştır. Bu kompleksler bölümümüzün anorganik kimya laboratuvarında sentezlenmiştir. İR, NMR ve kütle spektrumları ligand ve metal komplekslerinin yapısal karakterizasyonlarının araştırılmasında kullanılmıştır. Sentezlenen komplekslerin ısısal bozunması azot atmosferi altında, 3 °C/dak., 6 °C/dak., 9 °C/dak. ve 12 °C/dak. lık ısırma hızlarında Shimadzu DTG- 60H termogravimetri cihazı kullanılarak incelenmiştir. Bu komplekslerin bozunma kinetiği; integral, diferansiyel ve fark- diferansiyel termogravimetri yöntemleri kullamlarak araştırılmıştır. Ozawa, Friedman ve Freeman-Carroll yöntemlerini uygulayarak, aktivasyon enerjisi, E, pre-eksponansiyel faktör, A, ve tepkime mertebesi, n gibi kinetik parametreler üç farklı yöntemle TG eğrilerinin analizinden elde edilmiştir. En iyi değerler Osawa'nin integral eğri çakıştırma yöntemi ile Cr(SAT) için E=202.04±4.02kJ/mol, n=l ve logA=24.761±0.644, Mo(SAT) için E=123.48±1.05, n=l ve logA=14.074±0.070, W(SAT) için ise E=78.76±3.43, n=l ve logA=l 1.055±0.016 olarak bulunmuştur. Dinamik termogravimetrik yöntemlerinin karşılaştırma sonuçları, metal karbonil komplekslerinin ısısal bozunmasına ilişkin kinetik parametrelerinin araştırılmasında en uygun yöntemin integral yöntemler, özellikle Osawa yöntemi olduğunu göstermiştir. Diferansiyel ve fark-diferansiyel yöntemlerin ise hatalı sonuç verdikleri gözlenmiştir. Anahtar Kelimeler : Kompleks, ısısal bozunma, kinetik parametre, termogravimetri
V SUMMARY INVESTIGATION OF THERMAL DECOMPOSITION KINETICS OF Cr, Mo AND W HEXACARBONYL COMPLEXES OF THE SCHIFF BASE SALICYLIDENE-3-AMINO-l,2,4-TRIAZOLE USING THERMOGRAVIMETRIC METHODS GÜNSEVER, Gülden MS Degree Thesis, Department of Chemistry Supervisor: Prof. Dr. Mehmet YÜREKLİ February 2006, 77 pages In this study thermal decomposition kinetics of Cr, Mo and W hexacarbonyl complexes of the Schiff base salicylidene-3 -amino- 1,2,4-triazol (SAT) was investigated by non-isothermal (dynamic) thermogravimetric methods. These complexes were synthesised in inorganic chemistry laboratory. IR, NMR and mass spectra were used for the investigation of the structural characterization of the ligand and the metal complexes. The thermal decomposition of the synthesised complexes was studied in nitrogen atmosphere at the heating rate of 3 °C/min, 6 °C/min, 9 °C/min and 12 °C/min by using Shimadzu DTG-60H thermogravimetry apparatus. The decomposition kinetics of these complexes were examined by using integral, differential and difference-differential thermogravimetric methods. Applying the Ozawa, Friedman and Freeman-Carroll methods, kinetic parameters like activation energy, E, pre-exponential factor, A, and reaction order, n, were obtained from the analysis of TG curves with three different methods. The best values were found to be E=202.04±4.02 n=l andVI logA=24.761±0.644 for Cr(SAT), E=123.48±1.05 kJ/mol, n=l and logA=14.074±0.070 for Mo(SAT), and E=78.76±3.43 kJ/mol, n=l and logA=11.055±0.016 for W(SAT) by means of Ozawa's integral curve fitting method. Results of the comparison of the dynamic thermogravimetric methods indicated that the most appropriate methods for investigation of kinetic parameters related to the thermal decomposition of metal carbonyl complexes were the integral methods, especially Ozawa's method. And it was observed that differential and difference-differential methods lead to erratic results. Keywords : Complex, thermal decomposition, kinetic parameter, thermogravimetry.
V SUMMARY INVESTIGATION OF THERMAL DECOMPOSITION KINETICS OF Cr, Mo AND W HEXACARBONYL COMPLEXES OF THE SCHIFF BASE SALICYLIDENE-3-AMINO-l,2,4-TRIAZOLE USING THERMOGRAVIMETRIC METHODS GÜNSEVER, Gülden MS Degree Thesis, Department of Chemistry Supervisor: Prof. Dr. Mehmet YÜREKLİ February 2006, 77 pages In this study thermal decomposition kinetics of Cr, Mo and W hexacarbonyl complexes of the Schiff base salicylidene-3 -amino- 1,2,4-triazol (SAT) was investigated by non-isothermal (dynamic) thermogravimetric methods. These complexes were synthesised in inorganic chemistry laboratory. IR, NMR and mass spectra were used for the investigation of the structural characterization of the ligand and the metal complexes. The thermal decomposition of the synthesised complexes was studied in nitrogen atmosphere at the heating rate of 3 °C/min, 6 °C/min, 9 °C/min and 12 °C/min by using Shimadzu DTG-60H thermogravimetry apparatus. The decomposition kinetics of these complexes were examined by using integral, differential and difference-differential thermogravimetric methods. Applying the Ozawa, Friedman and Freeman-Carroll methods, kinetic parameters like activation energy, E, pre-exponential factor, A, and reaction order, n, were obtained from the analysis of TG curves with three different methods. The best values were found to be E=202.04±4.02 n=l andVI logA=24.761±0.644 for Cr(SAT), E=123.48±1.05 kJ/mol, n=l and logA=14.074±0.070 for Mo(SAT), and E=78.76±3.43 kJ/mol, n=l and logA=11.055±0.016 for W(SAT) by means of Ozawa's integral curve fitting method. Results of the comparison of the dynamic thermogravimetric methods indicated that the most appropriate methods for investigation of kinetic parameters related to the thermal decomposition of metal carbonyl complexes were the integral methods, especially Ozawa's method. And it was observed that differential and difference-differential methods lead to erratic results. Keywords : Complex, thermal decomposition, kinetic parameter, thermogravimetry.
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Anahtar Kelimeler
Kimya, Chemistry
