İmmobilize hümik asitlerin katı faz ekstraksiyon sistemlerinde kullanımı
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2006-12-22
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Selçuk Üniversitesi Fen Bilimleri Enstitüsü
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info:eu-repo/semantics/openAccess
Abstract
Doğal olarak oluşmuş, çok çeşitli fonksiyonel gruplara sahip hümik asitlerin, sulu ortamlarda metal iyonlarını tutabilme ve düşük pH`larda bırakabilme özelliği, metal iyonlarının uzaklaştırılması, geri kazanılması ve zenginleştirilmesi için çok uygun bir yöntem olan katı faz ektraksiyonu (SPE) sistemlerinde etkin bir madde olarak kullanılabilmesini sağlamıştır. Hümik asitlerin pH>3 olan sulu çözeltilerde az veya çok çözünmesi, bu maddelerin doğrudan adsorban olarak kullanılmalarını kısıtlamakta ve bu maddeler ancak çözünürsüzleştirme ve immobilizasyon gibi çeşitli işlemlerden geçirildikten sonra iyon değiştirici/adsorban madde olarak SPE sistemlerinde kullanılabilmektedir. Sunulan bu çalışmada; aminopropil silika (APS) üzerine immobilizasyonu yapılan ve pH 10`a kadar çözünme kararlılığı sağlanan hümik asit sabit faz olarak kullanılmış ve Cu, Ni, Co iyonlarının tutulma özelliklerine besleme çözeltisinin pH`sının ve konsantrasyonunun etkisi incelenmiştir. Deneylerde Cu tuzlarının tutulma etkilerini incelemek için Cu(NO3)2, Cu(CH3COO)2 ve CuNa2Y tuzları kullanılmıştır. Cu(II), Ni(II) ve Co(II) iyonlarının SPE işlemleri ImNaA ile doldurulmuş bir kolonda yürütülmüş ve sürekli sistemden elde edilen ?breakthrough eğrileri? ile işlemler takip edilmiştir. Cu(II), Ni(II) ve Co(II) iyonlarının her üçü için de, besleme çözeltisinin konsantrasyonu ve pH'sı attıkça, ImNaA tarafından tutulan miktarlarında da bir artış gözlenmiştir. Cu(II) ve Ni(II) iyonları Langmuir, Co (II)iyonlarının ise hem Freundlich hemde Langmuir izotermlerine uyan tutulma davranışı sergilediği gözlenmiştir. Sorpsiyonun mekanizmasını incelemek için Dubinin-Radushkevich adsorpsiyon izotermleri çıkarılmış ve ortalama adsorpsiyon enerjisi Cu(II), Ni(II) ve Co(II) iyonlarının için sırasıyla; 17,68kJ/mol, 26,73 kJ/mol ve 40,82 kJ/mol olarak hesaplanmıştır. Scatchard eğri analizleri ile izotermlerin uygunluluğu irdelenmiştir. Scatchard eğri analizinden iki doğru elde edilmiştir. Bu doğrulardan yüksek ve düşük enerjili etkileşimlerle tutunmanın gerçekleştiği görülmüştür. Adsorpsiyon izotermlerinden, Cu(II) ve Ni(II)'nin ağırlıklı olarak kimyasal etkileşmelerle ve Co(II)'nin ise hem fiziksel hemde kimyasal etkileşmeler ile tutulduğu sonucuna varılmıştır. SPE işlemlerinin sürekli olarak gözlenmesi için HPLC sistemi kullanılmıştır. Sonuç olarak; SPE işlemlerinde sabit faz olarak ImNaA'nın verimli olduğu ve kromatografik analizlerde sabit faz olarak kullanılabilirliğinin uygun olduğu görülmüştür.
Which naturally occurres, that humic acids have different functional groups, in watery mediums sorption of metal ions and desorption of low pH properties,a method to suit in solid phase extraction (SPE) systems ensure for remove, recover and enrich of metal ions a effective as substence availability. n SPE systems are availability, of humic acids pH>3 high or low solubility in water solutions, to restrict of this substances as direct adsorbent used and however this substances after different operations like the insolubilization and the immobilization that as the ion exchange/adsorbent matter. In the present study, investigated as solid phase the immobilized of humic acid on the amino prophylsilica used and of Cu, Ni, Co ions sorption properties of the pH and the concentration of the feeding sollution. n experiments, for properties of sorption effect of Cu ions used Cu(NO3)2, Cu(CH3COO)2 and CuNa2Y salts. The SPE steps were carried out for Cu(II), Ni(II) and Co(II) in a column filled with ImNaA and each step was monitored by breakthrough curves, which obtained by joined to the outlet end of the column. It was found that by increasing concentration and pH of the loading solution, there was an increment in the amount of the metal ions sorbed by ImNaA. It was observed that sorption behaviors of metal ions were fitted to the Langmuir and the both Langmuir and Freundlich isotherms on the large scale for Cu(II), Ni(II) and Co(II) respectively. To evaluate the sorption mechanism Dubinin-Radushkevich adsorption isotherms were got and average adsorption energies for Cu(II), Ni(II) and Co(II) were calculated as 17,68 kJ/mol, 26,73 kJ/mol and 40,82 kJ/mol, respectively. Appropriateness of the isotherms were examined by Scatchard Plot Analysis. To obtain two correct by Scatchard Plot Analysis. From this corrects has been seen low and high energy sorptions. From the adsorption isotherms it was concluded that Cu(II), Ni(II) were sorbed via chemical interactions and Co(II) was sorbed via ,both phisycal and chemical interactions, on the large scale. It was concluded that ImNaA was effective as a stationary phase for SPE processes and it is correspond its efficiency as a stationary phase for chromotographyc analysis.
Which naturally occurres, that humic acids have different functional groups, in watery mediums sorption of metal ions and desorption of low pH properties,a method to suit in solid phase extraction (SPE) systems ensure for remove, recover and enrich of metal ions a effective as substence availability. n SPE systems are availability, of humic acids pH>3 high or low solubility in water solutions, to restrict of this substances as direct adsorbent used and however this substances after different operations like the insolubilization and the immobilization that as the ion exchange/adsorbent matter. In the present study, investigated as solid phase the immobilized of humic acid on the amino prophylsilica used and of Cu, Ni, Co ions sorption properties of the pH and the concentration of the feeding sollution. n experiments, for properties of sorption effect of Cu ions used Cu(NO3)2, Cu(CH3COO)2 and CuNa2Y salts. The SPE steps were carried out for Cu(II), Ni(II) and Co(II) in a column filled with ImNaA and each step was monitored by breakthrough curves, which obtained by joined to the outlet end of the column. It was found that by increasing concentration and pH of the loading solution, there was an increment in the amount of the metal ions sorbed by ImNaA. It was observed that sorption behaviors of metal ions were fitted to the Langmuir and the both Langmuir and Freundlich isotherms on the large scale for Cu(II), Ni(II) and Co(II) respectively. To evaluate the sorption mechanism Dubinin-Radushkevich adsorption isotherms were got and average adsorption energies for Cu(II), Ni(II) and Co(II) were calculated as 17,68 kJ/mol, 26,73 kJ/mol and 40,82 kJ/mol, respectively. Appropriateness of the isotherms were examined by Scatchard Plot Analysis. To obtain two correct by Scatchard Plot Analysis. From this corrects has been seen low and high energy sorptions. From the adsorption isotherms it was concluded that Cu(II), Ni(II) were sorbed via chemical interactions and Co(II) was sorbed via ,both phisycal and chemical interactions, on the large scale. It was concluded that ImNaA was effective as a stationary phase for SPE processes and it is correspond its efficiency as a stationary phase for chromotographyc analysis.
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İmmobilize hümik asit, Katı faz ekstraksiyonu, Immobilized humic acid, Solid phase extraction, Breakthrough eğrileri, Breakthrough curves, İyon değişimi, Ion exchange, Adsorpsiyon, Adsorption, Langmuir adorpsiyon izotermi, Freundlich adorpsiyon izotermi, Dubinin-Radushkevich adorpsiyon izotermi, Scatchard eğri analizi, Langmuir adsorption isotherm, Freundlich adsorption isotherm, Dubinin-Radushkevich adsorption isotherm, Scatchard plot analysis
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Topkafa, M. (2006). İmmobilize hümik asitlerin katı faz ekstraksiyon sistemlerinde kullanımı. Selçuk Üniversitesi, Yayımlanmış yüksek lisans tezi, Konya.
