N,N'-bis-(2-hidroksi-5-brombenzil)-2-hidroksi-1,3-diiminopropan kullanarak ekstraksiyon kromatografisi ile demir spesiasyonu
Iron speciation by extraction chromatography using N'N-bis-(2-hydroxy-5-bromobenzyl)-2-hydroxy-1,3-diiminopropane
- Tez No: 169013
- Danışmanlar: DOÇ.DR. DERYA KARA
- Tez Türü: Yüksek Lisans
- Konular: Kimya, Chemistry
- Anahtar Kelimeler: Solid phase extraction, silicagel, N'-bis(2-hydroxy-5- bromobenzyI)-2-hydroxy-l, 3-diiminopropane, iron(III), iron(II)
- Yıl: 2005
- Dil: Türkçe
- Üniversite: Balıkesir Üniversitesi
- Enstitü: Fen Bilimleri Enstitüsü
- Ana Bilim Dalı: Kimya Ana Bilim Dalı
- Bilim Dalı: Belirtilmemiş.
- Sayfa Sayısı: 85
Özet
N, N'-bis-
Özet (Çeviri)
Iron Speciation by Extraction Chromatography using N'N-bis-(2- hydroxy-5-bromobenzyI)-2-hydroxy-13-düminopropane Emre PEHLİVAN Balıkesir University, Institute of Science, Department Of Chemistry ( Master Thesis / Supervisor : Doç. Dr. Derya KARA ) Balıkesir, 2005 Metal speciation and monitoring is very important for environmental protection and control. The presence and mobility of the metal species in water systems depend on the inter-changeable physicochemical forms and reactivity of these species. Many of the analytical methods in the literature have insufficient sensitivity and hence do not have the limit of detection necessary for trace element determination in natural water and sediment samples. Therefore preconcentration methods have become very important. In this work, the new Schiff base, N,N'-bis(2-hydroxy-5-bromobenzyl)-2- hydroxy-l,3-diiminopropane, has been synthesized for the very sensitive determination of iron(III) and iron(II) in natural water samples, enabling a very selective and rapid method for iron determination to be developed. The method has also been applied to total iron determination in sediment samples. In the preconcentration system, the Schiff base reagent is mixed with the samples and chelates with the iron. These complexes are men adsorbed on the silica gel within a column system. Elution of the adsorbed chelate from the silica gel was with a small volume of a suitable eluent. In this method that can be applied for preconcentration, separation and speciation of iron, the effects of parameters such as pH, sample flow rate, eluent flow rate, foreign ions and ligand concentration have been investigated. The effect of humic acid that can produce complexes with metal ions in natural systems has also been investigated on the complexation of the Schiff base and iron(III) ions. The results obtained indicate that the method is not affected in the IVpresence of up to 10 ppm humic acid, which would be a very high concentration to be present in natural systems. Acetone containing 2,5 % nitric acid has been used as an effective eluent and the eluted iron has been measured using FAAS. The solid phase extraction method developed has been applied successfully to the determination of iron in both natural water samples and sediment samples. The LOD was found to be 0.17 mg/L when no preconcentration was used. The recovery values for spiked samples were between 100 and 104 %. The results obtained from the method developed were compared statistically with those from the 1,10 phenanthroline method, used as a standard method for iron speciation in water systems. The results of the student t-test indicated no significant difference between the two methods. In addition, this method was applied successfully to the analysis of a certified sediment sample, LGC 6156. Generally, a 10-fold preconcentration factor was required for the analysis of water samples.
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