Chromosorb-105 reçinesi ve membran filtre kullanılarak bazı eser elementlerin zenginleştirilmesi ve türlemesi
Preconcentration and speciation of some trace elements by using chromosorb-105 resin and membrane filter
Yazar: ASLIHAN KARATEPE
Danışman: PROF.DR. LATİF ELÇİ ; PROF.DR. MUSTAFA SOYLAK
Erciyes Üniversitesi / Fen Bilimleri Enstitüsü / Kimya Ana Bilim Dalı
Derece: Doktora, 2006
Konu: Kimya = Chemistry
Dizin: Talyum = Thallium

Özet:
Bu çalısmada, katı faz kolon tekniği ve membran üzerinde biriktirme ile bazı eser metaliyonlarının deristirilmesi ve türlemesi için dört ayrı yöntem gelistirildi.Kolon tekniğinde, Chromosorb-105 reçinesi kullanılarak eser Cu(II), Pb(II) ve Cd(II)iyonları hat dısı Chromosorb 105 kolununda dietilditiyofosfonik asit ile selatlarıhalinde kantitatif alıkondu ve asetonda 1 M HNO3 ile elüe edildi. Önerilen hat dısıyöntemin bağıl Standard sapması (BSS) % 1,4-4,6 ve bağıl hatası,(BH) %(-0,2)-(+5,6)aralığındadır. Zenginlestirme Faktörü (ZF) 250'dir. Yöntem su örneklerine alevli AASile kombine uygulanmıstır.Küçük bir Chromosorb-105 kolonu (4 cm x 0,5 cm) hat dısı sistemde kobaltderistirilmesi için optimize edilmistir. Co(II), NH4/NH3 ile pH 9'a tamponlanan birçözeltiden kolonda amin kompleksleri seklinde kantitatif tutulmus ve 1 mL 1 M HCl ilegeri kazanılmıstır. Yöntemin BSS % 2 ve BH'sı en fazla % -5,5'tir. ZF'ü 50 ve Co(II)için Gözlenebilme Sınırı (GS) 2,5

Abstract:
In this study, four different methods were developed for preconcentration and speciationof some trace metal ions with solid phase extraction and collection on membranetechniques.In the column technique, Cu(II), Pb(II) ve Cd(II) ions were quantitatively retained astheir diethyldithiophosphonic acid chelate forms in the Chromosorb-105 column offline, and then eluted with 1 M HNO3 in acetone. The proposed off line method has aRelative Standard Deviation (RSD) of % 1,4-4,6 and the Relative Error (RE) is in therange %(-0,2)-(+5,6). The Enrichment Factor (EF) is 250. The method was combinedwith Flame Atomic Absorbtion technique and applied to water samples.A small Chromosorb-105 column (4 cm x 0,5 cm) was optimized in an off line systemto enrich cobalt ions. Co(II) was collected in the column from a solution which wasbuffered to pH 9 with NH4/NH3 mixture as amine complexes, and then it was elutedwith 1 mL 1 M HCl. The method has a RSD of % 2 and the RE is at the most % -5,5.The EF is 50 and the Detection Limit (DL) for Co(II) is 2,5 ?g/L. The method wasapplied for the determination of cobalt in table salt and drinking water samples.When the off line column system was used for preconcentration and speciation ofthallium, Tl(III) was selectively recovered in the presence of Tl(I) ions, in the 0,5 MHCl medium. Total thallium was recovered as Tl(I) from 0,5 M NaI in 0,5 M HClsolution or as Tl(III) from 0,01 M KBrO3 in 0,5 M HCl solution. The Tl(I) amount inthe mixture was calculated by subtracting the selectively recovered Tl(III) amount fromthe total thallium amount. The EF is 50, RSD is less than % 2 and RE is in the range%(-8,2) -(+4,8). The method was applied to some soil, cement, sediment and zincsamples. Thallium amounts in the samples were determined by graphite furnace AAS.Cellulose nitrate membrane filter was used for the preconcentration of thebenzopurpurine complexes of Cu(II), Fe(III), Pb(II) and Cr(III) ions. The method wasalso applied for the determination of Fe in water. RSD was found as % 2,6 and RE as %5,7. The DL for the method is found between 1,4 - 10,5 ?g/L and the EF as 200maximum.Keywords : Chromosorb-105, thallium speciation, trace element, preconcentration,benzopurpurine, diethyldithiophosphonic acid