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
- Tez No: 177689
- Danışmanlar: PROF.DR. LATİF ELÇİ, PROF.DR. MUSTAFA SOYLAK
- Tez Türü: Doktora
- Konular: Kimya, Chemistry
- Anahtar Kelimeler: Belirtilmemiş.
- Yıl: 2006
- Dil: Türkçe
- Üniversite: Erciyes Üniversitesi
- Enstitü: Fen Bilimleri Enstitüsü
- Ana Bilim Dalı: Kimya Ana Bilim Dalı
- Bilim Dalı: Belirtilmemiş.
- Sayfa Sayısı: 180
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
Özet (Çeviri)
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
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