C18-silika dolgulu mini kolon kullanılarak doğal sulardan Bakır(II) ve Demir(III) iyonlarının önderiştirilmesi ve alevli AAS ile tayini

Bu çalışmada, doğal su örneklerinden bakır(II) ve demir(III) iyonlarının aynı anda önderiştirilmesi için yeni bir katı faz ekstraksiyon yöntemi geliştirilmiştir. Analitler 4-aminoantipirin ile pH 8.0’de kompleksleştirilmiş ve C18-silika ile paketlenmiş mini kolondan geçirilmiştir. Kolonda alıkonunan analitler %10 etanolde hazırlanmış 1 mL 0,5 M nitrik asit çözeltisi ile elüe edilmiş ve alevli atomik absorpsiyon spektrometresi ile tayin edilmiştir. Örnek pH’sı, ligand miktarı, elüent türü, örnek ve elüent akış hızları ve örnek hacmi gibi çeşitli değişkenlerin analitlerin alıkonması veya elüsyonu üzerine etkisi incelenmiş ve optimize edilmiştir. Ayrıca analitlerin C18-silika kolonunda alıkonmasına bazı yabancı iyonların etkileri incelenmiştir. Gözlenebilme sınırları 20 kat önderiştirme faktörü ile Cu için 0,89 µg/L ve Fe için 1,41 µg/L olarak belirlenmiştir. Kalibrasyon grafikleri 5,0-125 µg/L bakır(II) ve demir(III) derişimi aralığında doğrusaldır. Kalibrasyon eşitlikleri Cu için A=2,36x10-3 C + 4,55x10-4 ve Fe için A=1,45x10-3 C + 8,88x10-4 olarak belirlenmiştir. Önerilen yöntemin doğruluğu sertifikalı referans su örneğinin (SPSSW2 Batch 127) analizi ile doğrulanmıştır. Geliştirilen yöntem nehir suyu ve deniz suyu örneklerine % 95- 99 arasındaki geri kazanım değerleri ile başarılı bir şekilde uygulanmıştır.

Preconcentration of Copper(II) and Iron(III) from natural waters using a C18-silica packed mini-column and their determination by FAAS

In the present study, a new solid phase extraction method was developed for simultaneous preconcentrationof copper(II) and iron(III) ions from natural waters. The analytes were first complexed with 4-aminoantipyrine at pH 8.0 and then passed through the column packed with C18-silica. The retainedanalytes on the C18-silica were eluted with 1.0 mL of 0.5 M nitric acid in 10% ethanol and determinedusing flame atomic absorption spectrometer. The influence of several variables such as sample pH, ligandamount, eluent type, sample and eluent flow rates, and sample volume on the retention/or elution of theanalytes were examined and optimized. The effects of some interfering ions on the retentions of analyteson C18-silica were also enquired. The detection limits were 0.89 µg/L for Cu and 1.41 µg/L for Fe with apreconcentration factor of 20. The calibration graphs were linear in the concentration range of 5.0-125 µg/Lof the analytes. The calibration equations were A=2.36x10-3 C + 4.55x10-4 for Cu and A=1.45x10-3 C +8.88x10-4 for Fe. The accuracy of the proposed method was verified by the analysis of SPS-SW2 Batch 127certified reference water. The method was applied to river water and seawater samples with recoveries inthe range of 95-99%.

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