Kobalt(II)’nin Amberlit XAD-4/SCHD Reçinesi Kullanılarak Yeni bir Katı-Faz Ekstraksiyon Yöntemi ile Zenginleştirilmesi ve Spektrofotometrik Tayini

Bu çalışmada, çevresel su numunelerinden eser miktardaki Co(II)’nin, Amberlit XAD–4-N,N-bis(salisilidin)-siklohegzandiamin (SCHD) reçinesi kullanılarak katı faz ekstraksiyon yöntemiile ön deriştirilmesi, ayrılması ve UV-VIS spektrofotometrik yöntemle tayini için yeni bir metot önerilmiştir. Bu amaçla, Co(II) için XAD–4-SCHD reçinesi ile sorpsiyon ve elüsyon parametreleri (pH, elüent tipi ve konsantrasyonu, elüent hacmi, maksimum numune hacmi, numune akış hızı, elüent akış hızı) incelenmiştir. Box Behnken Dizayn Programı kullanılarak katı faz ekstraksiyonu ile Co(II)’nin geri kazanımı için sorpsiyon ve elüsyon bağımsız değişkenleri optimize edilmiştir. Önerilen yöntemin kalibrasyon grafiğinin 0.06–3 μgmL−1 aralığında doğrusal olduğu tespit edilmiştir (r2 = 0.9980). Önderiştirme faktörü ve gözlenebilme sınırı sırasıyla 100 ve 8.4 µgL-1’dir. Yöntemin doğruluğu, sertifikalı standart su numunesinin (NW-TMDA-70.2) analizi ile kontrol edilerek % 90’ın üzerinde geri kazanım değerleri elde edilmiştir. Ayrıca, bu çalışmada önerilen metot kullanılarak eser miktarda Co(II) içeren farklı çevresel su numunelerinden elde edilen ölçüm sonuçları, ICP-MS ölçüm sonuçları ile benzer bulunmuştur. Önerilen metot, çevresel su numunelerinde eser miktardaki Co(II)’nin tayini için başarıyla uygulanmıştır.

Anahtar Kelimeler:

Co(II), Amberlit XAD-4/SCHD reçinesi, Box-behnken dizayn, Katı-faz ekstraksiyonu, UV-VIS spektrofotometri

Preconcentration of Co(II) by a New Solid-PhaseExtraction Method using Amberlite XAD-4/SCHD Resin and Spectrophotometric Determination

The study presents a novel method for the separation/enrichmentand UV-VIS spectrophotometric determination of traceCo(II) from environmental water samples using Amberlite XAD–4 resin modified with N,N-bis(salisilidin)-siklohegzandiamin (SCHD). For this aim, sorption and elütion parameters of Co(II) (pH, eluent type and concentration, eluent volume, maximum sample volume, sample flow rate, eluent flow rate) with XAD–4-SCHD resin were investigated. Sorption and elution independent variables were optimized using Box Behnken Design (BBD) program for there covery of Co(II) by solid phase extraction. Calibration graph was linear in the range of 0.06–3 μgmL−1(r2 = 0.9980). Preconcentration factor and dedection limit of the proposed methods were100 and 8,4µgL-1, respectively. The accuracy of the method was checked by analysis of the certified standard water sample (NW-TMDA-70.2), and recovery values above 90% were obtained. In addition, using the proposed method in this study, the measurement results obtained from different environmental water samples containing trace amounts of Co(II) were found to be similar to the ICP-MS measurement results. The proposed method was successfully applied for the determination of trace amount of Co(II) in environmentalwatersamples.

Keywords:

Amberlite XAD-4/SCHD resin, Box-behnken design, Co(II), Solid phaseextraction, UV-VIS spectrophotometry,

PDF

___

Alpdoğan, G., 2016. Solid phaseextraction of Cu (II), Ni (II), Co (II) and Fe (III) ions in water samples using salicylaldehydebenzoylhydrazone on Amberlite XAD-4 and their determinations by flame atomic absorption spectrometry, Toxicological & Environmental Chemistry, 98(2), 179-188.
Baliza, P.X.,Teixeira L.S.G., ve Lemos.V. A., 2009. A procedure for determination of cobalt in water samples after dispersive liquid–liquid microextraction, Microchemical Journal, 93(2), 220-224.
Box, G.E.P., ve Behnken, D.W., 1960. Some new three level designs for the study of quantative variables, Technometrics, 2, 455–475. Camel, V., 2003. Solid phaseextraction of trace elements, Spectrochimica Acta Part B: Atomic Spectroscopy, 58(7), 1177-1233.
Citak, D., ve Tuzen, M., 2010. A novel preconcentration procedure using cloud point extraction for determination of lead, cobalt and copper in water and food samples using flame atomic absorption spectrometry, Food and Chemical Toxicology, 48(5), 1399-1404.
Ferreira, S.L.C., ve De brito, C.F., 1999. Separation and preconcentration of cobalt after sorption onto Amberlite XAD-2 loaded with 2-(2-thiazolylazo)-p-cresol, AnalyticalSciences, 15(2), 189-191.
Hejazi, L.,Mohammadi, D.E., Yamini, Y., ve Brereton, R.G., 2004. Solid-phase extraction and simultaneous spectrophotometric determination of trace amounts of Co, Ni and Cu using partial leasts quares regression, Talanta, 62(1), 183-189.
Jamali, M.R.,Soleimani, B., ve Rahnama, R., 2017. A novelseparation/preconcentration procedure using in situ sorbent formation microextraction for the determination of cobalt (II) in water and food samples by flame atomic absorption spectrometry, Arabian Journal of Chemistry, 10, 3150–3155.
Khoddami, N., ve Shemirani, F., 2016. A new magneticion-imprintedpolymer as a highly selective sorbent for determination of cobalt in biological and environmental samples, Talanta, 146, 244-252.
Lemos, V.A.,Santos, J.S., Nunes, L.S., De Carvalho, M.B., Baliza, P.X., ve Yamaki, R.T., 2003. Amberlite XAD-2 functionalized with Nitroso R salt: synthesis and application in an online system for preconcentration of cobalt, AnalyticaChimicaActa, 494(1-2), 87-95.
Lemos, V.A., Gama, E.M., ve Da Silva Lima, A. 2006. On-linepreconcentration and determination of cadmium, cobalt and nickel in food samples by flame atomic absorption spectrometry using a new functionalized resin, MicrochimicaActa, 153(3-4), 179-186.
Montgomery, D.C., 1991. Design and Analysis of Experiments, John WileySonsInc., Singapore.
Safavi, A.,Iranpoor, N., Saghir, N., ve Momeni, S., 2006. Glycerol–silica gel: a new solid sorbent for preconcentration and determination of traces of cobalt (II) ion, AnalyticaChimicaActa, 569(1), 139-144.
Sivrikaya, S.,Imamoglu, M., Yıldız, S.Z., ve Kara, D., 2016. Novel Functionalized Silica Gel for On-line Preconcentration of Cadmium (II), Copper (II) and Cobalt (II) with Determination by Flame Atomic Absorption Spectrometry, Analytical Letters, 49(7), 943-957. Soylak, M., Kaya, B. ve Tuzen, M., 2007. Copper (II)-8-hydroxquinoline coprecipitation system for preconcentration and separation of cobalt (II) and manganese (II) in real samples, Journal of Hazardous Materials,147(3). 832-837.
Soylak, M., Karatepe, A.U., Elçi, L., ve Doğan, M., 2003. Column preconcentration/separation and atomic absorption spectrometric determinations of some heavy metals in table salt samples using amberlite XAD-1180, Turkish Journal of Chemistry, 27(2), 235-242.
Teixeira Tarley, C.R., Fernandes, F.F., Luccas, P.O.,ve Segatelli, M.G., 2011. Enhanced Selectivity and Sensitivity for Flow Injection Spectrophotometric Determination of Cobalt Using Solid Phase Extraction with a 2D Ion-Imprinted Adsorbent, Analytical Letters, 44(1-3), 216-231.
Topuz, B., 2004. Potasyum 2.6-dimetilmorfolin-ditiyokarbamat sentezi ve bazı içeceklerde bakır ve kurşunun faas ile tayininde kullanılması,Yüksek lisans Tezi, Ondokuz Mayıs Üniversitesi Fen Bilimleri Enstitüsü, Samsun, 85s.
Topuz, B., ve Macit. M., 2011. Solid phase extraction and preconcentration of Cu (II), Pb (II) and Ni (II) in environmental samples on chemically modified Amberlite XAD-4 with a proper Schiffbase, Environmental Monitoring and Assessment, 173(1), 709-722.
Wang, L., Zhou, J.B., Wang, X., Wang, Z.H., ve Zhao, R.S., 2016. Simultaneous determination of copper, cobalt and mercury ions in water samples by solid-phase extraction using carbon nanotubesponges as adsorbent after chelating with sodiumdiethyldithiocarbamate prior to high performance liquid chromatography, Analytical and Bioanalytical Chemistry, 408(16), 4445-4453.