Çok Değişkenli Kalibrasyon Teknikleri Kullanılarak Demir, Kobalt ve Nikelin Birlikte Spektrofotometrik Tayini

Abstract

Bu çalışmada, çok değişkenli kalibrasyon teknikleri kullanılarak demir kobalt ve nikel tayininde, spektrofotometrik olarak elde edilen veriler kemometrik yöntemler ile hesaplanmıştır. 5-seviyeli tasarıma göre Fe(III), Co(II), Ni(II) metalleri ile 0; 0.1; 0.2; 0.3; 0.4 mg/L seviyelerinde training set (kalibrasyon çözeltileri) hazırlanmıştır. Metal katyonlarının kompleksleştirilmesinde ligand olarak [4-(2-Piridilazo) rezorsinol] (PAR) reaktifi kullanılmıştır. pH, sıcaklık, kompleksleşme süresi, kompleks stokiyometrisi, alt tayin sınırı ve yabancı türlerin bozucu etkileri gibi deneysel parametreler araştırılmış ve optimum koşullar belirlenmiştir. Absorpsiyon spektrumları, Ultraviyole-Görünür bölge (UV-GB) spektrofotometresi ile alınmış ve sonuçlar klasik en küçük kareler (CLS), temel bileşen regresyonu (PCR) ve kısmi en küçük kareler (PLS1) teknikleri ile hesaplanmıştır. Bu tekniklerden PRESS (prediction error sum of squares) değerleri hesaplanarak en uygun yöntem olarak PCR yöntemi seçilmiştir. Cross validasyon (çapraz validasyon) işlemine göre training set içerisindeki her bir çözelti numune kabul edilerek hesaplamalar yapılmış ve % geri kazanımlar Fe(III) için 97,16±2,98, Co(II) için 98,78±3,24 ve Ni(II) için 101,89±2,98 olarak hesaplanmıştır.

Keywords

• çok değişkenli kalibrasyon
• UV-Görünür Bölge Spektroskopisi
• PAR
• Demir
• Kobalt
• Nikel

Simultaneously Spectrophotometric Determination of Iron, Cobalt and Nickel by Using Multivariate Calibration Techniques

Abstract

In this study, for the simultaneously determination of iron, cobalt and nickel, the data obtained spectrophotometrically using multivariate techniques were calculated by the chemometric methods. According to the 5-level design, training set (calibration solutions) were prepared at 0; 0.1; 0.2; 0.3; 0.4 mg/L levels for Fe(III), Co(II), Ni(II) ions. For the complexation of metal cations [4-(2-Pyridylazo) resorcinol] (PAR) reagent was used as ligand. Experimental parameters such as pH, temperature, complexation time, stoichiometry of the complex, limit of detection and effects of interfering species were investigated and optimum conditions were determined. Absorption spectra were obtained by Ultraviolet-Visible (UV-VIS) spectrophotometer and results were calculated by classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS1) techniques. Among these techniques, PRESS (prediction error sum of squares) values were calculated and decided that the most suitable method was PCR. According to the cross validation process, each solution in the training set was accepted as a sample and calculations were made and the % recoveries were found to be as 97.16±2.98, 98.78±3.24 and 101.89±2.98 for Fe(III), Co(II) and Ni(II), respectively.

Keywords

• multivariate calibration
• UV-VIS Spectroscopy
• PAR
• Iron
• Cobalt
• Nickel

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