Orijinal Yağ Matriksinde Hızlı Nikel Tayini için UV-Vis Spektrofotometrik Metot Geliştirilmesi

Bu çalışmada, yenilebilir yağlarda nikel tayini için yeni bir metot sunulmuştur. Önerilen prosedür, N, N’-bis(4-metoksisalisiliden) etilendiamin ve nikelin yağ ortamında kompleksleşmesi ve 396 nm’de UV-görünür bölgede spektrofotometrik tayinine dayanmaktadır. Kompleks oluşumu 20 saniyede tamamlanmaktadır. n-Hekzan ve aseton karışımı (1:4, h/h) çözücü olarak kullanılmış ve kompleksin molar absorpsiyon katsayısı 6540 L mol-1 cm-1 olarak hesaplanmıştır. Tayin ve gözlenebilme sınırları sırasıyla 0,24 ve 0,82 µg g-1 olarak bulunmuştır. Kalibrasyon grafiği 0,25-1,50 mg L-1 nikel derişimi aralığında doğrusaldır ve korelasyon katsayısı 0,9995’dir. Önerilen yöntemin gerçekliği organometalik nikel standardı kullanılarak test edilmiş; % geri kazanım ve % bağıl standart sapma değerleri sırasıyla % 97,0 ve % 3,8 olarak bulunmuştur. Ayrıca, geliştirilen yöntem nikel katılmış gerçek örneklerde de başarıyla uygulanmış ve % geri kazanım değerleri %90,0 -104,0 aralığında bulunmuştur.

Development of UV-Vis Spectrophotometric Method for Rapid Nickel Determination in Original Oil Matrix

A novel method for the determination of nickel in edible oils was proposed. The suggested procedure was on the basis of complexation of N, N’- bis(4-methoxysalicylidene) ethylenediamine and nickel in oily media and UVVisible spectrophotometric determination at 396 nm. The complex formation was completed within 20 seconds. The mixture of n-hexane and acetone (1:4, v/v) was used as solvent and the molar absorptivity of the complex was calculated as 6540 L mol-1 cm-1. The limits of detection and quantification were 0.24 and 0.82 µg g-1, respectively. The calibration graph was linear between 0.25-1.50 mg L-1 nickel concentration with 0.9995 correlation coefficient. The reliability of the suggested method was tested by analysis of organometallic nickel standard and the recovery and relative standard deviation were found as 97.0 % and 3.8 %, respectively. Furthermore, the developed method was successfully applied on nickel spiked real samples and recovery values were between 90.0 - 104.0 %.

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