Preconcentrations of Cd(II) and Cu(II) by solid phase extraction on thermophilic Bacillus firmus loaded Amberlite XAD-4 prior to their determinationsin food samples by ICP-OES

Year 2016, Volume: 21 Issue: 2, 152 - 166, 30.12.2016

Sadin Özdemir

Abstract

 

Abstract: It is well known that sensitivity of ICP-OES is not enough when ultra trace levels are concerned. From this perspective a new method was developed for the determinations of Cd(II) and Cu(II). It was based on the use of thermophilic Bacillus firmus loaded Amberlite XAD-4 as a biosorbent for solid phase extraction. The optimum pH, flow rate, eluent concentration and volume, amount of biomass and amount of Amberlit XAD-4 were found as 5.5, 3 mL min^-1, 5 mL of 1 mol L^-1 of HCl, 250 mg of biomass and 750 mg of Amberlite XAD-4, respectively for recovery of tested metal ions. Preconcentration factor was achieved as 35 for Cd and 50 for Cu. Resuability of the column were tested and same column could be used for 35 cycle. LODs were calculated as 0.09 and 0.08 ng mL^-1, respectively for Cd and Cu. RSDs were found as lower than 5.9%. The developed method was successfully applied to food samples to determine analyte concentrations.

 

Özet: Eser elemenler söz konusu olduğunda ICP-OES'in hassasiyetinin yeterli olmadığı iyi bilinmektedir. Bu bakımdan Cd(II) ve Cu(II)'nin belirlenmesi için yeni bir metod geliştirilmiştir. Amberlit XAD-4 üzerine tutturulmuş termofilik Bacillus firmus temel baz alınarak katı faz ekstraksiyon için biyosorbent olarak kullanılmıştır. Test edilen metal iyonlarının geri kazanımı için optimum pH, akış hızı, eluent konsantrasyonu ve hacmi, biyokütle miktarı ve Amberlit XAD-4 miktarı sırasıyla; 5.5, 3 ml dk^-1, 1 mol L^-1 5 mL HCl, 250 mg ve 750 mg olarak tespit edildi. Prekonsantrasyon faktörü Cd için 35 ve Cu için 50 olarak elde edildi. Kolonun geri kullanımı test edildi ve aynı kolon 35 defa kullanılabilir. LODs Cd ve Cu için sırasıyla  0.09 and 0.08 ng mL^-1 olarak hesaplandı. RSDs'nin %5.9'dan daha düşük olarak bulundu. Geliştirlen yöntem gıda örneklerindeki analit konsantrasyonlarının belirlenmesi için başarılı bir şekilde uygulandı.

 

Preconcentrations of Cd(II) And Cu(II) by Solid Phase Extraction on Thermophilic Bacillus firmus Loaded Amberlite XAD-4 Prior to Their Determinationsin Food Samples by ICP-OES

Abstract

It is well known that sensitivity of ICP-OES is not enough when ultra trace levels are concerned. From this perspective a new method was developed for the determinations of Cd(II) and Cu(II). It was based on the use of thermophilic Bacillus firmus loaded Amberlite XAD-4 as a biosorbent for solid phase extraction. The optimum pH, flow rate, eluent concentration and volume, amount of biomass and amount of Amberlit XAD-4 were found as 5.5, 3 mL min^-1, 5 mL 1 mol L^-1 of HCl, 250 mg of biomass and 750 mg of Amberlite XAD-4, respectively for recovery of tested metal ions. Preconcentration factor was achieved as 35 for Cd(II) and 50 for Cu(II). Resuability of the column were tested and same column could be used for 35 cycle. LODs were calculated as 0.09 and 0.08 ng mL^-1, respectively for Cd(II) and Cu(II). RSDs were found as lower than 5.9%. The developed method was successfully applied to food samples to determine analyte concentrations.

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