Publication: Tersane bölgesi deniz suyunda ağır metallerin eser analizi için yöntem geliştirilmesi
Abstract
TERSANE BÖLGESİ DENİZ SUYUNDA AĞIR METALLERİN ESER ANALİZİ İÇİN YÖNTEM GELİŞTİRİLMESİ Bu çalışma; tersane bölgesi deniz suyunda bulunan ağır metal iyonlarının miktarının tayini için bir önderiştirme yöntemi geliştirilmesi amacıyla yapılmıştır. Çalışmada ağır metal iyonlarının tayini için alevli atomik absorpsiyon spektroskopisi yöntemi kullanılmıştır. Ancak deniz suyunda bulunan ağır metal iyonlarını, düşük konsantrasyonda bulunmaları ve matris bileşenlerinin bozucu etkileri nedeniyle sadece AAS ile doğrudan tayin etmek oldukça zordur. Bu nedenle AAS yanında bir ayırma ve deriştirme tekniğinin kullanılması gerekmektedir. Bu amaçla geliştirilen yöntemde, katı faz ekstraksiyon yönteminin kullanılması tercih edilmiştir. Çalışmada, 3-fenil-1-(2-piridil)tiyoüre ligandı sentezlenerek Cu(II), Ni(II), Cd(II), Pb(II) ve Fe(II) iyonlarının ön deriştirilmesi için yeni bir katı faz ekstraksiyon yöntemi geliştirilmiştir. Sentezlenen adsorban üzerinde detaylı karakterizasyon çalışmaları FTIR, NMR, MS-MS ve elementel analiz teknikleri kullanılarak yapılmıştır. En iyi geri alma çözeltileri sırasıyla; 0,1M EDTA Cu(II), 0,5M EDTA (Ni(II), Cd(II)) ve 0,01M EDTA (Pb(II), Fe(II)) olarak belirlenmiştir. Çalışma süresince pH, çalkalama süresi, adsorban miktarı ve yabancı iyon etkisi incelenmiş olup optimum koşullar belirlenmiştir. Optimum koşullar altında tüm metaller için geri kazanım verimi % 95 güven seviyesinde ≥% 98 den büyük olarak elde edilmiştir. İncelenen iyonlar için derişiklendirme sonrası gözlenebilme sınırları Cu(II), Ni(II), Cd(II), Pb(II) ve Fe(II) iyonları için sırasıyla; 0,13 µgL-1, 0,79 µgL-1, 0,33 µgL-1, 0,79 µgL-1 ve 0,51 µgL-1 olarak bulunmuştur. Önerilen yöntemin bağıl standart sapma değerleri, tüm iyonlar için ≤ % 5 olmuştur. Geliştirilen yöntem, tersane bölgelerinden alınan deniz suyu ve musluk suyu örnekleri üzerine uygulanmış ve başarılı sonuçlar elde edilmiştir.
THE DEVELOPMENT OF A METHOD FOR TRACE ANALYSIS OF HEAVY METALS IN THE SEA WATER OF SHIPYARD REGIONS This study was conducted in order to develop a preconcentration method for determining the quantities of heavy metal ions that sea water of shipyard regions contain. In the present study, the Flame Atomic Absorption Spectrometer (AAS) method was employed to determine heavy metal ions. However, it is quite difficult to determine heavy metal ions via AAS alone due to their low concentration levels and the distortionary effects of matrices. Thus, it is necessary to use separation and concentration methods as well as AAS. The Solid Phase Extraction (SPE) technique was preferred for the method developed for this purpose. By synthesizing 3-phenyl-1(2-pyridyl)thiourea ligand, a new solid phase extraction method was developed for preconcentration of Cu(II), Ni(II), Cd(II), Pb(II) and Fe(II) ions. Detailed characterizations studies on synthesized adsorbent were made using FTIR, NMR, MS-MS and Elemental Analysis methods. The best recovery solutions were found to be 0.1M EDTA Cu(II), 0.5M EDTA (Ni(II), Cd(II)) and 0.01M EDTA (Pb(II), Fe(II)) respectively. pH, stirring period, adsorbent quantity and foreign ion effect were analyzed during the study and optimum conditions were defined. Under optimum conditions, recovery efficiency for all metals was found as ≥% 98 with a reliability level of % 95. Detection limit of the post-concentration period for analyzed ions were found as 0.13 µgL-1, 0.79 µgL-1, 0.33 µgL-1, 0.79 µgL-1 and 0.51 µgL-1 for Cu(II), Ni(II), Cd(II), Pb(II) and Fe(II) ions respectively. Relative standard deviation values of the proposed method turned out to be ≤% 5 for all ions. The developed method was implemented on samples of sea waters obtained from shipyard regions and tap waters. The application yielded rather successful results.
THE DEVELOPMENT OF A METHOD FOR TRACE ANALYSIS OF HEAVY METALS IN THE SEA WATER OF SHIPYARD REGIONS This study was conducted in order to develop a preconcentration method for determining the quantities of heavy metal ions that sea water of shipyard regions contain. In the present study, the Flame Atomic Absorption Spectrometer (AAS) method was employed to determine heavy metal ions. However, it is quite difficult to determine heavy metal ions via AAS alone due to their low concentration levels and the distortionary effects of matrices. Thus, it is necessary to use separation and concentration methods as well as AAS. The Solid Phase Extraction (SPE) technique was preferred for the method developed for this purpose. By synthesizing 3-phenyl-1(2-pyridyl)thiourea ligand, a new solid phase extraction method was developed for preconcentration of Cu(II), Ni(II), Cd(II), Pb(II) and Fe(II) ions. Detailed characterizations studies on synthesized adsorbent were made using FTIR, NMR, MS-MS and Elemental Analysis methods. The best recovery solutions were found to be 0.1M EDTA Cu(II), 0.5M EDTA (Ni(II), Cd(II)) and 0.01M EDTA (Pb(II), Fe(II)) respectively. pH, stirring period, adsorbent quantity and foreign ion effect were analyzed during the study and optimum conditions were defined. Under optimum conditions, recovery efficiency for all metals was found as ≥% 98 with a reliability level of % 95. Detection limit of the post-concentration period for analyzed ions were found as 0.13 µgL-1, 0.79 µgL-1, 0.33 µgL-1, 0.79 µgL-1 and 0.51 µgL-1 for Cu(II), Ni(II), Cd(II), Pb(II) and Fe(II) ions respectively. Relative standard deviation values of the proposed method turned out to be ≤% 5 for all ions. The developed method was implemented on samples of sea waters obtained from shipyard regions and tap waters. The application yielded rather successful results.