Ultrasonik destekli bulutlanma noktası ektraksiyonu (UA-CPE) ile ayırma ve zenginleştirme sonrası alevli atomik absorpsiyon spektrometresi (FAAS) ile gıdalarda molibden ve vanadyumun eşanlı belirlenme olanaklarının araştırılması
Küçük Resim Yok
Tarih
2019
Yazarlar
Dergi Başlığı
Dergi ISSN
Cilt Başlığı
Yayıncı
Sivas Cumhuriyet Üniversitesi
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Gıda, süt ve sebze örneklerinde molibden ve vanadyumun alevli atomik absorpsiyon spektrometresiyle (FAAS) tayini öncesi yeni ultrasonik destekli-bulutlanma noktası ekstraksiyon yöntemi (UA-CPE) geliştirildi. Yöntem, pH 4.5'te molibden ve vanadyumun kararlı anyonik oksalat komplekslerinin [9-(diethylamino)benzo[a]phenoxazin-5-ylidene]azanium; sulfate (Nile blue A) ile hidrofobik iyon-çifti kompleksler oluşturması, ardından oluşan iyon-çifti komplekslerin polyoxyethylene(7.5)nonylphenyl ether (PONPE 7.5)'in misel fazına ekstrakte edilmesi temeline dayanır. UA-CPE, geleneksel CPE ile karşılaştırıldığında büyük oranda basitleştirilmiş ve hızlandırılmıştır. Ultrasonik etki altında yöntemin analitik parametrelerini etkileyebilecek değişkenler (pH, oksalat ve Nile blue derişimi, PONPE 7.5 derişimi, elektrolit derişimi, örnek hacmi, sıcaklık ve ultrasonik güç gibi) optimize edildi. Optimum koşullar altında, molibden ve vanadyum için değerlendirilen analitik parametreler sırasıyla, doğrusal çalışma aralığı, (Mo: 3-340 µg L-1 ve V: 5–250 µg L-1), duyarlık iyileştirme faktörü (Mo:145 ve V:115), gözlenebilme sınırı (Mo: 0.86 µg L-1 ve V:1.55 µg L-1), % bağıl standart sapma (Mo: %2.7 ve V: %3.5) ve % geri kazanım (Mo: %95.7–102.3 ve % 96.3–101.8) idi. Yöntemin doğruluğu iki standart referans materyalin (SRM) analizi ve standart eklenmiş örneklerden geri kazanım çalışması ile test edildi. Geliştirilen yöntem daha sonra seçilen örneklerde bulunabilecek eser düzeylerde molibden ve vanadyumun tayinine memnuniyet verici sonuçlarla başarılı bir şekilde uygulandı.
A new ultrasonic assisted-cloud point extraction procedure (UA-CPE) was developed for preconcentration at the trace levels of vanadium (V) and molybdenum (Mo) in milk, vegetables and foodstuffs prior to determination via flame atomic absorption spectrometry (FAAS). The method is based on the ion-association of stable anionic oxalate complexes of V(V) and Mo(VI) with [9-(diethylamino)benzo[a]phenoxazin-5-ylidene]azanium; sulfate (Nile blue A) at pH 4.5, and then extraction of the formed ion-association complexes into micellar phase of polyoxyethylene(7.5)nonylphenyl ether (PONPE 7.5). The UA-CPE is greatly simplified and accelerated compared to traditional cloud point extraction (CPE). The analytical parameters (solution pH, the concentrations of complexing reagents oxalate and Nile blue A, the PONPE 7.5 concentration, electrolyte concentration, sample volume, temperature and ultrasonic power). Of the method under the ultrasonication effect were optimized optimum conditions, the calibration curves for Mo(VI) and V(V) are obtained in the concentration range of 3–340 µg L?1 and 5–250 µg L?1 with high sensitivity enhancement factors (EFs) of 145 and 115, respectively. The limits of detection (LODs) for Mo(VI) and V(V) are 0.86 and 1.55 µg L?1, respectively. The proposed method demonstrated good performances such as relative standard deviations (as RSD %) (?3.5%) and spiked recoveries (95.7–102.3%). The accuracy of the method was assessed by analysis of two standard reference materials (SRMs) and recoveries of the spiked solutions. The method was successfully applied to the food samples for the determination of trace amounts of Mo(VI) and V(V) with the satısfactory results.
A new ultrasonic assisted-cloud point extraction procedure (UA-CPE) was developed for preconcentration at the trace levels of vanadium (V) and molybdenum (Mo) in milk, vegetables and foodstuffs prior to determination via flame atomic absorption spectrometry (FAAS). The method is based on the ion-association of stable anionic oxalate complexes of V(V) and Mo(VI) with [9-(diethylamino)benzo[a]phenoxazin-5-ylidene]azanium; sulfate (Nile blue A) at pH 4.5, and then extraction of the formed ion-association complexes into micellar phase of polyoxyethylene(7.5)nonylphenyl ether (PONPE 7.5). The UA-CPE is greatly simplified and accelerated compared to traditional cloud point extraction (CPE). The analytical parameters (solution pH, the concentrations of complexing reagents oxalate and Nile blue A, the PONPE 7.5 concentration, electrolyte concentration, sample volume, temperature and ultrasonic power). Of the method under the ultrasonication effect were optimized optimum conditions, the calibration curves for Mo(VI) and V(V) are obtained in the concentration range of 3–340 µg L?1 and 5–250 µg L?1 with high sensitivity enhancement factors (EFs) of 145 and 115, respectively. The limits of detection (LODs) for Mo(VI) and V(V) are 0.86 and 1.55 µg L?1, respectively. The proposed method demonstrated good performances such as relative standard deviations (as RSD %) (?3.5%) and spiked recoveries (95.7–102.3%). The accuracy of the method was assessed by analysis of two standard reference materials (SRMs) and recoveries of the spiked solutions. The method was successfully applied to the food samples for the determination of trace amounts of Mo(VI) and V(V) with the satısfactory results.
Açıklama
Fen Bilimleri Enstitüsü, Kimya Ana Bilim Dalı, Kimya Bilim Dalı
Anahtar Kelimeler
Kimya, Chemistry