Bir akışkan sisteme enjeksiyon tekniği ile voltametrik tayinler
Küçük Resim Yok
Tarih
1990
Yazarlar
Dergi Başlığı
Dergi ISSN
Cilt Başlığı
Yayıncı
Ege Üniversitesi
Erişim Hakkı
info:eu-repo/semantics/closedAccess
Özet
83 O Z E T Endüstriyel kontrol, çevre kirliliği ve klinik kimya gibi bazı alanlarda, aynı yada farklı örneklerdeki birçok parametrenin hızlı ölçümünün gerekmesi, otomatikleştiril- miş sürekli analiz yöntemlerinin gelişmesini zorlamakta dır. Akışkan sistemde gerçekleştirilen sürekli analizle rin bir türü olan enjeksiyon tekniği (Fi A) ile ilgili çalışmaların son yıllarda büyük bir gelişme göstermesine karşın yöntemin ticari yönü henüz sınırlıdır. Bu nedenle, bu çalışmada tek yollu bir FIA sistemi kurulmuştur. Volta- metrik detektör olarak döner platin tel, doygun kalomel ve platin elektroddan oluşan üç elektrodlu yeni bir flow-cell tasarlanmış ve bu sistemde akış hızı, enjeksiyon hacmi ve kolon uzunluğunun sinyallere etkisi incelenmiştir.Elektro- aktif tür olarak doğrudan ve dolaylı ölçmeyi birlikte sağ layan adrenalin ve periyodat seçilerek bunların duyar ana lizleri en uygun akış ve taşıyıcı çözelti koşullarında gerçekleştirilmiştir. Korelasyon katsayısı en az 0.998 olan kalibrasyon doğrularından (i = f (C)) adrenalin ve periyodat sırasıyla -7 -6 5.0x10 M ve 5.0x10 M düzeyine kadar tayin edilebil miştir. Sonuçlar, aynı elektrod sistemiyle statik koşullar da yapılan çalışmalarda bulunanlarla karşılaştırılmıştır. Elektrodun dönmesinden kaynaklanan konveksiyon etkisinin duyarlığı arttırdığı, çözelti akışının ise hem duyarlığı hemde örnekleme frekansını! 50-60 enjeksiyon/saat ) arttır dığı saptanmıştır
84 SUMMARY The requirement of the fast measurement of many parameters in the same and different samples in the fields such as industrial control, environmental pollution and clinical chemistry has urged the development of automated continuous analysis methods. Although research on flow injection analysis (FIA), which is the type of continuous flow analysis, has undergone great development in recent years, commercialisation of the method is still limited. For this reason, a FIA system with a sigle-line was constructed in this study. A new flow-cell having three electrodes -rotating platinum wire, saturated calomel and platinum -was designed as a voltammetric detector and the effects of flow rate, injection volume and column length on the signals were studied. Adrenaline and periodate were selected as electroactive species which allow direct and indirect determinations and sensitive analysis of them were made at optimum flow and carrier solution conditions. From the calibration lines of current versus concentration with a correlation coefficient of at least 0.998, adrenaline and periodate were determined at the detection -7 -6 limited of 5.0x10 M and 5.0x10 M respectively. The results were compared with the results of the experiments using the same electrodes in static conditions. It was observed that the convection created by the rotation electrode increased the sensitivity and the flow of the solution increased both sensitivity and the frequency of injection (50-60 samplcs/hr).
84 SUMMARY The requirement of the fast measurement of many parameters in the same and different samples in the fields such as industrial control, environmental pollution and clinical chemistry has urged the development of automated continuous analysis methods. Although research on flow injection analysis (FIA), which is the type of continuous flow analysis, has undergone great development in recent years, commercialisation of the method is still limited. For this reason, a FIA system with a sigle-line was constructed in this study. A new flow-cell having three electrodes -rotating platinum wire, saturated calomel and platinum -was designed as a voltammetric detector and the effects of flow rate, injection volume and column length on the signals were studied. Adrenaline and periodate were selected as electroactive species which allow direct and indirect determinations and sensitive analysis of them were made at optimum flow and carrier solution conditions. From the calibration lines of current versus concentration with a correlation coefficient of at least 0.998, adrenaline and periodate were determined at the detection -7 -6 limited of 5.0x10 M and 5.0x10 M respectively. The results were compared with the results of the experiments using the same electrodes in static conditions. It was observed that the convection created by the rotation electrode increased the sensitivity and the flow of the solution increased both sensitivity and the frequency of injection (50-60 samplcs/hr).
Açıklama
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Anahtar Kelimeler
Kimya Mühendisliği, Chemical Engineering, Akışkan sistemler, Fluid systems, Enjeksiyon yöntemi, Injection method