Katı faz ekstraksiyon tekniği ile talyum türlendirme çalışması

06.03.2018 tarihli ve 30352 sayılı Resmi Gazetede yayımlanan “Yükseköğretim Kanunu İle Bazı Kanun Ve Kanun Hükmünde Kararnamelerde Değişiklik Yapılması Hakkında Kanun” ile 18.06.2018 tarihli “Lisansüstü Tezlerin Elektronik Ortamda Toplanması, Düzenlenmesi ve Erişime Açılmasına İlişkin Yönerge” gereğince tam metin erişime açılmıştır.Bu çalışmada, katı faz ekstraksiyon tekniği ile çeşitli ticari reçineler kullanılarak (Amberlit IR-120 H+ formlu (Fluka) reçine ve Dowex Monosphere 550 A (OH) anyon değiştirme reçinesi) Tl (I) ve Tl (III)'ü içeren çözeltiden bu iki türün birbirinden ayrılma şartları incelendi.Bu reçineler ile Tl (I) ve Tl (III) iyonlarının zenginleştirilmesi ve türlendirilmesi kolon yöntemi ile incelendi. Çözeltinin pH sı, hacmi, akış hızı, matriks bileşenleri ile elüsyon çözeltisinin türü, hacmi ve konsantrasyonu gibi faktörlerin bu elementin türlenmesi ve zenginleştirilmesi üzerine etkileri araştırıldı. Böylece Tl (I) ve Tl (III)'ü içeren çözeltiden bu iki türün birbirinden ayrılma şartları ve zenginleştirilmesi için optimum koşullar tespit edildi. Bu metot, talyum tayini amacıyla sentetik çözeltiler ve nehir suyuna uygulandı. Belirlenen yöntem aynı şekilde uygulanarak, eser miktarda talyum içeren ve standart referans madde olarak kullanılan bir sediment numunesinde talyum tayini talyum türlenmesi yapılarak sonuçların güvenirliliği ve talyum (III) türünün % geri kazanımı hesaplandı. Çalışmada ayrıca, Tl (I) ve Tl (III)'ün kararlılık sabitlerini içeren termodinamik verileri kullanarak sulu ortamda talyum türlerinin bilgisayar yazılımı ile teorik tahminleri yapıldı.Sonuç olarak, talyumun eser miktarını belirlemek için, yeni, basit, oldukça duyarlı, seçici ve fazla maliyet gerektirmeyen spektrofotometrik bir metot geliştirildi. Yapılan türlendirme çalışmasında ayrıca hem Tl (I) hem de Tl (III) için geniş bir pH aralığında çalışılabileceği ortaya kondu. Böylelikle yapılan deneyler ile çalışmada kullanılan Dowex Monosphere 550 A (OH) anyon değiştirme reçinesinin Tl (I) ve Tl (III)'ü içeren çözeltiden bu iki türün birbirinden ayrılması amacıyla kullanılabileceği sonucuna varıldı. Bu metot sentetik çözeltilerde, gerçek örneklerde ve standart referans maddeler üzerinde talyum türlendirme ve tayininde başarılı bir şekilde uygulandı.In this study, separation and speciation of Tl (I) and Tl (III) species from the solution with using various commercial resins (Amberlite IR-120 H+ form (Fluka) resin and Dowex Monosphere 550 A (OH), anion exchange resin) by solid phase extraction (SPE) technique.Preconcentration and speciation of Tl (I) and Tl (III) ions were investigated in the of are mentioned resins using SPE column technique. Enfluents of pH, volume, flow rate, matrix components of solution and type, volume and concentration of elutionsolution were investigated for the element studied over the speciation and preconcentration. Thus, optimum conditions were determined for seperation and preconcentration of Tl (I) and Tl (III) species in the solution. This method was applied fort he determination of Thallium species in synthetic and river water samples. The method was also applied to the Cerified Reference Material containing trace Thallium element as river sediment sample for the purpose of method validation. Percentages of Thallium recoveries were calculated using CRM. Comparison of the results obtained from the experimental data were made using computer simulation program Minteqa2.As a result, a new, simple, highly sensitive, selective and low cost spectrophotometric method has been developed to determine trace amounts of thallium species. In addition, it was found that both Tl (I) and Tl (III) species can be studied in a wide range of pH. Thus, the experimental results showed that Dowex Monosphere 550 A (OH) anion exchange resin can be used to separate Tl (I) and Tl (III) species. This developed method was applied to synthetic solutions, real sample solutions, and standard referans materials for thallium speciation and determination study

The effect of nickel phytotoxicity on photosystem II activity and antioxidant enzymes in barley

In this study, the effect of mild (100 µM), moderate (300 µM) and severe (500 µM) nickel (NiSO4.7H2O) toxicity on the photosynthetic activity, photosynthetic pigment content and some antioxidant enzymes in the leaves of a barley cultivars (Hordeum vulgare L. cv. Tarm-92) was investigated. Moderate and severe nickel toxicity decreased root length while shoot length was not affected by nickel stress, probably due to over accumulation of nickel in roots. Similarly, biomass accumulation was declined by moderate and severe nickel toxicity as reflected by the lowered fresh and dry weight. Chlorophyll a, chlorophyll b and consequently total chlorophyll content decreased by all nickel applications, presumably because the reduced level of carotenoids. Chlorophyll a fluorescence measurements showed that nickel toxicity blocked electron movement in some specific points of the photosynthetic electron transport system. The constant Fo value indicated that PSII reaction centers was not damaged in the leaves of barley under nickel toxicity while the reduced Fm value showed that acceptor side of PSII was more sensitive to nickel toxicity as compared to donor side. Changes in JIP test parameters in the leaves of barley showed that primary photochemical reactions are reduced, and thermal dissipation of excess energy is increased. SOD and CAT activity is elevated in the leaves of barley under moderate and severe nickel toxicity which demonstrate an efficient superoxide dismutation. Severe nickel toxicity, however, did not affect SOD and CAT activity. The ascorbate-glutathione cycle was activated in the leaves of barley plants under nickel toxicity, probably indicating an efficient H2O2 detoxification. However, considerable H2O2 and MDA accumulation was observed in the leaves of barley under nickel stress. As a result, it may be concluded that the barley genotype Tarm-92 is moderately tolerant to nickel toxicity

Determination of some major and trace elements in the lower Sakarya River water by ICP-MS

In this paper, water and sediment samples were collected along the Lower Sakarya River basin for a twelve month period between February 2007 and January 2008. The samples were analysed for trace elements (31 elements in sediment and 33 elements in water) using the ICP-MS technique as pollution indicators. The results indicated that the Sakarya River water was polluted by sources of beryllium and thallium which exceeded the limits set by US Environmental Protection Agency (USEPA 2003). Sediments were polluted by Antimony, Tin, Rhodium and Selenium. The results also provide useful data for the conservation of the Black Sea where it is joined by the Sakarya River. (C) 2018 ACG Publications. All rights reserved

Determination of some heavy metals by ICP-OES in edible parts of fish from Sapanca Lake and streams

In this study, 20 fish taken from Sapanca Lake, Sakarya River and Western Black Sea (Karasu) in total and heavy metal accumulation (Cu, Fe abd Zn) in the muscles of 15 species was determined with ICP-OES (Inductively Coupled Plasma-Optical Emission Spectometer) device. When the results were examined, Cu, Fe and Zn concentration was determined to be 2.60-5.31 mu g/g, 0.25-54.36 mu g/g and 13.66-47.11 mu g/g respectively in fish samples. In addition, the same procedures were applied with the standard reference material DORM-3 reference material (Fish Protein Certified Reference Material for Trace Metals) to determine the accuracy of the method. As a result, it has been determined that the amount of heavy metals contained in the analyzed fish samples is below the limit values provided by the Turkish Food Codex, Food and Agriculture Organization and World Health Organization and therefore consumption of these does not constitute a threat to health

Determination of Boron in hazelnut varieties with the addition of sorbitol by using ICP-OES and ultrasonic nebulization after microwave digestion system

Boron is an essential nutrient for plants and an essential element for many organisms, but can be toxic to aquatic and terrestrial organisms above certain concentrations. The aim of this research is determining the Boron content of four varieties of Hazelnut (Corylus avellana L.) from Sakarya. Inductively coupled plasma optical emission spectrometry (ICP-OES) with ultrasonic nebulization (USN) was used for the determination of Boron contents. This method is based on microwave digestion system and reduced memory effect of Boron by using sorbitol. Different conditions were optimized for this method. Four hazelnut varieties, eight soil samples and certificated reference material (NIM-GBW10012) were analyzed. The Boron contents were found as 18.27, 28.3, 38.6, 17.6 mg/kg in Kara, Sivri, Delisava and Tombul hazelnut varieties, respectively. And Boron contents of soil samples were between 30.44 to 196.79 mg/kg. The results revealed that the Turkish hazelnut is a good natural source of Boron. (C) 2018 ACG Publications. All rights reserved

Speciation of Antimony Using Dithizone Ligand via Cloud Point Extraction and Determination by USN-ICP-OES

In this paper, a cloud point extraction (CPE) method is described and inorganic antimony species were determined by using an inductively coupled plasma optic emission spectrometer coupled to an ultrasonic nebulizer (USN-ICPOES). Dithizone complexed Sb(III) species were trapped in the micelle front the aqueous phase using the Triton X-114 surfactant with an increase in temperature. After centrifugation and phase separation, the surfactant-rich phase was dissolved with 2 M HNO3 and measured in the USN-ICP-OES. Indium (In) was used as an internal standard in order to reduce noise and random systematic errors. The effects of phi, surfactant concentration, ligand concentration, heating time, temperature, and interfering ions were optimized. The effects of the rate of foreign ions and their species, as well as the parameters such as pH, surfactant concentration, ligand concentration, heating time and temperature, were optimized. In the proposed method, Sb(V) was reduced to Sb(III) with L-cysteine for the determination of total antimony. For Sb(III), the determined 1.01) value was 0.04 mu g with an RSD of 2.59% (n=12) [pH = 4, 0.04 mu g mol L-1 dithizone, and 0.06% (w/v) Triton X-114]. The developed method was applied to the analysis of real water and fruit juices, and validated using a certified reference material