Ozgur Dogan Uluozlu

Mercury(II) and methyl mercury speciation on Streptococcus pyogenes loaded Dowex Optipore SD-2

A solid phase extraction procedure based on speciation of mercury(II) and methyl mercury on Streptococcus pyogenes immobilized on Dowex Optipore SD-2 has been established. Selective and sequential elution with 0.1 mol L(-1) HCl for methyl mercury and 2 mol L(-1) HCl for mercury(II) were performed at pH 8. The determination of mercury levels was performed by cold vapour atomic absorption spectrometry (CVAAS). Optimal analytical conditions including pH, amounts of biosorbent, sample volumes, etc., were investigated. The influences of the some alkaline and earth alkaline ions and some transition metals on the recoveries were also investigated. The capacity of biosorbent for mercury(II) and methyl mercury was 4.8 and 3.4 mg g(-1). The detection limit (3 sigma) of the reagent blank for mercury(II) and methyl mercury was 2.1 and 1.5 ng L(-1). Preconcentration factor was calculated as 25. The relative standard deviations of the procedure were below 7%. The validation of the presented procedure is performed by the analysis of standard reference material (NRCC-DORM 2 Dogfish Muscle). The procedure was successfully applied to the speciation of mercury(II) and methyl mercury in natural water and environmental samples.

Characterization of biosorption process of As(III) on green algae Ulothrix cylindricum

Arsenic (As) is generally found as As(III) and As(V) in environmental samples. Toxicity of As(III) is higher than As(V). This paper presents the characteristics of As(III) biosorption from aqueous solution using the green algae (Ulothrix cylindricum) biomass as a function of pH, biomass dosage, contact time, and temperature. Langmuir, Freundlich and Dubinin-Radushkevich (D-R) models were applied to describe the biosorption isotherm of As(III) by U. cylindricum biomass. The biosorption capacity of U. cylindricum biomass was found as 67.2mg/g. The metal ions were desorbed from U. cylindricum using 1M HCl. The high stability of U. cylindricum permitted 10 times of adsorption-elution process along the studies with a slightly decrease about 16% in recovery of As(III) ions. The mean free energy value evaluated from the D-R model indicated that the biosorption of As(III) onto U. cylindricum biomass was taken place by chemical ion-exchange. The calculated thermodynamic parameters, DeltaG degrees , DeltaH degrees and DeltaS degrees showed that the biosorption of As(III) onto U. cylindricum biomass was feasible, spontaneous and exothermic under examined conditions. Experimental data were also tested in terms of biosorption kinetics using pseudo-first-order and pseudo-second-order kinetic models. The results showed that the biosorption processes of As(III) followed well pseudo-second-order kinetics.

Determination of As(III) and As(V) species in some natural water and food samples by solid-phase extraction on Streptococcus pyogenes immobilized on Sepabeads SP 70 and hydride generation atomic absorption spectrometry

The speciation of arsenic(III) and arsenic(V) by using Streptococcus pyogenes immobilized on Sepabeads SP 70 resin has been investigated with solid-phase extraction method. The arsenic levels were determined hydride generation atomic absorption spectrometry (HGAAS) in sample solutions. The procedure presented based on quantitative recoveries of As(III) as >95%. Also the As(V) recoveries were obtained as <5% using the presented method. After reduction of As(V) by using KI and ascorbic acid and waiting 1h later, the system was applied to determination of total arsenic. As(V) was found as the difference between the total As and As(III) content. Various experimental parameters such as pH, amount of microorganism, sample volume, etc. were investigated. The capacity of biosorbent for arsenic(III) was calculated as 7.3 mg/g. The preconcentration factor was found as 36. The relative standard deviation was calculated below 8%. Limit of detection was calculated as 13 ng/L. The validation of the presented procedure was tested by analysis of standard reference materials (NIST SRM 1568a Rice floor and GBW 07605 Tea) and obtained fairly compatible results. The procedure was also successfully applied to arsenic speciation and determination of some natural water and food samples.

Investigation of the levels of some element in edible oil samples produced in Turkey by atomic absorption spectrometry

The element contents (Fe, Mn, Zn, Cu, Pb, Co, Cd, Na, K, Ca and Mg) in edible oils (olive oil, hazelnut oil, sunflower oil, margarine, butter and corn oil) from Turkey were determined using atomic absorption spectrometry after microwave digestion. The concentrations of trace element in the samples were found to be 291.0-52.0, 1.64-0.04, 3.08-1.03, 0.71-0.05, 0.03-0.01, 1.30-0.50, 84.0-0.90, 50.1-1.30, 174.2-20.8 and 20.8-0.60 microg/g for iron, manganese, zinc, copper, lead, cobalt, sodium, potassium, calcium, and magnesium, respectively. Cadmium was found to be 4.57-0.09 microg/kg. The high heavy metal and minerals accumulation levels in the samples were found in olive oil for Cu, Pb, Co, margarine for Fe, K, corn oil for Zn, Mn, butter for Na, Mg, sunflower oil for Ca and hazelnut oil for Cd, respectively.

Assessment of trace element contents of chicken products from turkey

Due to the consumption of chicken and chicken products in Turkey at high ratio, trace metal content of chicken and chicken products from Turkey were determined by atomic absorption spectrometry after microwave digestion. The accuracy of the method was confirmed by analysis of standard reference material (NIST SRM 1577b Bovine liver). Trace element content in various parts of chicken samples and chicken products were to be in the range of 0.10-114 microg/g for copper, 0.25-6.09 microg/kg for cadmium, 0.01-0.40 microg/g for lead, 0.10-0.91 microg/g for selenium, 0.05-3.91 microg/g for manganese, 0.06-0.10 microg/g for arsenic, 0.01-0.72 microg/g for chromium, 0.01-2.08 microg/g for nickel, 0.01-0.02 microg/g for cobalt, 0.10-1.90 microg/g for aluminium, 1.21-24.3 microg/g for zinc, 2.91-155 microg/g for iron. The levels of lead in some analyzed chicken products were higher than the recommended legal limits for human consumption.

Assessment of trace element levels in Rhododendron honeys of Black Sea Region, Turkey.

Rhododendron and multi-flower honeys obtained from Black Sea Region of Turkey (12 Rhododendron and 8 multi-flower honeys) were studied to determine the presence of the 14 trace elements such as Cu, Cd, Pb, Co, Cr, Ni, Al, Se, Zn, Mn, Fe, K, Ca and Mg. Trace element determination was performed by atomic absorption spectrometry (AAS) after microwave digestion. The results revealed that Rhododendron honeys exhibited higher concentrations of Cu, Co, Cr, Ni, Se, Zn, Ca and Mg but lower concentrations of Al, Mn, Fe and K than in the multi-flower honeys. Trace element levels in analyzed honey samples were generally lower than literature values.

Coprecipitation of trace elements with Ni2+/2-Nitroso-1-naphthol-4-sulfonic acid and their determination by flame atomic absorption spectrometry

Ni(2+)/2-Nitroso-1-naphthol-4-sulfonic acid precipitate was used for the coprecipitation of Co, Pb, Cu, Fe and Zn prior to their flame atomic absorption spectrometric (FAAS) determinations in environmental samples. The precipitate could be easily dissolved with concentrated nitric acid. The recovery values for analyte ions were higher than 95%. The parameters including pH, sample volume, centrifuge time, amounts of nickel and matrix effects were optimized for the quantitative recoveries of the analytes. The relative standard deviations of cobalt, lead, copper, iron and zinc were found 4.5, 5.7, 3.8, 6.1 and 7.5%, respectively. The limit of detection was calculated as 1.05, 2.67, 1.30, 1.38, and 0.50 microg L(-1) for cobalt, lead, copper, iron and zinc. The validation of the procedure was checked by the analysis of IAEA 336 lichen and SLRS 4 Riverine water standard reference materials were analyzed with satisfactory results. The presented coprecipitation procedure was successfully applied to some environmental samples for determination of analyte ions.

Speciation and separation of Cr(VI) and Cr(III) using coprecipitation with Ni2+/2-Nitroso-1-naphthol-4-sulfonic acid and determination by FAAS in water and food samples

A speciation procedure for chromium(III) and chromium(VI) in the water and food samples has been established in the presented work. The procedure presented based on quantitative recoveries of Cr(III)>95% using coprecipitation of Ni(2+)/2-Nitroso-1-naphthol-4-sulfonic acid. The total chromium was measured after reduction of Cr(VI) by concentrated H(2)SO(4) and ethanol. The Cr(VI) was calculated as the difference between the total Cr content and the Cr(III) contents. The analytical variables, pH, amounts of precipitate, sample volume for optimum recoveries of Cr(III) were investigated. The influences of the some alkaline and earth alkaline ions and some transition metals on the recoveries of analyte ions were also investigated. The preconcentration factor was 50. The detection limit (3 sigma) of the reagent blank for chromium(III) was 1.33 microg L(-1). The relative standard deviations for determinations were found to be <7%, and % of relative error was calculated <6%. The method was validated by certified reference materials of tea (GBW 07605) and bush branches and leaves (GBW 0703). The procedure was successfully applied to the speciation of chromium in natural water and food samples (fish, white cheese, cows meat, black tea, boiled wheat).

3-Ethyl-4-(p-chlorobenzylidenamino-4,5-dihydro-1H-1,2,4-triazol-5-one (EPHBAT) as precipitant for carrier element free coprecipitation and speciation of chromium(III) and chromium(VI).

A method for the separation and speciative determination of Cr(VI) and Cr(III) has been developed. The procedure is based on coprecipitation of Cr(III) on 3-ethyl-4-(p-chlorobenzylidenamino-4,5-dihydro-1H-1,2,4-triazol-5-one (EPHBAT) without carrier element. The Cr(III) can be selectively precipitated on EPHBAT in the pH range of 8.0-9.0, while Cr(VI) cannot be retained. Total chromium was determined after the reduction of Cr(VI) to Cr(III) with 0.5 mL of concentrated H2SO4 and 0.5 mL of ethanol. Cr(VI) concentrations were obtained as the respective differences between total chromium and Cr(III). Experiments were performed to optimize conditions, such as pH, amounts of EPHBAT, sample volume, etc. A preconcentration factor of 50-fold was achieved for Cr(III). The detection limit of the method for Cr(III) was 1.0 microg L(-1). To validate the developed method, the certified reference materials (NIST SRM 1573a and GBW 0703) were analyzed. The method was applied for the speciation of chromium in spiked natural water samples with satisfactory results.

A new separation and preconcentration method for selenium in some foods using modified silica gel with 2,6-diamino-4-phenil-1,3,5-triazine

A novel and simple solid phase extraction method was improved and recommended for selenium. Silica gel was modified with 2,6-diamino-4-phenil-1,3,5-triazine and characterized by FTIR, SEM and elemental analysis and used adsorbent for column solid phase extraction of selenium ions. The experimental parameters (pH, flow rates, amounts of the modified silica gel, concentration and type of eluent, volume of sample, etc.) on the recoveries of selenium were optimized. Standard reference materials were analyzed for validation of method. The present method was successfully applied to the detection of total selenium in water and microwave digested some food samples with quantitative recoveries (> 95%). The relative standard deviations were<8%. Matrix influences were not observed. The adsorption capacity of modified silica gel was 5.90mgg-1. The LOD was 0.015μgL-1. Enrichment factor was obtained as 50 for the introduced method.