Volkan Numan Bulut

Removal of fluoride ions from aqueous solution by waste mud.

The present study was carried out to assess the ability of original waste mud (o-WM) and different types of activated waste mud which are acid-activated (a-WM) and precipitated waste mud (p-WM), in order to remove excess of fluoride from aqueous solution by using batch technique. The p-WM exhibited greater performance than the others. Adsorption studies were conducted as a function of pH, contact time, initial fluoride concentration, adsorbent concentration, temperature, etc. Studies were also performed to understand the effect of some co-existing ions present in aqueous solutions. Adsorption process was found to be almost independent of pH for all types of waste mud. Among the kinetic models tested for p-WM, pseudo-second-order model fitted the kinetic data well with a perfect correlation coefficient value of 1.00. It was found that the adequate time for the adsorption equilibrium of fluoride was only 1h. Thermodynamic parameters including the Gibbs free energy (DeltaG degrees ), enthalpy (DeltaH degrees ), and entropy (DeltaS degrees ) revealed that adsorption of fluoride ions on the p-WM was feasible, spontaneous and endothermic in the temperature range of 0-40 degrees C. Experimental data showed a good fit with the Langmuir and Freundlich adsorption isotherm models. Results of this study demonstrated the effectiveness and feasibility of WM for removal of fluoride ions from aqueous solution.

Carrier element-free coprecipitation (CEFC) method for the separation, preconcentration and speciation of chromium using an isatin derivative

A new, simple, rapid and sensitive separation, preconcentration and speciation procedure for chromium in environmental liquid and solid samples has been established. The present speciation procedure for Cr(III) and Cr(VI) is based on combination of carrier element-free coprecipitation (CEFC) and flame atomic absorption spectrometric (FAAS) determinations. In this method a newly synthesized organic coprecipitant, 5-chloro-3-[4-(trifluoromethoxy) phenylimino]indolin-2-one (CFMEPI), was used without adding any carrier element for coprecipitation of chromium(III). After reduction of chromium(VI) by concentrated H(2)SO(4) and ethanol, the procedure was applied for the determination of total chromium. Chromium(VI) was calculated as the difference between the amount of total chromium and chromium(III). The optimum conditions for coprecipitation and speciation processes were investigated on several commonly tested experimental parameters, such as pH of the solution, amount of coprecipitant, sample volume, etc. No considerable interference was observed from the other investigated anions and cations, which may be found in natural water samples. The preconcentration factor was found to be 40. The detection limit for chromium(III) corresponding to three times the standard deviation of the blank (N=10) was found 0.7 microg L(-1). The present procedure was successfully applied for speciation of chromium in several liquid and solid environmental samples. In order to support the accuracy of the method, the certified reference materials (CRM-TMDW-500 Drinking Water and CRM-SA-C Sandy Soil C) were analyzed, and standard APDC-MIBK liquid-liquid extraction method was performed. The results obtained were in good agreement with the certified values.

Preconcentration, separation and spectrophotometric determination of aluminium(III) in water samples and dialysis concentrates at trace levels with 8-hydroxyquinoline-cobalt(II) coprecipitation system.

A separation-preconcentration procedure was developed for the determination of trace amounts of aluminium in water samples and dialysis concentrates by UV-vis Spectrophotometry after coprecipitation using 8-hydroxyquinoline (8-HQ) as a chelating agent and Co(II) as a carrier element. This procedure is based on filtration of the solution containing precipitate on a cellulose nitrate membrane filter following aluminium(III) coprecipitation with Co/8-HQ and then the precipitates together with membrane filter were dissolved in concentrated nitric acid. The metal contents of the final solution were determined by UV-vis Spectrophotometry with Erio Chrome Cyanine-R standard method. Several parameters including pH of sample solution, amount of carrier element and reagent, standing time, sample volume for precipitation and the effects of diverse ions were examined. The enrichment factor was calculated as 50 and the detection limits, corresponding to three times the standard deviation of the blank (N: 10), was found to be 0.2 microg L(-1). The accuracy of the method was tested with standard reference material (CRM-TMDW-500) and spiked addition. Determination of aluminium(III) was carried out in sea water, river water, tap water and haemodialysis fluids samples. The recoveries were >95%. The relative standard deviations of determination were less than 6%.

A new approach to separation and pre-concentration of some trace metals with co-precipitation method using a triazole

A new co-precipitation method was developed to separate and pre-concentrate Fe(3+), Cu(2+), Cr(3+), Zn(2+), and Pb(2+) ions using an organic co-precipitant, 3-benzyl-4-p-nitrobenzylidenamino-4,5-dihydro-1,2,4-triazole-5-on (BPNBAT) without adding any carrier element, following flame atomic absorption spectrometric (FAAS) determinations. Effect of some analytical conditions, such as pH of the solution, quantity of the co-precipitant, standing time, centrifugation rate and time, sample volume, and interference of concomitant ions were investigated over the recovery yields of the metal ions. The recoveries of the analyte ions were in the range of 95-102%. The detection limits, corresponding to three times the standard deviation of the blank, were found to be in the range of 0.3-2.0 microg L(-1). The precision of the method, evaluated as the relative standard deviation (R.S.D.) obtained after analyzing a series of 10 replicates, was between 1.6% and 6.0% for the trace metal ions. The method was validated by analyzing two certified reference materials and spiked addition. The proposed procedure was applied for the trace metal ions in some environmental samples.

Carrier element-free coprecipitation with 3-phenly-4-o-hydroxybenzylidenamino-4,5-dihydro-1,2,4-triazole-5-one for separation/preconcentration of Cr(III), Fe(III), Pb(II) and Zn(II) from aqueous solutions.

A separation/preconcentration procedure, based on the coprecipitation of Cr(3+), Fe(3+), Pb(2+) and Zn(2+) ions using a new organic coprecipitant, 3-phenly-4-o-hydroxybenzylidenamino-4,5-dihydro-1,2,4-triazole-5-one (POHBAT) without adding any carrier element has been developed. The method, thus, has been called carrier element-free coprecipitation (CEFC). The resultant concentrated elements were determined by flame atomic absorption spectrometric determinations. The influences of some analytical parameters including pH of the solution, amount of the coprecipitant, standing time, centrifugation rate and time, sample volume and diverse ions were investigated on the quantitative recoveries of analyte ions. The validation of the present preconcentration procedure was performed by the analysis of two certified reference materials. The recoveries of understudy analytes were found in the range of 93-98%, while the detection limits were calculated in the range of 0.3-2.0 microg L(-1). The precision of the method evaluated as relative standard deviation (R.S.D.), was in the range of 3-7% depend on the analytes. The proposed method was successfully applied to environmental samples for the determination of the analytes.

Cadmium and nickel determinations in some food and water samples by the combination of carrier element-free coprecipitation and flame atomic absorption spectrometry

A procedure for separation and enrichment of Cd(II) and Ni(II) ions based upon carrier element-free coprecipitation by using an organic coprecipitant, 2-{4-[2-(1H-Indol-3-yl)ethyl]-3-(4-methylbenzyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl}-N′-(3-fluoro-phenylmethyliden) acetohydrazide, prior to their flame atomic absorption spectrometric detections has been developed. The effects of varied experimental conditions on the performance of the developed method such as pH, sample volume, amount of coprecipitating agent, etc. were evaluated in detail on the recovery of analyte ions, and the influences of some anions and cations were investigated. The limits of detection for Cd(II) and Ni(II) ions based on three times the standard deviation of the blanks (N: 10) were obtained as 0.70 μg L−1 and 1.21 μg L−1, respectively. The accuracy of the method was tested by analyzing a certified reference material and by spike tests. The method was applied to determine the levels of cadmium and nickel in stream and sea water, rice, red lentil, and wheat samples.

Separation and pre-concentration of palladium(II) from environmental and industrial samples by formation of a derivative of 1,2,4-triazole complex on Amberlite XAD–2010 resin

A simple separation/pre-concentration method was developed for extraction of Pd(II) in various environmental samples, based on its adsorption of 4–phenyl–5–{[(4–phenyl–5–pyridin–4–yl–4H–1,2,4–triazole–3–yl)thio]methyl}–4H–1,2,4–triazole–3–thyol (PPTTMET) complex on Amberlite XAD–2010 resin in a mini column. The ligand has high affinity for Pd(II) among many other metals that are taken into consideration. The flame atomic absorption spectrometry is employed to determine the concentration of Pd(II). The optimum working conditions which were determined are as follows: 0.05 mol L−1 HNO3 as working medium, 1.0 mol L−1 HCI in acetone as elution solvent, 0.75 mg of PPTTMET amount and 750 mL of sample volume. The system was independent from the flow rates between 3.1 and 23.1 mL min−1. The Pd(II) adsorption capacity of Amberlite XAD–2010 resin was found to be 12.8 mg g−1 and the enrichment factor was calculated as 375. The method was successfully applied for the determination of Pd(II) in motorway dust samples, anodic sludge, gold ore, industrial electronic waste materials and various water samples.

A sensitive method for the determination of gold and palladium based on dispersive liquid–liquid microextraction combined with flame atomic absorption spectrometric determination using N-(6-morpholin-4-ylpyridin-3-yl)-N′-phenylthiourea

A new method for the determination of gold and palladium was developed by dispersive liquid–liquid microextraction separation–preconcentration and flame atomic absorption spectrometry detection. In the proposed approach, N-(6-morpholin-4-ylpyridin-3-yl)-N′-phenylthiourea (MPPT) was synthesized as a complexing agent. The complexation ability of the MPPT was explored by examining the effect of a series of heavy metal ions, including Mn2+, Pd2+, Ni2+, Cd2+, Co2+, Cu2+, Au3+, Pb2+, Zn2+ and Fe3+, using the DLLME procedure. The MPPT exhibited pronounced selectivity toward Pd2+ and Au3+ ions at different pH levels. Factors influencing the extraction efficiency and complex formation were examined, i.e. the pH of the sample solution, the concentration of the chelating agent, the extraction and dispersive solvent type and volume, the sample volume, and foreign ions, etc. Optimal conditions for quantitative recoveries were pH 5.5 for gold and pH 1.5 for palladium, 125 μL of % 0.4 MPPT, 1200 μL of methanol and 125 μL of carbon tetrachloride. The presented method showed a good linearity within a range of 30–230 and 25–200 μg L−1 with the detection limits of 1.75 and 1.65 μg L−1 for Au and Pd, respectively. The relative standard deviation (RSD) was below 2.8% at 50 μg L−1 for both ions (n = 10). The developed method was simple, fast, cost efficient, and sensitive for the extraction and preconcentration of gold and palladium in samples of liquids (sea, stream water) and solids (stream sediment, ores, and electronic waste).

Determination of Au(III) and Pd(II) ions by flame atomic absorption spectrometry in some environmental samples after solid phase extraction

ABSTRACT A simple and sensitive solid phase extraction method was developed for simultaneous separation and preconcentration of gold and palladium ions with N-(4-methylphenyl)-2-{[(4-phenyl-5-pyridine-4-yl-4H-1,2,4-triazol-3-yl)thio]acetyl}hydrazine carbo thioamide complex on Amberlite XAD-1180 resin before their determination by flame atomic absorption spectrometry. Some analytical parameters such as HNO3 concentration of the sample solution, amount of complexing agent, sample volume, eluent type and volume, effects of foreign ions and adsorption capacity of the resin were investigated for quantitative recovery of gold and palladium ions. The effects of some anions and cations were also examined. Under optimum conditions, the detection limits for gold and palladium ions were found to be 0.29 and 0.19 μg L−1, respectively. The preconcentration factor for gold and palladium was 250. After being validated by standard addition and analysis of standard reference material, the procedure was successfully applied to the analysis of sea and stream water, anodic slime, gold ore, soil and electronic waste.