Determination of Pb(II), Zn(II), Cd(II), and Co(II) ions by flame atomic absorption spectrometry in food and water samples after preconcentration by coprecipitation with Mo(VI)-diethyldithiocarbamate.

A new, simple, and rapid separation and preconcentration procedure, for determination of Pb(II), Cd(II), Zn(II), and Co(II) ions in environmental real samples, has been developed. The method is based on the combination of coprecipitation of analyte ions by the aid of the Mo(VI)-diethyldithiocarbamate-(Mo(VI)-DDTC) precipitate and flame atomic absorption spectrometric determinations. The effects of experimental conditions like pH of the aqueous solution, amounts of DDTC and Mo(VI), standing time, centrifugation rate and time, sample volume, etc. and also the influences of some foreign ions were investigated in detail on the quantitative recoveries of the analyte ions. The preconcentration factors were found to be 150 for Pb(II), Zn(II) and Co(II), and 200 for Cd(II) ions. The detection limits were in the range of 0.1-2.2 µg L(-1) while the relative standard deviations were found to be lower than 5 % for the studied analyte ions. The accuracy of the method was checked by spiked/recovery tests and the analysis of certified reference material (CRM TMDW-500 Drinking Water). The procedure was successfully applied to seawater and stream water as liquid samples and baby food and dried eggplant as solid samples in order to determine the levels of Pb(II), Cd(II), Zn(II), and Co(II) ions.

Cloud-point extraction of rhodamine 6G by using Triton X-100 as the non-ionic surfactant.

Cloud-point extraction (CPE) using the non-ionic surfactant Triton X-100 was used successfully to remove a highly toxic dye, rhodamine 6G (R6G), from water and wastewater. The effects of different analytical parameters such as pH, concentration of Triton X-100 (TX-100) and salts, equilibrium temperature, and incubation time on the efficiency of the extraction of R6G were studied in detail, and optimum conditions for dye extraction were obtained. Thermodynamic parameters including changes in Gibbs free energy, enthalpy, and entropy were also calculated, and these parameters indicated that the CPE of R6G was feasible, spontaneous, and endothermic in the temperature range of 75-95 degrees C. The equilibrium solubilization capacity of TX-100 was found to be 1.10 mmol/mol by using Langmuir isotherm models. No significant interference effects were observed in the presence of phenol and its derivatives, some acidic and basic dyes and most of the anions and cations. It was concluded that the CPE process described in this paper can be an alternative technique for removal of dyes and other pollutants from waters and wastewaters.

Variation of total organic carbon content along the stream Harsit, Eastern Black Sea Basin, Turkey.

The TOC in surface waters and wastewater is an important analytical parameter describing the total content of all organic substances containing carbon. In practice, the TOC originated from natural and anthropogenic sources, and even if it is not directly responsible for dangers on human health, its determination is important for any kind of water that is used by public. The aim of this study was to determine variation of total organic carbon (TOC) and total carbon (TC) content in the stream Harsit, which courses in Eastern Black Sea Region, Turkey. Sampling was fortnightly conducted in each of the four seasons between March 2009 and February 2010. A total of 230 water samples were collected from ten sampling stations along the main branch of the stream Harsit with 143 km of length. Obtained TOC values were evaluated and used to classify the water quality of stream Harsit, according to the Turkish Water Pollution Control Regulation (TWPCR). The annual average TOC content values for the stations were found between 2.33 and 6.97 mg/L. It was seen that the TOC content have increased along the streamcourse of Harsit until the fourth station, where reaches its maximum value. The TOC content, then, has decreased and the minimum value was observed in the eighth station. The results showed that, except in winter season, maximum TOC content observed in many of the water samples were above Class I water standard indicated in TWPCR, which classifies the water resources according to the different area of uses. It was also found that TOC has a small contribution to TC and the highest TOC content in stream waters were measured in Gumushane station where direct discharge of city wastewaters and solid waste dumping to the stream were observed.

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%.

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.

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.

Separation and enrichment of gold(III) from environmental samples prior to its flame atomic absorption spectrometric determination.

A simple and accurate method was developed for separation and enrichment of trace levels of gold in environmental samples. The method is based on the adsorption of Au(III)-diethyldithiocarbamate complex on Amberlite XAD-2000 resin prior to the analysis of gold by flame atomic absorption spectrometry after elution with 1 molL(-1) HNO3 in acetone. Some parameters including nitric acid concentration, eluent type, matrix ions, sample volume, sample flow rate and adsorption capacity were investigated on the recovery of gold(III). The recovery values for gold(III) and detection limit of gold were greater than 95% and 16.6 microgL(-1), respectively. The preconcentration factor was 200. The relative standard deviation of the method was <6%. The adsorption capacity of the resin was 12.3 mg g(-1). The validation of the presented procedure was checked by the analysis of CRM-SA-C Sandy Soil certified reference material. The presented procedure was applied to the determination of gold in some environmental samples.

A multi-element solid-phase extraction method for trace metals determination in environmental samples on Amberlite XAD-2000.

A method for the preconcentration of some transition elements at trace level was proposed using a column filled with Amberlite XAD-2000 resin. Metal ions were adsorbed on XAD-2000 as their diethyldithiocarbamate chelates, then analytes retained on the resin were eluted by 1 mol L(-1) nitric acid in acetone and determined by flame atomic absorption spectrometry (FAAS). The influences of some analytical parameters including pH of sample solution, ligand amount, the type, concentration and volume of elution solution, flow rates of the sample and eluent solutions, adsorption capacity of the resin and sample volume on the preconcentration efficiency have been investigated. The influences of some matrix elements were also examined. The detection limit (N=20, 3 sigma) for Mn(II), Fe(II), Co(II), Cu(II), Cd(II), Zn(II), Pb(II) and Ni(II) were found as 0.20, 0.35, 0.25, 0.20, 0.20, 0.15, 0.45 and 0.25 microg L(-1), respectively. The validation of the procedure was carried out by analysis of certified reference materials. The proposed method was applied to natural waters and kale vegetable (Brassica oleracea var. acephala).

Solid-phase extraction of Mn(II), Co(II), Ni(II), Cu(II), Cd(II) and Pb(II) ions from environmental samples by flame atomic absorption spectrometry (FAAS).

A new method using a column packed with Amberlite XAD-2010 resin as a solid-phase extractant has been developed for the multi-element preconcentration of Mn(II), Co(II), Ni(II), Cu(II), Cd(II), and Pb(II) ions based on their complex formation with the sodium diethyldithiocarbamate (Na-DDTC) prior to flame atomic absorption spectrometric (FAAS) determinations. Metal complexes sorbed on the resin were eluted by 1 mol L(-1) HNO3 in acetone. Effects of the analytical conditions over the preconcentration yields of the metal ions, such as pH, quantity of Na-DDTC, eluent type, sample volume and flow rate, foreign ions etc. have been investigated. The limits of detection (LOD) of the analytes were found in the range 0.08-0.26 microg L(-1). The method was validated by analyzing three certified reference materials. The method has been applied for the determination of trace elements in some environmental samples.