Spectrofluorimetric Determination of Beryllium by Mean Centering of Ratio Spectra.

Trace amounts of beryllium has been determined by spectrofluorimetric method that used morin as fluorimetric reagent. Beryllium gives a highly fluorescent complex with morin. The excitation wavelength of morin and Be-morin complex were 410 and 430. The fluorescence spectra of morin and Be-morin complex were overlaped in excitation wavelength of 430 nm. A method based on mean centering of ratio spectra has been performed to remove the interference caused by morin as it overlaps with the Be-morin spectra. The linear range of beryllium concentration is in 0.2-200 ppb range. The parameters of detection limit and RSD were 0.18 ppb and 4.6 % respectively. This method was used for determination of beryllium in copper-beryllium alloy as a real sample. In determination of Be(II), the interference by Cu(II) was very serious, which was eliminated by adding triethanolamine.

Vortex-assisted surfactant-enhanced emulsification microextraction based on solidification of floating organic drop followed by electrothermal atomic absorption spectrometry for speciation of antimony (ΙΙΙ, V).

Vortex-assisted surfactant-enhanced emulsification microextraction based on solidification of floating organic drop (VASEME-SFO) was used for preconcentration and speciation of antimony (ΙΙΙ, V) followed by electrothermal atomic absorption spectrometry (ETAAS). In this procedure, Triton X-114 was used as emulsifier and 1-undecanol was used as extraction solvent. This method is based on the complexation of Sb(ΙΙΙ) with dithizone (as complexing agent) at pH 2 and extraction of the resulting hydrophobic complex into the extraction solvent (1-undecanol) with vortex-assisted liquid phase microextraction, whereas Sb(V) remained in solution. Sb(ΙΙΙ) in extraction solvent was directly analyzed by ETAAS after dilution with ethanol, and Sb(V) was calculated by subtracting Sb(ΙΙΙ) from the total antimony after reducing Sb(V) to Sb(ΙΙΙ) by L-cysteine. Under the optimized condition, the calibration curve was linear in the range of 0.4-8 µg L(-1) of Sb(ΙΙΙ) with a correlation coefficient of 0.9995. The detection limit based on three times of the standard deviation of the blank (n = 8) was 0.09 µg L(-1). The validation and the recovery of the proposed method were performed by the analysis of a certified reference material and spike method. The obtained results were in very good agreements with certified values. The proposed method was successfully applied for the determination of antimony species at trace levels in different water samples.

Hydride generation coupled to microfunnel-assisted headspace liquid-phase microextraction for the determination of arsenic with UV-Vis spectrophotometry.

In this research, a microfunnel-assisted headspace liquid-phase microextraction technique has been used in combination with hydride generation to determine arsenic (As) by UV-Vis spectrophotometry. The method is based on the reduction of As to arsine (AsH3) in acidic media by sodium tetrahydroborate (NaBH4) followed by its subsequent reaction with silver diethyldithiocarbamate (AgDDC) to give an absorbing complex at 510 nm. The complexing reagent (AgDDC) has been dissolved in a 1:1 (by the volume ratio) mixture of chloroform/chlorobenzene microdroplet and exposed to the generated gaseous arsine via a reversed microfunnel in the headspace of the sample solution. Several operating parameters affecting the performance of the method have been examined and optimized. Acetonitrile solvent has been added to the working samples as a sensitivity enhancement agent. Under the optimized operating conditions, the detection limit has been measured to be 0.2 ng mL(-1) (based on 3sb/m criterion, n b = 8), and the calibration curve was linear in the range of 0.5-12 ng mL(-1). The relative standard deviation for eight replicate measurements was 1.9 %. Also, the effects of several potential interferences have been studied. The accuracy of the method was validated through the analysis of JR-1 geological standard reference material. The method has been successfully applied for the determination of arsenic in raw and spiked soft drink and water samples with the recoveries that ranged from 91 to 106 %.

Preconcentration of lead using solidification of floating organic drop and its determination by electrothermal atomic absorption spectrometry.

A simple microextraction method based on solidification of a floating organic drop (SFOD) was developed for preconcentration of lead prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Ammonium pyrolidinedithiocarbamate (APDC) was used as complexing agent, and the formed complex was extracted into a 20 µL of 1-undecanol. The extracted complex was diluted with ethanol and injected into a graphite furnace. An orthogonal array design (OAD) with OA16 (4(5)) matrix was employed to study the effects of different parameters such as pH, APDC concentration, stirring rate, sample solution temperature and the exposure time on the extraction efficiency. Under the optimized experimental conditions the limit of detection (based on 3 s) and the enhancement factor were 0.058 µg L(-1) and 113, respectively. The relative standard deviation (RSD) for 8 replicate determinations of 1 µg L(-1) of Pb was 8.8%. The developed method was validated by the analysis of certified reference materials and was successfully applied to the determination of lead in water and infant formula base powder samples.

Evaluation of electrochemical generation of volatile zinc hydride by heated quartz tube atomizer atomic absorption spectrometry.

Electrochemical hydride generation (EcHG) as a sample introduction system for determination of zinc was developed. It was directly coupled to an electrically heated quartz tube atomizer (QTA) atomic absorption spectrometry (AAS) system. The hydride generator is a laboratory-made semi-batch electrolytic cell that consists of a lead-tin alloy cathode and a platinum anode. The effects of typical parameters on the generation efficiency of the technique, such as types of cathode material and catholyte and anolyte solutions, were studied. The influences of numerical experimental operating parameters on the analytical signal were evaluated in detail and optimum conditions were obtained. The analytical figures of merit for the developed method were determined. The calibration curve was linear up to 300 ng mL(-1) of Zn. A concentration detection limit (3σ, n = 9) of 11 ng mL(-1) Zn and a relative standard deviation of 5.0% (RSD, n = 9) for 200 ng mL(-1) Zn were accessed. In addition, the susceptibility of interference from various ions was evaluated. The accuracy of the method was verified by determination of Zn in a certified reference material and in tap water. The achieved concentrations were found to be in good agreement with both the certified value and the data obtained using flame AAS.

Speciation and analysis of arsenic(III) and arsenic(V) by electrochemical hydride generation spectrophotometric method.

A simple method was developed for speciation and spectrophotometric determination of inorganic As(III) and As(V) using an electrochemical hydride generation technique. For speciation of As(III) and As(V), a graphite rod was used as cathode to reduce As(III) to AsH(3), the rod was then replaced with a tin-lead alloy wire for reducing As(V) to AsH(3). The spectrophotometric determination was based on the reaction of AsH(3) with silver diethyldithiocarbamate to give an absorbing complex at 510 nm. Under the optimized conditions, the calibration curves were linear over the ranges of 0.1-5 microg ml(-1) for As(III) and 0.5-4.0 microg ml(-1) for As(V). The concentration detection limits of 0.02 and 0.06 microg ml(-1) were achieved for As(III) and As(V), respectively. The relative standard deviations for five replicate speciation and determination of 3.0 microg ml(-1) As(III) and As(V) were 0.8 and 7.2%, respectively. The accuracy and recovery of the method were evaluated by analyzing tap water spiked with As(III) and As(V).