scholarly journals Determination of beryllium in various types of natural waters by electrothermal atomic absorption spectrometry

2013 ◽  
Vol 14 (1) ◽  
pp. 40-47

The procedure for the reliable determination of Be in natural waters by ETAAS was elaborated. Various modifiers (EDTA, Ca(NO3)2, Mg(NO3)2, Pd(NO3)2 and the mixture of Pd(NO3)2 and Mg(NO3)2) for the determination of beryllium was examined. The applicability of the selected Mg(NO3)2 as the appropriate and generally used modifier for the determination of Be in the different types of natural waters by ETAAS has been confirmed. The accuracy of the method was verified by analyzing of the certified reference material of drinking water ("Trace Metals in Drinking Water"). The real drinking waters and waste waters with the reference values of Be concentration, spiked tap water, mineral waters and model river water were utilized for the determination of Be. Using Mg(NO3)2 for modification, the detection limit of 0.07 μg L-1, the quantification limit of 0.22 μg L-1 and characteristic mass of 3.7 pg of Be were obtained. The recovery was in the range 95–111% and (%) RSD value was less than 8%.

2010 ◽  
Vol 75 (1) ◽  
pp. 113-128 ◽  
Author(s):  
Simona Murko ◽  
Radmila Milacic ◽  
Marjan Veber ◽  
Janez Scancar

The applicability of nitric acid, palladium nitrate and a mixture of palladium and magnesium nitrate as matrix modifiers was estimated for the accurate and reproducible determination of cadmium (Cd), lead (Pb) and arsenic (As) in sediments of the Sava River by electrothermal atomic absorption spectrometry, ETAAS. Decomposition of the samples was done in a closed vessel microwave-assisted digestion system using nitric, hydrochloric and hydrofluoric acids, followed by the addition of boric acid to convert the fluorides into soluble complexes. The parameters for the determination of Cd, Pb and As in sediments were optimized for each individual element and for each matrix modifier. In addition, two sediment reference materials were also analyzed. In determination of Cd and Pb, nitric acid was found to be the most appropriate matrix modifier. The accurate and reliable determination of Cd and Pb in sediments was possible also in the presence of boric acid. The use of a mixture of palladium and magnesium nitrate efficiently compensated for matrix effects and enabled the accurate and reliable determination of As in the sediments. Quantification of Cd and As was performed by calibration using acid matched standard solutions, while the standard addition method was applied for the quantification of Pb. The repeatability of the analytical procedure for the determination of Cd, Pb and As in sediments was ?5 % for Cd, ?4 % for Pb and ?2 % for As. The LOD values of the analytical procedure were found to be 0.05 mg/kg for Cd and 0.25 mg/kg for Pb and As, while the LOQ values were 0.16 mg/kg for Cd and 0.83 mg/kg for Pb and As. Finally, Cd, Pb and As were successfully determined in sediments of the Sava River in Slovenia.


2008 ◽  
Vol 33 (1) ◽  
pp. 49-56 ◽  
Author(s):  
V. R.. Amorim Filho ◽  
V. P. Franzini ◽  
J. A. Gomes Neto

National Health Surveillance Agency (ANVISA) established in the decree number 54 maximum allowed levels for Ni and Pb in mineral and natural waters at 20 µg L-1 and 10 µg L-1, respectively. For screening analysis purposes, the high-resolution continuum source flame atomic absorption spectrometry technique (HR-CS FAAS) was evaluated for the fast-sequential determination of nickel and lead in mineral waters.Two atomic lines for Ni (232.003 nm - main and 341.477 nm - secondary) and Pb (217.0005 nm - main and 283.306 nm - secondary) at different wavelength integrated absorbance (number of pixels) were evaluated. Sensitivity enhanced with the increase of the number of pixels and with the summation of the atomic lines absorbances. The main figures of merit associated to the HR-CS FAAS technique were compared with that obtained by line-source flame atomic absorption spectrometry (LS FAAS). Water samples were pre-concentrated about 5-fold by evaporation before analysis. Recoveries of Pb significantly varied with increased wavelength integrated absorbance. Better recoveries (92-93%) were observed for higher number of pixels at the main line or summating the atomic lines (90-92%). This influence was irrelevant for Ni, and recoveries in the 92-104% range were obtained in all situations.


2012 ◽  
Vol 66 (3) ◽  
Author(s):  
Jordan Mouhovski ◽  
Albena Detcheva

AbstractNatural fluorite is used for growing CaF2 boules from melt by an improved technique. Chemical treatment of the starting ore decomposes the accessory minerals, thus producing small amounts of the oxides of Si, Al, and Fe insoluble in the melt, whereas the overall content of rare earth elements (REEs) of hundreds of μg g−1, remains unchanged. Analytical techniques and optical measurements provide for assessing the concentration range and trends in the distribution of residual metal impurities along the height of the boules. Solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS) gives good reproducibility for impurities’ distribution within a large concentration range of 0.1–10 μg g−1. The concentrations of Zn and Cu determined were found to vary within the lowest tenths of μg g−1 range in the starting portions of chemically treated fluorspar and a batch of boules produced subsequently. The concentrations of both elements show a decreasing trend towards the top section within the confidential interval, the width of which confirms the definite in homogeneities in their distribution at those concentration levels. The Fe occurs in the boules below the detection limit, while the content of lead diminishes rapidly towards their upper section, probably due to a shorter path in the liquid phase before any vapour phase transition proceeds. A satisfactory correlation is found between the Pb concentration in ng g−1-range and light-absorption peak intensity at 204 nm, the precise determination of which is impeded due to the overlapping bands and the light-scattering effect. Reliable determination of impurities enables optimisation of the basic purification — growing stages for the production of high grade crystals.


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