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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' journal of analytical chemistry 364 (1999), S. 533-540 
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Solid sampling graphite furnace atomic absorption spectroscopy (SS-GFAAS) has been used for the determination of traces of heavy metals (Cd, Pb, Cu, Cr, Ni, V and As) in barytes over a wide concentration range, e.g. Cd from 0.023 to 27.0 μg/g and Pb from 1.54 to 3509 μg/g.The necessity of determining heavy metals in commercial barytes (naturally occurring barium sulfate), a mineral important to the oil industry because of its use in drilling muds, is discussed. The problems presented by the analysis of this difficult matrix are elegantly solved by using SS-GFAAS for the direct determination of heavy metals. A high-performance graphite furnace AAS with D2-background correction system and a transversely heated graphite atomizer was used for the investigations. The spectrometer was combined with a mechanical sampling module and an ultramicrobalance. The transfer of solid samples (sample weights 0.031–0.686 mg) into the atomizer was carried out by using an optimized graphite platform as the sample carrier. Calibration curve techniques and standard addition methods were employed using external standards (CRMs). Problems associated with signal deformations like multiple peaks, tailing or shoulders are also discussed and possibilities to solve the problems are given. The influence of the homogeneity of solid samples on the precision and accuracy are shown in a real example. The results obtained by SS-GFAAS were compared with results by other methods like X-ray fluorescence spectroscopy (XRF) and flame AAS after aqua regia microwave extraction. This study has demonstrated that SS-GFAAS is a very powerful and easy-to-use method for quick and accurate analysis of barytes.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An instrumental design for the analysis of heavy metals in solid samples (certified reference materials, river sediments, cements) by direct graphite furnace atomic absorption spectroscopy (SSGF-AAS) is presented and outlined. A high performance atomic absorption spectrometer with a D2-background corrector and a transversely heated graphite atomizer was modified. Solid sampling was achieved by a mechanical module combined with an ultra microbalance. Cadmium, lead and chromium in different samples (sample weights between 20–400 μg) have been determined in the μg/g- to ng/g-range with the graphite-platform technique. Different ways of calibration and inhomogeneity problems are discussed. The precision of SSGF-AAS is equal to the precision of the conventional AAS-technique with chemical digestion (microwave digestion system, Zeeman-AAS). It is shown that SSGF-AAS is a reasonable alternative to the conventional technique for selected analytical problems.
    Type of Medium: Electronic Resource
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