Direct analysis of solid samples by GFAAS – determination of trace heavy metals in barytes |
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Authors: | R Nowka I L Marr T M Ansari and H Müller |
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Institution: | (1) Martin-Luther-Universit?t Halle Wittenberg, Fachbereich Chemie, Institut für Analytik und Umweltchemie, Geusaer Str. 88, D-06217 Merseburg, Germany, DE;(2) University of Aberdeen, Department of Chemistry, Meston Walk, Old Aberdeen, AB24 3UE, Scotland, GB |
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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.
Received: 9 November 1998 / Revised: 29 January 1999 / Accepted: 2 February 1999 |
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