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Irina V. Nikolaeva, Anastasia S. Shaibalova, Stanislav V. Palesskiy
ICP-MS elemental analysis of candidates for
reference materials of black shales composition
Abstract
Abstract.
For the
elemental analysis of candidates for reference materials of black shale
composition – SLg-1A and SChS-1A – inductively coupled plasma mass spectrometry
(ICP-MS) was used after fusing the samples with lithium metaborate and
microwave acid decomposition without preliminary ashing. The proposed sample
preparation methods are characterized by speed and ease of implementation, and
made it possible to use ICP-MS to determine a wide range of elements in each
sample, including Cd, Mo, Sb, Sn, Te, W, Tl, Bi, data on the content of which
were previously unavailable or were estimated approximately during the
certification of SLg-1 and SChS-1. The determination of analyte concentrations
was performed within a single measurement cycle on the magnetic sector mass
spectrometer ELEMENT in low, medium and high resolution using external
calibration with solutions of similar matrix composition in combination with an
internal standard to reduce non-spectral matrix influence. The relative
standard deviation of ICP-MS analysis for most elements after fusion is less
than 10%, after acid decomposition from 6 to 20%.The
necessity of increasing the sample weight to 1 g has been experimentally
established to ensure the representativeness of the sample during ICP-MS
determination of Ag and Au in samples.
Key words:
reference
materials, SLg-1A (SLg-1), SChS-1A (SChS-1), sample preparation, inductively
coupled plasma mass spectrometry (ICP-MS)
Copyright (C) Chemistry Dept., Moscow State University, 2002
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