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Multitechnique Determination of Halogens in Soil after Selective Volatilization Using Microwave-Induced Combustion
journal contribution
posted on 2016-11-29, 00:00 authored by L. S.
F. Pereira, M. F. Pedrotti, M. S. P. Enders, C. N. Albers, J. S. F. Pereira, E. M. M. FloresA method
for digestion of soils with high inorganic matter content
(ranging from 50 to 92%) by microwave-induced combustion (MIC) is
proposed for the first time for further halogens (F, Cl, Br, and I)
determination by ion chromatography (IC) and also by inductively coupled
plasma mass spectrometry (ICP-MS). Microcrystalline cellulose (100–500
mg), used as a combustion aid, was mixed with sample and water or
NH4OH solutions (10–100 mmol L–1) were investigated for analytes absorption. The use of cellulose
(400 mg) was mandatory to volatilize the halogens from soils with
high inorganic matter. It was possible to use diluted absorbing solutions
(up to 100 mmol L–1 NH4OH) for halogens
retention, providing limits of quantification in the range of 0.06
(I) to 60 (Cl) μg g–1. Accuracy was evaluated
using certified reference materials (CRMs), spiked samples, and pyrohydrolysis
method. Recoveries for halogens after spiked samples were in the range
of 94 to 103% and the results after digestion of CRMs by MIC were
in agreement better than 95% to certified values. Blanks were low,
relative standard deviation was below 8% for all soils and no statistical
difference was observed for results by pyrohydrolysis and MIC methods
showing the feasibility of the proposed method for further halogens
determination in soil samples.
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Multitechnique Determinationhalogens retentionOHsolutioncombustion aidsoil samplesMicrowave-Induced Combustionreference materialsCRMmicrowave-induced combustioncellulosemmolpyrohydrolysis methodion chromatographyplasma mass spectrometryNHanalytes absorptionmgClhalogens determinationmatter contentMIC methodsSelective VolatilizationICP-MS
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