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A study of sample mineralization methods for arsenic analysis of blood and urine by hydride generation and graphite furnace atomic absorption spectrometry

100%
Sysalova J., Spevackova V.
|
EN
Mineralization procedures for blood and urine suitable for the determination of arsenic by Hydride Generation Atomic Absorption Spectrometry (HGAAS) are studied on model samples, and the results are utilized in biological monitoring investigations. The objective of this work is to obtain good total As recoveries for both matrices regardless of added As species (As(III), As(V), DMA, MMA, AsB, or AsC). Prior to the HGAAS analyses, preparation procedures were controlled under optimised conditions by graphite furnace atomic absorption spectrometry (GFAAS). Two preparation procedures for urine give As recoveries close to 100% by HGAAS: a) dry ashing at 420°C with Mg(NO3)2 on a hot plate, and b) microwave oven decomposition with (NH4)2S2O8. For blood samples, As recoveries by HGAAS range between 95 and 108% for all species when using dry ashing after a pretreatment of samples with HNO3 and H2O2 in a microwave oven. Wet digestion with (NH4)2S2O8 in a microwave oven gives recoveries very near 100% for Asinorg. and MMA. For other As species in spiked blood samples, recoveries of less than 20% As are found. Precision and detection limits obtained by both techniques are evaluated as well. For arsenic concentrations of 20 μg dm−3 or more in blood and urine, a chemical modifier is recommended for GFAAS analysis; it may or may not be proceeded by a mineralization step. For low As levels encountered in the unexposed population, the HGAAS technique provides reliable results only if a very complete mineralization procedure is used.
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Methodological study of extraction procedures applied to urban particulate matter

81%
Sysalova J., Szakova J., Goessler W., Tremlova J.
Open Chemistry
|
2011
|
vol. 9
|
issue 6
1071-1079
EN
The modified BCR three-step sequential extraction procedure has been applied to two different samples of urban particulate matters (PM). The distribution of selected trace elements As, Cd, Cr, Mn, Ni, Pb, Zn was investigated and, in a comparative study, the presence of common organic air filters in extraction procedures was evaluated. Analytes in separate fractions were determined by ICP-OES and GFAAS, respectively, depending on concentration levels. While, due to air filters, a significant increase of some analytes mobility in individual fractions has been observed in case of the jet-milled PM (tunnel Letna), but in case of the PKC sample such effect was not found. The analyte impurities built in some filters has been tested, and the impact on the reliability of analyte results has been discussed. The arsenic species occurrence and their stability in presence of air filters (size 47 mm) were investigated in both urban PM samples as well, using HPLC-ICP-MS technique. Water soluble and by three-step BCR procedure extractable arsenic forms are shown in chromatograms
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