C. Harzdorf et al., APPLICATION OF MICROWAVE DIGESTION TO TRACE ORGANOELEMENT DETERMINATION IN WATER SAMPLES, Analytica chimica acta, 374(2-3), 1998, pp. 209-214
Microwave digestion is a powerful tool for converting various types of
samples into a solution ready for instrumental measurement. In trace
analysis for heavy metals in water and waste water it may show some li
mitations due to the comparatively high dilution of the digestion reag
ent by the water sample itself. This is proved in this study with orga
nically bound elements to be analyzed, after digestion, by cold vapor
or hydride generation atomic absorption spectrometry, because these te
chniques require the elements to be completely mineralized. The experi
ments were carried out with 2-[(ethylmercury)thio]benzoic acid, D,L-se
lenomethionine and tetraphenylarsonium chloride using microwave digest
ion devices allowing high- and low-pressure digestion. The selenium co
mpound yielded satisfactory results with both digestion modes; in cont
rast the arsenic compound yielded very low recoveries under all test c
onditions applied. The mercury compound gave good recoveries only with
the high-pressure digestion device. Low-pressure digestion revealed s
ignificantly lower results. High concentrations of organic matter may
lead to incomplete digestion and low results because of the developmen
t of high carbon dioxide pressure which causes the feed-back system of
the microwave device to reduce microwave power and, hence, temperatur
e in the batch. Also the digestion mixture may play an important role
as shown by the organoarsenic compound. The quoted limitations should
be taken into account in water analysis particularly if it is intended
to incorporate microwave digestion in standardized procedures. (C) 19
98 Elsevier Science B.V. All nights reserved.