COMPLETELY INTEGRATED ONLINE DETERMINATION OF DISSOLVED SELENIUM(IV) AND TOTAL INORGANIC SELENIUM IN SEA-WATER BY FLOW-INJECTION HYDRIDE GENERATION ATOMIC FLUORESCENCE SPECTROMETRY
Yz. He et al., COMPLETELY INTEGRATED ONLINE DETERMINATION OF DISSOLVED SELENIUM(IV) AND TOTAL INORGANIC SELENIUM IN SEA-WATER BY FLOW-INJECTION HYDRIDE GENERATION ATOMIC FLUORESCENCE SPECTROMETRY, Journal of analytical atomic spectrometry (Print), 13(11), 1998, pp. 1291-1296
Highly sensitive on-line pre-treatment methods were developed for the
direct determination of trace amounts of selenite and total inorganic
Se in sea-water. Selenite determination was carried out on samples aci
dified with HCl and merged on-line with 5% m/v KH2PO4, which was emplo
yed as an interference eliminating reagent. For total inorganic Se det
ermination, acidified samples were merged with 30% m/v NaBr, used for
reduction of Se(VI), and pre-reduced on-line by microwave irradiation
at 210 W for 60 s. After pre-treatment, the sample zone was stored in
a coil and then transported at a how rate of 22 ml min(-1) for reactio
n with 1.5% m/v NaBH4. The hydride produced was separated and dried an
d Se was determined in a mini-hydrogen diffusion flame by non-dispersi
ve atomic fluorescence spectrometry. The interface developed for this
purpose makes possible the integration, within the same manifold, of t
wo steps involving very different reaction times. The detection limits
were 5 ng l(-1) for Se(IV) and 4 ng l(-1) for total inorganic Se. The
recoveries of selenite at the: 30 ng l(-1) level were 94-104% and tho
se of total inorganic Se, at the same concentration level, were 92-98%
. The methods developed are suitable for the accurate and direct analy
sis of natural waters, and the results obtained for total inorganic Se
determination in a freshwater reference material were in good agreeme
nt with the certified value.