An automated and high-throughput (36 h–1) method
for extremely sensitive determination of the two main tellurium species
in the environment, namely, tellurite (TeIV) and tellurate
(TeVI), was developed. Flow injection hydride generation
was interfaced for the first time with inductively coupled plasma
triple quadrupole mass spectrometry (ICP–MS/MS) detection to
assure interference-free tellurium analysis. ICP–MS/MS conditions
were studied in detail. Using a mixture of He + O2 gases
in the reaction cell, the background signals significantly dropped
and Xe isobaric interference was eliminated, allowing measurement
with the most abundant Te isotopes, that is, 128Te and 130Te, and offering a huge increase in sensitivity. Volatile
H2Te was selectively generated by a HCl/NaBH4 reaction from TeIV or from both TeIV and TeVI (TeIV+VI) after pre-reduction of TeVI by a TiCl3 solution. The optimum conditions for TiCl3 as a pre-reductant and the pre-reduction kinetics were also
investigated. Different reduction rates were found depending on the
sample stabilization media (HCl, HNO3, or EDTA). The same
sensitivity was found for TeIV and TeVI, measured
after pre-reduction, and no significant matrix effect was observed
in both fresh and seawaters. Therefore, external calibration was used
for quantification in real samples. Under optimal conditions, this
method reached an unprecedented limit of detection of 0.07 ng L–1 for both TeIV and TeIV+VI and
an intra-day repeatability of 5.2% at the 5 ng L–1 level. The methodology was successfully applied to the speciation
analyses in commercially available certified reference materials of
river water and seawater, and in bottled water and lake water samples.