Determination of Pb2+ in water by isotope dilution gas chromatography-mass spectrometry of tetraethyllead formed by reaction with SODIUM TETRAETHYLBORATE (cas 15523-24-7)

Add time:08/27/2019    Source:sciencedirect.com

Aqueous Pb2+ samples in the low ng/g concentration range were spiked with stable isotope 206Pb standards and subsequently ethylated by a simple room-temperature reaction with sodium tetraethylborate. After extraction into heptane, samples were analyzed by gas chromatography-mass spectrometry on a bench-top quadrupole instrument. Detection was performed by single ion monitoring at m/z 293 (triethyl-206Pb ion) and 295 (triethyl-208Pb ion). The technique is rapid, convenient and has good linearity over the tested concentration range of 0.5−100 ng/g. Internal standardization by stable isotope dilution improves the relative standard deviation (for 20−50 ng/g samples, from 24.9% (for externally calibrated determinations) to 4.2% for intra-assay precision and from 35.0% to 8.7% for inter-assay precision. The 206Pb internal standard also discriminates against interference by other metals. The detection limit (3σ) of 0.3 ng/g (for a 2-ml sample) is due primarily to the large relative standard deviation of the blank. Applications to biological matrices are discussed.

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