Extraction, clean-up and determination of ionic alkyllead compounds in road dust by gas chromatography–mass spectrometry

Abstract

An experimental study of the clean-up before and after derivatization with BuMgCl in the determination of Me3Pb+, Et3Pb+ and Pb2+ in road dust is described. The analytical procedure consisted of an extraction at pH 9.0 (buffer) of the diethyldithiocarbamate complex in pentane followed by the evaporation to dryness and derivatization in hexane with BuMgC1. Me3BuPb, Et3BuPb and Bu4Pb are separated and quantified by gas chromatography-mass spectrometry in the selected ion monitoring mode. The adsorbents Florisil, Silicagel, alumina, Amberlite (XAD-2 and XAD-7) and Chromosorb with 3% and 10% deactivation degree were investigated for the clean-up. Prior to derivatization, Florisil, Silicagel and Alumina retained all the diethyldithiocarbamate complexes. The Amberlites (XAD-2 and XAD-7) and Chromosorb did not trap either diethyldithiocarbamate complexes or other interference compounds. After derivatization, alumina was to be the most effective adsorbent. Under these conditions, a recovery of 86.5% of Me3Pb+ was obtained using a road dust sample.

Speciation analysis of lead in marine animals by using capillary electrophoresis couple online with inductively coupled plasma mass spectrometry

“…The extraction method must be capable of completely extracting each lead species from samples without altering the individual lead species. So far, some methods including traditional liquid extraction and supercritical fluid extraction have been developed to extract different lead compounds in sand, road dust, and mussels . However, these methods can only effectively extract organolead compounds since they used hexane as solvent.…”

Isotope ratio measurements using gas chromatography inductively coupled plasma mass spectrometry for the assessment of organolead sources

“…The peak from inorganic lead was small due to the fact that EDTA was added during the extraction as DDTC complexes to prevent the extraction of inorganic lead. 37 Fig. 4 was modified according to a referee to show the inorganic Pb peak.…”

“…The compounds are almost completely degraded to inorganic lead during combustion, but both diand trialkyllead compounds have been detected in most environmental samples during recent years. [31][32][33][34][35][36][37][38][39] The isotopic composition of lead in compounds found in environmental samples should reflect the average isotopic composition of lead in the petrol used in the area and could be quite different from the isotopic composition found for inorganic lead in the same samples. In that sense, the sources of lead in environmental samples should be investigated.…”

Speciation of mercury, tin, and lead compounds by gas chromatography with microwave-induced plasma and atomic-emission detection (GC–MIP–AED)

“…The extraction of lead compounds from sediments and particulate matter can be performed under mild conditions by use of organic solvents in the presence of complexing agents [107,130], supercritical CO 2 modified with methanol [131], buffer solutions of pH 4, or direct dissolution in water containing NaCl [121]. Most of these procedures give satisfactory yields for Me 3 Pb + and Et 3 Pb + , but not for dialkyllead species.…”