Speciation of trimethyllead in rainwater by gas chromatography-mass spectrometry after ethylation with sodium tetraethylborate comparison with other alkylation methods

In situ ethylation of organolead, organotin and organomercury species by bromomagnesium tetraethylborate prior to GC‐ICP‐MS analysis

“…Thus, characteristic peaks were detected at m/z 120, 197 and 351 for triphenyltin; 121, 179, 235, 291 for tributyltin; 149, 207, 263, for dibutyltin and 149, 177, 235 for monobutyltin. The characteristic peaks for methyllead and inorganic lead compounds were also consistent with those reported in the literature [25,26]; at m/z 207, 236, 266 for trimethyllead; 208, 223, 267 for dimethyllead and 208, 237 and 295 for tetraethyllead. Figure 1a shows the chromatogram obtained for the speciation of organotin by GC-MS analyses.…”

Mass spectrometry studies of organolead compounds

“…Figure 6 shows a common fragmentation pathway for these two compounds. It is similar, in many respects, to the reaction pathway for R 3 PbCl compounds. For example, there is an initial loss of either an R group or a chlorine atom.…”

“…The EI À spectra of these two compounds indicate the presence of a very stable Ph 3 Pb À ion (m/z 439, RA = 100%, when R = Ph and RA = 95% when R = Cl). This is in contrast to the analogous species Ph 3 Sn À and Ph 3 Ge À , which were not detected in the EI À mass spectra of similar compounds.…”

“…Organolead compounds are of great environmental interest. For example, tetraalkyllead (TAL) compounds in air, 1 road dust 2 and rainwater 3 have been trapped and measured using gas chromatography-mass spectrometry (GC-MS) in the single ion monitoring (SIM) mode. Furthermore, there is some evidence for formation of alkyllead compounds in the natural environment from inorganic lead.…”

Hybrid Methods of Speciation

“…However, the systems used often lacked sensitivity. This area has expanded recently as inexpensive, smaller and more sensitive instruments have become available (Zufiaurre et al, 1997). Tributyl tin and triphenyl tin compounds have recently been determined in seawater using GC negative ion chemical ionisation MS (Mizuishi et al, 1998).…”