Determination of trimethyl‐lead in rainwater and road dust by capillary GC MIP‐AE spectrometry after <i>in situ</i> ethylation and extraction

Witte, Claudia; Szpunar-Łobińska, Joanna; Łobiński, Ryszard; Adams, F.

doi:10.1002/aoc.590080712

Cited by 16 publications

(4 citation statements)

References 28 publications

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“…Sample Treatment. The sample treatment procedure for the determination of trimethyllead in road dust was adapted from the work of Witte et al, which was optimized for the isotope dilution technique. The recommended minimum sample intake of 1 g was weighed together with 0.3−0.4 g of a diluted stock spike solution (usually in the range of∼10 ng g -1 , but exactly determined) into a 7-mL vial with screw cap.…”

Section: Methodsmentioning

confidence: 99%

Species-Specific GC/ICP-IDMS for Trimethyllead Determinations in Biological and Environmental Samples

Poperechna

Heumann

2004

Anal. Chem.

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An accurate and sensitive species-specific isotope dilution GC/ICPMS method was developed for the determination of trimethyllead (Me3Pb+) in biological and environmental samples. A trimethyllead spike was synthesized from 206Pb-enriched metallic lead by reaction of lead halide with methyllithium and subsequent formation of trimethyllead iodide. The isotopic composition of the spike solution was determined by GC/ICPMS after derivatization with tetraethylborate, and its concentration was determined by reverse isotope dilution analysis. The species-specific GC/ICP-IDMS method was validated by reference material CRM 605 (urban dust) certified for Me3Pb+. The method was also applied to determine the Me3Pb+ content in six biological reference materials (DORM 2, CRM 278, CRM 422, CRM 463, CRM 477, MURST-ISS-A2) and one sediment reference material (CRM 580) for which no certified values of this species exist. The Me3Pb+ concentrations in the biological reference materials vary in the range of 0.3-17 ng g(-1) (as Pb) except for the Antarctic Krill (MURST-ISS-A2), where the concentration was less than the detection limit of 0.09 ng g(-1), which was also found for the sediment. Up to 20% of total lead was methylated in the biological reference materials, whereas much higher methylation fractions were found for mercury. The method was also applied to seafood samples purchased from a supermarket with Me3Pb+ concentrations in the limited range of 0.3-0.7 ng g(-1). On the contrary, the portion of methylated lead in these samples varied over more than 2 orders of magnitude from 0.02 to 7.5%.

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Section: Methodsmentioning

confidence: 99%

Species-Specific GC/ICP-IDMS for Trimethyllead Determinations in Biological and Environmental Samples

Poperechna

Heumann

2004

Anal. Chem.

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“…The European Community Bureau of Reference (BCR) has started a project aiming to organise an intercomparison study on analysis of Me3Pb + and Et3Pb + species [121]. The analysis of trimethyllead and the preparation of the certificate reference materials (rainwater and urban road dust) are in progress [11,84].…”

Section: Validation Of the Resultsmentioning

confidence: 99%

“…Elution with acetate buffer + CH3OH. HPLC-photometry R 3Pb + rainwater [11] rain and tap water [15] polar snow [3,16], tap water [72] surface [8], lake, river [51], rain water [52] river, lake surface water [54] water [58,59] rainwater [70] drinking, harbour and rain water [79,80] " QT---quartz t~zbe. b R = Me or Et.…”

Section: Sample Pretreatmentmentioning

confidence: 99%

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Organolead speciation in environmental samples: a review

Pyrzyńska

1996

Mikrochim Acta

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Gas Chromatography with Atomic Emission Detection in Environmental Analysis

Pedersen‐Bjergaard

2000

Encyclopedia of Analytical Chemistry

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When capillary gas chromatography (GC) is coupled with atomic emission detection (AED), mixtures of volatile and semivolatile organic compounds are first separated based on different retention in a capillary GC column, whereafter the separated compounds are introduced directly into a helium (or argon) plasma. The high temperature of this plasma results in atomization of the separated compounds followed by excitation of the constituent atoms. From the excited states, the atoms emit light of characteristic wavelengths which are monitored continuously during the chromatographic separation by an optical spectrometer. This results in element‐selective chromatograms, where all elements from the periodic table (except helium or argon) may be monitored selectively with a simple change of wavelength on the spectrometer. With the use of multichannel spectrometers, several elements may be monitored simultaneously resulting in multielemental detection. Both nonmetallic and metallic elements are detected with a very high selectivity. This enables environmental contaminants containing heteroatoms to be determined in dirty extracts without extensive sample cleanup. However, since detection limits (DLs) in GC/AED range from 1–100 pg s −1 , extensive analyte enrichment is often required prior to environmental analysis. Because the separated compounds are atomized within the plasma, only minor structural variations are observed for the detector responses. This, in combination with the multielemental capability, enables estimation of empirical formulas for each of the separated compounds, which may be utilized to support identification of environmental micropollutants. In addition, the structure‐independent detector responses enable simplified calibration for quantitative purposes because different compounds may be quantified based on a single elemental calibration curve.

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Determination of trimethyl‐lead in rainwater and road dust by capillary GC MIP‐AE spectrometry after in situ ethylation and extraction

Cited by 16 publications

References 28 publications

Species-Specific GC/ICP-IDMS for Trimethyllead Determinations in Biological and Environmental Samples

Species-Specific GC/ICP-IDMS for Trimethyllead Determinations in Biological and Environmental Samples

Organolead speciation in environmental samples: a review

Gas Chromatography with Atomic Emission Detection in Environmental Analysis

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