Determination of lead isotope ratios in seawater by quadrupole inductively coupled plasma mass spectrometry after Mg(OH)2 co-precipitation

Dominik Weiss, Edward A. Boyle, Valérie Chavagnac, Marco Herwegh, Jingfeng Wu

Research output: Contribution to journalArticle

35 Citations (Scopus)

Abstract

A low blank Mg(OH)2 pre-concentration method was evaluated for the determination of lead isotope ratios (208Pb/206Pb, 207Pb/206Pb) in seawater using a quadrupole ICP-MS VG Plasma Quad II+. Possible matrix effects derived from the Mg(OH)2 co-precipitate were assessed by spiking lead-free seawater (PbFS) and 1% (v/v) HNO3 with the certified common lead standard NBS 981 to give solutions with concentrations in the lower picogram per millilitre range. The standard curves for all three masses were linear in both matrices with minor signal loss (approximately 18%) in the Mg matrix. Mass fractionation showed similar mass biases (<2% frac./amu) for 208Pb/206Pb and 207Pb/206Pb in both seawater and 1% (v/v) HNO3, indicating that there is no significant matrix influence on the isotope ratio determination. Using the Mg(OH)2 precipitation method, real seawater samples were pre-concentrated approximately 28-fold, and 1 ml of 5% (v/v) HNO3 end volume was used for the subsequent measurement. The data acquisition parameters dwell time, replicates per analysis, and acquisition time were first varied to optimize analytical precision and accuracy of the ICP-MS measurements. On the basis of these results, approximately 0.5 ml of pre-concentrated solution was finally used employing a low-flow, CETAC microconcentric nebulizer to minimize sample consumption and extend acquisition time. Analyzing 18 seawater samples from the North Atlantic, the average 1 σ external precision of triplicate measurements was approximately 0.3% for both ratios, 208Pb/206Pb and 207Pb/206Pb, at the level of approximately 20 pg ml-1 Pb. Blanks accounted for less than 3% of total lead analyzed for each sample. Six samples were also measured with TIMS and agreed in average within 0.26% for 207Pb/206Pb and 0.37% for 208Pb/206Pb. Three surface water samples from the Sargasso Sea, collected in 1989, showed ratios in line with previous published ratios from the western North Atlantic.

Original languageEnglish (US)
Pages (from-to)363-374
Number of pages12
JournalSpectrochimica Acta, Part B: Atomic Spectroscopy
Volume55
Issue number4
DOIs
StatePublished - Apr 28 2000
Externally publishedYes

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lead isotopes
Inductively coupled plasma mass spectrometry
inductively coupled plasma mass spectrometry
isotope ratios
Coprecipitation
Seawater
Isotopes
Lead
quadrupoles
blanks
matrices
Sargasso Sea
acquisition
Inductively coupled plasma
spiking
Fractionation
Surface waters
dwell
Precipitates
Data acquisition

ASJC Scopus subject areas

  • Analytical Chemistry
  • Spectroscopy

Cite this

Determination of lead isotope ratios in seawater by quadrupole inductively coupled plasma mass spectrometry after Mg(OH)2 co-precipitation. / Weiss, Dominik; Boyle, Edward A.; Chavagnac, Valérie; Herwegh, Marco; Wu, Jingfeng.

In: Spectrochimica Acta, Part B: Atomic Spectroscopy, Vol. 55, No. 4, 28.04.2000, p. 363-374.

Research output: Contribution to journalArticle

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abstract = "A low blank Mg(OH)2 pre-concentration method was evaluated for the determination of lead isotope ratios (208Pb/206Pb, 207Pb/206Pb) in seawater using a quadrupole ICP-MS VG Plasma Quad II+. Possible matrix effects derived from the Mg(OH)2 co-precipitate were assessed by spiking lead-free seawater (PbFS) and 1{\%} (v/v) HNO3 with the certified common lead standard NBS 981 to give solutions with concentrations in the lower picogram per millilitre range. The standard curves for all three masses were linear in both matrices with minor signal loss (approximately 18{\%}) in the Mg matrix. Mass fractionation showed similar mass biases (<2{\%} frac./amu) for 208Pb/206Pb and 207Pb/206Pb in both seawater and 1{\%} (v/v) HNO3, indicating that there is no significant matrix influence on the isotope ratio determination. Using the Mg(OH)2 precipitation method, real seawater samples were pre-concentrated approximately 28-fold, and 1 ml of 5{\%} (v/v) HNO3 end volume was used for the subsequent measurement. The data acquisition parameters dwell time, replicates per analysis, and acquisition time were first varied to optimize analytical precision and accuracy of the ICP-MS measurements. On the basis of these results, approximately 0.5 ml of pre-concentrated solution was finally used employing a low-flow, CETAC microconcentric nebulizer to minimize sample consumption and extend acquisition time. Analyzing 18 seawater samples from the North Atlantic, the average 1 σ external precision of triplicate measurements was approximately 0.3{\%} for both ratios, 208Pb/206Pb and 207Pb/206Pb, at the level of approximately 20 pg ml-1 Pb. Blanks accounted for less than 3{\%} of total lead analyzed for each sample. Six samples were also measured with TIMS and agreed in average within 0.26{\%} for 207Pb/206Pb and 0.37{\%} for 208Pb/206Pb. Three surface water samples from the Sargasso Sea, collected in 1989, showed ratios in line with previous published ratios from the western North Atlantic.",
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AU - Wu, Jingfeng

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