Precise isotope-ratio measurements of lead species by capillary gas chromatography hyphenated to hexapole Multicollector ICP-MS

Eva Maria Krupp, C Pecheyran, S Meffan-Main, O F X Donard

Research output: Contribution to journalArticle

42 Citations (Scopus)

Abstract

The precision and accuracy of lead isotope-ratio determination on a short transient signal has been assessed by coupling capillary gas chromatography to the Isoprobe (Micromass, UK), a single-focusing inductively coupled plasma mass spectrometer with multicollector detection. A T-piece connecting the GC transfer line to the torch enabled continuous aspiration of thallium solution for mass-bias correction. The volatile lead species PbEt4 was derivatized from NIST isotopic certified lead standard SRM 981 and different amounts of PbEt4 dissolved in iso-octane were injected into the GC. Chromatograms were recorded in multicollection mode by use of Faraday cups; seven isotopes (Pb-204, Pb-206, Pb-207, Pb-208, Tl-203, Tl-205, and Hg-202) were monitored simultaneously at a transient resolution of 160 ms. PbEt4 peaks were obtained with a half-width of 1.2 s and a base width of 3.5 s. Lead isotope ratios were calculated from the peak areas integrated for each lead isotope, giving precision in the range of 0.02 to 0.07% for ratios of high-abundant isotopes and injections of 5 and 50 pg absolute amount as lead (five replicates). Mass bias was found to be about 0.5% per mass unit and was corrected by using the continuously measured thallium signals at Tl-203 and Tl-205. After mass-bias correction, deviation of the certified lead ratio values was found to be in the range of 0.02 to 0.15% accuracy.

Original languageEnglish
Pages (from-to)573-580
Number of pages8
JournalFresenius’ Journal of Analytical Chemistry
Volume370
Issue number5
Publication statusPublished - Jul 2001

Keywords

  • PLASMA-MASS SPECTROMETRY
  • SPECIATION ANALYSIS
  • TRACE-METAL
  • FRACTIONATION
  • SEDIMENTS
  • DILUTION
  • PB
  • REDUCTION
  • SAMPLES
  • WINE

Cite this

Precise isotope-ratio measurements of lead species by capillary gas chromatography hyphenated to hexapole Multicollector ICP-MS. / Krupp, Eva Maria; Pecheyran, C ; Meffan-Main, S ; Donard, O F X .

In: Fresenius’ Journal of Analytical Chemistry, Vol. 370, No. 5, 07.2001, p. 573-580.

Research output: Contribution to journalArticle

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abstract = "The precision and accuracy of lead isotope-ratio determination on a short transient signal has been assessed by coupling capillary gas chromatography to the Isoprobe (Micromass, UK), a single-focusing inductively coupled plasma mass spectrometer with multicollector detection. A T-piece connecting the GC transfer line to the torch enabled continuous aspiration of thallium solution for mass-bias correction. The volatile lead species PbEt4 was derivatized from NIST isotopic certified lead standard SRM 981 and different amounts of PbEt4 dissolved in iso-octane were injected into the GC. Chromatograms were recorded in multicollection mode by use of Faraday cups; seven isotopes (Pb-204, Pb-206, Pb-207, Pb-208, Tl-203, Tl-205, and Hg-202) were monitored simultaneously at a transient resolution of 160 ms. PbEt4 peaks were obtained with a half-width of 1.2 s and a base width of 3.5 s. Lead isotope ratios were calculated from the peak areas integrated for each lead isotope, giving precision in the range of 0.02 to 0.07{\%} for ratios of high-abundant isotopes and injections of 5 and 50 pg absolute amount as lead (five replicates). Mass bias was found to be about 0.5{\%} per mass unit and was corrected by using the continuously measured thallium signals at Tl-203 and Tl-205. After mass-bias correction, deviation of the certified lead ratio values was found to be in the range of 0.02 to 0.15{\%} accuracy.",
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