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

cited By 40International audienceThe 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 (204Pb, 206Pb, 207Pb, 208Pb, 203Tl, 205Tl, and 202Hg) 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 203Tl and 205Tl. 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

Precise isotope-ratio determination by CGC hyphenated to ICP- MCMS for speciation of trace amounts of gaseous sulfur, with SF6 as example compound

cited By 33International audienceCapillary gas chromatography coupled to an inductively coupled plasma mass spectrometer with multiple-collector detection (GC-ICP-MCMS) has been used to assess the precision and instrumental mass bias in sulfur isotope-ratio determination for the gaseous sulfur species SF6. The isotopic composition of the compound was certified by the institute for reference materials and measurements (IRMM, Belgium) and is available as PIGS 2010. Integration of the peaks (peak half-width 1.4 s) was performed using a special peak-integration method based on definition of the integration area by assessment of a uniform isotope-ratio area within the chromatographic peak. Instrumental mass bias was determined to be approximately 12% per mass unit and proved to be stable in the concentration range measured. Replicate injections of 2, 10, 20, and 30 ng (as S) SF6 diluted in argon gave precision for the 32S/34S ratio from 0.6% RSD for 2-ng injections to 0.03% RSD for 30-ng injections. The 32S/33S and 33S/34S isotope-ratio precision was better than 0.4% RSD for injections of 10 ng (as S) and higher. Detection limits were in the absolute pg range for all measured sulfur isotopes. © Springer-Verlag 2004