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Fast and precise method for Pb isotope ratio determination in complex matrices using GC-MC-ICPMS: application to crude oil, kerogen, and asphaltene samples.

Analytical chemistry (2012-08-01)
Georgia Sanabria-Ortega, Christophe Pécheyran, Sylvain Bérail, Olivier F X Donard
ABSTRACT

A new method to determine Pb isotope ratio without ion-exchange-matrix separation is proposed. After acid digestion, Pb was ethylated to Et(4)Pb, separated from the digested solution (black shale, asphaltene, crude oil and kerogen) by extraction in isooctane, and then injected into a gas chromatograph coupled to a multicollector inductively coupled plasma mass spectrometer. Seven isotopes ((202)Hg, (203)Tl, (204)Pb, (205)Tl, (206)Pb, (207)Pb, (208)Pb) were monitored simultaneously with peak duration of 23 s. GC elution was operated under wet plasma conditions where a thallium standard solution was introduced to the mass spectrometer for mass bias correction. The total time of the procedure (sample preparation and analysis, after acid digestion) was reduced by a factor of 15 compared to conventional-continuous sample introduction. Data treatment was carried out using the linear regression slope method. Mass bias was corrected using the double correction method (first thallium normalization followed by classical bracketing). For the (208/206)Pb and (207/206)Pb ratios, precision (2RSD(EXT), n = 21) was 49 and 69 ppm, and the bias between experimental results and reference values was better than 0.0033 and 0.0007 ‰, when injecting 1.2 ng of ethylated Pb SRM NIST 981 solution. Results obtained by this method were validated by comparison with those obtained via conventional-continuous sample introduction. The applicability of this approach was demonstrated with the analysis of black shale, asphaltene, crude oil and kerogen samples.

MATERIALS
Product Number
Brand
Product Description

Supelco
2,2,4-Trimethylpentane, analytical standard
Sigma-Aldrich
2,2,4-Trimethylpentane, anhydrous, 99.8%
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2,2,4-Trimethylpentane, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.5%
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2,2,4-Trimethylpentane, puriss. p.a., ACS reagent, ≥99.5% (GC)
Sigma-Aldrich
2,2,4-Trimethylpentane, ReagentPlus®, ≥99%
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2,2,4-Trimethylpentane, puriss. p.a., ≥99.5% (GC)
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2,2,4-Trimethylpentane, ACS reagent, ≥99.0%
Supelco
Density Standard 692 kg/m3, H&D Fitzgerald Ltd. Quality