High precision lead isotope ratio measurements by multicollector-ICP-MS in variable matrices

Ehrlich, Sarah; Karpas, Zeev; Ben‐Dor, L.; Halicz, Ludwik

doi:10.1039/b102454j

Cited by 41 publications

(33 citation statements)

References 12 publications

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“…In this way, the internal precision for each analytical session and the long-term reproducibility over a year were obtained. Reproducibility values (calculated as 2 s) for the δ 65 Cu values obtained for the NIST 976 standard along the period of an entire year (n0113) were ±0.027‰ and ±0.039‰ for Ni and Zn, respectively, showing that, as concluded in other recent Cu isotope ratio studies [49][50][51][52][53][54], the use of Ni as internal standard provides superior precision (F-test; F value 02.155; F critical, (P00.05) 0 1.366). In any case, both elements are well-suited for mass bias correction of Cu ratios.…”

Section: Resultssupporting

confidence: 51%

“…For Cu isotopic analysis, two elements are commonly used for this purpose, Zn [5,[43][44][45][46][47][48] and Ni [49][50][51][52][53][54]. According to the literature, both elements seem to be well-suited for mass bias correction affecting the Cu isotope ratio, although marginal precision improvements have been recorded when Ni is used [49][50][51][52][53][54]. As a consequence, a comparative study of Ni and Zn performance was carried out in our investigation.…”

Section: Resultsmentioning

confidence: 99%

“…This chromatographic separation, however, is not perfect and still shows problems related to the poor specificity of the resin for this element: (1) difficulty to obtain quantitative recovery and therefore, the necessity to check for possible on-column fractionation; (2) non-efficient removal of potentially interfering elements (e.g., Na, giving rise to formation of 40 Ar 23 Na + , the signal of which overlaps with that of 63 Cu + ); (3) strong dependence of the elution protocol on the sample characteristics. For these reasons, some authors have avoided the use of Cu column isolation and have proposed alternative approaches such as hand-picking of Cu-containing fractions in Cu minerals [28,59], or even direct Cu isotopic analysis without target element isolation, which could provide acceptable results in some instances [54,56].…”

Section: Isolation Of the Target Elementsmentioning

confidence: 99%

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Copper and tin isotopic analysis of ancient bronzes for archaeological investigation: development and validation of a suitable analytical methodology

et al. 2012

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Although in many cases Pb isotopic analysis can be relied on for provenance determination of ancient bronzes, sometimes the use of "non-traditional" isotopic systems, such as those of Cu and Sn, is required. The work reported on in this paper aimed at revising the methodology for Cu and Sn isotope ratio measurements in archaeological bronzes via optimization of the analytical procedures in terms of sample pre-treatment, measurement protocol, precision, and analytical uncertainty. For Cu isotopic analysis, both Zn and Ni were investigated for their merit as internal standard (IS) relied on for mass bias correction. The use of Ni as IS seems to be the most robust approach as Ni is less prone to contamination, has a lower abundance in bronzes and an ionization potential similar to that of Cu, and provides slightly better reproducibility values when applied to NIST SRM 976 Cu isotopic reference material. The possibility of carrying out direct isotopic analysis without prior Cu isolation (with AG-MP-1 anion exchange resin) was investigated by analysis of CRM IARM 91D bronze reference material, synthetic solutions, and archaeological bronzes. Both procedures (Cu isolation/no Cu isolation) provide similar δ 65 Cu results with similar uncertainty budgets in all cases (±0.02-0.04 per mil in delta units, k02, n0 4). Direct isotopic analysis of Cu therefore seems feasible, without evidence of spectral interference or matrix-induced effect on the extent of mass bias. For Sn, a separation protocol relying on TRU-Spec anion exchange resin was optimized, providing a recovery close to 100 % without oncolumn fractionation. Cu was recovered quantitatively together with the bronze matrix with this isolation protocol. Isotopic analysis of this Cu fraction provides δ 65 Cu results similar to those obtained upon isolation using AG-MP-1 resin. This means that Cu and Sn isotopic analysis of bronze alloys can therefore be carried out after a single chromatographic separation using TRU-Spec resin. Tin isotopic analysis was performed relying on Sb as an internal standard used for mass bias correction. The reproducibility over a period of 1 month (n042) for the mass bias-corrected Sn isotope ratios is in the range of 0.06-0.16 per mil (2 s), for all the ratios monitored.

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Section: Resultssupporting

confidence: 51%

Section: Resultsmentioning

confidence: 99%

Section: Isolation Of the Target Elementsmentioning

confidence: 99%

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Copper and tin isotopic analysis of ancient bronzes for archaeological investigation: development and validation of a suitable analytical methodology

et al. 2012

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“…Some of the previous studies demonstrated that there was no significant effect on the analytical performance of MC-ICPMS when the total ion concentration was less than 400 or 700 mg kg -1 , 22,23 and thus was more robust than TIMS. In this study, however, the results shown above demonstrated that the matrix elements in the sample solutions affected the accuracy of the Pb isotope ratio measurement by MC-ICPMS.…”

Section: Effect On Biasmentioning

confidence: 99%

Isotope Ratio Analysis of Lead in Blood and Environmental Samples by Multi-collector Inductively Coupled Plasma Mass Spectrometry

et al. 2011

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“…Therefore, it enables the precise measurement of isotope compositions for a wide range of elements combined with excellent detection limits. Isotope ratio determinations by MC-ICP-MS can provide external precision as low as 0.002% RSD (2 sigma) [7,8,9] for different elements. However, these results are based entirely on measurements using continuous sample introduction.…”

Section: Introductionmentioning

confidence: 99%

Measurement of isotope ratios on transient signals by MC-ICP?MS

Günther-Leopold

Wernli

Kopajtic

et al. 2004

Analytical and Bioanalytical Chemistry

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Precise and accurate isotope ratio measurements are an important task in many applications such as isotope-dilution mass spectrometry, bioavailability studies, or the determination of isotope variations in geological or nuclear samples. The technique of MC-ICP-MS has attracted much attention because it permits the precise measurement of isotope compositions for a wide range of elements combined with excellent detection limits due to high ionisation efficiencies. However, the results are based mainly on measurements using continuous sample introduction. In the present study the determination of isotope ratios on various transient signals with a time duration of 30 to 60 s has been achieved by coupling high-performance liquid chromatography to a multicollector inductively coupled plasma mass spectrometer. In order to investigate the origin of ratio drifts across the transient signals for this hyphenated technique, measurements with the same standard solutions were also carried out using a flow-injection device for sample introduction. As a result of this application it could be concluded that the main source of the bias in the measured isotope ratios is within the ICP-MS instead of fractionation effects on the chromatographic column material. Preliminary studies on short transient signals of gaseous samples (dry plasma) showed a reverse fractionation effect compared with wet plasma conditions (flow injection and HPLC).

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High precision lead isotope ratio measurements by multicollector-ICP-MS in variable matrices

Cited by 41 publications

References 12 publications

Copper and tin isotopic analysis of ancient bronzes for archaeological investigation: development and validation of a suitable analytical methodology

Copper and tin isotopic analysis of ancient bronzes for archaeological investigation: development and validation of a suitable analytical methodology

Isotope Ratio Analysis of Lead in Blood and Environmental Samples by Multi-collector Inductively Coupled Plasma Mass Spectrometry

Measurement of isotope ratios on transient signals by MC-ICP?MS

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