A method for Se isotope analysis of low ng-level geological samples via double spike and hydride generation MC-ICP-MS

Kurzawa, Timon; König, Stephan; Labidi, Jabrane; Yierpan, Aierken; Schoenberg, Ronny

doi:10.1016/j.chemgeo.2017.06.012

Cited by 38 publications

(58 citation statements)

References 75 publications

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“…Most of the samples analysed in this work were received as fine powder materials, except for sample 15-EDL/007, which was cut by a rock saw into smaller pieces that were then crushed and finally pulverised using an agate disc mill. Analytical procedures are described in detail in 20 , 21 , and only a brief summary of the most important aspects is given here.…”

Section: Methodsmentioning

confidence: 99%

“…For this study, we selected a set of representative mantle peridotites that range in age from Mid-Proterozoic to late Paleozoic and are from different geological settings and localities, including nine samples from orogenic and transitional peridotite massifs (Ronda, Pyrenees, Lanzo and External Ligurides) and two xenoliths from the French Massif Central ( Supplementary Table 1 ). Samples were analysed for Se isotopes on a multi-collector inductively coupled plasma mass spectrometer (MC-ICP-MS) at the University of Tuebingen (Germany) using a double spike and methane-boosted hydride generation technique 20 , 21 (see Methods ). Data are reported in δ 82/76 Se notation ( Supplementary table 2 ), that is, the per mil (‰) variation of 82 Se /76 Se relative to the reference material NIST SRM 3149.…”

Section: Se Isotope Signature Of the Bse Inferred From Peridotitesmentioning

confidence: 99%

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Selenium isotopes as tracers of a late volatile contribution to Earth from the outer Solar System

et al. 2019

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The origin of Earth’s volatiles has been attributed to a late addition of meteoritic material after core-mantle differentiation. The nature and consequences of this 'late veneer' are debated, but may be traced by isotopes of the highly siderophile, or iron-loving, and volatile element selenium. Here we present high-precision selenium isotope data for mantle peridotites, from double spike and hydride generation multi-collector inductively coupled plasma mass spectrometry. These data indicate that the selenium isotopic composition of peridotites is unaffected by petrological processes, such as melt depletion and melt-rock reaction, and thus a narrow range is preserved that is representative of the silicate Earth. We show that selenium isotopes record a signature of late accretion after core formation and that this signature overlaps only with that of the CI-type carbonaceous chondrites. We conclude that these isotopic constraints indicate the late veneer originated from the outer Solar System and was of lower mass than previously estimated. Thus, we suggest a late and highly concentrated delivery of volatiles enabled Earth to become habitable.

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Section: Methodsmentioning

confidence: 99%

Section: Se Isotope Signature Of the Bse Inferred From Peridotitesmentioning

confidence: 99%

Selenium isotopes as tracers of a late volatile contribution to Earth from the outer Solar System

et al. 2019

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“…[ 33 ]. A detailed description of the analytical method for Se isotope measurements employed in this study is given by [ 34 ]. For mass bias correction, a Double Spike approach was used according to [ 35 ] and following [ 34 ].…”

Section: Methodsmentioning

confidence: 99%

“…A detailed description of the analytical method for Se isotope measurements employed in this study is given by [ 34 ]. For mass bias correction, a Double Spike approach was used according to [ 35 ] and following [ 34 ]. This techniques offers the advantage that it is able to correct isotope fractionation occurring at sample preparation, which is essential for Se due to its sensitivity to isotope fractionation and the difficulty to recover Se quantitatively [ 34 , 35 ].…”

Section: Methodsmentioning

confidence: 99%

“…For mass bias correction, a Double Spike approach was used according to [ 35 ] and following [ 34 ]. This techniques offers the advantage that it is able to correct isotope fractionation occurring at sample preparation, which is essential for Se due to its sensitivity to isotope fractionation and the difficulty to recover Se quantitatively [ 34 , 35 ]. An adequate amount of the Se Double Spike solution, calculated from the determined Se concentration to yield a Double Spike/sample-Se ratio of 1:1 [ 36 ], was added to the digested sample before Se purification, which is described in section 2.3.…”

Section: Methodsmentioning

confidence: 99%

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Preparation and purification of organic samples for selenium isotope studies

et al. 2018

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Selenium (Se) is an important micronutrient but also a strong toxin with a narrow tolerance range for many organisms. As such, a globally heterogeneous Se distribution in soils is responsible for various disease patterns (i.e. Se excess and deficiency) and environmental problems, whereby plants play a key role for the Se entrance into the biosphere. Selenium isotope variations were proved to be a powerful tracer for redox processes and are therefore promising for the exploration of the species dependent Se metabolism in plants and the Se cycling within the Critical Zone. Plant cultivation setups enable systematic controlled investigations, but samples derived from them–plant tissue and phytoagar–are particularly challenging and require specific preparation and purification steps to ensure precise and valid Se isotope analytics performed with HG-MC-ICP-MS. In this study, different methods for the entire process from solid tissue preparation to Se isotope measurements were tested, optimized and validated. A particular microwave digestion procedure for plant tissue and a vacuum filtration method for phytoagar led to full Se recoveries, whereby unfavorable organic residues were reduced to a minimum. Three purification methods predominantly described in the literature were systematically tested with pure Se solution, high concentrated multi-element standard solution as well as plant and phytoagar as target matrices. All these methods efficiently remove critical matrix elements, but differ in Se recovery and organic residues. Validation tests doping Se-free plant material and phytoagar with a reference material of known Se isotope composition revealed the high impact of organic residues on the accuracy of MC-ICP-MS measurements. Only the purification method with no detectable organic residues, hydride generation and trapping, results in valid mass bias correction for plant samples with an average deviation to true δ82/76Se values of 0.2 ‰ and a reproducibility (2 SD) of ± 0.2 ‰. For phytoagar this test yields a higher deviation of 1.1 ‰ from the true value and a 2 SD of ± 0.1 ‰. The application of the developed methods to cultivated plants shows sufficient accuracy and precision and is a promising approach to resolve plant internal Se isotope fractionations, for which respective δ82/76Se values of +2.3 to +3.5 ‰ for selenate and +1.2 to +1.9 ‰ for selenite were obtained.

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Chemical Sample Processing for Combined Selenium Isotope and Selenium‐Tellurium Elemental Investigation of the Earth's Igneous Reservoirs

Yierpan

König

Labidi

et al. 2018

Geochem Geophys Geosyst

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The redox‐sensitive, chalcophile, and volatile Se stable isotope system offers new perspectives to investigate the origin and evolution of terrestrial volatiles and the roles of magmatic and recycling processes in the development of the redox contrast between Earth's reservoirs. Selenium isotope systematics become more robust in a well‐constrained petrogenetic context as can be inferred from Se‐Te elemental signatures of sulfides and igneous rocks. In this study, we present a high‐yield chemical sample processing method that allows the determination of Se‐Te concentrations and Se isotope composition from the same sample digest of silicate rocks by hydride generation isotope dilution (ID) quadrupole inductively coupled plasma mass spectrometry (ICP‐MS) and double spike (DS) multicollector (MC)‐ICP‐MS, respectively. Our procedure yields ∼80% Se‐Te recoveries with quantitative separation of relevant interfering elements such as Ge and HG‐buffering metals. Replicate analyses of selected international reference materials yield uncertainties better than 0.11‰ (2 s.d.) on δ82/76Se and 3% (r.s.d.) on Se concentration for DS MC‐ICP‐MS determinations for as low as ∼10 ng sample Se. The precision of Se‐Te concentration measurements by ID ICP‐MS is better than 3% and 5% (r.s.d.) for total amounts of ∼0.5–1 ng Se and ∼0.2–0.5 ng Te, respectively. The basaltic reference materials have variable Se‐Te contents, but their δ82/76Se values are rather uniform (on average 0.23 ± 0.14‰; 2 s.d.) and different from the chondritic value. This altogether provides the methodology and potential to extend the limited data set of coupled Se isotope and Se‐Te elemental systematics of samples relevant to study the terrestrial igneous inventory.

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A method for Se isotope analysis of low ng-level geological samples via double spike and hydride generation MC-ICP-MS

Cited by 38 publications

References 75 publications

Selenium isotopes as tracers of a late volatile contribution to Earth from the outer Solar System

Selenium isotopes as tracers of a late volatile contribution to Earth from the outer Solar System

Preparation and purification of organic samples for selenium isotope studies

Chemical Sample Processing for Combined Selenium Isotope and Selenium‐Tellurium Elemental Investigation of the Earth's Igneous Reservoirs

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