Development of reference materials for in-situ Rb-Sr isotopic dating by laser ablation ICP-MS/MS and its application to W-Sn deposits in the French Massif Central

Abstract. Latest advances in laser ablation inductively coupled plasma mass spectrometer (LA-ICPMS) allow for accurate in situ U−Pb dating of carbonate material, with final age uncertainties usually >3 % 2σ. Cross-laboratory reference materials (RMs) used for sample-bracketing are currently limited to WC1 calcite with an age of 254.4±6.5 (2σ). The minimum uncertainty on any age determination with the LA-ICPMS method is therefore ≥2.5 %, and validation by secondary RMs is usually performed on in-house standards. This contribution presents a new reference material, ASH-15, a flowstone that is dated here by isotope dilution (ID) thermal ionization mass spectrometry (TIMS) analysis using 37 sub-samples, 1–7 mg each. Age results presented here are slightly younger compared to previous ID isotope ratio mass spectrometry (IRMS) U−Pb dates of ASH-15 but within uncertainties and in agreement with in situ analyses using WC1 as the primary RM. We provide new correction parameters to be used as primary or secondary standardization. The suggested 238U∕206Pb apparent age, not corrected for disequilibrium and without common-lead anchoring, is 2.965±0.011 Ma (uncertainties are 95 % confidence intervals). The new results could improve the propagated uncertainties on the final age with a minimal value of 0.4 %, which is approaching the uncertainty of typical ID analysis on higher-U materials such as zircon. We show that although LA-ICPMS spot analyses of ASH-15 exhibit significant scatter in their isotopic ratios, the down-hole fractionation of ASH-15 is similar to that of other reference materials. This high-U (≈1 ppm) and low-Pb (<0.01 ppm) calcite is most appropriate as a reference material for other speleothem-type carbonates but requires more-sensitive ICP-MS instruments such as the new generation of single-collector and multi-collector ICP-MS. Reference materials with high-Pb and low-U or both low-U and low-Pb compositions are still needed to fully cover the compositional range of carbonate material but may introduce analytical challenges.

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Further characterization of SA01 and SA02 zircon reference materials for Si and Zr isotopic compositions via femtosecond laser ablation MC-ICP-MS

Journal of Analytical Atomic Spectrometry ◽

10.1039/d1ja00160d ◽

2021 ◽

Vol 36 (10) ◽

pp. 2192-2201

Author(s):

Chao Huang ◽

Hao Wang ◽

Hui-Min Yu ◽

Lan-Ping Feng ◽

Lie-Wen Xie ◽

...

Keyword(s):

Laser Ablation ◽

Femtosecond Laser ◽

Reference Materials ◽

Analytical Methods ◽

Femtosecond Laser Ablation ◽

Isotopic Analysis ◽

Isotopic Data ◽

Icp Ms

We present Si and Zr isotopic data of SA01 and SA02 zircons via multi-technique analytical methods to evaluate the suitability of the two zircon reference materials for in situ Si and Zr isotopic analysis using fs-LA-MC-ICP-MS.

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In situ Fe isotopic analyses of fourteen reference materials using a synthetic Cr standard for mass bias and isobaric interference corrections by femtosecond LA-MC-ICP-MS

Journal of Analytical Atomic Spectrometry ◽

10.1039/d0ja00465k ◽

2021 ◽

Author(s):

Lei Xu ◽

Wen Zhang ◽

Tao Luo ◽

Jin-Hui Yang ◽

Zhaochu Hu

Keyword(s):

Reference Materials ◽

Isotope Ratios ◽

Isobaric Interference ◽

Analytical Technique ◽

Mass Bias ◽

Icp Ms ◽

Isotopic Analyses

High precise and accurate measurements of Fe isotope ratios for fourteen reference materials from the USGS, MPI-DING and CGSG were successfully carried out using a developed analytical technique by fs...

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In-situ determination of antimony isotope ratios in Sb minerals by femtosecond LA-MC-ICP-MS

Journal of Analytical Atomic Spectrometry ◽

10.1039/d1ja00089f ◽

2021 ◽

Author(s):

Andreas Benjamin Kaufmann ◽

Marina Lazarov ◽

Stefan Kiefer ◽

Juraj Majzlan ◽

Stefan Weyer

Keyword(s):

Laser Ablation ◽

Femtosecond Laser ◽

Femtosecond Laser Ablation ◽

Isotope Ratios ◽

Icp Ms

Here we present a method for in-situ determination of stable antimony (Sb) isotope compositions by ultraviolet (UV)-femtosecond-laser-ablation-multi-collector-ICP-MS (fs-LA-MC-ICP-MS). Metallic antimony and a number of Sb minerals (stibnite, senarmontite, chalcostibite, tetrahedrite,...

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In-situ trace element characterization of three gold reference materials using EPMA and LA-ICP-MS

10.4095/299097 ◽

2016 ◽

Author(s):

D Milidragovic ◽

G Beaudoin ◽

S E Jackson

Keyword(s):

Trace Element ◽

Reference Materials ◽

Icp Ms

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In situ determination of precise stable Si isotope ratios by UV-femtosecond laser ablation high-resolution multi-collector ICP-MS

Chemical Geology ◽

10.1016/j.chemgeo.2007.12.003 ◽

2008 ◽

Vol 249 (1-2) ◽

pp. 155-166 ◽

Cited By ~ 57

Author(s):

Jérôme Chmeleff ◽

Ingo Horn ◽

Grit Steinhoefel ◽

Friedhelm von Blanckenburg

Keyword(s):

Laser Ablation ◽

High Resolution ◽

Femtosecond Laser ◽

Femtosecond Laser Ablation ◽

Isotope Ratios ◽

Icp Ms ◽

Si Isotope

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Development of sulfide reference materials for in situ platinum group elements and S–Pb isotope analyses by LA-(MC)-ICP-MS

Journal of Analytical Atomic Spectrometry ◽

10.1039/c8ja00305j ◽

2018 ◽

Vol 33 (12) ◽

pp. 2172-2183 ◽

Cited By ~ 6

Author(s):

Yantong Feng ◽

Wen Zhang ◽

Zhaochu Hu ◽

Yongsheng Liu ◽

Kang Chen ◽

...

Keyword(s):

Hydrothermal Synthesis ◽

Reference Materials ◽

Platinum Group Elements ◽

Pb Isotopes ◽

Synthetic Method ◽

Pb Isotope ◽

Icp Ms ◽

Platinum Group ◽

Isotope Analyses

A new synthetic method has been used to prepare sulfide reference materials for the in situ analysis of PGEs and S–Pb isotopes. The results indicate that the hydrothermal synthesis of the nanoparticles can serve as a potentially effective approach for the preparation of microanalysis reference materials.

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In situ 87Sr/86Sr investigation of igneous apatites and carbonates using laser-ablation MC-ICP-MS

Geochimica et Cosmochimica Acta ◽

10.1016/s0016-7037(02)01048-7 ◽

2003 ◽

Vol 67 (2) ◽

pp. 289-302 ◽

Cited By ~ 69

Author(s):

Martin Bizzarro ◽

Antonio Simonetti ◽

R.K. Stevenson ◽

Stephan Kurszlaukis

Keyword(s):

Laser Ablation ◽

Icp Ms

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Assessment of Five Monazite Reference Materials for U-Th/Pb Dating Using Laser-Ablation ICP-MS

Geosciences ◽

10.3390/geosciences9090391 ◽

2019 ◽

Vol 9 (9) ◽

pp. 391

Author(s):

Richter ◽

Nebel-Jacobsen ◽

Nebel ◽

Zack ◽

Mertz-Kraus ◽

...

Keyword(s):

Laser Ablation ◽

Reference Material ◽

Reference Materials ◽

Operational Conditions ◽

Inductively Coupled ◽

Phosphate Mineral ◽

Icp Ms ◽

Wide Range ◽

Absolute Age ◽

Key Aspects

Monazite is a common accessory phosphate mineral that occurs under a wide range of pressure and temperature conditions in sedimentary, metamorphic and igneous rocks. Monazite contains high amounts of Th and U, rendering single monazite grains suitable for in-situ U-Th/Pb dating using laser ablation inductively-coupled mass spectrometry (LA-ICP-MS). Two key aspects of monazite dating that are critical for accurate age data with maximum precision are (i) optimized instrumental conditions to minimize analytical scatter and (ii) a well characterized reference material to ensure the accuracy of the obtained aged. Here, we analyzed five monazite reference materials (USGS 44069, 94-222, MAdel, Moacir and Thompson Mine Monazite) for their U-Th/Pb ages using LA-ICP-MS technique and applied a variety of laser spot diameters and repetition rates to find the best operational conditions to achieve accurate age data while maintaining maximum precision. We find that a spot diameter of 10 µm and a repetition rate of 10 Hz yield the most precise ages with a deviation of ±2.0% from their respective high-precision U/Pb literature age data. Ages were reproduced in three different LA-ICP-MS laboratories using these parameters. Each reference material was tested for its suitability as a matrix-matched age reference material. For this, a rotating, iterative approach was adopted in which one reference monazite was used as calibration reference material against all others, which were treated as unknowns. The results reveal that USGS 44069, 94-222, Thompson Mine Monazite and MAdel all agree with their respective calculated ages and ID-TIMS reference ages and thus are suggested as suitable calibration reference materials. Moacir, however, appears slightly older than previously suggested (up to 4%), thus, caution is advised here when using Moacir as reference material for U-Th/Pb LA-ICP-MS dating in the absence of further absolute age calibration.

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