Femtosecond laser ablation-ICP-mass spectrometry analysis of a heavy metallic matrix: Determination of platinum group metals and gold in lead fire-assay buttons as a case study

In situ laser ablation analyses rely on the microanalytical homogeneity of reference materials (RMs) and a similar matrix and mass fraction between unknown samples and RMs to obtain reliable results. Suitable carbonate and phosphate RMs for determination of Sr isotope ratios in such materials are limited. Thus, we determined 87Sr/86Sr ratios of several carbonate (JCt-1, JCp-1, MACS-1, MACS-3) and phosphate (MAPS-4, MAPS-5, NIST SRM 1400, NIST SRM 1486) international RMs using dissolved samples and two different multi-collector inductively coupled plasma-mass spectrometers (MC-ICP-MS). Our Sr isotope data are in agreement with published data and have an improved measurement precision for some RMs. For MACS-1, we present the first 87Sr/86Sr value. We tested the suitability of these materials for microanalytical analyses by LA-MC-ICP-MS, with two different laser ablation systems: a conventional nanosecond laser and a state-of-the-art femtosecond laser. We investigated the RMs micro-homogeneity and compared the data with our solution data. Both laser ablation systems yielded identical 87Sr/86Sr ratios within uncertainty to the solution data for RMs with low interferences of REEs. Therefore, these carbonate and phosphate RMs can be used to achieve accurate and precise results for in situ Sr isotope investigations by LA-MC-ICP-MS of similar materials

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“…, Vanhaecke et al . ). However, the refractory Sr is less influenced by these factors than for example the volatile Rb.…”

Section: Analytical Techniquesmentioning

confidence: 97%

Calcium Carbonate and Phosphate Reference Materials for Monitoring Bulk and Microanalytical Determination of Sr Isotopes

Weber

Lugli

Jochum

et al. 2017

Geostandard Geoanalytic Res

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“…In comparison with solution‐based analytical techniques, in situ analyses, such as LA‐(MC‐)ICP‐MS or SIMS, of unknown samples are limited by the availability of suitable RMs with microhomogeneity in the range of the respective test portion masses (µg–ng range). Furthermore, for laser ablation analysis, a similar matrix composition and mass fraction of the element of interest of the RM and the unknown sample are preferable (Jochum and Enzweiler ), in particular if femtosecond laser ablation systems are not available (Poitrasson et al , Vanhaecke et al ).…”

mentioning

confidence: 99%

NanoSr – A New Carbonate Microanalytical Reference Material for In Situ Strontium Isotope Analysis

Weber

Lugli

Hattendorf

et al. 2019

Geostandard Geoanalytic Res

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The in situ measurement of Sr isotopes in carbonates by MC‐ICP‐MS is limited by the availability of suitable microanalytical reference materials (RMs), which match the samples of interest. Whereas several well‐characterised carbonate reference materials for Sr mass fractions > 1000 µg g−1 are available, there is a lack of well‐characterised carbonate microanalytical RMs with lower Sr mass fractions. Here, we present a new synthetic carbonate nanopowder RM with a Sr mass fraction of ca. 500 µg g−1 suitable for microanalytical Sr isotope research (‘NanoSr’). NanoSr was analysed by both solution‐based and in situ techniques. Element mass fractions were determined using EPMA (Ca mass fraction), as well as laser ablation and solution ICP‐MS in different laboratories. The 87Sr/86Sr ratio was determined by well‐established bulk methods for Sr isotope measurements and is 0.70756 ± 0.00003 (2s). The Sr isotope microhomogeneity of the material was determined by LA‐MC‐ICP‐MS, which resulted in 87Sr/86Sr ratios of 0.70753 ± 0.00007 (2s) and 0.70757 ± 0.00006 (2s), respectively, in agreement with the solution data within uncertainties. Thus, this new reference material is well suited to monitor and correct microanalytical Sr isotope measurements of low‐Sr, low‐REE carbonate samples. NanoSr is available from the corresponding author.

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“…25 Organic materials such as charred wood, vegetable remains and animal hairs were found in the casting cores and used for the analysis. Vanhaecke et al described the determination of platinum group metals (PGM) in lead, produced from fire assay, using the analytical technique of laser ablation (LA)-ICP-MS. 27 The fire assay lead button acted as a separation and pre-concentration step for the analytes Ir, Pd, Pt, Rh, and Ru extracted from ore samples. 26 Isotope ratio precision values for 207 Pb/ 206 Pb and 208 Pb/ 206 Pb were in the range of 0.15-0.30% with Pb occurring at an average concentration of 5% in these bronze alloys.…”

Section: Non-ferrous Metals and Alloysmentioning

confidence: 99%

Atomic spectrometry update. Industrial analysis: metals, chemicals and advanced materials

Carter

Fisher

Goodall

et al. 2011

J. Anal. At. Spectrom.

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Metals 1.1 Ferrous metals and alloys 1.2 Non-ferrous metals and alloys 2 Chemicals 2.1 Petroleum and petroleum products 2.1.1 Petroleum products -gasoline, diesels, gasohol, exhaust particulates 2.1.2 Fuel -coal, fly ash, particulates/emissions 2.1.3 Oils -crude oil, lubricants 2.1.4 Alternative fuels 2.2 Organic chemicals and solvents 2.2.1 The analysis of archaeological and art objects 2.2.2 LIBS and other laser techniques 2.2.3 Mass spectrometric techniques 2.2.4 Ion beam techniques 2.2.5 Speciation 2.2.6 Extraction, preconcentration and sample introduction 2.3 Inorganic chemicals and acids 2.3.1 Reviews, overviews and CRMs 2.3.2 Cements, concretes and plasters 2.3.3 Matrix modifiers 2.3.4 Forensic applications 2.3.5 Other applications 2.3.6 The analysis of nano-structures 2.3.6.1 Reviews and CRMs 2.3.6.2 Methods of analysis 2.4 Nuclear materials 2.4.1 Reviews and overviews 2.4.2 Nuclear forensic and safeguards applications 2.4.3 Other nuclear applications 3 Advanced materials 3.1 Polymeric materials and composites

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Femtosecond laser ablation-ICP-mass spectrometry analysis of a heavy metallic matrix: Determination of platinum group metals and gold in lead fire-assay buttons as a case study

Cited by 45 publications

References 29 publications

Calcium Carbonate and Phosphate Reference Materials for Monitoring Bulk and Microanalytical Determination of Sr Isotopes

Calcium Carbonate and Phosphate Reference Materials for Monitoring Bulk and Microanalytical Determination of Sr Isotopes

NanoSr – A New Carbonate Microanalytical Reference Material for In Situ Strontium Isotope Analysis

Atomic spectrometry update. Industrial analysis: metals, chemicals and advanced materials

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