TC1725 - A Proposed Chalcopyrite Reference Material for LA-MC-ICP-MS Sulfur Isotope Determination

2021 ◽  
Author(s):  
Zhian Bao ◽  
Kaiyun Chen ◽  
Chunlei Zong ◽  
Honglin Yuan
Keyword(s):  
Reference Material ◽  
Reference Materials ◽  
Sulfur Isotope ◽  
Accuracy And Precision ◽  
Icp Ms ◽  
Geochemical Tracer ◽  
Isotope Determination

Sulfur isotope is an important geochemical tracer in diverse fields of geosciences. Controlling the accuracy and precision of microanalysis of sulfur isotope requires well-characterized reference materials with matrices similar to...

ICP-MS AND ICP-AES ANALYSIS OF PLANT REFERENCE MATERIALS

2019 ◽  
Vol 85 (6) ◽  
pp. 11-24
Author(s):  
I. V. Nikolaeva ◽  
A. A. Kravchenko ◽  
S. V. Palessky ◽  
S. V. Nechepurenko ◽  
D. V. Semenova
Keyword(s):  
Reference Material ◽  
Mass Spectrometer ◽  
Reference Materials ◽  
Atomic Emission ◽  
Icp Ms ◽  
Lithium Metaborate ◽  
Relative Standard ◽  
Microwave System ◽  
Total Analysis ◽  
Siberian Pine

Two methods — ICP-MS and ICP-AES are used for certification of the new reference material — needles of Siberian pine (NSP-1). Techniques of the analysis include decomposition of plant samples in two different ways: acid digestion in a microwave system MARS-5 and lithium metaborate fusion followed by ICP-MS and ICP-AES analysis of the solutions. Simultaneous determinations of all the elements were carried out in low, medium and high resolution using SF-mass-spectrometer ELEMENT and atomic-emission spectrometer IRIS Advantage with external calibrations and internal standards (In — ICP-MS, Sc —ICP-AES). Middle and high resolutions of ICP mass spectrometer were used for interference corrections. Data obtained by ICP-MS and ICP-AES with different decomposition techniques are in good agreement. The ICP-MS and ICP-AES techniques have been validated by the analysis of three plant reference materials: LB-1 (leaf of a birch), Tr-1 (grass mixture) and EK-1 (Canadian pondweed). These techniques were used for the determination of 38 elements in the new reference material NSP-1. Relative standard deviations for most of the determined elements were below 10%. Combination of ICP-MS and ICP-AES techniques for certification of the new reference material makes it possible to expand the set of elements to be determined and to reduce the total analysis time.

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

Geosciences ◽  
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.

A Method for the Routine Determination of Methylmercury in Marine Tissue by GC Isotope Dilution-ICP-MS

2012 ◽  
Vol 95 (4) ◽  
pp. 1189-1194 ◽  
Author(s):  
Stig Valdersnes ◽  
Amund Maage ◽  
Daniel Fliegel ◽  
Kåre Julshamn
Keyword(s):  
Reference Material ◽  
Reference Materials ◽  
Isotope Dilution ◽  
Isotope Dilution Mass Spectrometry ◽  
Standard Reference Materials ◽  
Statistical Measures ◽  
Icp Ms ◽  
Wide Range ◽  
Z Scores

Abstract Currently, there is no legal limit for methyl mercury (MeHg) in food; thus, no standardized method for the determination of MeHg in seafood exists within the European jurisdiction. In anticipation of a future legislative limit an inductively coupled plasma isotope dilution mass spectrometry (GC-ICP-ID-MS) method was developed in collaboration with the European Standardization Organization (CEN). The method comprises spiking the tissue sample with Me201Hg, followed by decomposition with tetramethylammonium hydroxide, pH adjustment and derivatization with sodium tetraethylborate, and finally organic extraction of the derivatized MeHg in a hexane phase. Subsequently, the sample is analyzed via GC-ICP-MS and the result calculated using the ID equation. The working range of the method was 0.0005–1.321 mg/kg MeHg in marine tissue, with an internal reproducibility (RSD) of 12–1%. The method was validated based on statistical measures, such as the z-scores, using the commercially available reference materials from National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1566b, NIST SRM 2977 and National Research Council of Canada (NRCC) TORT 2, NRCC, DORM 3, NRCC DOLT 4, and European Reference Material (ERM) CE 464. Z-scores for all standard reference materials, except for NIST SRM 1566b, were better than |1.5|. The wide range of marine tissues used during the validation ensures that the method will be applicable for measuring of MeHg in seafood matrixes of all kinds.

scholarly journals The use of ASH-15 flowstone as a matrix-matched reference material for laser-ablation U − Pb geochronology of calcite

Geochronology ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 35-47
Author(s):  
Perach Nuriel ◽  
Jörn-Frederik Wotzlaw ◽  
Maria Ovtcharova ◽  
Anton Vaks ◽  
Ciprian Stremtan ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Laser Ablation ◽  
Reference Material ◽  
Reference Materials ◽  
Inductively Coupled Plasma ◽  
Age Determination ◽  
Ionization Mass ◽  
Icp Ms ◽  
Carbonate Material

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.

A New Basaltic Glass Microanalytical Reference Material for Multiple Techniques

2012 ◽  
Vol 20 (1) ◽  
pp. 12-16 ◽  
Author(s):  
Steve Wilson ◽  
Alan Koenig ◽  
Heather Lowers
Keyword(s):  
Mass Spectrometry ◽  
Reference Material ◽  
Reference Materials ◽  
Secondary Ion Mass Spectrometry ◽  
Ion Beam ◽  
Round Robin ◽  
Inductively Coupled ◽  
Icp Ms ◽  
Ultra Trace ◽  
New Generation

The U.S. Geological Survey (USGS) has been producing reference materials since the 1950s. Over 50 materials have been developed to cover bulk rock, sediment, and soils for the geological community. These materials are used globally in geochemistry, environmental, and analytical laboratories that perform bulk chemistry and/or microanalysis for instrument calibration and quality assurance testing. To answer the growing demand for higher spatial resolution and sensitivity, there is a need to create a new generation of microanalytical reference materials suitable for a variety of techniques, such as scanning electron microscopy/X-ray spectrometry (SEM/EDS), electron probe microanalysis (EPMA), laser ablation inductively coupled mass spectrometry (LA-ICP-MS), and secondary ion mass spectrometry (SIMS). As such, the microanalytical reference material (MRM) needs to be stable under the beam, be homogeneous at scales of better than 10–25 micrometers for the major to ultra-trace element level, and contain all of the analytes (elements or isotopes) of interest. Previous development of basaltic glasses intended for LA-ICP-MS has resulted in a synthetic basaltic matrix series of glasses (USGS GS-series) and a natural basalt series of glasses (BCR-1G, BHVO-2G, and NKT-1G). These materials have been useful for the LA-ICP-MS community but were not originally intended for use by the electron or ion beam community. A material developed from start to finish with intended use in multiple microanalytical instruments would be useful for inter-laboratory and inter-instrument platform comparisons.This article summarizes the experiments undertaken to produce a basalt glass reference material suitable for distribution as a multiple-technique round robin material. The goal of the analytical work presented here is to demonstrate that the elemental homogeneity of the new glass is acceptable for its use as a reference material. Because the round robin exercise is still underway, only nominal compositional ranges for each element are given in the article.

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

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...

scholarly journals Development and certification of a reference material for zearalenone in maize germ oil

2021 ◽  
Author(s):  
Juliane Riedel ◽  
Sebastian Recknagel ◽  
Diana Sassenroth ◽  
Tatjana Mauch ◽  
Sabine Buttler ◽  
...  
Keyword(s):  
Reference Material ◽  
Reference Materials ◽  
Mass Fraction ◽  
High Performance ◽  
Certified Reference Materials ◽  
Maximum Level ◽  
Whole Process ◽  
Commission Regulation ◽  
Maize Oil ◽  
Maize Germ

AbstractZearalenone (ZEN), an estrogenic mycotoxin produced by several species of Fusarium fungi, is a common contaminant of cereal-based food worldwide. Due to frequent occurrences associated with high levels of ZEN, maize oil is a particular source of exposure. Although a European maximum level for ZEN in maize oil exists according to Commission Regulation (EC) No. 1126/2007 along with a newly developed international standard method for analysis, certified reference materials (CRM) are still not available. To overcome this lack, the first CRM for the determination of ZEN in contaminated maize germ oil (ERM®-BC715) was developed in the frame of a European Reference Materials (ERM®) project according to the requirements of ISO Guide 35. The whole process of CRM development including preparation, homogeneity and stability studies, and value assignment is presented. The assignment of the certified mass fraction was based upon an in-house study using high-performance liquid chromatography isotope dilution tandem mass spectrometry. Simultaneously, to support the in-house certification study, an interlaboratory comparison study was conducted with 13 expert laboratories using different analytical methods. The certified mass fraction and expanded uncertainty (k = 2) of ERM®-BC715 (362 ± 22) μg kg−1 ZEN are traceable to the SI. This reference material is intended for analytical quality control and contributes to the improvement of consumer protection and food safety. Graphical abstract

scholarly journals Comparison of Serum, Plasma, and Liver Zinc Measurements by AAS, ICP-OES, and ICP-MS in Diverse Laboratory Settings

2021 ◽  
Author(s):  
Andrew G. Hall ◽  
Janet C. King ◽  
Christine M. McDonald
Keyword(s):  
Inductively Coupled Plasma ◽  
Method Development ◽  
Geometric Mean ◽  
Zinc Content ◽  
Plasma Zinc ◽  
Icp Oes ◽  
Percent Error ◽  
Accuracy And Precision ◽  
Icp Ms ◽  
Standardized Method

AbstractProgress improving zinc nutrition globally is slowed by limited understanding of population zinc status. This challenge is compounded when small differences in measurement can bias the determination of zinc deficiency rates. Our objective was to evaluate zinc analytical accuracy and precision among different instrument types and sample matrices using a standardized method. Participating laboratories analyzed zinc content of plasma, serum, liver samples, and controls, using a standardized method based on current practice. Instrument calibration and drift were evaluated using a zinc standard. Accuracy was evaluated by percent error vs. reference, and precision by coefficient of variation (CV). Seven laboratories in 4 countries running 9 instruments completed the exercise: 4 atomic absorbance spectrometers (AAS), 1 inductively coupled plasma optical emission spectrometer (ICP-OES), and 4 ICP mass spectrometers (ICP-MS). Calibration differed between individual instruments up to 18.9% (p < 0.001). Geometric mean (95% CI) percent error was 3.5% (2.3%, 5.2%) and CV was 2.1% (1.7%, 2.5%) overall. There were no significant differences in percent error or CV among instrument types (p = 0.91, p = 0.15, respectively). Among sample matrices, serum and plasma zinc measures had the highest CV: 4.8% (3.0%, 7.7%) and 3.9% (2.9%, 5.4%), respectively (p < 0.05). When using standardized materials and methods, similar zinc concentration values, accuracy, and precision were achieved using AAS, ICP-OES, or ICP-MS. However, method development is needed for improvement in serum and plasma zinc measurement precision. Differences in calibration among instruments demonstrate a need for harmonization among laboratories.

scholarly journals Geochemical signatures of mineralizing events in the Juomasuo Au–Co deposit, Kuusamo belt, northeastern Finland

2021 ◽  
Author(s):  
Mikael Vasilopoulos ◽  
Ferenc Molnár ◽  
Hugh O’Brien ◽  
Yann Lahaye ◽  
Marie Lefèbvre ◽  
...  
Keyword(s):  
Trace Element ◽  
Sulfur Isotope ◽  
Mineral Chemistry ◽  
Chemical Compositions ◽  
Metasedimentary Rocks ◽  
Metavolcanic Rocks ◽  
Icp Ms ◽  
Stage 1 ◽  
Host Rocks ◽  
Relationship Of

AbstractThe Juomasuo Au–Co deposit, currently classified as an orogenic gold deposit with atypical metal association, is located in the Paleoproterozoic Kuusamo belt in northeastern Finland. The volcano-sedimentary sequence that hosts the deposit was intensely altered, deformed, and metamorphosed to greenschist facies during the 1.93–1.76 Ga Svecofennian orogeny. In this study, we investigate the temporal relationship between Co and Au deposition and the relationship of metal enrichment with protolith composition and alteration mineralogy by utilizing lithogeochemical data and petrographic observations. We also investigate the nature of fluids involved in deposit formation based on sulfide trace element and sulfur isotope LA-ICP-MS data together with tourmaline mineral chemistry and boron isotopes. Classification of original protoliths was made on the basis of geochemically immobile elements; recognized lithologies are metasedimentary rocks, mafic, intermediate-composition, and felsic metavolcanic rocks, and an ultramafic sill. The composition of the host rocks does not control the type or intensity of mineralization. Sulfur isotope values (δ34S − 2.6 to + 7.1‰) and trace element data obtained for pyrite, chalcopyrite, and pyrrhotite indicate that the two geochemically distinct Au–Co and Co ore types formed from fluids of different compositions and origins. A reduced, metamorphic fluid was responsible for deposition of the pyrrhotite-dominant, Co-rich ore, whereas a relatively oxidized fluid deposited the pyrite-dominant Au–Co ore. The main alteration and mineralization stages at Juomasuo are as follows: (1) widespread albitization that predates both types of mineralization; (2) stage 1, Co-rich mineralization associated with chlorite (± biotite ± amphibole) alteration; (3) stage 2, Au–Co mineralization related to sericitization. Crystal-chemical compositions for tourmaline suggest the involvement of evaporite-related fluids in formation of the deposit; boron isotope data also allow for this conclusion. Results of our research indicate that the metal association in the Juomasuo Au–Co deposit was formed by spatially coincident and multiple hydrothermal processes.

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