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.

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...

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.

Microwave acid digestion of mafic and ultramafic rocks in ICP-MS determination of the rare earth elements

2020 ◽  
Vol 86 (10) ◽  
pp. 10-17
Author(s):  
A. A. Kravchenko ◽  
I. V. Nikolaeva ◽  
S. V. Palessky
Keyword(s):  
Rare Earth ◽  
Rare Earth Elements ◽  
Reference Materials ◽  
Detection Limits ◽  
Ultramafic Rocks ◽  
Maximum Pressure ◽  
Icp Ms ◽  
Microwave System ◽  
The Rare Earth

A technique of the microwave digestion of mafic and ultramafic rocks is developed for ICP-MS determination of the rare earth elements. A series of experiments was carried out to optimize the digestion parameters (temperature, acid ratio, sample mass) in a microwave system MARS-5. A mixture of acids HF and HNO3 in a volume ratio of 4:1 was used at the first stage (60 min, 190°C, maximum pressure 20 atm), and after distilling off the excess fluorides in the form of SiF4 the dry residue was treated with aqua regia (60 min, 190°C, maximum pressure 20 atm). Measurements were carried out using a double-focusing ICP mass spectrometer ELEMENT Finnigan Mat. Multielement standard solution with an acidic composition similar to the analyzed solutions was used for external calibration and indium was used as an internal standard. The detection limits were 0.0002 – 0.008 μg/g. The digestion technique was validated by analysis of the geological reference materials BHVO-2 and BCR-2 (basalts), UB-N (serpentinite), JP-1 (peridotite). The relative standard deviations for the determined elements were below 8% for reference materials BHVO-2, BCR-2, and UB-N, and ranged within 10 – 35% for JP-1 sample. The developed technique was used for determination of the rare earth elements in Kola Peninsula rocks. The correctness of the results was confirmed by comparison with the results of ICP-MS analysis after fusion with lithium metaborate. The rapidity compared to acid decomposition without using a microwave system and low detection limits compared to fusion are the apparent advantages of the developed technique.

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.

Plasma parameters in atomic-emission spectral analysis of phosphate concentrates of the fission products

2019 ◽  
Vol 85 (2) ◽  
pp. 17-22
Author(s):  
M. I. Khamdeev ◽  
E. A. Erin
Keyword(s):  
Spectral Analysis ◽  
Chemical Composition ◽  
Reference Materials ◽  
Fission Products ◽  
Atomic Emission ◽  
Electric Arc ◽  
Physical Parameters ◽  
Arc Plasma ◽  
Atomic Emission Spectral Analysis ◽  
Excitation Processes

Physical parameters of electric arc plasma as well as their time dependences are calculated when analyzing phosphate precipitates of the fission products of irradiated nuclear fuel. Phosphate concentrates of the fission products are known for their complex chemical composition and high thermal and chemical stability. Hence, direct atomic emission spectral analysis of phosphate powders without transferring them into solutions is advisable. Different conditions of sample preparation and synthesis of the reference materials determine the different chemical forms of the elements to be determined. This, in turn, affects the kinetics of their evaporation in the electrode crate and excitation processes in the plasma. The known mechanisms of those processes cannot always be transferred to specific conditions of the given method of analysis thus entailing the necessity of studying the effect of the samples chemical composition on the results of determination, proper choice of spectroscopic carriers, detailed study of spectra excitation processes in spectral analysis, and analysis of the physical parameters of the electric arc plasma. We used the lines Zn I 307.206 nm and Zn I 307.589 nm to measure the effective temperature of the central hot sections of the arc in a range of4500 - 6500 K. NaCl, BaCl2 and NaCl + T1C1 were studied to reduce the effect of the sample elemental composition on excitation conditions of the spectra and their stabilization as a spectroscopic carrier. In control experiments we used carrier-free samples. The coincidence of the values of the plasma physical parameters within the measurement error not exceeding 20%, as well as the identity of the nature of the kinetic curves for samples of phosphate precipitates and synthetic reference materials prove their correctness. The result of the study substantiate correctness of the direct atomic-emission spectral procedure in analysis of phosphate concentrates of fission when using synthetic reference materials.

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

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