1.6 Anorganische Referenzmaterialien
Filtern
Dokumenttyp
- Vortrag (54)
- Zeitschriftenartikel (31)
- Posterpräsentation (23)
- Dissertation (1)
- Newsletter (1)
- Sonstiges (1)
Schlagworte
- HR-CS-MAS (15)
- Isotope analysis (11)
- Machine learning (9)
- CRM (8)
- Isotope (8)
- Lithium (8)
- Optical spectroscopy (8)
- GD-OES (7)
- Reference material (7)
- HR-CS-AAS (6)
- Lithium Ion Batteries (6)
- Magnesium (6)
- ISO-Guide 35 (5)
- Isotopes (5)
- Spectrometry (5)
- Fluorine (4)
- GDMS (4)
- Graphite furnace (4)
- LIBS (4)
- Lithium isotope (4)
- Microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) (4)
- Multi-element analysis (4)
- Nitrogen plasma (4)
- Reference materials (4)
- Soil (4)
- Atomic absorption spectrometry (3)
- Battery (3)
- Borosilicate glass (3)
- Calibration (3)
- Certified reference material (3)
- Diatomic molecule (3)
- Hydrolytic resistance (3)
- Isotopenanalyse (3)
- Lithium-ion batteries (3)
- Provenance (3)
- Referenzmaterialien (3)
- Steel (3)
- ZRM (3)
- AAS (2)
- Boden (2)
- Boron (2)
- CCQM (2)
- Cadmium (2)
- Calcium (2)
- Calcium monofluoride (2)
- Certification (2)
- Cocoa (2)
- Cyanide in soil (2)
- Depth-profiling (2)
- EDX (2)
- FIB (2)
- Food analysis (2)
- Graphite (2)
- Halogene (2)
- Halogens (2)
- Herkunftsbestimmung (2)
- Human serum (2)
- Hydrogen (2)
- ICP-MS (2)
- ISO Guide 35 (2)
- Isotope dilution (2)
- Isotopic shift (2)
- Laser-induced XUV spectroscopy (2)
- Lithium batteries (2)
- MC-ICP-MS (2)
- MOSES (2)
- Mass spectrometry (2)
- Massenspektrometrie (2)
- Messunsicherheit (2)
- Molecular absorption spectrometry (2)
- Mono-hydride (2)
- Multivariate data analysis (2)
- Non-metals (2)
- Optischer Spektroskopie (2)
- Quality assurance (2)
- Referenzmaterial (2)
- Referenzmaterial-Herstellung (2)
- SEM (2)
- Spectroscopy (2)
- Sulfur (2)
- Total cyanide (2)
- Trace elements (2)
- Traceability (2)
- Zinc (2)
- AFM (1)
- Absorption spectrometry (1)
- Acrylamide (1)
- Additive manufacturing (1)
- Aging Mechanisms (1)
- Aging mechanisms (1)
- AlCl (1)
- Algorithms (1)
- Aluminium (1)
- Anode (1)
- Anti-cancer (1)
- Applied optical spectroscopy (1)
- Atomabsorptionsspektrometrie (1)
- Atomic Absorption Spectrometry (1)
- Atomic absorption spectroscopy (1)
- Atomic spectrometry (1)
- Atomic spectroscopy (1)
- BERM (1)
- Battery aging (1)
- Boron monohydride (1)
- Bunsen-Kirchhoff-Preis (1)
- CaCl emission bands (1)
- CaF (1)
- Capecitabine (1)
- Carbon (1)
- Carbon cycle (1)
- Cathode (1)
- CdSe/ZnS quantum Dots (1)
- Cellular substructure (1)
- Cellular uptake (1)
- Chemometric (1)
- Chemometrics (1)
- Chemometry (1)
- Chlorides (1)
- Chlorine (1)
- Chlorine determination (1)
- Collaborative trial (1)
- Coltan (1)
- Continuum source atomic absorption spectrometry (1)
- Cooper (1)
- Crude oil (1)
- DC-Arc (1)
- Dating (1)
- Depht profiling (1)
- Diatomic (1)
- Diatomic molecules (1)
- Doppler effect (1)
- ELISA (1)
- ETV (1)
- Eignungsprüfung (1)
- Electrochemistry (1)
- Elemental Impurities (1)
- Elemental impurities (1)
- European Reference Material (1)
- Fast flow GD (1)
- Fast single pulse response (1)
- Fluorescence (1)
- Fluorouracil (1)
- Food (1)
- Fusarium mycotoxin (1)
- GD-MS (1)
- GDOES (1)
- Gas analysis (1)
- Genauigkeit (1)
- Geological thermometer (1)
- Germanium sulfide (1)
- Gesamtcyanid (1)
- Glow Discharge (1)
- Glow discharge optical emission spectroscopy (1)
- Graphit (1)
- HT22 (1)
- HeLa (1)
- Heat accumulation (1)
- Heavy crude oil (1)
- High purity (1)
- High purity material (1)
- High-resolution (1)
- High-resolution absorption isotopic spectrometry (1)
- High-resolution continuum source atomic absorption spectrometer (1)
- High-resolution continuum source graphite furnace atomic absorption spectrometry (1)
- High-resolution continuum source molecular absorption spectrometry (1)
- Hot-pressing (1)
- ICH guideline Q3D (1)
- ICP-AES (1)
- ICP-OES (1)
- ICP-ToF-MS (1)
- ISO REMCO (1)
- Iisotopic signature (1)
- In-situ process monitoring (1)
- Industrial gypsum (1)
- Inorganic Reference Materials (1)
- Inter layer time (1)
- Interferences (1)
- Iron (1)
- Isotope anaylsis (1)
- Isotopic fingerprints (1)
- LA-ICP-SFMS (1)
- Laser Ablation/Imaging (1)
- Laser ablation (1)
- Laser induced XUV spectroscopy (1)
- Laser induced breakdown Spectrocopy (LIBS) (1)
- Laser powder bed fusion (1)
- Laser spectroscopy (1)
- Li-ion battery (1)
- MALDI (1)
- MICAP-MS (1)
- MKW (1)
- MS-ICP-MS (1)
- Magnesium monofluoride (1)
- Magnetically stabilized (1)
- Material Science (1)
- Matrix independent calibration (1)
- Medicinal products (1)
- Mercury solution (1)
- Metrology (1)
- Microemulsion (1)
- Microwave plasma (1)
- Molecular spectra (1)
- Molecular spectrum (1)
- Monoelemental solutions (1)
- Multielemental analysis (1)
- Multivariate analysis (1)
- Nanomaterials (1)
- Nanoparticles (1)
- Nichtmetall-Analytik (1)
- Nichtmetalle (1)
- Nickel (1)
- Niobcarbid (1)
- Nitrogen (1)
- Nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (1)
- Non metals (1)
- Non-metal analysis (1)
- Non-metals analysis (1)
- Non-target (1)
- Optical Spectroscopy (1)
- Optical emission spectroscopy (1)
- Optical isotopic spectrometry (1)
- Optical spectrometry (1)
- Oxygen (1)
- PCB (1)
- Peristaltic pumps (1)
- Pharmacopea (1)
- Pharmacopoeial Reference Standards (1)
- Planetary science (1)
- Plasma (1)
- Plasmaspectrochemistry (1)
- Pouch cell (1)
- Primary standard (1)
- Primäre Kalibriersubstanzen (1)
- Präzision (1)
- Pulsed-GD-SFMS (1)
- Quantitative bioimaging (1)
- RIchtigkeit (1)
- Reference standards (1)
- Reinstmetalle (1)
- Reinststoffe (1)
- SI Traceability (1)
- SI-traceable (1)
- Safety (1)
- Selenium (1)
- Simultaneous determination (1)
- Single cell (1)
- Soda-lime glass (1)
- Software (1)
- Solid microanalysis (1)
- Spurenelemente (1)
- Sputtering (1)
- Statistics (1)
- Storage Technologies (1)
- Sub-doppler spectroscopy (1)
- Thermography (1)
- Thin metal alloy layers (1)
- Titanium hydride (1)
- Trace Analysis (1)
- Trace analysis (1)
- Two-phase system (1)
- Unsicherheitsabschätzung (1)
- VO (1)
- Validierung (1)
- Vanadium (1)
- Vanadiumcarbid (1)
- Vegetable edible oil (1)
- Water (1)
- Wolframcarbid (1)
- X-ray fluorescence (1)
- Xerogel (1)
- ZIF (1)
- Zertifizierung (1)
- Zirconium (1)
- Zn (1)
- Zr-Modifier (1)
- battery aging mechanism (1)
- current collector corrosion (1)
- depth profiles (1)
- discharge (1)
- emission (1)
- glow (1)
- optical (1)
- pL-droplets (1)
- spectroscopy (1)
Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (111)
- 1.6 Anorganische Referenzmaterialien (111)
- 1.1 Anorganische Spurenanalytik (19)
- P Präsident (14)
- P.0 Präsident und andere (14)
- S Qualitätsinfrastruktur (8)
- S.1 Qualität im Prüfwesen (8)
- 1.3 Instrumentelle Analytik (7)
- 1.7 Organische Spuren- und Lebensmittelanalytik (7)
- 3 Gefahrgutumschließungen; Energiespeicher (6)
Paper des Monats
- ja (1)
In this study, we demonstrate the applicability of nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) for Ca, Fe, and Se quantification in human serum using isotope dilution (ID) analysis. The matrix tolerance of MICAP-MS in Na matrix was investigated, uncovering that high Na levels can suppress the signal intensity. This suppression is likely due to the plasma loading and the space charge effect. Moreover, 40Ca and 44Ca isotopic fractionation was noted at elevated Na concentration. Nine certified serum samples were analyzed using both external calibration and ID analysis. Overestimation of Cr, Zn, As, and Se was found in the results of external calibration, which might be resulted from C-induced polyatomic interference and signal enhancement, respectively. Further investigations performed with methanol showed a similar enhancement effect for Zn, As, and Se, potentially supporting this assumption. The mass concentrations determined with ID analysis show metrological compatibility with the reference values, indicating that MICAP-MS combined with ID analysis can be a promising method for precise Ca, Fe, and Se determination. Moreover, this combination reduces the influences of matrix effects, broadening the applicability of MICAP-MS for samples with complex matrix.
The statistical tool eCerto was developed for the evaluation of measurement data to assign property values and associated uncertainties of reference materials. The analysis is based on collaborative studies of expert laboratories and was implemented using the R software environment. Emphasis was put on comparability of eCerto with SoftCRM, a statistical tool based on the certification strategy of the former Community Bureau of Reference. Additionally, special attention was directed towards easy usability from data collection through processing, archiving, and reporting. While the effects of outlier removal can be flexibly explored, eCerto always retains the original data set and any manipulation such as outlier removal is (graphically and tabularly) documented adequately in the report. As a major reference materials producer, the Bundesanstalt für Materialforschung und -prüfung (BAM) developed and will maintain a tool to meet the needs of modern data processing, documentation requirements, and emerging fields of RM activity. The main features of eCerto are discussed using previously certified reference materials.
Referenzmaterialien sind unter anderem ein wichtiges Werkzeug zur Qualitätskontrolle von Messungen bestimmter Merkmalswerte. Dabei ist zu berücksichtigen, dass zertifizierte Merkmalswerte immer eine gewisse Unsicherheit haben. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Vortrags. Referenzmaterialien sind gleichzeitig ein wertvolles Werkzeug zur Ermittlung der Unsicherheit von Messverfahren und -Analysen unbekannter Proben. Die Vorgehensweise bei der Ermittlung der Messunsicherheit mit Hilfe eines Referenzmaterials wird beschrieben.
Referenzmaterialien sind unter anderem ein wichtiges Werkzeug zur Qualitätskontrolle von Messungen bestimmter Merkmalswerte. Dabei ist zu berücksichtigen, dass zertifizierte Merkmalswerte immer eine gewisse Unsicherheit haben. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Vortrags. Referenzmaterialien sind gleichzeitig ein wertvolles Werkzeug zur Ermittlung der Unsicherheit von Messverfahren und -Analysen unbekannter Proben. Die Vorgehensweise bei der Ermittlung der Messunsicherheit mit Hilfe eines Referenzmaterials wird beschrieben.
Research into new sources for EUV lithography is driving advancements in experimental methods tailored for this short wavelength range. This progress enables the exploration of spectroscopic techniques aimed at monitoring electronic transitions within this energy spectrum. Laser-induced breakdown spectroscopy (LIBS) serves as a rapid tool for elemental analysis, primarily established in the UV-vis range. However, LIBS encounters challenges such as limited repeatability precision and elevated background noise resulting from continuum radiation.
In parallel, laser-induced extreme UV spectroscopy (LIXS) delves into the initial stages of plasma evolution, characterized by the emergence of soft X-ray and extreme UV radiation. The method benefits from a fast timeframe and constrained plasma confinement, leading to better precision. Nevertheless, LIXS encounters convoluted spectra arising from unresolved transition arrays (UTA), particularly pronounced for heavier elements. This complexity renders conventional univariate data analysis impractical, demanding the adoption of a multivariate data analysis approach.
Multiple cathode samples, each coated with varying stoichiometries of lithium nickel manganese cobalt oxide (NMC), were prepared and used for calibration purposes. Through the application of Partial Least Squares (PLS) regression, a robust correlation with an R2 value exceeding 0.97 was achieved. The LIXS technique underwent a comparative evaluation against UV-vis LIBS. Furthermore, a comparison between univariate and multivariate analysis approaches was conducted, incorporating validation through y-randomization to mitigate overfitting risks.
The viability of this approach was confirmed through the testing of an NMC reference material. The results showed metrological compatibility with reference values, underscoring the potential capability of the proposed methodology.
The application of multivariate data analysis is essential in extracting the full potential of laser-induced XUV spectroscopy (LIXS) for high-precision elemental mapping. LIXS offers significant advantages over traditional laser-induced breakdown spectroscopy in UV-vis (LIBS), including higher precision and a wider dynamic range,[1,2] while making it possible to determine light elements like lithium and fluorine. However, it is challenged by the presence of unresolved transition arrays (UTAs) for heavier elements. These UTAs add considerable complexity to the spectral data, often concealing crucial information. In this study, we employ well-established multivariate data analysis techniques and intensive data preprocessing to unravel this contained information.
The refined analysis reveals a high level of detail, enabling the precise identification of inhomogeneities within material samples. Our approach has particular relevance for studying aging processes in lithium-ion batteries (LIBs), specifically in relation to varying cathode materials and fluorine-containing polymer binder content. By combining elemental distribution with structural information, this improved method can offer a more comprehensive understanding of sample inhomogeneities and aging processes in LIBs, contributing to the development of more reliable and sustainable battery technologies.
Laser-induced XUV spectroscopy (LIXS) is an emerging technique for elemental mapping. In comparison to conventional laser-induced breakdown spectroscopy in UV-vis (LIBS), it has a higher precision and wider dynamic range, and it is well suited for the quantification light elements like lithium and fluorine. Further it can spot oxidation states. The XUV spectra are produced at a very early stage of the plasma formation. Therefore, effects from plasma evolution on the reproducibility can be neglected. It has been shown, that high-precision elemental quantification in precursor materials for lithium-ion batteries (LIBs) can be performed using LIXS. Based on these results, LIXS mapping was used to investigate aging processes in LIBs. Different cathode materials with varying compositions of fluorine containing polymer binders were compared at different stages of aging. Due to effects comparable to X-ray photoelectron spectroscopy but in reverse, monitoring of changes in the oxidation state is envisioned, which makes information about the chemical environment of the observed elements accessible. The combination of elemental distribution and structural information leads to a better understanding of aging processes in LIBs, and the development of more sustainable and safe batteries.
Introduction
Lithium-ion batteries (LIBs) are one key technology to overcome the climate crisis and energy transition challenges. Demands of electric vehicles on higher capacity and power drives research on innovative cathode and anode materials. These high energy-density LIBs are operated at higher voltages, leading to increased electrolyte decay and the current collectors' degradation. Even though this fundamental corrosion process significantly affects battery performance, insufficient research is being done on the aluminum current collector. Fast and convenient analytical methods are needed for monitoring the aging processes in LIBs.
Methods
In this work glow-discharge optical emission spectrometry (GD-OES) was used for depth profile analysis of aged cathode material. The measurements were performed in pulsed radio frequency mode. Under soft and controlled plasma conditions, high-resolution local determination (in depth) of the elemental composition is possible. Scanning electron microscopy (SEM) combined with a focused ion beam (FIB) cutting and energy dispersive X-ray spectroscopy (EDX) was used to confirm GD-OES results and obtain additional information on elemental distribution.
Results
The aging of coin cells manufactured with different cathode materials (LCO, LMO, NMC111, NMC424, NMC532, NMC622, and NMC811) was studied. GD-OES depth profiling of new and aged cathode materials was performed. Quantitative analysis was possible through calibration with synthetic standards and correction by sputter rate. Different amounts of aluminum deposit on the cathode surface were found for different materials. The deposit has its origin in the corrosion of the aluminum current collector. The results are compatible with results from FIB-EDX. However, GD-OES is a faster and less laborious analytical method. Therefore, it will accelerate research on corrosion processes in high energy-density batteries.
Innovative aspects
- Quantitative depth profiling of cathode material
-Monitoring of corrosion processes in high energy-density lithium-ion batteries
- Systematic investigation of the influence of different cathode materials
We investigated the performance of nitrogen microwave inductively coupled atmospheric-pressure plasma mass spectrometry (MICAP-MS) under matrix effects and its applicability to trace element analysis in steels. Influences of different gas flows and ion optics on the matrix tolerance are studied, indicating that nebulizer gas flow has the most significant impact. Optimization of ion optics improves matrix tolerance for light elements due to the reduction of the inelastic collisional scattering effect. With optimized operating conditions, MICAP-MS achieves an internal standard intensity recovery of over 90% at an Fe concentration of 500 mg L−1. Even at an Fe concentration of 1 g L−1, the recovery remains above 80%. Three certified reference materials – non-alloy, low-alloy and high-alloy steel – were analyzed using MICAP-MS. The determined mass concentrations of the trace and minor components show metrological compatibility to the reference values. No significant differences are observed between the results obtained with aqueous and matrix-matched calibration, demonstrating the strong matrix tolerance of MICAP-MS, and its promising applicability to steel analysis.