Chemische Charakterisierung und Spurenanalytik
Filtern
Erscheinungsjahr
- 2023 (112) (entfernen)
Dokumenttyp
- Vortrag (44)
- Zeitschriftenartikel (42)
- Posterpräsentation (18)
- Dissertation (2)
- Sonstiges (2)
- Buchkapitel (1)
- Beitrag zu einem Tagungsband (1)
- Handbuch (1)
- Forschungsbericht (1)
Schlagworte
- PFAS (11)
- Fluorine (7)
- HR-CS-GFMAS (7)
- Microplastics (6)
- Per- and Polyfluoroalkyl substances (PFAS) (6)
- Process Analytical Technology (6)
- TED-GC/MS (6)
- Benchtop-NMR (5)
- Metrology (5)
- Reference material (4)
- Synchrotron (4)
- Traceability (4)
- Absolute isotope ratio (3)
- BAMline (3)
- Biosensor (3)
- Combustion Ion Chromatography (3)
- Conventional isotope ratio (3)
- Isotope ratio (3)
- LC-MS/MS (3)
- Lithium Ion Batteries (3)
- Mass spectrometry (3)
- Messunsicherheit (3)
- Mycotoxins (3)
- Polymer 3R (3)
- SPM (3)
- Sewage sludge (3)
- Soil (3)
- WWTP (3)
- XRF (3)
- Amperometry (2)
- Analytical Chemistry (2)
- Benchtop NMR (2)
- Cement (2)
- D2XRF (2)
- Degradation (2)
- Depth-profiling (2)
- Ergot alkaloids (2)
- Fertilizer (2)
- Food analysis (2)
- GD-OES (2)
- General Earth and Planetary Sciences (2)
- Gold (2)
- Hydrogen Storage (2)
- ISO Guide 35 (2)
- Immunoassay (2)
- Isotope fractionation (2)
- Isotope reference material (2)
- Laser-induced XUV spectroscopy (2)
- Lithium-ion batteries (2)
- MefHySto (2)
- Multivariate data analysis (2)
- Mykotoxine (2)
- NMR spectroscopy (2)
- Online-NMR-Spektroskopie (2)
- Prozessanalytik (2)
- Referenzmaterial (2)
- Remediation (2)
- Risk assessment (2)
- Schwebstoffe (2)
- Steel (2)
- Uncertainty (2)
- Volatile organic compounds (2)
- qNMR (2)
- 6xHis (1)
- AAS (1)
- ABC (1)
- AF4 (1)
- ANAKON (1)
- Acoustic levitation (1)
- Acute myocardial infarction (1)
- Additive (1)
- Affinity chromatography (1)
- Aging mechanisms (1)
- Aluminum oxide (1)
- Amoxicillin (1)
- Antibiotics (1)
- Antibodies (1)
- Anwendungsmöglichkeiten (1)
- Arbeitsanleitung (1)
- Atomabsorptionsspektrometrie (1)
- Atomic weights (1)
- Automation (1)
- BAM Data Store (1)
- Bacterial lysates (1)
- Bayes (1)
- Bayesian Optimization (1)
- Betonschwellen (1)
- Biomarker (1)
- Bioseparation (1)
- Bitumen und bitumenhaltige Bindemittel (1)
- CXC (1)
- Calibration standards (1)
- Cardiac troponin (1)
- Carrier (1)
- Cascade filtration (1)
- Cconventional method (1)
- Cheese (1)
- Chemical Production (1)
- Chemiluminescence (1)
- Classical primary measurement method (CPM) (1)
- Cleaning (1)
- Cocoa (1)
- Cocrystal (1)
- Combustion ion chromatography (CIC) (1)
- Comparability (1)
- Compost (1)
- Comsumer good samples (1)
- Consumer products (1)
- Conventional isotope ratios (1)
- Core-shell nanoparticles (1)
- Corrosion (1)
- Counting detector (1)
- Cryoadsorption (1)
- Curse tablets (1)
- Cytoplasm (1)
- Datenerfassung (1)
- Derivatization (1)
- Detector deadtime (1)
- Diagnosis (1)
- Diclofenac (1)
- Dispersions (1)
- Downstream processing (1)
- Dual mode detector (1)
- EDTAD (1)
- ELISA (1)
- EMPIR (1)
- ESI-MS (1)
- Egypt (1)
- Electronic Lab Notebook (ELN) (1)
- Electronic lab notebook (ELN) (1)
- Elektronisches Laborbuch (1)
- Elemental fingerprints (1)
- Emergency (1)
- Emission reference materials (1)
- Emission test chamber (1)
- Energy input (1)
- Energy storage (1)
- Environmental impacts (1)
- Environmental pollutants (1)
- Escherichia coli (1)
- Ethylenediaminetetraacetic acid (1)
- Extended X-ray absorption fine structure (1)
- Extractable organic fluorine (1)
- Extraktion (1)
- FTIR-Spektroskopie (1)
- Feldintegration (1)
- Field integration (1)
- Filtration (1)
- Flow NMR (1)
- Flow injection immunoassay (1)
- Forschungsdatenmanagement (1)
- Fow injection analysis (1)
- GC/ICP-ToF-MS (1)
- GF-MAS (1)
- Gas chromatography (1)
- Gaussian Process (1)
- Geochemistry (1)
- Geochemistry and Petrology (1)
- Geological Storage (1)
- Geological material (1)
- Geophysics (1)
- Gleisoberbau (1)
- Gravimetric preparation (1)
- Ground water (1)
- Gypsum (1)
- HPLC-MS (1)
- HPLC-MS/MS (1)
- HR-CS-MAS (1)
- HRMS (1)
- Handbook (1)
- Heart attack (1)
- Heavy metals (1)
- HexaHis-Tag (1)
- High-resolution continuum source molecular absorption spectrometry (1)
- His6 (1)
- His8 (1)
- Hydrazinolysis (1)
- Hydrogen Metrology (1)
- Hydrogen Purity (1)
- Hydrogen adsorption storage (1)
- Hydrogen analysis (1)
- Hydrolysis products (1)
- ICP-MS (1)
- ICP-TOFMS (1)
- ILC (1)
- ILC on detection methods (1)
- IMAC purification (1)
- Immunocapture (1)
- Immunology (1)
- Immunometric assay (1)
- Immunometric biosensor (1)
- Immunosensor (1)
- Indoor air quality (1)
- Industry 4.0 (1)
- Inhalation exposure (1)
- Inorganic chemical analysis (1)
- Instrumental isotope fractionation (1)
- Interferences (1)
- Interlaboratory comparison (1)
- Internal Standard (1)
- Iron isotopes (1)
- Isotope (1)
- Isotope Dilution (1)
- Isotope Labelling (1)
- Isotope amount ratio (1)
- Isotope delta (1)
- Isotope delta value (1)
- Isotope dilution (1)
- Isotope dilution analysis (1)
- Isotope mixtures (1)
- Isotope ratios (1)
- Isotopenanalyse (1)
- LC-HRMS (1)
- Laser induced XUV spectroscopy (1)
- Lead ions (1)
- Li-ion battery (1)
- Lifetime (1)
- Lithium (1)
- Luminescence (1)
- Luminol (1)
- Lysergic acid hydrazide (1)
- MALDI TOF MS (1)
- MC-ICP-MS (1)
- MC-TIMS (1)
- MDG (1)
- MICAP-MS (1)
- Magnetic beads (1)
- Mass contents (1)
- Massenspektrometrie (1)
- Materials emissions test (1)
- Mathematics and Statistics (1)
- Matrix separation (1)
- Measurement uncertainty (1)
- Mechanochemistry (1)
- Mercury (1)
- Metals (1)
- Metal−organic frameworks (1)
- Method (1)
- Method development (1)
- Metrology in chemistry (1)
- Micro-chamber (1)
- Microfluidic system (1)
- Microplastic (1)
- Microplastic analysis (1)
- Microplastic mass (1)
- Microplastic pathways (1)
- Microplastics sampling (1)
- Microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) (1)
- Mobile analytics (1)
- Modular Production (1)
- Monitoring (1)
- Monoclonal antibodies (1)
- Monolithic column (1)
- Multi-element analysis (1)
- Mycotoxin (1)
- Mycotoxin Analysis (1)
- NMR Accreditation (1)
- NMR Validation (1)
- NMR spetroscopy (1)
- NMR-Spektroskopie (1)
- Nano (1)
- NanoPlattform (1)
- Nanopartikel (1)
- Near edge X-ray absorption fine structure spectroscopy (1)
- Neodymium (1)
- Nickel (1)
- Nickel chelate (1)
- Nitrogen plasma (1)
- Noise (1)
- Nondestructive testing techniques (1)
- On-site detection (1)
- Online NMR Spectroscopy (1)
- Online biosensor (1)
- OpenBIS (1)
- Optimization (1)
- Ordinary Portland cement (1)
- PARCI-MS (1)
- PET (1)
- PFAS TOP Assay soil contamination (1)
- Particle (1)
- Peptides and Proteins (1)
- Peroxidase (1)
- Phosphonate esters (1)
- Plants (1)
- Polishing (1)
- Pollution (1)
- Polymere (1)
- Polymorph (1)
- Polyurethanes (1)
- Portland cement (1)
- Primary difference measurement method (PDM) (1)
- Primary transfer standards (PTSs) (1)
- Probenvorbereitung (1)
- Process Monitoring (1)
- Process monitoring (1)
- Protein analysis (1)
- Provenance (1)
- Prozessindustrie (1)
- Präzision (1)
- PtNP (1)
- Purity (1)
- QI-Digital (1)
- Quality Assurance (1)
- Quality assurance (1)
- Quantitative NMR Spectroscopy (1)
- Quantitative NMR spectroscopy (1)
- Quantitative spectroscopy (1)
- Reaction Monitoring (1)
- Recombinant protein (1)
- Reference Material (1)
- Reference materials (1)
- Referenzmaterialien (1)
- Reliabiilty (1)
- Research Agenda (1)
- Research Data Infrastructure (1)
- Research Data Management (1)
- Research data management (1)
- SPE (1)
- Sapphire (1)
- Schieneninfrastruktur (1)
- Sensors (1)
- Si wafer filter (1)
- Silver artefacts (1)
- Single Cell (1)
- Single Particle (1)
- Solid microanalysis (1)
- Spannbetonschwelle (1)
- Sr and Nd isotope analysis (1)
- Sr isotope analysis (1)
- Stability (1)
- Standards (1)
- Statistical analysis (1)
- Strontium (1)
- Sum Parameter (1)
- Sum Parameter Method (1)
- Sum parameter (1)
- Sustainable Food Safety (1)
- Temperature (1)
- Temperature Control (1)
- Terminology (1)
- Tesserae (1)
- Textile fibres (1)
- Thermal degradation (1)
- Thermal treatment (1)
- Thermo-desorption (1)
- Thermoanalytical methods (1)
- Thermoanalytics (1)
- Thermostating (1)
- Trace Analysis (1)
- Ultraschall (1)
- Unsicherheit (1)
- VO (1)
- VOC (1)
- Validation (1)
- Vanadium (1)
- Vergleichuntersuchung (1)
- X-ray absorption spectroscopy (1)
- X-ray fluorescence spectroscopy (1)
- X-ray photoelectron spectroscopy (1)
- XANES (1)
- ZIF-8 (1)
- battery aging mechanism (1)
- current collector corrosion (1)
- depth profiles (1)
- openBIS (1)
- spICP-MS (1)
- β-lactam (1)
Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (85)
- 1.1 Anorganische Spurenanalytik (41)
- 6 Materialchemie (20)
- 1.4 Prozessanalytik (18)
- 1.6 Anorganische Referenzmaterialien (12)
- 4 Material und Umwelt (11)
- 1.7 Organische Spuren- und Lebensmittelanalytik (10)
- 1.8 Umweltanalytik (10)
- 6.3 Strukturanalytik (10)
- 6.6 Physik und chemische Analytik der Polymere (9)
Paper des Monats
- ja (5)
Inputs of plastic impurities into the environment via the application of fertilizers are regulated in Germany and the EU by means of ordinances. Robust and fast analytical methods are the basis of legal regulations. Currently, only macro- and large microplastic contents (>1 mm) are measured. Microplastics (1–1,000 µm), are not yet monitored. Thermal analytical methods are suitable for this purpose, which can determine the mass content and can also be operated fully automatically in routine mode. Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS) allows the identification of polymers and the determination of mass contents in solid samples from natural environments. In accordance with the German or European Commission (EC) Fertiliser Ordinance, composting plants should be monitored for microplastic particles with this method in the future. In this context a compost plant was sampled. At the end of the rotting process, the compost was sieved and separated in a coarse (>1 mm) and a fine fraction (<1 mm). The fine fraction was processed using density separation comparing NaCl and NaI as possible salt alternative and screened for microplastic masses by TED-GC/MS with additional validation and quality assurance experiments. With TED-GC/MS total microplastics mass contents of 1.1–3.0 μg/mg in finished compost could be detected with polyethylene mainly. What differs much to the total mass of plastics in the coarse fraction with up to 60 μg/mg, which were visually searched, identified via ATR-FTIR and gravimetrically weighted.
Iron isotopes are used in a variety of fields from e.g., geologic question to medical applications. Measurements of iron isotopes are usually performed as delta measurements to an artificial based delta zero standard. In the case of Fe isotopes is that delta zero standard IRMM-014, a pure Fe metal. Unfortunately, that conventional delta zero reference material defining the 56/54Fe scale is out of stock and therefore unavailable. To overcome that situation and fulfill the need for laboratories that measure Fe isotope on a regular basis we will provide a set of solutions with IRMM-014 and a second anchor point for Fe isotope ratio measurements that is based on a pure Fe metal. This new second anchor point, a high purity Fe from BAM, will be calibrated against IRMM-014 and can be used as bracketing standard or as reference value for stable Fe isotope measurements.
We are in the good situation that BAM ordered a large stock of IRMM-014 several years ago. That stock of IRMM-014 Fe cubes and IRMM-014 Fe wires will be dissolved in 6M HCl in a large quantity. The new anchor point, the high purity Fe metal, that is commercially available at BAM, is a pure Fe metal with only trace amounts of impurities. The high purity BAM material will also be dissolved in 6M HCl in large quantity. Several aliquots of both solutions will be measured on the Neptune Plus MC-ICP-MS to define this second anchor point with a low uncertainty. Further will we send several aliquots of both solutions to different laboratories to also measure this second anchor point of high purity Fe on the 56/54Fe scale.
We will report the values of that study on BAM high purity Fe and will provide a guide for scale conversion to the IRMM-014 scale and for uncertainty calculation to use that new anchor point instead of the exhausted IRMM-014.
Introduction
Per- and polyfluorinated alkyl substances (PFASs) are a group of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate realistic PFAS pollution levels.
Methods
For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. In our study we used high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) which is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L.
Results
Here, we present an improved method for the determination of PFASs using HR-CS-GFMAS via GaF detection. The optimized method includes a modifier pretreatment step using a mixture of Mg, Pd and Zr and a correction measurement using perfluorooctanoic acid. The combination of both resulted in increased accuracy and precision as well as overall lower detection limits. Furthermore, during optimization the influence of species-specific responses during HR-CS-GFMAS analysis was reduced resulting in a more accurate determination of PFAS sum parameters. To test the applicability of the improved method, we analysed soil samples from a former fire-fighting training area combining the improved method for detection with our previously optimized extraction method for extractable organically bound fluorine (EOF) determination in soils.
Innovative aspects
• Highly sensitive and selective method for fluorine/PFASs analysis based on HR-CS-GFMAS
• Increased accuracy for the determination of EOF
• Reduction of PFAS species-specific responses by optimized modifier conditions
HR-CS-GFMAS turned out to be a sensitive, fast and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) at a temperature of 1550°C. GaF can be detected at 211.248 nm providing limits of quantificationin the low μg/L range. However, several species specific effects where observed when analyzing PFASs.
Per- und polyfluorierte Alkylverbindungen (PFAS) sind eine Substanzklasse bestehend aus mehreren tausenden Einzelverbindungen. Unter PFAS zählen alle Verbindungen, die mindestens eine perfluorierte Methyl- (-CF3) oder Methylen-Gruppe (-CF2-) besitzen. Somit zählt auch ein großer Teil der fluorierten Medikamente, Pflanzenschutzmittel oder Biozide in die PFAS-Substanzklasse. Aufgrund der Persistenz, Bioakkumulation in Nahrungsketten, Toxizität und der ubiquitären Verbreitung von PFAS zählen sie zu den „emerging pollutants“. Die PFAS-Analytik ist wegen ihrer vielfältigen physikalisch-chemischen Eigenschaften und der sehr hohen Anzahl an PFAS eine große Herausforderung. Da es für viele Anwendungen noch ungewiss ist, welche PFAS verwendet werden, wie sie in die Umwelt gelangen und welche Transformations- bzw. Abbauprodukte entstehen, stoßen analytische Ansätze, die nur auf Einzelsubstanzen abzielen, hier an ihre Grenzen. PFAS-Summenparameter-Methoden, die darauf abzielen ein möglichst vollständiges Abbild der PFAS-Belastungssituation widerzuspiegeln, werden daher immer wichtiger.
Per- und polyfluorierte Alkylverbindungen (PFAS) sind eine Substanzklasse bestehend aus mehreren tausenden Einzelverbindungen. Unter PFAS zählen alle Verbindungen, die mindestens eine perfluorierte Methyl- (-CF3) oder Methylen-Gruppe (-CF2-) besitzen.[1] Somit zählt auch ein großer Teil der fluorierten Medikamente, Pflanzenschutzmittel oder Biozide in die PFAS-Substanzklasse. Aufgrund der Persistenz, Bioakkumulation in Nahrungsketten, Toxizität und der ubiquitären Verbreitung von PFAS zählen sie zu den „emerging pollutants“.[2] Die PFAS-Analytik ist wegen ihrer vielfältigen physikalisch-chemischen Eigenschaften und der sehr hohen Anzahl an PFAS eine große Herausforderung. Da es für viele Anwendungen noch ungewiss ist, welche PFAS verwendet werden, wie sie in die Umwelt gelangen und welche Transformations- bzw. Abbauprodukte entstehen, stoßen analytische Ansätze, die nur auf Einzelsubstanzen abzielen, hier an ihre Grenzen. PFAS-Summenparameter-Methoden, die darauf abzielen ein möglichst vollständiges Abbild der PFAS-Belastungssituation widerzuspiegeln, werden daher immer wichtiger.
The structure and composition of ancient gold objects retain information about their long history of manufacture, from the exploitation of the ore to the finishing touches, as well as evidence of their use, deposition, and degradation. By developing an efficient analytical strategy, it is possible to retrieve that information. This chapter sets the necessary foundation 131to explore fully the analytical results presented in the following chapters of this volume. The techniques employed in the analyses of the Egyptian jewellery are described and the analytical parameters provided. For more established techniques, only brief introductions are presented, while more recent developments are presented in greater detail.
With increasing demand and environmental concerns, researchers are exploring new materials that can perform as well or better than traditional materials while reducing environmental impact. The BAMline, a real-life sample materials research beamline, provides unique insights into materials’ electronic and chemical structure at different time and length scales. The beamline specializes in x-ray absorption spectroscopy, x-ray fluorescence spectroscopy, and tomography experiments. This enables real-time optimization of material properties and performance for various applications, such as energy transfer, energy storage, catalysis, and corrosion resistance. This paper gives an overview of the analytical methods and sample environments of the BAMline, which cover non-destructive testing experiments in materials science, chemistry, biology, medicine, and cultural heritage. We also present our own synthesis methods, processes, and equipment developed specifically for the BAMline, and we give examples of synthesized materials and their potential applications. Finally, this article discusses the future perspectives of the BAMline and its potential for further advances in sustainable materials research.
The use of benchtop-NMR instruments is constantly increasing during the recent years. Advantages of being affordable, portable and easy-to-operate without the need for trained staff make them especially interesting for industrial applications in quality control. However, applications of NMR spectroscopy as an online PAT tool are still very rare but offer a huge potential for process optimization and control. A key task to exploit this potential is hardware field integration of the lab-instruments in a rough environment of a chemical plant. Additionally, developments in automation and data evaluation are mandatory to ensure a robust unattended operation with low maintenance requirements. Here, we show an approach of a fully automated analyzer enclosure considering explosion safety, field communication, as well as environmental conditions in the field.
Temperature sensitivity is still a limitation of benchtop-NMR instruments in flow applications. Recent developments of manufacturers allow for limited operation at static temperature levels, however, a dynamic system for continuous operation is still not available. Using a prototype system offering a larger bore, active temperature shielding studies with thermostated air were performed evaluating the performance.
Automated data evaluation of NMR spectra using a modular indirect hard modeling (IHM) approach showed good results and flexibility. A second data analysis approach based on artificial neural networks (ANN) was evaluated.Therefore, amount of data was augmented to be sufficient for training. The results show comparable performance, while improving the calculation time tremendously, offering new ways to simultaneously evaluating large numbers of different models.