Filtern
Erscheinungsjahr
Dokumenttyp
- Zeitschriftenartikel (38)
- Posterpräsentation (34)
- Vortrag (26)
- Beitrag zu einem Tagungsband (6)
- Forschungsbericht (1)
Sprache
- Deutsch (53)
- Englisch (51)
- Mehrsprachig (1)
Schlagworte
- AHTN (6)
- Arsenolipids (5)
- LA-ICP-MS (5)
- Umweltsimulation (5)
- ESI-MS/MS (4)
- GC-MS (4)
- Metformin (4)
- Warfarin (4)
- XRF (4)
- BFR (3)
- Estrogens (3)
- Mass spectrometry (3)
- Polymer (3)
- Schadstoffe (3)
- Analytik (2)
- Arsenic species (2)
- Disinfection by-product (2)
- EDC (2)
- Environmental simulation (2)
- Fish (2)
- HPLC-ICP-MS/ESI-Q-TOF-MS (2)
- Marine fish (2)
- Materialien (2)
- Methyl mercury (2)
- Migration (2)
- PBFSM (2)
- PFAS (2)
- Pollutants (2)
- Polypropylen (2)
- Polystyrol (2)
- RFA (2)
- Schadstoffaustrag (2)
- Sewage sludge (2)
- Soil (2)
- Surface water (2)
- Tonalide (2)
- Transformationsprodukte (2)
- Umweltverhalten (2)
- WFD (2)
- Whole water samples (2)
- 13C (1)
- 13C labeling (1)
- AHTN-COOH (1)
- AHTN-COOMe (1)
- APCI (1)
- Accelerant (1)
- Advanced oxidation (1)
- Affinity (1)
- Analysis (1)
- Arsenic species analysis (1)
- Arsenobetaine (1)
- Arsenolipide (1)
- Arson analysis (1)
- Artificial weathering (1)
- Bewitterung (1)
- Bisphenol-A (1)
- Blood-brain barrier (1)
- Brand (1)
- Brandbeschleuniger (1)
- Brandgase (1)
- CCQM (1)
- Canned cod liver (1)
- Casein (1)
- Chemical analysis (1)
- Chlorination (1)
- Cod liver (1)
- Column percolation leaching (1)
- Combustion Ion Chromatography (1)
- Comparability (1)
- Cone calorimeter (1)
- Cyclic musk (1)
- Cyclilc musk (1)
- Degradation (1)
- Derivatization (1)
- Difenoconazole (1)
- Dimethylarsenate (1)
- Disinfection (1)
- Dynamic scanning calorimetry (1)
- EQS (1)
- EU-WFD (1)
- Effect based Method (1)
- Element species (1)
- Elutionsverfahren (1)
- Endocrine disrupting chemicals (1)
- Environmental Chemistry (1)
- Environmental simulations (1)
- Enzymatic digestion (1)
- Esterification (1)
- Estrogenes (1)
- Extraction (1)
- Fertilizer (1)
- Finow Canal (1)
- Fire debris (1)
- Flammschutzmittel (1)
- Fluoride (1)
- Forensic science (1)
- Fragmentation pathway (1)
- Freisetzung (1)
- Freshwater fish (1)
- GC (1)
- GC-PED (1)
- Gas chromatography (1)
- General Medicine (1)
- Glucose (1)
- HHCB (1)
- HHCB-lactone (1)
- HPLC-DAD (1)
- HPLC-ICP-MS/HR-MS (1)
- Haloform reaction (1)
- Health, Toxicology and Mutagenesis (1)
- Herring (1)
- Heterogeneous photocatalysis (1)
- High-resolution mass spectrometry (1)
- Hydroxy warfarin (1)
- Hypothalamus (1)
- ICP-TOF-MS (1)
- ILC (1)
- Ignitable liquids (1)
- Interlaboratory key comparison (1)
- Isotope dilution (1)
- Isotopic labeled (1)
- Kontaminierte Böden (1)
- LC-MS (1)
- LC-MS/MS (1)
- LC-UV (1)
- Lactate (1)
- Leaching (1)
- Legacy pollution (1)
- Linear alkylbenzenesulfonates (1)
- Liquid chromatography (1)
- MIP (1)
- MS based method (1)
- Mercury speciation (1)
- Metal contamination (1)
- Methylene blue (1)
- Methylmercury (1)
- Methylquecksilber (1)
- Metrology (1)
- Microdialysis (1)
- Microplastic (1)
- Modeling (1)
- Molecular imprinted polymers (1)
- Monomethylarsonate (1)
- Musk (1)
- NMR (1)
- NSO-Heterozyklen (1)
- Nanozirconia (1)
- Norfuraneol (1)
- Organische Schadstoffe (1)
- PET (1)
- POP (1)
- PP (1)
- PS (1)
- Partikel (1)
- Pathway (1)
- Peptide (1)
- Per- and Polyfluoroalkyl substances (PFAS) (1)
- Perfluorinated surfactants (1)
- Pesticides (1)
- Photocatalysis (1)
- Plastic debris (1)
- Pollution (1)
- Polymer-based products (1)
- Pressurised liquid extraction (1)
- Purity assessment (1)
- Rauchgase (1)
- Rauchgastemperaturen (1)
- Raumbrände (1)
- Reliable measurements (1)
- SPE (1)
- SPME (1)
- Sediment (1)
- Smoke density chamber (1)
- Soil contact (1)
- Soil organic matter (1)
- Solid-liquid-extraction (1)
- Solid-phase microextraction (1)
- Stoffwechselprodukte (1)
- Surfactants (1)
- Synthesis (1)
- Synthetische Moschusverbindungen (1)
- Säulenperkolationsverfahren (1)
- TBBPA-dbpe (1)
- Total petrol hydrocarbons (1)
- Toxicity (1)
- Transformation (1)
- Transformations products (1)
- Umweltschadstoffe (1)
- Water treatment (1)
- Weathering (1)
- Wärmefreisetzung (1)
- XANES (1)
Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (29)
- 1.8 Umweltanalytik (29)
- 1.7 Organische Spuren- und Lebensmittelanalytik (13)
- 1.1 Anorganische Spurenanalytik (12)
- 1.4 Prozessanalytik (10)
- 4 Material und Umwelt (10)
- 4.1 Biologische Materialschädigung und Referenzorganismen (7)
- 4.2 Material-Mikrobiom Wechselwirkungen (7)
- 4.0 Abteilungsleitung und andere (4)
- 4.3 Schadstofftransfer und Umwelttechnologien (3)
Paper des Monats
- ja (1)
Eingeladener Vortrag
- nein (26)
High polarity analyte(s) in aqueous media: determination of L-PFOA and L-PFOS in ground water
(2022)
The CCQM-K156 comparison was coordinated by TUBITAK UME on behalf of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) for National Measurement Institutes (NMIs) and Designated Institutes (DIs) which provide measurement services in organic analysis under the 'Comité International des Poids et Mesures' Mutual Recognition Arrangement (CIPM MRA).
Perfluoro alkyl substances (PFAS) such as PFOS and PFOA have been used in numerous industrial applications and products. Because of their high stability and resistance to biodegradation, atmospheric photooxidation, direct photolysis and hydrolysis, they are extremely persistent in the environment. The European Union (EU) Water Framework Directive lists PFOS as a priority hazardous substance that poses a significant risk to the aquatic environment. The use of PFOS-containing Aqueous Film-Forming Foams (AFFFs) has been banned since June 2011 in the EU. As relatively water-soluble, effectively non-degradable compounds, PFOS and PFOA migrate to ground water. They are not removed in the conventional drinking water treatment, and therefore cause health risks in polluted areas. The EU Drinking Water Directive and the European Commission has proposed a limit value of 100 ng/L for the sum of 20 PFAS, including PFOS and PFOA.
This study provides the means for assessing measurement capabilities for determination of high polarity measurands in a procedure that requires extraction, clean-up, analytical separation and detection. Successful participation in CCQM-K156 demonstrates measurement capabilities in determining mass fraction of organic compounds, with a molecular mass of 200 g/mol to 700 g/mol, having high polarity pKow -2, in a mass fraction range from 0.5 ng/kg to 500 ng/kg in aqueous media.
Nine NMIs and DIs participated in the CCQM-K156 key comparison. Seven institutes reported their results. SPE was applied in the sample pre-treatment and LC-MS was applied for detection. All participating laboratories applied isotope dilution mass spectrometry (IDMS) techniques for quantification. Participants established the metrological traceability of their results using certified reference materials (CRMs) from NMIs with stated traceability; where commercially available high purity materials were used the purity was determined in-house. The CCQM-K156 results for L-PFOA and L-PFOS range from 2.75 ng/kg to 5.50 ng/kg with a % RSD of 19.5 % for L-PFOA and from 2.04 ng/kg to 4.45 ng/kg with a % RSD of 21.3 % for L-PFOS. The KCRV was assigned using a Hierarchical Bayesian Random Effects Model (HB REM) estimator from the values reported by six of the participants. One participant result of L-PFOS and one result of L-PFOA were excluded from the KCRV for technical reasons. The KCRV was 4.9 ng/kg ± 0.4 ng/kg for L-PFOA and 3.8 ng/kg ± 0.4 ng/kg for L-PFOS. The six institutes that were included in the assignment of consensus KCRV all agreed within their standard uncertainties.
To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/.
The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).
For the first time, µ-X-ray fluorescence (µ-XRF) mapping combined with fluorine K-edge µ-X-ray absorption near-edge structure (µ-XANES) spectroscopy was applied to depict per- and polyfluoroalkyl substances (PFAS) contamination and inorganic fluoride in samples concentrations down to 100 µg/kg fluoride. To demonstrate the matrix tolerance of the method, several PFAS contaminated soil and sludge samples as well as selected consumer product samples (textiles, food contact paper and permanent baking sheet) were investigated. µ-XRF mapping allows for a unique element-specific visualisation at the sample surface and enables localisation of fluorine containing compounds to a depth of 1 µm. Manually selected fluorine rich spots were subsequently analysed via fluorine K-edge µ-XANES spectroscopy. To support spectral interpretation with respect to inorganic and organic chemical distribution and compound class determination, linear combination (LC) fitting was applied to all recorded µ-XANES spectra. Complementarily, solvent extracts of all samples were target-analysed via LC-MS/MS spectrometry. The detected PFAS sum values range from 20 to 1136 µg/kg dry weight (dw). All environmentally exposed samples revealed higher concentration of PFAS with a chain length >C8 (e.g. 580 µg/kg dw PFOS for Soil1), whereas the consumer product samples showed a more uniform distribution with regard to chain lengths from C4 to C8. Independent from quantified PFAS amounts via target analysis, µ-XRF mapping combined with µ-XANES spectroscopy was successfully applied to detect both point-specific concentration maxima and evenly distributed surface coatings of fluorinated organic contaminants in the corresponding samples.
Solid wastewater-based fertilizers were screened for per- and polyfluoroalkyl substances (PFAS) by the extractable organic fluorine (EOF) sum parameter method. The EOF values for ten sewage sludges from Germany and Switzerland range from 154 to 7209 mg kg−1. For thermal treated sewage sludge and struvite the EOF were lower with values up to 121 mg kg−1. Moreover, the application of PFAS targeted
and suspect screening analysis of selected sewage sludge samples showed that only a small part of the EOF sum parameter values can be explained by the usually screened legacy PFAS. The hitherto unknown part of EOF sum parameter contains also fluorinated pesticides, pharmaceutical and aromatic compounds. Because these partly fluorinated compounds can degrade to (ultra-)short PFAS in wastewater treatment plants they should be considered as significant sources of organic fluorine in the environment. The combined results of sum parameter analysis and suspect screening reveal the need to update current regulations, such as the German fertilizer ordinance, to focus not solely on a few selected PFAS such as perfluorooctane sulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) but
consider an additional sum parameter approach as a more holistic alternative. Moreover, diffusion gradient in thin-films (DGT) passive samplers were utilized as an alternative simplified extraction method for PFAS in solid wastewater-based fertilizers and subsequently quantified via combustion ion chromatography. However, the DGT method was less sensitive and only comparable to the EOF values
of the fertilizers in samples with >150 mg kg−1, because of different diffusion properties for various PFAS, but also kinetic exchange limitations.
AbstractSince the 1950s, Warfarin has been used globally as both a prescription drug and a rodenticide. Research has shown that warfarin and other rodenticides are present in the environment and food chain. However, emerging contaminants are subject to degradation by biotic and abiotic processes and advanced oxidation processes. In some cases, detecting the parent compound may not be possible due to the formation of structurally changed species. This approach aims to identify hydroxylated transformation products of warfarin in a laboratory setting, even after the parent compound has undergone degradation. Therefore, the Fenton reaction is utilized to insert hydroxylation into the parent compound, warfarin, by hydroxyl and hydroperoxyl radicals generated by Fe2+/Fe3+ redox reaction with hydrogen peroxide. Using multiple reaction monitoring, a GC–MS/MS method, incorporating isotopically labeled reference compounds, is used to quantify the expected derivatized species. The analytes are derivatized using trimethyl-3-trifluoromethyl phenyl ammonium hydroxide, and the derivatization yield of warfarin is determined by using isotopically labeled reference compounds. The method has a linear working range of 30 to 1800 ng/mL, with detection limits ranging from 18.7 to 67.0 ng/mL. The analytes are enriched using a C18-SPE step, and the recovery for each compound is calculated. The Fenton reaction generates all preselected hydroxylated transformation products of warfarin. The method successfully identifies that 4′-Me-O-WAR forms preferentially under the specified experimental conditions. By further optimizing the SPE clean-up procedures, this GC–MS-based method will be suitable for detecting transformation products in more complex matrices, such as environmental water samples. Overall, this study provides a better understanding of warfarin’s degradation and offers a robust analytical tool for investigating its transformation products.
The plant secondary metabolite families of coumarin and 4-hydroxy coumarin have a broad pharmacological spectrum ranging from antibacterial to anticancer properties. One prominent member of this substance class is the synthetic but naturally inspired anticoagulant drug and rodenticide warfarin (coumadin). A vast number of publications focus on the identification of warfarin and its major cytochrome P450-mediated phase I metabolites by liquid chromatography (LC) with mass spectrometry (MS) and tandem mass spectrometric (MS/MS) detection techniques. For the first time, electron ionization (EI) induced high-resolution quadrupole time-of-flight mass spectrometric (HR-qToF-MS) data of in-liner derivatized warfarin and selected hydroxylated species is provided in this study as an alternative to LC-MS/MS approaches. Furthermore, the characteristic fragments and fragmentation pathways of the analyzed methyl ethers are concluded. The obtained data of analytical standards, specific deuterated and 13C-labeled compounds prove inductive cleavage of the acyl or acetonyl side chain, methyl migration, and H-migration, along with consequential inductive cleavage as predominant fragmentation routes. Based on the HR-spectral data, commonalities and differences between the analyzed compounds and fragment groups were evaluated with future applicability in structure elucidation and spectra prediction of related compounds.