TY - JOUR A1 - Zweigle, J. A1 - Schmidt, A. A1 - Bugsel, B. A1 - Vogel, Christian A1 - Simon, Fabian A1 - Zwiener, C. T1 - Perfluoroalkyl acid precursor or weakly fluorinated organic compound? A proof of concept for oxidative fractionation of PFAS and organofluorines N2 - Organofluorine mass balance approaches are increasingly applied to investigate the occurrence of per- and polyfluoroalkyl substances (PFAS) and other organofluorines in environmental samples more comprehensively. Usually, complex samples prevent the identification and quantification of every fluorine-containing molecule. Consequently, large unidentified fractions between fluorine sum parameters such as extractable organic fluorine (EOF) and the sum of quantified analytes are frequently reported. We propose using oxidative conversion to separate (unidentified) weakly fluorinated compounds (e.g., pesticides, pharmaceuticals) from PFAA-precursors (perfluoroalkyl chain lengths ≥ C6). We show with three organofluorine model substances (flufenamic acid, diflufenican, pantoprazole) that CF3-groups or aromatic fluorine can be quantitatively converted to inorganic fluoride and trifluoroacetic acid (TFA) by applying PhotoTOP oxidation (UV/TiO2). The principle of fluorine separation in mixtures is demonstrated by the oxidation of the three weakly fluorinated compounds together with the PFAA-precursor 6:2/6:2 fluorotelomer mercaptoalkyl phosphate diester (FTMAP). After oxidation, the products F− and TFA were separated from PFCAs ( C4) by SPE, and the fractions were analyzed individually. Closed mass balances both with and without the addition of organic matrix were achieved. Eventually, the fluorine balance was verified by total fluorine measurements with combustion ion chromatography (CIC). The proposed methods should be considered a proof of concept to potentially explain unidentified fractions of the EOF, especially if compounds with low fluorine content such as pesticides, pharmaceuticals, and their transformation products contribute largely to the EOF. Future studies are needed to show the applicability to the complexity of environmental samples. Graphical Abstract KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613429 DO - https://doi.org/10.1007/s00216-024-05590-5 SP - 1 EP - 10 PB - Springer Science and Business Media LLC AN - OPUS4-61342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zweigle, J. A1 - Capitain, C. A1 - Simon, Fabian Michael A1 - Roesch, Philipp A1 - Bugsel, B. A1 - Zwiener, C. T1 - Non-extractable PFAS in functional textiles − Characterization by complementary methods: oxidation, hydrolysis, and fluorine sum parameters N2 - Per- and polyfluoroalkyl substances (PFAS) are widely used for durable water-repellent finishing of different fabrics and textiles like outdoor clothing, carpets, medical textiles and more. Existing PFAS extraction techniques followed by target analysis are often insufficient in detecting widely used side-chain fluorinated polymers (SFPs) that are barely or non-extractable. SFPs are typically copolymers consisting of a non-fluorinated backbone with perfluoroalkyl side-chains to obtain desired properties. We compared the accessible analytical information and performance of complementary techniques based on oxidation (dTOP assay, PhotoTOP), hydrolysis (THP assay), standard extraction, extractable organic fluorine (EOF), and total fluorine (TF) with five functional textiles and characterized 7 further textiles only by PhotoTOP oxidation. The results show that when applied directly to textile samples, oxidation by dTOP and PhotoTOP and also hydrolysis by the THP are able to capture large fractions of the TF in form of perfluoroalkyl side-chains present in the textiles while methods relying on extracts (EOF, target and non-target analysis) were much lower (e.g., factor ~25-50 lower). The conversion of large fractions of the measured TF into PFCAs or FTOHs from fluorinated side chains is in contrast to previous studies. Concentrations ranged from 0.9 and <0.4 mmol/g for both types of chitosan and activated carbon, respectively). Milled activated carbon proved to be the better adsorption material, considering the fixed volume of the adsorber (>99.9% PFOS adsorbed). Overall, the cross-linking agent concentration in chitosan is a crucial factor influencing its PFOS absorption potential. Our results feature cross-linked chitosan as an effective economic and ecologic alternative for PFOS adsorption in aqueous solutions. KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Remediation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618406 DO - https://doi.org/10.3390/app142311145 VL - 14 IS - 23 SP - 1 EP - 13 PB - MDPI AN - OPUS4-61840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Willms, Thomas A1 - Kryk, Holger A1 - Hampel, Uwe T1 - An improved method for the analysis of the reaction products of the partial isobutane oxidation by gas chromatography using a green solvent N2 - In the present work, an improved GC/MS method for the analysis of the reaction products of the non-catalytic partial oxidation of isobutane at a starting temperature of 25°C has been developed and compared to a previously published method. Two green GC-solvents (dimethyl carbonate (DMC), diethyl carbonate (DEC)) and several internal standards (hexane, benzene, toluene, DEC) have been tested. The separation of the products at low retention times (methanol, isobutane, isobutene) could be significantly improved. For the liquid main products t-butyl hydroperoxide (TBHP), di-t-butyl peroxide (DTBP), t-butanol (TBA), propanone and most trace products (isopropanol, isobutanal, methyl formate, isopropyl formate, t-butyl formate and some acetates – 24 compounds in total), a coefficient of determination CoD > 0.999 has been achieved. For all weighing and GC/MS measurements uncertainties have been calculated. The peaks of the peak pair t-butyl formate (CoD >0.999) and isobutanol (CoD >0.99), have been simulated and used for calibrations. DEC gave a decomposition of TBHP on the column. With DMC, a problem of peak purity of TBHP appeared but could be resolved. The use of the green solvent DMC, compared to also studied traditional solvents like heptane and toluene, proved to be very beneficial, since it also permitted to determine polar compounds, e. g. carbon dioxide and formic acid. KW - GC/MS KW - Green solvent KW - Method development KW - Peroxide KW - Measurement uncertainties KW - Oxidation products KW - Simulation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632026 DO - https://doi.org/10.1016/j.chroma.2025.465892 SN - 0021-9673 VL - 1753 SP - 1 EP - 16 PB - Elsevier CY - Amsterdam AN - OPUS4-63202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Scholz, Philipp A1 - Kalbe, Ute A1 - Caliebe, W. A1 - Tayal, A. A1 - Vasala, S. J. A1 - Simon, Franz-Georg T1 - Speciation of antimony and vanadium in municipal solid waste incineration ashes analyzed by XANES spectroscopy N2 - The use of ashes from municipal solid waste incineration as secondary building materials is an important pillar for the circular economy in Germany. However, leaching of potential toxic elements from these materials must be at environmentally acceptable levels. Normally, a three-month ageing period immobilizes most hazardous heavy metals, but antimony (Sb) and vanadium (V) showed previously unusual leaching. In order to clarify the mechanisms, we analyzed the Sb and V species in various bottom and fly ashes from municipal waste incineration by XANES spectroscopy. Antimony oxidizes from Sb(+ III) species used as flame retardants in plastics to Sb(+ V) compounds during waste incineration. However, owing to the similarity of different Sb(+ V) compound in the Sb K- and L-edge XANES spectra, it was not possible to accurately identify an exact Sb(+ V) species. Moreover, V is mainly present as oxidation state + V compound in the analyzed ashes. However, the coarse and magnetic fraction of the bottom ashes contain larger amounts of V(+ III) and V(+ IV) compounds which might enter the waste incineration from vanadium carbide containing steel tools. Thus, Sb and V could be critical potential toxic elements in secondary building materials and long-term monitoring of the release should be taken into account in the future. KW - Müllverbrennung KW - XANES spectroscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599841 DO - https://doi.org/10.1007/s10163-024-01954-2 SN - 1438-4957 VL - 26 SP - 2152 EP - 72158 PB - Springer Science and Business Media LLC AN - OPUS4-59984 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Roesch, Philipp A1 - Wittwer, Philipp A1 - Sommerfeld, Thomas A1 - Riedel, Maren A1 - Leube, Peter A1 - Kalbe, Ute A1 - Schoknecht, Ute A1 - Simon, Franz-Georg T1 - Per- and Polyfluoroalkyl Substances (PFAS) in Ski Waxes and Snow from Cross-Country Skiing in Germany - Comparative study of Sum Parameter and Target Analysis N2 - Per- and polyfluoroalkyl substances (PFAS) are often environmentally exposed via discharge through human consumer products, such as ski waxes. In our study we analyzed various ski waxes from the 1980s and 2020s, to determine both the sum parameter values total fluorine (TF), extractable organically bound fluorine (EOF), hydrolysable organically bound fluorine (HOF) as well as targeted PFAS analysis. This showed that modern high-performance waxes contain up to 6 % TF, but also PFAS-free labelled ski waxes contain traces of PFAS with EOF/HOF values in the low mg kg-1 range. With the ban of all fluorine-based waxes with the start of the 2023/2024 winter season this will probably change soon. Moreover, we applied our analysis methods to snow samples from a frequently used cross country ski trail (Kammloipe) in the Ore Mountain region in Germany, assessing the potential PFAS entry/discharge through ski waxes. Melted snow samples from different spots were analyzed by the adsorbable organically bound fluorine (AOF) sum parameter and PFAS target analysis and confirmed the abrasion of the ski waxes into the snow. Moreover, on a PFAS hotspot also soil samples were analyzed, which indicate that PFAS from the ski waxes adsorb after snow melting into the soil. KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Consumer Products PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612760 DO - https://doi.org/10.1016/j.hazadv.2024.100484 VL - 16 SP - 1 EP - 5 PB - Elsevier B.V. AN - OPUS4-61276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Roesch, Philipp A1 - Wittwer, Philipp A1 - Piechotta, Christian A1 - Lisec, Jan A1 - Sommerfeld, Thomas A1 - Kluge, Stephanie A1 - Herzel, Hannes A1 - Huthwelker, T. A1 - Borca, C. A1 - Simon, Franz-Georg T1 - Levels of per- and polyfluoroalkyl substances (PFAS) in various wastewater-derived fertilizers - Analytical investigations from different perspectives N2 - 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. KW - Combustion ion chromatography KW - Per- and polyfluoroalkyl substances (PFAS) KW - Sewage sludge KW - Fertilizer PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583429 DO - https://doi.org/10.1039/d3va00178d SN - 2754-7000 VL - 2 IS - 10 SP - 1436 EP - 1445 PB - Royal Society of Chemistry (RSC) CY - London AN - OPUS4-58342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Helfenstein, J. A1 - Massey, M. A1 - Kretzschmar, R. A1 - Schade, U. A1 - Verel, R. A1 - Chadwick, O. A1 - Frossard, E. T1 - Spectroscopic analysis shows crandallite can be a major component of soil phosphorus N2 - Phosphorus (P) bioavailability is crucial for the productivity of natural and agricultural ecosystems, and soil P speciation plays a major role therein. Better understanding of P forms present in soil is thus essential to predict bioavailability. However, P speciation studies are only as powerful as the reference spectra used to interpret them, and most studies rely on a limited set of reference spectra. Most studies on soil P forms differentiate between Ca-bound P (e.g. apatite), organic P, Fe-bound P, and Al-bound P. In our analysis of a Ca, Al, and P rich soil from the Kohala region of Hawaii, we identified the mineral crandallite, CaAl3(PO4)2(OH)5·H2O, a mineral previously not considered to play a significant role in soils. Crandallite was first identified with powder X-ray diffraction. Subsequently reference spectra were collected, and the presence of crandallite was confirmed using micro-focused P K-edge X-ray absorption near edge structure (XANES) spectroscopy, micro-infrared spectroscopy, and solid-state 31P nuclear magnetic resonance (NMR) spectroscopy. Crandallite XANES spectra were distinct from other common XANES spectra due to the presence of features in the post-edge region of the spectrum. Linear combination fitting of bulk P K-edge XANES spectra allowed the determination of the proportion of crandallite to the total P content, indicating that crandallite comprises up to half, possibly even more of the soil P in the samples. Crandallite is therefore an important and potentially overlooked component of soil P, which pedogenically forms in soils with high P, Al, and Ca contents, where it could play an important role in P bioavailability. KW - Phosphorus KW - XANES spectrosocpy KW - Infrared spectroscopy KW - NMR spectrocopy PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654968 DO - https://doi.org/10.1016/j.geoderma.2026.117712 SN - 0016-7061 VL - 467 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-65496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Smol, M. A1 - Adam, Christian A1 - Kugler, Stefan T1 - Analiza możliwości wykorzystania w Polsce popiołów ze spalania komunalnych osadów ściekowych na cele nawozowe T1 - Use of municipal sewage sludge ash for fertilizing purposes. An analysis of possibilities in Poland N2 - Popioły pochodzące z instalacji do spalania komunalnych osadów ściekowych, znajdującej się na terytorium Polski, poddano procesom termochemicznego przekształcania, dzięki czemu otrzymano produkty nawozowe spełniające kryteria dopuszczające je do obrotu jako nawozy mineralne. Ponadto dokonano analizy możliwości wykorzystania popiołów na cele nawozowe zgodnie z obecnie przyjętymi dokumentami strategicznymi i planistycznymi dotyczącymi gospodarki odpadami na poziomie krajowym i europejskim. N2 - Ashes from thermal transformation of municipal sewage sludge were thermochem. modified at 1000°C in the presence of NaHCO3 and sewage sludge to obtain CaNaPO4 and reduce the content of heavy metals in the produced fertilizer. Its bioavailability was more than 99% higher than that of raw ashes (50%). The nutrient content was 13.56 % Ca, 6.33% P, 4.36% K and 5.0% Fe. The content of heavy metals in fertilizer products met the std. requirements and was exceeded only in the case of Pb (278.3 mg/kg d.m.). KW - Ashes KW - Waste KW - Phosphorus KW - Recovery KW - Fertilizer PY - 2020 DO - https://doi.org/10.15199/62.2020.8.14 VL - 99 IS - 8 SP - 1186 EP - 1191 AN - OPUS4-51267 LA - pol AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - von der Au, Marcus A1 - Wittwer, Phillip A1 - Roesch, Philipp A1 - Pfeifer, Jens A1 - Cossmer, Antje A1 - Meermann, Björn T1 - A fast and simple PFAS extraction method utilizing HR–CS–GFMAS for soil samples N2 - Here, we describe an optimized fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) in soils utilizing high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR–CS–GFMAS). To omit the bias of the solid phase extraction (SPE) step commonly used during the analysis of extractable organically bound fluorine (EOF) we optimized a fast and simple SPE-free extraction method. The developed extraction method consists of a liquid-solid extraction using acidified methanol without any additional SPE. Four extraction steps were representative to determine a high proportion of the EOF (>80% of eight extractions). Comparison of the optimized method with and without an additional SPE clean-up step revealed a drastic underestimation of EOF concentrations using SPE. Differences of up to 94% were observed which were not explainable by coextracted inorganic fluoride. Therefore, not only a more accurate but also a more economic as well as ecologic method (bypassing of unnecessary SPE) was developed. The procedural limit of quantification (LOQ) of the developed method was 10.30 μg/kg which was sufficient for quantifying EOF concentrations in all tested samples. For future PFAS monitoring and potential regulative decisions the herein presented optimized extraction method can offer a valuable contribution. KW - Per- and polyfluorinated alkly substances (PFASs) KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Soils KW - Solid phase extraction (SPE) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction PY - 2022 DO - https://doi.org/10.1016/j.chemosphere.2022.133922 VL - 295 SP - 1 EP - 9 PB - Elsevier Ltd. AN - OPUS4-54359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulze-Makuch, D. A1 - Haque, S. A1 - Beckles, D. A1 - Schmitt-Kopplin, P. A1 - Harir, M. A1 - Schneider, Beate A1 - Stumpp, C. A1 - Wagner, D. T1 - A chemical and microbial characterization of selected mud volcanoes in Trinidad reveals pathogens introduced by surface water and rain water N2 - Terrestrial mud volcanoes are unique structures driven by tectonic pressure and fluids from the deep subsurface. These structures are mainly found in active tectonic zones, such as the area near the Los Bajos Fault in Trinidad. Here we report a chemical and microbiological characterization of three mud volcanoes, which included analyses of multiple liquid and solid samples from the mud volcanoes. Our study confirms previous suggestions that at least some of the mud volcano fluids are a mixture of deeper salt-rich water and surficial/precipitation water. No apparent water quality differences were found between sampling sites north and south of a major geological fault line. Microbiological analyses revealed diverse communities, both aerobic and anaerobic, including sulfate reducers, methanogens, carbon dioxide fixing and denitrifying bacteria. Several identified species were halophilic and likely derived from the deeper salt-rich subsurface water, while we also cultivated pathogenic species from the Vibrionaceae, Enterobacteriaceae, Shewanellaceae, and Clostridiaceae. These microorganisms were likely introduced into the mud volcano fluids both from surface water or shallow ground-water, and perhaps to a more minor degree by rain water. The identified pathogens are a major health concern that needs to be addressed. KW - Water stable isotope analysis KW - Mud volcanoe fluids KW - Metabolomics PY - 2020 DO - https://doi.org/10.1016/j.scitotenv.2019.136087 VL - 707 SP - 136087 PB - Elsevier B.V. AN - OPUS4-50499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholz, Philipp A1 - Vogel, Christian A1 - Schuck, G. A1 - Simon, Franz-Georg T1 - Speciation of copper and zinc compounds relevant for the hazard property (HP) 14 classification of municipal solid waste incineration bottom and fly ashes N2 - The analysis of the presence and content of substances that are toxic to aquatic life in waste is essential for classification of waste with regard to hazard property (HP) 14 ‘ecotoxic’. For the determination of HP14 classified copper (Cu) and zinc (Zn) compounds in various municipal solid waste incineration bottom ashes (IBA) and one fly ash (FA) from Germany we applied X-ray absorption near-edge structure (XANES) spectroscopy in combination with linear combination fitting. The analysis showed that approx. 50–70% of Cu in the IBA are Cu(I) compounds and elemental Cu(0), but these compounds were not equally distributed in the different IBA. In contrast, the majority (approx. 50–70%) of Zn in all IBA is elemental zinc, which originates from brass or other alloys and galvanized metals with a large content of zinc in the waste. The FA contain higher mass fraction on Zn and other toxic elements, but similar Cu and Zn species. Additional performed selective extraction at a pH of 4 with an organic acid of some IBA showed that the ecotoxic Zn fraction is mainly elemental zinc and zinc oxide. In contrast, for the ecotoxic Cu fraction within the IBA no specific compound could be identified. Furthermore, the XANES analysis showed that the HP14 properties of especially Cu in IBA is overestimated with current best-practice guidelines for sample processing for the current substance-related approach with the 0.1% cut-off rule for each substance. However, it should be considered whether it would not be better from an environmental point of view to take the ecotoxicologically leachable copper and zinc as a reference value. KW - Thermal waste treatment KW - XANES spectroscopy KW - Ecotoxicity KW - Incineration bottom ash PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609584 DO - https://doi.org/10.1016/j.wasman.2024.09.001 VL - 189 SP - 421 EP - 426 PB - Elsevier Ltd. AN - OPUS4-60958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sathiyamani, S. A1 - Ngiam, S. A1 - Bonnerot, O. A1 - Jaengsawang, S. A1 - Panarut, P. A1 - Helman-Wazny, Agnieszka A1 - Colini, C. T1 - Material Characterisation of 19–20th Century Manuscripts from Northern Thailand N2 - Material analysis was carried out on four manuscripts from Northern Thailand, which included two palm-leaf manuscripts and two paper manuscripts. The two palm-leaf manuscripts MS 6 and MS 7 were found to have been written in the traditional method, wherein text was incised on the surface of the leaves, and then soot applied to the surfaces, confirmed by the identification of carbon ink. MS 7 additionally showed the presence of trace levels of iron in the ink, either from soot paste or from the stylus used for inscribing. The paper manuscript MS 3 was written in iron-gall ink, with sections written using a methyl-violet based ink while MS 4 was written in carbon ink. The paper used in the case of MS 3 was found to be machine made, while khoi fibres (Streblus asper) were used for making the paper used for MS 4. A combination of traditional and modern pigments, like molybdenum orange, was used for decorating the edges and cover. The results improved our understanding of these manuscripts in particular, and also provided us with insights about the rapid adoption of modern materials and their incorporation into the production of written artefacts from Northern Thailand in the late 19th and early 20th centuries. KW - Materials analysis KW - Paper manuscript KW - Palm-leaf manuscript KW - Writing inks PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652586 DO - https://doi.org/10.1515/res-2023-0028 SN - 0034-5806 VL - 45 IS - 2-3 SP - 117 EP - 140 PB - Walter de Gruyter GmbH AN - OPUS4-65258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruyle, B. A1 - Pickard, H. A1 - Schultes, L. A1 - Fredriksson, F. A1 - Heffernan, A. A1 - Knappe, D. A1 - Lord, H. A1 - Meng, P. A1 - Mills, M. A1 - Ndungu, K. A1 - Roesch, Philipp A1 - Rundberget, J.T. A1 - Tettenhorst, D. A1 - Van Buren, J. A1 - Vogel, Christian A1 - Westerman, D. A1 - Yeung, L. A1 - Sunderland, E. T1 - Interlaboratory Comparison of Extractable Organofluorine Measurements in Groundwater and Eel (Anguilla rostrata): Recommendations for Methods Standardization N2 - Research on per- and polyfluoroalkyl substances (PFAS) frequently incorporates organofluorine measurements, particularly because they could support a class-based approach to regulation. However, standardized methods for organofluorine analysis in a broad suite of matrices are currently unavailable, including a method for extractable organofluorine (EOF) measured using combustion ion chromatography (CIC). Here, we report the results of an international interlaboratory comparison. Seven laboratories representing academia, government, and the private sector measured paired EOF and PFAS concentrations in groundwater and eel (Anguilla rostrata) from a site contaminated by aqueous film-forming foam. Among all laboratories, targeted PFAS could not explain all EOF in groundwater but accounted for most EOF in eel. EOF results from all laboratories for at least one replicate extract fell within one standard deviation of the interlaboratory mean for groundwater and five out of seven laboratories for eel. PFAS spike mixture recoveries for EOF measurements in groundwater and eel were close to the criterion (±30%) for standardized targeted PFAS methods. Instrumental operation of the CIC such as replicate sample injections was a major source of measurement uncertainty. Blank contamination and incomplete inorganic fluorine removal may introduce additional uncertainties. To elucidate the presence of unknown organofluorine using paired EOF and PFAS measurements, we recommend that analysts carefully consider confounding methodological uncertainties such as differences in precision between measurements, data processing steps such as blank subtraction and replicate analyses, and the relative recoveries of PFAS and other fluorine compounds. KW - Extractable organic fluorine KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Combustion ion chromatography (CIC) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587726 DO - https://doi.org/10.1021/acs.est.3c04560 SN - 0013-936X VL - 57 IS - 48 SP - 20159 EP - 20168 PB - American Chemical Society (ACS) AN - OPUS4-58772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Bresch, Harald A1 - Kipphardt, Heinrich A1 - Resch-Genger, Ute A1 - Koch, Matthias A1 - Rosner, M. T1 - Trends in selected fields of reference material production N2 - For more than 110 years, BAM has been producing reference materials for a wide range of application fields. With the development of new analytical methods and new applications as well as continuously emerging more stringent requirements of laboratory accreditation with regard to quality control and metrological traceability, the demand and requirements for reference materials are increasing. This trend article gives an overview of general developments in the field of reference materials as well as developments in selected fields of application in which BAM is active. This includes inorganic and metal analysis, gas analysis, food and consumer products, and geological samples. In addition to these more traditional fields of application, developments in the areas of optical spectroscopy, particulary fluorescence methods, and nanomaterials are considered. T2 - 150 years BAM: Science with impact CY - Berlin, Germany DA - 01.01.2021 KW - Reference material KW - ISO REMCO KW - Gas analysis KW - Food KW - Nanomaterials KW - Fluorescence PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548407 DO - https://doi.org/10.1007/s00216-022-03996-7 SN - 1618-2642 SN - 1618-2650 VL - 414 IS - Topical collection: Analytical methods and applications in the materials and life sciences SP - 4281 EP - 4289 PB - Springer CY - Berlin AN - OPUS4-54840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Poelke, B. A1 - Klein, Luise A1 - Hoffmann, H. A1 - Wilke, Olaf A1 - Roloff, A. T1 - Bestimmung von VOC-Emissionen aus Verbraucherprodukten in mikroskaligen Emissionsprüfkammern: Ergebnisse eines Rundversuchs T1 - Determining VOC Emissions from Consumer Products in Micro-Scale Emission Test Chambers: Results of a Round Robin Test N2 - Die Bestimmung der Anfangskonzentrationen flüchtiger organischer Verbindungen, die innerhalb der ersten Stunden des Gebrauchs aus Verbraucherprodukten emittiert werden, wurde in einem Ringversuch getestet, bei dem Mikro-Kammern verwendet wurden. Neun Labore nahmen an dem Ringversuch teil, der sich aus zwei Teilen zusammensetzte: Im ersten Teil wurde die analytische Leistungsfähigkeit beurteilt. Jedes beteiligte Labor erhielt zwei mit Analyten dotierte Tenax® TA Desorptionsröhrchen zur Qualitätskontrolle (QC). Im zweiten Teil führte jedes Labor Emissionsmessungen über einen Zeitraum von 48 Stunden in Mikro-Kammern mit Volumina von 44 oder 114 ml durch. Als Probenmaterial dienten Stücke eines Regenponchos, der Cyclohexanon, Phenol, 2-Ethylhexanol, Naphthalin und Isophoron in signifikanten Konzentrationen emittierte. Für den QC-Test wurden sehr geringe relative Standardabweichungen (9 14 %) erhalten. Die Ergebnisse der Emissionsmessungen waren ebenfalls sehr gut. In der frühen Phase (0,5 4 Stunden) wurden akzeptable z-Scores (|z| ≤ 2,00) von mindestens sieben Laboren erhalten, nach 24 und 48 Stunden erhielten alle Labore akzeptable z-Scores. KW - Emissionsprüfkammer KW - Ringversuch KW - Verbraucherprodukt KW - VOC-Emission PY - 2025 DO - https://doi.org/10.37544/0949-8036-2025-03-04-71 VL - 85 IS - 03-04 SP - 71 EP - 76 AN - OPUS4-63561 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Musyanovych, A. A1 - Grimmer, Christoph A1 - Sadak, A. E. A1 - Heßling, L. A1 - Lüdicke, M. A1 - Bilsel, M. A1 - Horn, Wolfgang A1 - Richter, Matthias T1 - Polymer Capsules with Volatile Organic Compounds as Reference Materials for Controlled Emission N2 - Encapsulation of volatile organic compounds (VOCs) that could evaporate at a defined rate is of immense interest for application in emission reference materials (ERMs). Polyurethane/polyurea microcapsules with various VOC active ingredients (limonene, pinene, and toluene) were successfully produced by interfacial polymerization with Shirasu porous glass membrane emulsification in a size range between 10 and 50 μm. The effect of surfactant, VOC, monomer(s) type, and ratio has a great effect on the formulation process and morphology of capsules. The type of VOC played a significant role in the encapsulation efficiency. Due to the difference in vapor pressure and VOC/water interfacial tension, the formulation for encapsulation was optimized for each individual VOC. Furthermore, to achieve effective stability of the large droplets/capsules, a combination of ionic and nonionic surfactants was used. Optical and scanning electron microscopy, Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA), were used to characterize the optimized microcapsules. The results showed that the obtained microcapsules exhibited a spherical shape and core–shell morphology and featured characteristic urethane-urea bonds. The amount of encapsulated VOC ranges between 54 and 7 wt %. The emission tests were performed with the help of the emission test chamber procedure (EN 16516). The limonene-loaded polyurethane/polyurea microcapsules show a change in emission rate of less than 10% within 14 days and can be considered as a potential candidate for use as an ERM. KW - Polymer microcapsules KW - Membrane emulsification KW - Polyaddition KW - Volatile organic compound (VOC) KW - Emission testing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-619227 DO - https://doi.org/10.1021/acsami.4c12826 SN - 1944-8252 VL - 16 IS - 50 SP - 69999 EP - 70009 PB - ACS AN - OPUS4-61922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meiers, Emelie A1 - Scholl, Juliane A1 - Droas, Morten A1 - Vogel, Christian A1 - Leube, Peter A1 - Sommerfeld, Thomas A1 - Bagheri, A. A1 - Adam, Christian A1 - Seubert, A. A1 - Koch, Matthias T1 - Development and evaluation of analytical strategies for the monitoring of per- and polyfluoroalkyl substances from lithium-ion battery recycling materials N2 - Per- and polyfluoroalkyl substances (PFAS) are well-known as “forever chemicals” and persistent pollutants released by different anthropogenic sources. The potential release of PFAS from accumulating electronic waste and lithium-ion battery (LIB) recycling activities has gained increasing attention in the past years. This creates a need for analytical methods tailored for the determination of PFAS out of environmental matrices related to the named activities or directly out of the concerned materials. In this work, analytical strategies for the monitoring of PFAS in LIB recycling materials were explored for a group of legacy perfluoro sulfonic- and carbonic acids (PFSA and PFCA) and of fluorinated sulfonylimides suspected to be LIB electrolyte ingredients. These analytical strategies comprehend PFAS target approaches with a herein optimized liquid chromatography tandem mass spectrometry (LC–MS/MS) method equipped with a HILIC (hydrophilic interaction liquid chromatography) column in combination with the TOP (total oxidizable precursor) assay and an adapted sample preparation method for high-matrix LIB recycling materials. The validated target method was applied to a set of LIB recycling materials: end-of-life batteries, black masses from hydrometallurgical recycling, and gas absorption solutions from thermal treatment of black masses as part of the recycling procedure. Investigation results show that the LIB industry can be connected to the release of both “LIB”-PFAS, such as the target sulfonylimides, and “already-legacy” PFAS, like the PFSA and PFCA. Especially, the presence of trifluoroacetic acid (TFA) as an emerging pollutant in every investigated LIB material type underlines the threat of PFAS emissions from LIB waste and recycling activities. KW - Per- and polyfluoroalkyl substances (PFAS) KW - Battery PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647015 DO - https://doi.org/10.1007/s00216-025-06165-8 SN - 1618-2642 VL - 417 SP - 6567 EP - 6583 PB - Springer Science and Business Media LLC AN - OPUS4-64701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liaskos, C. A1 - Rhoderick, G. A1 - Hodges, J. A1 - Possolo, A. A1 - Wilke, Olaf T1 - Pilot comparison CCQM-P177 - monoterpenes in nitrogen at 2.5 nmol/mol - final report N2 - Growing awareness of the impact of monoterpenes on climate, atmospheric chemistry, and indoor air quality has necessitated the development of measurement standards to globally monitor and control their emissions. For National Metrology Institutes to develop such standards, it is essential that they demonstrate measurement equivalence for assigned values at the highest levels of accuracy. This report describes the results of a pilot comparison for 4 key monoterpene species: α-pinene, 3-carene, R-limonene and 1,8-cineole, at a nominal amount-of-substance fraction of 2.5 nmol mol-1. The objective of this comparison is to evaluate participant capabilities to measure trace-level monoterpenes using their own calibration techniques. KW - Pilot comparison KW - CCQM KW - Monoterpene KW - Accuracy PY - 2020 DO - https://doi.org/10.1088/0026-1394/57/1A/08018 SN - 0026-1394 SN - 1681-7575 VL - 57 IS - 1A SP - 08018-1 EP - 08018-21 PB - IOP Science AN - OPUS4-51111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalbe, Ute A1 - Piechotta, Christian A1 - Bandow, Nicole T1 - Comparing PFAS analysis in batch leaching and column leaching tests N2 - Laboratory leaching tests are tools to assess the mobility of environmental contaminants released from granular materials. Comparative leaching tests were performed using four PFAS-contaminated soils whose concentration patterns of 10 selected perfluoroalkyl and polyfluoroalkyl substances (PFAS) differed due to the two types of contamination sources. This study aimed to evaluate the equivalence of two usual laboratory-scale leaching test procedures, batch and column percolation tests, at liquid-to-solid ratios (L/S) of 2 l/kg, which is the current practice within the German assessment framework, and 10 l/kg (relevant for some EU regulations such as the landfill directive). The differences between the replicates of leaching tests investigating PFAS were smaller for column percolation tests than for batch tests, probably mainly due to the greater sample size and the better representativeness of the sample portion analyzed. It was observed that batch tests overestimate the release of shorter-chain PFAS, whereby the effect was greater with carboxylic than with sulfonic acids. Currently, the limits of detection of analyses given by the DIN standard with regard to PFCA and PFSA in soils are partly not sufficient to detect very low contents, whereas the detection of selected PFCA and PFSA in eluates is more sensitive, in accordance with the available standards. This results in limitations when calculating mass balances. KW - PFAS KW - Leaching KW - Column percolation test KW - Batch test KW - Soil PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618187 DO - https://doi.org/10.1007/s11356-024-35510-0 SN - 1614-7499 VL - 31 IS - 57 SP - 65233 EP - 65251 PB - Springer Science and Business Media LLC AN - OPUS4-61818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grzelec, Małgorzata A1 - Haas, Sylvio A1 - Helman-Ważny, Agnieszka T1 - Application of scanning small-angle X-ray scattering in the identification of sheet formation techniques in historical papers N2 - Among writing substrates produced historically in different regions of the world, paper is one of the most complex materials. Its complexity results not only from a variety of highly processed ingredients, which can be used in its production, but also from a variety of methods in which these materials are combined to form the fibrillar network referred to as paper. While material identification methods are well established in the analysis of historical papers, the identification of manufacturing technologies is still an under-researched topic, that requires the development of appropriate methods and measurement protocols. This paper reports on the results of a research project aimed at the application of synchrotron scanning small angle X-ray scattering (SAXS) method in the characterization of paper structure, with emphasis on the assessment of fibrillar orientation as a marker characteristic for different, historical papermaking technologies. The main objective of this study consists of the development of a measurement protocol involving the SAXS technique complemented by other analytical methods in the characterization of the fibrous paper structure. KW - SAXS KW - Paper analysis KW - Papermaking technology KW - Fiber orientation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651594 DO - https://doi.org/10.1007/s00339-024-08157-4 SN - 0947-8396 VL - 131 IS - 1 SP - 1 EP - 16 PB - Springer Science and Business Media LLC AN - OPUS4-65159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grimmer, Christoph A1 - Richter, Matthias A1 - Neuhaus, T. A1 - Prinz, Carsten A1 - Strzelczyk, Rebecca Skadi A1 - Colakoglu, Irem A1 - Horn, Wolfgang T1 - Towards a multi-VOC emission reference material with temporally constant emission profile for QA/QC of materials emission testing procedures N2 - Emission reference materials (ERMs) are sought after to further control and improve indoor air quality. The impregnation of porous materials with volatile organic compounds (VOCs) is a promising approach to produce ERMs. Different VOCs were used to impregnate various porous materials (mainly zeolites, activated carbons and a metal organic framework). The influence of different methodological parameters and material properties were studied to optimize the impregnation procedure and to find the best material/VOC combination. The impregnation procedure remains quite irreproducible, nevertheless, very good ERM candidates were identified. Two materials (zeolite 4 and AC 1 impregnated with n-hexadecane) showed a very stable emission over 14 days (<10 % change). Another material (AC 1 impregnated with toluene) showed a declining emission profile but with a very good in-batch reproducibility and a storage stability of up to 12 months. KW - Emission reference material KW - Porous materials KW - Indoor air quality KW - Emission test chamber KW - CO2 assisted impregnation KW - EN 16516 PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612238 DO - https://doi.org/10.1016/j.chemosphere.2024.143437 SN - 1879-1298 VL - 366 SP - 1 EP - 8 PB - Elsevier AN - OPUS4-61223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - Roesch, Philipp A1 - Fischer, E. A1 - von der Au, Marcus A1 - Pfeifer, Jens A1 - Cossmer, Antje A1 - Wittwer, Philipp A1 - Vogel, Christian A1 - Simon, Franz-Georg A1 - Meermann, Björn T1 - Determination of organically bound fluorine sum parameters in river water samples - Comparison of combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) N2 - In this study, we compare combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) with respect to their applicability for determining organically Bound fluorine sum parameters. Extractable (EOF) and adsorbable (AOF) organically bound fluorine as well as total fluorine (TF) were measured in samples fromriver Spree in Berlin, Germany, to reveal the advantages and disadvantages of the two techniques used as well as the two established fluorine sum Parameters AOF and EOF. TF concentrations determined via HR-CS-GFMAS and CIC were comparable between 148 and 270 μg/L. On average, AOF concentrations were higher than EOF concentrations, with AOF making up 0.14–0.81% of TF (determined using CIC) and EOF 0.04–0.28% of TF (determined using HR-CSGFMAS). The results obtained by the two independent methods were in good agreement. It turned out that HR-CS-GFMAS is a more sensitive and precise method for fluorine analysis compared to CIC. EOF and AOF are comparable tools in Risk evaluation for the emerging pollutants per- and polyfluorinated alkyl substances; however, EOF is much faster to conduct. KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Combustion ion chromatography (CIC) KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Adsorbable organically bound fluorine (AOF) KW - Extractable organically bound fluorine (EOF) KW - Surface waters PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515351 DO - https://doi.org/10.1007/s00216-020-03010-y SN - 1618-2650 VL - 413 IS - 28 SP - 103 EP - 115 PB - Springer CY - Berlin AN - OPUS4-51535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Even, Morgane A1 - Juritsch, Elevtheria A1 - Richter, Matthias T1 - Measurement of very volatile organic compounds (VVOCs) in indoor air by sorbent-based active sampling: Identifying the gaps towards standardisation N2 - The ISO 16000-6 standard describes a method for the determination of volatile organic compounds (VOCs) in indoor and test chamber air by sorbent-based active sampling, thermal desorption and gas chromatography coupled with mass spectrometry (GC/MS). It also gives directions to adapt this methodology to very volatile organic compounds (VVOCs). Indeed, toxicologically based guideline values are being implemented for these compounds and it becomes necessary to measure them. But a comprehensive and robust measurement method is lacking. This work highlights the points that still need to be explored towards the standardisation of a suitable procedure: investigations on sorbent combinations, the suitability of chromatography columns and the use of gaseous standards are required. The biggest challenge remains in the fact that strong sorbents adsorb water together with VVOCs. Water may impair the analysis and the optimal approach to eliminate it is still to be found and integrated into the sampling strategy. KW - Solvents KW - Air analysis KW - VOC KW - Thermal desorption KW - Gas chromatography KW - ISO 16000-6 PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523919 DO - https://doi.org/10.1016/j.trac.2021.116265 VL - 140 SP - 116265 PB - Elsevier B.V. AN - OPUS4-52391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duarte-Ruiz, D. A1 - Saßnick, H.-D. A1 - Ferreira De Araujo, F. A1 - Gentzmann, Marie A1 - Huthwelker, T. A1 - Cocchi, C T1 - X-ray absorption spectroscopy of scandium oxide polymorphs N2 - Scandium oxide (Sc2O3) is a rare-earth oxide with significant potential in key technological areas, but due to its limited supply a deep understanding of its characteristics in different crystalline phases is still missing. Here, we present a combined experimental and ab initio X-ray absorption spectroscopy investigation of Sc2O3 focusing on excitations from the O K-edge and the Sc L2,3-edge. While measurements are performed on a cubic sample, the most stable phase under ambient conditions, six different polymorphs are computed, including two high-pressure phases with a trigonal and monoclinic lattice in addition to the cubic phase, as well as three computationally predicted structures. Our analysis of the structural and electronic properties reveals significant similarities between the cubic polymorph and the high-pressure trigonal phase, while the monoclinic crystal exhibits distinct features. The spectra simulated for these similar phases from the solution of the Bethe–Salpeter equation show very good agreement with measurements. Additional comparison with results computed in the independent-particle approximation highlights the dominant role of electron–hole correlations in shaping the absorption features, particularly at the O K-edge, where a common pattern with the features of other sesquioxides is identified. Our findings offer new insight into the spectral fingerprints of Sc2O3 polymorphs, aiding in situ characterization and informing sustainable materials management. KW - Scandium PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650806 DO - https://doi.org/10.1039/d5ra06446e VL - 15 IS - 56 SP - 47814 EP - 47825 AN - OPUS4-65080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Desvergnes, Amélie Couvrat A1 - Helman-Wazny, Agnieszka T1 - Sialkoti paper used by Pahari artists: Raw materials and fibre analysis N2 - This study aims to characterise the so-called Sialkoti paper used to produce Pahari drawings preserved today in the Wereldmuseum in Leiden (Netherlands) (WML). These works originate from the Punjab Hills in India (today Himachal Pradesh) and are commonly known as ‘Pahari miniature paintings’. The paper upon which these drawings are executed is said to have been produced in Sialkot during the eighteenth and nineteenth centuries when papermaking was an integral part of an overall regional economy correlated with other sectors such as agriculture and the textile industry. Although the term Sialkoti refers to identified papermills in Sialkot (now Pakistan), the paper from this region is yet to be subjected to a systematic study. This article therefore explores the paper(s) in question through macro- and microscopic observations of structure, pulp and fibres. The study of historical sources, complemented by the analysis of paper samples and fibre identification, has revealed that the pulp would have been prepared from a variety of manufactured products using different technologies, such as rags, cloth, mats, rope and other plant-based materials made from local bast fibres which, once tattered, were recycled to prepare the pulp. Microscopic study reveals that a variety of fibre combinations under different conditions and processing steps were used, in particular sunn hemp fibre (Crotalaria juncea L.), a plant species that has until now rarely been identified in historical paper. In addition, the presence of kenaf and jute fibres, as well as a significant quantity of cotton fibres, have also been demonstrated. To overcome the lack of comparative materials, our work was supported by a comparative study of several materials made from sunn hemp now held in the Ethnobotany Collection at Kew Gardens. Samples were taken from these materials and provided useful reference micrographs for the identification of the WML samples. The quality of the paper used by Pahari artists, as well as the raw materials available and their processing, are discussed in detail. Putting all the data, including technical and historical information into perspective, we conclude that the Pahari artists used a paper of inferior quality compared to other types of paper used for other purposes such as the creation of illuminated manuscripts in the Punjab plains. This study therefore provides useful analytical and material evidence that complements previous historical, technical and anthropological studies. KW - Sialkoti paper KW - Pahari drawings KW - Indian handmade paper KW - Sunn hemp KW - Fibre identification KW - Microscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-645216 DO - https://doi.org/10.1186/s40494-024-01360-9 SN - 2050-7445 VL - 12 SP - 1 EP - 18 PB - Springer CY - Cham AN - OPUS4-64521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cohen, Zina A1 - Hahn, Oliver A1 - Rabin, Ira A1 - Ward, Aengus T1 - Centenary Paper: Of Inks and Scribes: The Composition of a Thirteenth-Century Castilian Manuscript – British Library Res 20787 N2 - This article presents the results of the first scientific analysis of the inks of a thirteenth-century Castilian manuscript – British Library Res 20787, a copy of the Fuero de las leyes. The analysis reveals the fingerprint of the inks used in the codex and points the way to future cross-disciplinary research based on a wider corpus of evidence. KW - Archaeometry KW - Manuscript KW - Colorant KW - Cinnabar PY - 2024 DO - https://doi.org/10.3828/bhs.2024.56 SN - 1475-3839 VL - 101 SP - 703 EP - 720 PB - Liverpool University Press AN - OPUS4-61435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Capitain, C. A1 - Schüßler, M. A1 - Bugsel, B. A1 - Zweigle, J. A1 - Vogel, Christian A1 - Leube, Peter A1 - Zwiener, C. T1 - Implementation of matrix-matched semiquantification of PFAS in AFFF-contaminated soil N2 - This study presents a novel semiquantification approach for nontarget screening (NTS), combining matrix-matched calibration and ionization class-specific average calibration curves (ACCs) to address the lack of analytical reference standards for most per- and polyfluoroalkyl substances (PFAS). Ionization class-specific ACCs for carboxylic and sulfonic acids, sulfonamides, and cationic PFAS result in high accuracy, with median absolute accuracy quotients below 2.27×. The approach was applied to soil impacted by aqueous film-forming foam (AFFF) contamination. A total of 96 tentatively identified PFAS were semiquantified in addition to 28 quantified compounds based on available standards. Semiquantified concentrations exceeded those of target analytes, demonstrating the critical role of this method in capturing broader PFAS contamination. In this case, validation against extractable organofluorine (EOF) showed a 102% closed mass balance. The innovative approach not only enables comprehensive PFAS contamination assessment in complex matrices but also expands the scope of the NTS for environmental monitoring, remediation, and risk assessment of AFFF-contaminated sites. KW - Per- and polyfluoroalkyl substances (PFAS) KW - Contaminated soil KW - Non-targeted analysis KW - Combustion ion chromatography PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629445 DO - https://doi.org/10.1021/acs.est.4c14255 SN - 1520-5851 VL - 59 IS - 14 SP - 7338 EP - 7347 PB - American Chemical Society (ACS) CY - Columbus, Ohio AN - OPUS4-62944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Harald A1 - Hodoroaba, Vasile-Dan A1 - Schmidt, Alexandra A1 - Rasmussen, K. A1 - Rauscher, H. T1 - Counting Small Particles in Electron Microscopy Images — Proposal for Rules and Their Application in Practice N2 - Electron microscopy (EM) is the gold standard for the characterisation of the morphology (size and shape) of nanoparticles. Visual observation of objects under examination is always a necessary first step in the characterisation process. Several questions arise when undertaking to identify and count particles to measure their size and shape distribution. In addition to challenges with the dispersion and identification of the particles, more than one protocol for counting particles is in use. This paper focuses on precise rules for the counting of particles in EM micrographs, as this influences the measurement accuracy of the number of particles, thus implicitly affecting the size values of the counted particles. We review and compare four different, commonly used methods for counting, which we then apply in case studies. The impact of the selected counting rule on the obtained final particle size distribution is highlighted. One main aim of this analysis is to support the application of a specific, well-defined counting approach in accordance with regulatory requirements to contribute to achieving more reliable and reproducible results. It is also useful for the new harmonised measurement procedures for determining the particle size and particle size distribution of nanomaterials. KW - Nano KW - Particle size distribution KW - Nanoparticle KW - Nanomaterial KW - OECD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551891 DO - https://doi.org/10.3390/nano12132238 SN - 2079-4991 VL - 12 IS - 13 SP - 2238 PB - MDPI CY - Basel AN - OPUS4-55189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Scholz, Philipp A1 - Jung, Christian A1 - Weidner, Steffen T1 - Thermo-Desorption Gas Chromatography-Mass Spectrometry for investigating the thermal degradation of polyurethanes N2 - Thermo-Desorption Gas Chromatography-Mass Spectrometry (TD-GC-MS) was used to investigate the thermal degradation of two different polyurethanes (PU). PU samples were heated at different heating rates and the desorbed products were collected in a cold injection system and thereafter submitted to GC-MS. Prospects and limitations of the detection and quantification of semi-volatile degradation products were investigated. A temperature dependent PU depolymerization was found at temperatures above 200 °C proved by an increasing release of 1,4-butanediol and methylene diphenyl diisocyanate (MDI) representing the main building blocks of both polymers. Their release was monitored quantitatively based on external calibration with authentic compounds. Size Exclusion Chromatography (SEC) of the residues obtained after thermodesorption confirmed the initial competitive degradation mechanism indicating an equilibrium of crosslinking and depolymerization as previously suggested. Matrix-Assisted Laser Desorption Ionization (MALDI) mass spectrometry of SEC fractions of thermally degraded PUs provided additional hints on degradation mechanism. KW - Thermo-desorption KW - Mass spectrometry KW - Polyurethanes KW - Thermal degradation PY - 2023 DO - https://doi.org/10.1039/D3AY00173C SN - 1759-9660 SP - 1 EP - 6 PB - Royal Society for Chemistry AN - OPUS4-57307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Albarrán Martínez, M. J. A1 - Ghigo, Tea T1 - The practice of writing inside an Egyptian monastic settlement N2 - Over the last few years, the Federal Institute for material research (BAM, Berlin) together with the Centre for the Study of Manuscript Cultures (CSMC, University of Hamburg) have initiated a systematic material investigation of black inks produced from Late Antiquity to the Middle Ages (ca. fourth century CE–fourteenth/fifteenth centuries CE), aimed primarily at extending and complementing findings from previous sporadic studies. Part of this systematic investigation has focused on Egyptian Coptic manuscripts, and the present preliminary study is one of its outputs. It centres on a corpus of 45 Coptic manuscripts—43 papyri and 2 ostraca—preserved at the Palau-Ribes and Roca-Puig collections in Barcelona. The manuscripts come from the Monastery of Apa Apollo at Bawit, one of the largest monastic settlements in Egypt between the Late Antiquity and the Early Islamic Period (sixth–eighth centuries CE). The composition of their black inks was investigated in situ using near-infrared reflectography (NIRR) and X-ray fluorescence (XRF). The analyses determined that the manuscripts were written using different types of ink: pure carbon ink; carbon ink containing iron; mixed inks containing carbon, polyphenols and metallic elements; and iron-gall ink. The variety of inks used for the documentary texts seems to reflect the articulate administrative system of the monastery of Bawit. This study reveals that, in contrast to the documents, written mostly with carbon-based inks, literary biblical texts were written with iron-gall ink. The frequent reuse of papyrus paper for certain categories of documents may suggest that carbon-based inks were used for ephemeral manuscripts, since they were easy to erase by abrasion. KW - Papyrus KW - Ink analysis KW - Coptic manuscripts KW - Bawit KW - Mixed ink KW - Near-infrared refectography KW - X-ray fuorescence PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528833 DO - https://doi.org/10.1186/s40494-021-00541-0 SN - 2050-7445 VL - 9 IS - 1 SP - 1 EP - 15 PB - Springer Open CY - Rome, Italy AN - OPUS4-52883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -