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 JF - Environmental Science: Processes & Impacts 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 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 VL - 2 IS - 10 SP - 1436 EP - 1445 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58342 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 JF - Przemysł Chemiczny 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 JF - Chemosphere 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 JF - Science of The Total Environment 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 - 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 JF - Environmental Science and Technology 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 JF - Analytical and bioanalytical chemistry 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 - 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 JF - Metrologia 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 - Lehnik-Habrink, Petra A1 - Bandow, Nicole A1 - Sauer, Andreas T1 - Validation of European horizontal methods for the analysis of PAH, PCB and dioxins in sludge, treated biowaste and soil JF - Environmental Science Europe N2 - Draft standards for the determination of organic pollutants in the solid matter of environmental matrices such as sludge, treated biowaste and soil have been basically developed in the framework of the European standardization project HORIZONTAL. A research project financed by the German Federal Environment Agency was initiated to finalize some of these CEN standard drafts, since fully validated standard procedures are crucial for the evaluation of their reliability in the context of implementation in legislation on environmental health. Approach: Appropriate test materials (< 2mm particle size) were prepared and homogenized from contaminated soils, sludge and treated biowaste containing polycyclic aromatic hydrocarbons (PAH), polychlorinated biphenyls (PCB), dioxins, furans and dioxin-like-PCB and served, along with reference solutions, as the basis for international interlaboratory comparisons. Performance data of three analytical standard procedures were obtained by the statistical evaluation of results received from 11 to 29 participants per test material. Results: The overall variation coefficients of reproducibility (between-lab standard deviations) for the sum parameters were roughly between 10 and 35 %. The variation coefficients of repeatability (within-lab standard deviations) range between 3 % and 8 % and show no trend considering the substance groups or matrices. The highest coefficients of reproducibility were found for the analysis of PAHs, which were between 26 and 35 %, depending on the matrix, whereas 7-17 % reproducibility was observed for toxicity equivalents (TEQ) comprising dioxins, furans and dl-PCB. Conclusions: Overall, the results confirm that the procedures described in the Technical Specifications are fit for purpose for all three matrices and that the feasibility of the HORIZONTAL approach, to cover several matrices with one standard per analyte, was thereby proven. KW - Standardization KW - Analytical methods KW - Organic contaminants KW - Validation trial KW - Interlaboratory comparison PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479914 DO - https://doi.org/10.1186/s12302-019-0211-3 SN - 2190-4715 VL - 31 SP - 29, 1 EP - 10 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-47991 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) JF - Analytical and bioanalytical chemistry 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 JF - TrAC Trends in Analytical Chemistry 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 - 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 JF - Nanomaterials 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 - Borzekowski, Antje A1 - Drewitz, T. A1 - Keller, Julia A1 - Pfeifer, Dietmar A1 - Kunte, Hans-Jörg A1 - Koch, Matthias A1 - Rohn, S. A1 - Maul, R. T1 - Biosynthesis and characterization of zearalenone-14-sulfate, zearalenone-14-glucoside and zearalenone-16-glucoside using common fungal strains JF - Toxins N2 - Zearalenone (ZEN) and its phase II sulfate and glucoside metabolites have been detected in food and feed commodities. After consumption, the conjugates can be hydrolyzed by the human intestinal microbiota leading to liberation of ZEN that implies an underestimation of the true ZEN exposure. To include ZEN conjugates in routine analysis, reliable standards are needed, which are currently not available. Thus, the aim of the present study was to develop a facilitated biosynthesis of ZEN-14-sulfate, ZEN-14-glucoside and ZEN-16-glucoside. A metabolite screening was conducted by adding ZEN to liquid fungi cultures of known ZEN conjugating Aspergillus and Rhizopus strains. Cultivation conditions and ZEN incubation time were varied. All media samples were analyzed for metabolite formation by HPLC-MS/MS. In addition, a consecutive biosynthesis was developed by using Fusarium graminearum for ZEN biosynthesis with subsequent conjugation of the toxin by utilizing Aspergillus and Rhizopus species. ZEN-14-sulfate (yield: 49%) is exclusively formed by Aspergillus oryzae. ZEN-14-glucoside (yield: 67%) and ZEN-16-glucoside (yield: 39%) are formed by Rhizopus oryzae and Rhizopus oligosporus, respectively. Purities of ≥73% ZEN-14-sulfate, ≥82% ZEN-14-glucoside and ≥50% ZEN-16-glucoside were obtained by 1H-NMR. In total, under optimized cultivation conditions, fungi can be easily utilized for a targeted and regioselective synthesis of ZEN conjugates. KW - Mycotoxin KW - Zearalenone KW - Conjugate KW - Biosynthesis KW - Fusarium KW - Aspergillus KW - Rhizopus PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444246 DO - https://doi.org/10.3390/toxins10030104 SN - 2072-6651 VL - 10 IS - 3 SP - Article 104, 1 EP - 15 PB - MDPI CY - Basel AN - OPUS4-44424 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Borzekowski, Antje A1 - Anggriawan, R. A1 - Auliyati, M. A1 - Kunte, Hans-Jörg A1 - Koch, Matthias A1 - Rohn, S. A1 - Karlovsky, P. A1 - Maul, Ronald T1 - Formation of Zearalenone Metabolites in Tempeh Fermentation JF - Molecules N2 - Tempeh is a common food in Indonesia, produced by fungal fermentation of soybeans using Rhizopus sp., as well as Aspergillus oryzae, for inoculation. Analogously, for economic reasons, mixtures of maize and soybeans are used for the production of so-called tempeh-like products. For maize, a contamination with the mycoestrogen zearalenone (ZEN) has been frequently reported. ZEN is a mycotoxin which is known to be metabolized by Rhizopus and Aspergillus species. Consequently, this study focused on the ZEN transformation during tempeh fermentation. Five fungal strains of the genera Rhizopus and Aspergillus, isolated from fresh Indonesian tempeh and authentic Indonesian inocula, were utilized for tempeh manufacturing from a maize/soybean mixture (30:70) at laboratory-scale. Furthermore, comparable tempeh-like products obtained from Indonesian markets were analyzed. Results from the HPLC-MS/MS analyses show that ZEN is intensely transformed into its metabolites alpha-zearalenol (alpha-ZEL), ZEN-14-sulfate, alpha-ZEL-sulfate, ZEN-14-glucoside, and ZEN-16-glucoside in tempeh production. alpha-ZEL, being significantly more toxic than ZEN, was the main metabolite in most of the Rhizopus incubations, while in Aspergillus oryzae fermentations ZEN-14-sulfate was predominantly formed. Additionally, two of the 14 authentic samples were contaminated with ZEN, alpha-ZEL and ZEN-14-sulfate, and in two further samples, ZEN and alpha-ZEL, were determined. Consequently, tempeh fermentation of ZEN-contaminated maize/soybean mixture may lead to toxification of the food item by formation of the reductive ZEN metabolite, alpha-ZEL, under model as well as authentic conditions. KW - Modified mycotoxins KW - Zearalenone sulfate KW - a-zearalenol KW - Food fermentation KW - Rhizopus and Aspergillus oryzae PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-491126 DO - https://doi.org/10.3390/molecules24152697 VL - 24 IS - 15 SP - 2697 PB - MDPI AN - OPUS4-49112 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 JF - Analytical Methods 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 JF - Heritage Science 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 -