TY - CONF A1 - Even, Morgane T1 - Development of a procedure for the analysis of the emissions of VVOCs N2 - Several aspects were explored towards the standardization of a suitable procedure. The use of gaseous standards is necessary and a standard gas mixture containing 60 substances was successfully generated and employed for further investigations. The suitability of different chromatography columns was addressed: The use of PLOT (Porous Layer Open Tubular) columns is well suitable for VVOC analysis. The recoveries of the 60 analytes on several adsorbents and their combinations were determined: A combination of a graphitized carbon black and a carbon molecular sieve showed great results for all analytes. Carbon molecular sieves adsorb water which can impair the analysis. Different options such as purging, the use of a drying system or splitting were investigated for water removal. This contribution will present experimental results supporting the standardization of a method for VVOC analysis. T2 - Indoor Air conference CY - Kuopio, Finland DA - 12.06.2022 KW - Analytical method KW - EN 16516 KW - ISO 16000-6 KW - VVOCs PY - 2022 AN - OPUS4-55282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Raab, A. A1 - Vogl, Jochen A1 - Solovyev, N. T1 - Isotope signature of iron, copper and zinc in mouse models (L66 and 5XFAD) and their controls used for dementia research N2 - Introduction: The influence of copper, iron and zinc concentrations on the formation of ß-amyloid plaques and neurofibrillary tangles in Alzheimer’s disease (AD) is widely discussed in the community. The results from human and animal studies so far are mixed with some studies showing a correlation and others not. From a number of studies, it is known that disease state and isotopic composition of essential elements can be coupled. Aim: The aim of the study was to identify changes in element content and isotopic composition in two transgenic mouse models used in AD research compared to their genetic WT relatives and to establish whether element content and isotopic signature between different laboratories is comparable. Methods: ß-amyloid (5xFAD) and tau overexpressing (L66) mice together with their matching wild-types were bred at dedicated facilities in accordance with the European Communities Council Directive (63/2010/EU). Serum and brain were sampled after sacrifice and the samples distributed among the participants of the study. The tissues were acid digested for total element determination and high-precision isotope ratio determination. Element content was determined by either sector-field or quadrupole-based inductively coupled plasma mass spectrometry (ICPMS). For the determination of isotope ratios multi-collector ICPMS was used. Results: Total copper content was significantly higher for L66 and their matched WT compared to 5xFAD and WT. Brains of L66 mice contained more Fe in brain than their WT, Zn and Cu were not significantly different between L66 and WT. Whereas 5xFAD mice had a slightly lower Cu and slightly higher Zn concentration in brain compared to WT. The isotopic signature in brain of L66 mice for Fe was different from their controls, whereas Zn isotope ratios were influenced in 5xFAD mice compared to their WT. The Cu isotopic ratio did not seem to be influenced in either strain. In serum, the shifts were less pronounced. Conclusion: Even though neither Tau-protein nor amyloid precursor protein are known to be metal-dependent / -containing proteins, the overexpression of both influences the Fe, Cu and Zn metabolism in brain and to some extent also in serum as can be seen not only using total element determination but probably more clearly studying the isotopic signature of Fe, Cu and Zn. T2 - The International Conference of Trace Elements and Minerals (ICTEM) 2022 CY - Aachen, Germany DA - 05.06.2022 KW - Isotope ratio KW - Isotope delta value KW - Metrology KW - Alzheimer disease KW - Measurement uncertainty PY - 2022 AN - OPUS4-55204 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schühle, Florian T1 - Bereitstellung qualitätsgesicherter VOC-Aufnahmeraten für axiale Passivsammler N2 - Quality assured uptake rates for passive sampling of indoor air VOCs Passive sampling of VOCs with Tenax® TA and thermal desorption GC-MS analysis is a simple, cost efficient and representative method to determine VOCs concentrations in indoor air. In theory, the uptake into the passive sampler is only dependent on the diffusion coefficient of the analyte in air and the geometry of the sampler (ideal adsorption). For characterization, the uptake rate (UR) is used, defined as the ratio of the uptaken mass and the product of ambient concentration and exposure time. Various reported effective uptake rates (UR,eff) differ considerably from ideal values (UR,id). Literature values in national and international standards, are essentially sorted by the applicable exposure time, while detailed information about the corresponding concentration range is lacking. Moreover the number of itemized substances is limited. The aim of this study was to review and expand this set of uptake rates by determination of own quality assured laboratory values.The determined uptake rates are considered accurate in terms of RSD and comparability to literature values and can be recommended for exposure times of seven days at 50 100 µg/m³ (approximately 100 300 ppm min). Seven day uptake rates in ISO16017 2 and ASTM D6196 are not generally suited for this purpose, as has been exemplarily shown for benzene. N2 - Die passive Probenahme von VOC (Volatile Organic Compounds) mit Tenax® TA und Thermodesorption GC/MS Analytik ist eine einfache, kosteneffiziente und repräsentative Methode zur Bestimmung der VOC-Konzentrationen in der Innenraumluft. In der Theorie ist die Stoffaufnahme in den Passivsammler nur abhängig vom Diffusionskoeffizienten der Substanz in Luft und der Geometrie des Sammlers (ideale Adsorption). Um sie zu charakterisieren, wird die Aufnahmerate (UR), definiert als Quotient der Massenaufnahme und dem Produkt aus Konzentration und Expositionszeit, verwendet. Viele effektive Aufnahmeraten (UR,eff) unterscheiden sich beträchtlich von idealen (theoretischen) Werten (UR,id). Literaturwerte sind in nationalen und internationalen Normen lediglich für bestimmte Expositionszeiten vorgegeben, während detaillierte Informationen über den zugehörigen Konzentrationsbereich fehlen. Außerdem ist die Anzahl der insgesamt in der Literatur beschriebenen Substanzen begrenzt. Das Ziel der vorgestellten Studie ist es diesen Fundus an Aufnahmeraten zu begutachten und zu prüfen und ihn durch die Bestimmung eigener qualitätsgesicherter Laborwerte zu ergänzen. Die bestimmten Aufnahmeraten werden als akkurat bezüglich ihrer relativen Standardabweichung und Vergleichbarkeit zu Literaturwerten betrachtet und können für Expositionszeiten von 7 Tagen bei Konzentrationen von 50 100 µg/m³ (ca. 100 300 ppm min) empfohlen werden. Die Sieben Tage Aufnahmeraten aus ISO16017 2 und ASTM D6196 sind nicht generell für diesen Zweck geeignet, wie exemplarisch für Benzol gezeigt wurde. T2 - Kongress 29. WaBoLu-Innenraumtage CY - Berlin, Germany DA - 24.05.2022 KW - IAQ KW - VOC KW - Passive sampling KW - Uptake rate PY - 2022 SN - 978-3-949241-04-8 AN - OPUS4-55209 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von der Au, Marcus A1 - Faßbender, Sebastian A1 - Chronakis, Michail A1 - Vogl, Jochen A1 - Meermann, Björn T1 - Size determination of nanoparticles by ICP-ToF-MS using isotope dilution in microdroplets N2 - Within this work, the combination of a microdroplet generator and an ICP-ToF-MS for nanoparticle analysis is presented. For the size determination of platinum nanoparticles an on-line isotope dilution analysis approach was developed. The 194Pt/195Pt isotopic ratio was used for the characterization of the particles, while the 182W/183W isotopic ratio was monitored simultaneously for mass bias correction. The on-line ID-MDG-sp-ICP-ToF-MS approach was deployed for the size determination of three platinum nanoparticle samples (50 nm, 63 nm, 70 nm); for validation, complementary size characterization techniques (sp-ICP-ToF-MS and TEM) were used. The robustness of this technique was evidenced, by using sodium chloride concentrations up to 100 mg L−1 as a matrix component. Our new on-line ID MDG-sp-ICP-ToF-MS approach is a promising tool for the fast and reliable determination of nanoparticles' size in severe matrix concentrations, e.g., environmental samples. KW - ICP-ToF-MS KW - Nanoparticles KW - Isotope Dilution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552727 DO - https://doi.org/10.1039/D2JA00072E SN - 0267-9477 VL - 37 IS - 6 SP - 1203 EP - 1207 PB - Royal Society of Chemistry AN - OPUS4-55272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Even, Morgane T1 - Weiterentwicklung und Validierung eines leistungsfähigen Verfahrens zur Bestimmung von VVOCs aus Bauprodukten und in der Innenraumluft N2 - Mehrere Aspekte wurden im Hinblick auf die Standardisierung eines geeigneten Verfahrens für die Analyse sehr flüchtiger organischer Verbindungen (VVOCs) untersucht. Die Verwendung gasförmiger Standards ist notwendig und es wurde ein stabiles Standardgasgemisch aus 60 Substanzen erfolgreich erzeugt und auf Stabilität und Reaktivität überprüft. Die Eignungsuntersuchung verschiedener Chromatographiesäulen ergab, dass PLOT-Säulen (Porous Layer Open Tubular) für die VVOC-Analytik gut geeignet sind. Für die 60 Analyten wurden Wiederfindungsraten auf mehreren Adsorbenzien und deren Kombinationen bestimmt. Dabei zeigte eine Kombination aus einem graphitierten Ruß und einem Kohlenstoff-Molekularsieb hervorragende Ergebnisse für alle Zielkomponenten. Nachteilig an Kohlenstoff-Molekularsieben ist, dass sie Wasser adsorbieren, was die Analyse beeinträchtigen kann. Zur Wasserentfernung wurden verschiedene Optionen wie das Trockenspülen oder der Einsatz eines Trocknungssystems untersucht. T2 - WaBoLu Innenraumtage CY - Berlin, Germany DA - 24.05.2022 KW - Analytische Methode KW - EN 16516 KW - ISO 16000-6 KW - VVOCs PY - 2022 AN - OPUS4-55281 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - Meermann, Björn T1 - Schnelle und einfache Extraktion von PFAS aus Bodenproben: Optimierte EOF-Bestimmung mittels HR-CS-GFMAS N2 - Per- und polyfluorierte Alkylsubstanzen (PFAS) bilden eine sehr komplexe Schadstoffgruppe mit über 6300 Einzelsubstanzen, die in vielfältiger Form in die Umwelt eingetragen werden. Für ein effektives Monitoring dieser Schadstoffklasse benötigt es ein Zusammenspiel aus Summenparameter-Analytik zur hot-spot-Identifizierung und Klassifizierung von Belastungssituationen sowie einer nachgeschalteten target-Analytik zur Identifizierung von Eintragswegen, die zugleich ein tieferes Verständnis von Transformationsprozessen ermöglicht. In diesem Beitrag präsentieren wir eine optimierte Extraktions-Methode für die PFAS-Summenparameteranalytik. Mit Hilfe dieser können bisher verwendete zeit- und kostenintensive Festphasenextraktionen (SPE) umgangen und PFAS-Extraktionseffizienzen gesteigert werden. Die methodische Bestimmungsgrenze (LOQ) war mit 10,30 μg/kg (Fluor pro Bodenprobe) ausreichend für alle 9 untersuchten Realbodenproben. KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - PFAS KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction KW - Böden PY - 2022 UR - https://www.gdch.de/fileadmin/downloads/Netzwerk_und_Strukturen/Fachgruppen/Umweltchemie_Oekotoxikologie/mblatt/2022/Heft122.pdf SN - 1618-3258 VL - 28 IS - 1 SP - 12 EP - 15 PB - Gesellschaft Deutscher Chemiker AN - OPUS4-54417 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Even, Morgane T1 - Development of a procedure for the analysis of the emissions of VVOCs – Results of a research project N2 - Since 1997, the Committee for Health-related Evaluation of Building Products (AgBB) has been developing the basis for building regulations for protection against indoor health risks that may arise when building products are used. In 2009, the AgBB decided to include relevant VVOCs in the assessment procedure. The ISO 16000-6 (2021) states that the use of the thermal desorption gas chromatography technique is appropriate for VVOCs, if adaptations are considered. However, a suitable method for the trustworthy quantification of VVOC emissions from building products and in the indoor air is still missing. This webinar will present the results of a research project on the development of a procedure for VVOC analysis: • identification of the gaps towards standardization • investigations on gas standards and the suitability of chromatography columns • investigations on sorbent combinations and water management • validation of the method and screening of VVOC emissions from building products. T2 - Webinar organized by Umweltbundesamt and BAM CY - Online meeting DA - 13.09.2022 KW - Analytical method KW - EN 16516 KW - ISO 16000-6 KW - VVOCs PY - 2022 AN - OPUS4-55693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - An improved method for the determination of PFAS using HR-CS-GFMAS via GaF detection N2 - Per- and polyfluorinated alkyl substances (PFASs) are a group of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate realistic PFAS pollution levels. PFAS sum parameters display the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L. Here, we present an improved method for the determination of PFASs using HR-CS-GFMAS via GaF detection. The optimized method includes a Ga pretreatment as described by Gawor et al. resulting in overall lower detection limits. Furthermore, during optimization the influence of species-specific responses during HR-CS-GFMAS analysis was reduced resulting in a more accurate determination of PFAS sum parameters. To test the applicability of the improved method, we analyzed soil samples from a former fire-fighting training area combining the improved method for detection with our previously optimized extraction method for EOF determination in soils. T2 - ESAS - CSSC CY - Brno, Czech Republic DA - 04.09.2022 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine PY - 2022 AN - OPUS4-55782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - An improved method for the determination of PFAS using HR-CS-GFMAS via GaF detection N2 - Per- and polyfluorinated alkyl substances (PFASs) are a group of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate realistic PFAS pollution levels. PFAS sum parameters display the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L. Here, we present an improved method for the determination of PFASs using HR-CS-GFMAS via GaF detection. The optimized method includes a Ga pretreatment as described by Gawor et al. resulting in overall lower detection limits. Furthermore, during optimization the influence of species-specific responses during HR-CS-GFMAS analysis was reduced resulting in a more accurate determination of PFAS sum parameters. To test the applicability of the improved method, we analyzed soil samples from a former fire-fighting training area combining the improved method for detection with our previously optimized extraction method for EOF determination in soils. T2 - SALSA - Communicating Make and Measure 2022 CY - Berlin, Germany DA - 15.09.2022 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine PY - 2022 AN - OPUS4-55783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Spallanzani, Roberta A1 - Koga, K. A1 - Cichy, S. A1 - Wiedenbeck, M. A1 - Schmidt, B. A1 - Oelze, Marcus A1 - Wilke, M. T1 - Lithium and boron difusivity and isotopic fractionation in hydrated rhyolitic melts N2 - Lithium and boron are trace components of magmas, released during exsolution of a gas phase during volcanic activity. In this study, we determine the difusivity and isotopic fractionation of Li and B in hydrous silicate melts. Two glasses were synthesized with the same rhyolitic composition (4.2 wt% water), having diferent Li and B contents; these were studied in difusion-couple experiments that were performed using an internally heated pressure vessel, operated at 300 MPa in the temperature range 700–1250 °C for durations from 0 s to 24 h. From this we determined activation energies for Li and B difusion of 57±4 kJ/mol and 152±15 kJ/mol with pre-exponential factors of 1.53 × 10–7 m2/s and 3.80× 10–8 m2 /s, respectively. Lithium isotopic fractionation during difusion gave β values between 0.15 and 0.20, whereas B showed no clear isotopic fractionation. Our Li difusivities and isotopic fractionation results difer somewhat from earlier published values, but overall confrm that Li difusivity increases with water content. Our results on B difusion show that similarly to Li, B mobility increases in the presence of water. By applying the Eyring relation, we confrm that B difusivity is limited by viscous fow in silicate melts. Our results on Li and B difusion present a new tool for understanding degassing-related processes, ofering a potential geospeedometer to measure volcanic ascent rates. KW - Hydrated silicate melts KW - Stable isotopes KW - Diffusion KW - Isotopic fractionation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554496 DO - https://doi.org/10.1007/s00410-022-01937-2 VL - 177 IS - 8 SP - 1 EP - 17 PB - Springer AN - OPUS4-55449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -