TY - CONF A1 - Simon, Fabian T1 - A fast and simple extraction method for the determination of PFASs in soil samples - HR-CS-GFMAS a new screening tool N2 - Here, we describe a fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) utilizing extractable organic fluorine (EOF) sum parameter analysis and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) in soil samples. After extraction and separation of inorganic and organic fluorinated compounds, organically bound fluorinated compounds were indirectly determined via the molecular absorption of gallium mono-fluoride at 211.248 nm. The implementation of the decisions of the “Stockholm Convention on persistent organic pollutants” as well as the “Protocol on Persistent Organic Pollutants of the Convention on Long-Range Transboundary Air Pollution” of the UNECE include the reduction respectively the elimination of PFASs in the environment. Currently, regulations aim to target single compounds (mostly C8-PFAS). But the PFAS group includes over 4700 substances, which are potentially persistent and toxic, thus target analytical approaches are not suitable for a holistic approach investigating the PFAS pollutant situation. Furthermore, forbidden PFASs are substituted by short-chain PFASs, thus the number of unknow substances is steadily increasing. For this reason, sum parameter approaches are more suitable to investigate and assess the pollution situation as well as derive exposure limits. Our developed analytical method was successfully applied to determine PFASs in soil samples from a polluted site. In view of steadily increasing numbers of PFAS substances, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFAS in the future. T2 - ENSOr - International Workshop on Emerging policy challenges on new soil contaminants CY - Online Meeting DA - 06.05.2021 KW - PFAS KW - HR-CS-GFMAS KW - Soil KW - Sediment PY - 2021 AN - OPUS4-52608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - A fast and simple PFAS extraction method for soil sample analysis using HR-CS-GFMAS N2 - Per- and polyfluorinated alkyl substances (PFASs) are a substance class of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their different chemical and physical properties as well as the high number of target substances. 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 a realistic PFAS pollution level. PFAS sum parameters compromise 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 indirect 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 describe a fast and simple extraction method for the determination of the EOF using HR-CS-GFMAS in soil samples. Common approaches for the EOF determination use solid phase extraction (SPE). To omit the bias of this time consuming and expensive step we optimized a fast and simple SPE-free extraction method. The developed extraction method consists of a liquid-solid extraction using acidified methanol. Comparison of the method with and without an SPE clean-up step revealed a drastic underestimation of EOF concentrations using SPE. In the next step, the applicability of our method was tested for other solid matrices. In view of steadily increasing numbers of PFASs, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFASs in the future. T2 - Analytica conference CY - München, Germany DA - 21.06.2022 KW - PFAS KW - HR-CS-GFMAS KW - Soil KW - Fluorine KW - SPE PY - 2022 AN - OPUS4-55124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - A fast and simple PFAS extraction method for soil samples utilizing HR-CS-GFMAS N2 - Here, we describe a fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) utilizing extractable organic fluorine (EOF) sum parameter analysis and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) in soil samples. After extraction and separation of inorganic and organic fluorinated compounds, organically bound fluorinated compounds were indirectly determined via the molecular absorption of gallium mono-fluoride at 211.248 nm. The implementation of the decisions of the “Stockholm Convention on persistent organic pollutants” as well as the “Protocol on Persistent Organic Pollutants of the Convention on Long-Range Transboundary Air Pollution” of the UNECE include the reduction respectively the elimination of PFASs in the environment. Currently, regulations aim to target single compounds (mostly C8-PFAS). But the PFAS group includes over 4700 substances, which are potentially persistent and toxic, thus target analytical approaches are not suitable for a holistic approach investigating the PFAS pollutant situation. Furthermore, forbidden PFASs are substituted by short-chain PFASs, thus the number of unknow substances is steadily increasing. For this reason, sum parameter approaches are more suitable to investigate and assess the pollution situation as well as derive exposure limits. Our developed analytical method was successfully applied to determine PFASs in soil samples from a polluted site. In view of steadily increasing numbers of PFAS substances, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFAS in the future. T2 - SALSA Make and Measure ... and Machines CY - Online meeting DA - 16.09.2021 KW - PFAS KW - HR-CS-GFMAS KW - IC KW - EOF KW - Soil PY - 2021 AN - OPUS4-53302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oelze, Marcus T1 - A second anchor Fe isotope reference material based on high purity Fe metal for the exhausted IRMM-014 N2 - Iron isotopes are used in a variety of fields from e.g., geologic question to medical applications. Measurements of iron isotopes are usually performed as delta measurements to an artificial based delta zero standard. In the case of Fe isotopes is that delta zero standard IRMM-014, a pure Fe metal. Unfortunately, that conventional delta zero reference material defining the 56/54Fe scale is out of stock and therefore unavailable. To overcome that situation and fulfill the need for laboratories that measure Fe isotope on a regular basis we will provide a set of solutions with IRMM-014 and a second anchor point for Fe isotope ratio measurements that is based on a pure Fe metal. This new second anchor point, a high purity Fe from BAM, will be calibrated against IRMM-014 and can be used as bracketing standard or as reference value for stable Fe isotope measurements. We are in the good situation that BAM ordered a large stock of IRMM-014 several years ago. That stock of IRMM-014 Fe cubes and IRMM-014 Fe wires will be dissolved in 6M HCl in a large quantity. The new anchor point, the high purity Fe metal, that is commercially available at BAM, is a pure Fe metal with only trace amounts of impurities. The high purity BAM material will also be dissolved in 6M HCl in large quantity. Several aliquots of both solutions will be measured on the Neptune Plus MC-ICP-MS to define this second anchor point with a low uncertainty. Further will we send several aliquots of both solutions to different laboratories to also measure this second anchor point of high purity Fe on the 56/54Fe scale. We will report the values of that study on BAM high purity Fe and will provide a guide for scale conversion to the IRMM-014 scale and for uncertainty calculation to use that new anchor point instead of the exhausted IRMM-014. T2 - EWCPS CY - Ljubljana, Slovenia DA - 30.01.2023 KW - Iron isotopes KW - Reference material PY - 2023 AN - OPUS4-58012 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Absolute isotope ratios - a proposed research topic N2 - An introduction into absolute isotope ratios is given, with application fields ranging from fundamental science to geochronology and forensics. This is followed by a proposal for developing new calibration approaches for obtaining absolute isotope ratios at unrivaled uncertainty levels. This new developments will set the basis for improvements in all scientific fields. T2 - EURAMET TC-MC Workshop on Isotope Ratio Analysis CY - Bern, Switzerland DA - 05.02.2020 KW - Absolute isotope ratio KW - Isotope fractionation KW - Metrology KW - Fundamental science PY - 2020 AN - OPUS4-50346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zuliani, T. T1 - Advancing Stable and Long-lived Radiogenic Isotope Ratio Measurements of Environmental Pollutants N2 - The isotopic compositions of elements vary in the environment due to processes such as radioactive decay, cosmic ray spallation, mass-dependent and mass-independent fractionation, and different anthropogenic sources such as industrial activities, nuclear weapon testing, nuclear accidents, as well as natural phenomena long-range atmospheric and water transport, climate change, etc. Isotope ratio data obtained by mass spectrometry now plays an important role as tracers of a multitude of processes in Earth and environmental sciences. Inductively coupled plasma mass spectrometry (ICP-MS) is a widely used technique for detecting variations in isotopic abundances in e.g., environmental samples. Recent advancements in mass spectrometric instrumentation have significantly enhanced sensitivity and precision, enabling the reliable detection of even minute variations in the isotopic composition of most elements with more than one natural isotope. However, to fully realize these new capabilities, a significant analytical challenge remains due to a vast number of analyte/matrix combinations, concomitant matrix effects, spectral interferences, and instrumental isotopic fractionation that must be characterized before and during the measurements. Success in developing new and improved methods for stable and long-lived radiogenic isotope ratio measurements by mass spectrometric methods depends on improvements in the reduction and quantification of uncertainties associated with sample preparation, instrumentation, and external calibration. The goal of this presentation is to show the key findings of the European Partnership on Metrology project “Metrology for the harmonisation of measurements of environmental pollutants in Europe” - MetroPOEM (https://www.npl.co.uk/euramet/metropoem), with a focus on the ICP-MS techniques used for isotope ratio measurements. Several elements were used as model systems for the development and optimisation of sample preparation and measurement procedures, including Li, B, Cr, Cd, Ni, Sb, Pb, and U. Isotope ratios of these elements determined by multi-collector ICP-MS, sector field ICPMS, quadrupole ICP-MS, and ICP-MS/MS will be assessed and compared. Data on their performance will be presented and assessed in terms of accuracy and precision. Comprehensive uncertainty budgets for the determination of the isotope ratios of the selected elements by different calibration approaches will be presented. The presented results will highlight the potential of recent advances in ICP-MS technology. T2 - 11th Nordic Conference on Plasma Spectrochemistry CY - Loen, Norway DA - 09.06.2024 KW - Isotope analysis KW - ICP-MS KW - Measurement uncertainty PY - 2024 AN - OPUS4-61599 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 - CONF A1 - Simon, Fabian T1 - An improved method for the determination of PFASs using HR CS GFMAS via GaF detection N2 - Introduction Per- and polyfluorinated alkyl substances (PFASs) are a group of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate realistic PFAS pollution levels. Methods For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. In our study we used high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) which is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L. Results Here, we present an improved method for the determination of PFASs using HR-CS-GFMAS via GaF detection. The optimized method includes a modifier pretreatment step using a mixture of Mg, Pd and Zr and a correction measurement using perfluorooctanoic acid. The combination of both resulted in increased accuracy and precision as well as overall lower detection limits. Furthermore, during optimization the influence of species-specific responses during HR-CS-GFMAS analysis was reduced resulting in a more accurate determination of PFAS sum parameters. To test the applicability of the improved method, we analysed soil samples from a former fire-fighting training area combining the improved method for detection with our previously optimized extraction method for extractable organically bound fluorine (EOF) determination in soils. Innovative aspects • Highly sensitive and selective method for fluorine/PFASs analysis based on HR-CS-GFMAS • Increased accuracy for the determination of EOF • Reduction of PFAS species-specific responses by optimized modifier conditions T2 - ANAKON23 CY - Vienna, Austria DA - 11.04.2023 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine PY - 2023 AN - OPUS4-57409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - An optimized HR-CS-GFMAS method for PFAS analysis N2 - HR-CS-GFMAS turned out to be a sensitive, fast and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) at a temperature of 1550°C. GaF can be detected at 211.248 nm providing limits of quantificationin the low μg/L range. However, several species specific effects where observed when analyzing PFASs. T2 - 1st Summer School of the CRC 1349 Fluorine-Specific Interactions Fundamentals and Functions CY - Berlin, Germany DA - 28.08.2023 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine PY - 2023 AN - OPUS4-58145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -