Chemische Charakterisierung und Spurenanalytik
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- 4 Material und Umwelt (80) (entfernen)
Eingeladener Vortrag
- nein (34)
Per- and polyfluoroalkyl substances (PFAS) are a group of more than 4700 anionic and cationic anthrophonic substances which have been used extensively in a variety of products and industries due to their inert chemical stability and resistance to degradation by heat or acids. As a result of continuous use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil and groundwater resources. However, because of the continuous use of fluorinated consumer products, also effluents and sewage sludge from wastewater treatment plants (WWTPs) have been shown to be an important source of PFAS contamination into the aquatic environment. Resulting from recent stricter regulations and restrictions in the last years on the use of long chain (≥C8) PFAS, there is a significant shift in the chemical industry towards production of short (C4-C7) and ultrashort (C1-C3) chain alternatives. With the amendment of the Sewage Sludge Ordinance in 2017 the German legislation banned sewage sludge application on agricultural land, and by 2029/2032 sewage sludge will be completely prohibited from agricultural application. While environmental exposure of organic pollutants like PFAS, pesticides and pharmaceuticals are no longer desirable, phosphorus (P) from sewage sludge must still be used to produce high-quality P-fertilizers for a circular economy. Currently, plant-available P-fertilizers from sewage sludge/wastewater can be produced using a variety of treatment approaches including precipitation, leaching, and thermal treatment. However, the fate of legacy and emerging PFAS compounds during P leaching, precipitation and treatment from sewage sludge and wastewater is for the most parts still unknown.
Per- und polyfluorierte Alkylsubstanzen (PFAS) im Klärschlamm - Analytische Methoden und Grenzwerte
(2022)
Per- und Polyfluoralkylsubstanzen (PFAS) sind eine Gruppe von mehr als 4700 anionischen und kationischen anthrophonen Stoffen, die aufgrund ihrer inerten chemischen Stabilität und ihrer Widerstandsfähigkeit gegen den Abbau durch Hitze oder Säuren in einer Vielzahl von Produkten verwendet werden. Infolge der ständigen Verwendung, vor allem in Feuerlöschschäumen für die Luftfahrt, wurden in Tausenden von Industrie- und Militäranlagen kontaminierte Böden und Grundwasservorkommen gefunden. Aufgrund der ständigen Verwendung von fluorierten Konsumgütern haben sich jedoch auch Abwässer und Klärschlamm aus Kläranlagen als Quelle für die Kontamination der aquatischen Umwelt mit PFAS erwiesen. Infolge der strengeren Vorschriften und Beschränkungen, die in den letzten Jahren für die Verwendung langkettiger (≥C8) PFAS erlassen wurden, findet in der chemischen Industrie eine deutliche Verlagerung hin zur Herstellung kurz- (C4-C7) und ultrakurzkettiger (C1-C3) Alternativen statt. Mit der Novellierung der Klärschlammverordnung im Jahr 2017 hat der deutsche Gesetzgeber die Ausbringung von Klärschlamm auf landwirtschaftlichen Flächen verboten, und bis 2029/2032 wird die Ausbringung von Klärschlamm in der Landwirtschaft vollständig verboten sein. Während die Belastung der Umwelt mit organischen Schadstoffen wie PFAS, Pestiziden und Arzneimitteln nicht mehr erwünscht ist, muss Phosphor (P) aus Klärschlamm weiterhin zur Herstellung hochwertiger P-Dünger für eine Kreislaufwirtschaft genutzt werden. Derzeit können pflanzenverfügbare P-Düngemittel aus Klärschlamm/Abwasser mit verschiedenen Behandlungsmethoden hergestellt werden, darunter Fällung, Auslaugung und thermische Behandlung. Der Verbleib von PFAS bei der Auslaugung, Ausfällung und Behandlung von Klärschlamm und Abwasser ist jedoch noch weitgehend unbekannt.
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.
Volatile organic compounds (VOCs) emitted by furniture and
building materials can cause health issues. For an
improvement of indoor air quality low emitting materials
should be used. Quality assurance and –control (QA/QC)
measures require an emission reference material (ERM) with a
predictable emission rate of VOCs. The idea is to use porous
materials as ERM, which store the VOCs inside their pores and
emit them constantly.
Per- and polyfluoroalkyl substances (PFAS) were classified as a group of highly concerning chemicals over the last decades. Because of the high persistence of PFAS, their previous use led to contamination of the environment and human population. Due to ongoing use and incomplete remediation or destruction methods, the PFAS background in the environment is growing continuously.
The presence of ultrashort PFAS (with ≤3 carbon atoms) in the environment is often overlooked despite their contributions to PFAS levels. These compounds may directly contaminate the environment and arise from degradation of polyfluorinated compounds as well as incomplete PFAS destruction in certain industrial processes. Nonetheless, few approaches for targeted analysis of ultrashort PFASs have been developed, except for trifluoroacetic acid (TFA). Beside liquid (LC-MS/MS), supercritical fluid (SFC-MS/MS), and ion chromatography (IC-MS)-based systems, gas chromatography coupled with mass spectrometry (GC-MS) is a promising method for detection and quantification of ultrashort PFAS.
The goal of this study was to develop a simple headspace GC-MS method for the quantification of ultrashort perfluorocarboxylic acids (PFCAs) and polyfluorinated alcohols (PFOHs) in water samples. In contrast to PFOHs, functionalization of PFCAs was required for quantification. This was done by esterification with methanol at 80 °C, which can be carried out directly in the headspace GC-MS system.
Moreover, several parameters were optimized to achieve a low limit of quantification (LOQ) for the analytes used: i) The ratio of the aqueous solution, methanol, and available gas phase within the analysis vessel, ii) the concentration of additional acid in esterification mixtures of PFCAs, iii) shaking frequency and iv) shaking time before analysis. After optimizing the procedure, we were able to quantify ultrashort PFCAs and PFOHs. Thus, our developed headspace GC-MS method has the potential to be used as an alternative target analysis for ultrashort-chain PFCAs and PFOHs in various water samples (groundwater, wastewater).
Ultrashort PFAS (≤ 3 carbon atoms) were overlooked for a long time in analytical monitoring. Beside through the use of these substances, they contribute to the PFAS background in the environment through (environmental/ bio-) degradation and incomplete destruction3 of PFAS with longer carbon chains or other fluorinated compounds. As part of the German-Israeli Cooperation in Water Technology Research project „Detection, quantification, and treatment of per- and polyfluoroalkyl substances in groundwater“ (DEFEAT-PFAS), we are developing an as simple as possible direct headspace (HS-)GC-MS method to detect trifluoroacetic acid (TFA) and perfluoropropanioc acid (PFPrA), as well as trifluoroethanol (TFEtOH), pentafluoropropanol(PFPrOH) and hexafluoroiospropanol (HFIP) in water samples. Here we present the results of the PFAS mentioned in spiked ultrapure water solutions.
In this paper, we discuss the importance of scientifically investigating cultural artefacts in a non-invasive way. Taking as test case Leonardo da Vinci’s Manuscript with anatomic drawings and notes, which is stored in Weimar, we clarify fundamental steps in the chronology of this folio. By means of microscopy, infrared reflectography, UV photography, and X-ray fluorescence analysis, we were able to identify various types of sketching material and several varieties of iron gall ink. For his sketches, Leonardo used two different sketching tools, a lead pencil and a graphite pencil, as well as several types of ink for developing these sketches into drawings. With regard to ink, it is important to observe that there is no difference between the ink Leonardo used for drawing and the ink he used for writing text. Based on the materials analysed, we suggest a chronology for the creation of this unique folio.
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.
Gegenstand des Projekts ist die Prüfung der Umweltbeständigkeit und -verträglichkeit von Materialien und Produkten hinsichtlich der Emission von potenziellen Schadstoffen in die Umwelt. Hierzu werden chemisch-physikalische Einflüsse (Bewitterung) und mikrobielle Beanspruchungen an Modellmaterialien evaluiert. So werden die Freisetzungsraten von Schadstoffen in Abhängigkeit der Beanspruchung beschrieben. Als Modellmaterialien kommen die Polymere Polycarbonat, Polytetrafluorethylen, Polystyrol und Polypropylen zum Einsatz. Synergistische Effekte der Bewitterungsparameter und der mikrobiologischen Beanspruchung sollen dabei ebenso betrachtet werden, wie die gezielte Alterung. Auch findet eine Beschreibung des Verhaltens der ausgetragenen Schadstoffe in den Umweltkompartimenten Boden oder Wasser statt. Hier sind mit Hilfe der zu entwickelnden Screening- und non-Target-Analyseverfahren die Transformation und der Metabolismus durch Mikroorganismen zu beschreiben. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden, die es gestatten, Schnellprüfverfahren zu etablieren, die die Simulation der realen Beanspruchungen im Zeitraffermodell anwendbar machen. Somit sollen standardisierbare Schnellbeanspruchungs-verfahren erarbeitet werden, die als Prüfeinrichtungen etabliert werden und von externen Auftraggebern zur Prüfung der Umweltbeständigkeit und -verträglichkeit von neuen Materialien genutzt werden können. Die Umweltwirkungen (chemisch-physikalisch und mikrobiologisch) sollen so definiert eingesetzt werden, dass eine reproduzierbare Prüfung möglich wird. Aus diesen Verfahren und Methoden sollen Normen abgeleitet werden, die eine standardisierte Materialprüfung ermöglichen.
The BAM Data Store
(2023)
As a partner in several NFDI consortia, the Bundesanstalt für Materialforschung und -prüfung (BAM, German federal institute for materials science and testing) contributes to research data standardization efforts in various domains of materials science and engineering (MSE). To implement a central research data management (RDM) infrastructure that meets the requirements of MSE groups at BAM, we initiated the Data Store pilot project in 2021. The resulting infrastructure should enable researchers to digitally document research processes and store related data in a standardized and interoperable manner. As a software solution, we chose openBIS, an open-source framework that is increasingly being used for RDM in MSE communities.
The pilot project was conducted for one year with five research groups across different organizational units and MSE disciplines. The main results are presented for the use case “nanoPlattform”. The group registered experimental steps and linked associated instruments and chemicals in the Data Store to ensure full traceability of data related to the synthesis of ~400 nanomaterials. The system also supported researchers in implementing RDM practices in their workflows, e.g., by automating data import and documentation and by integrating infrastructure for data analysis.
Based on the promising results of the pilot phase, we will roll out the Data Store as the central RDM infrastructure of BAM starting in 2023. We further aim to develop openBIS plugins, metadata standards, and RDM workflows to contribute to the openBIS community and to foster RDM in MSE.
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.
Thermal Destruction of PFAS
(2023)
Thermal treatment processes are currently the only full-scale option for thedestruction of per- and polyfluoroalkyl substances (PFAS) in large waste streams. While all organic molecules including PFAS are susceptible to thermal destruction, their decomposition rates are controlled by process variables such as temperature, reaction atmosphere, and residence time. Concerns exist about the formation of products of incomplete destruction and their emission from hazardous waste incinerators. This talk will summarize the current stateof-the-art of thermal PFAS destruction, identify research needs, and showcase future research designed to address critical knowledge gaps.
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.
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.
In der Berliner Sammlung "Manuscripta Americana" befinden sich Fragmente von Bilderhandschriften, die Alexander von Humboldt 1804 in Mexiko erwarb und der Königlichen Bibliothek schenkte. Die in der frühen Kolonialzeit hergestellten verschiedenartigen Codices waren damals schon nicht mehr an den Orten ihrer ursprünglichen Verwendung. Entsprechend ihres Seltenheitswertes gelangten einzelne Schriftstücke seit der Conquista in die Bestände bedeutender Persönlichkeiten. Hierzu fertigte man auch Abschriften oder Kopien an, oder zerstückelte sogar einzelne Blätter, so dass die Darstellungen auf den abgetrennten Fragmenten oft nur zum Teil abgebildet vorliegen.
Um herauszufinden, ob einige Schriftstücke der "Humboldt Codices" in Bezug zu einander stehen, werden die Dokumente, ihre Symbole und Schriftzeichen und das zur Herstellung verwendete Material miteinander verglichen.
Mit den für die Analyse von Manuskripten bewährten Untersuchungsmethoden werden Papier und Farbmittel identifiziert. Hierzu zählen Raman-, FTIR-, Röntgenfluoreszenz- und VIS- Spektroskopie. Charakteristisch für die Herstellung von schriftlichen Dokumenten in der Kolonialzeit von Amerika ist die Verwendung von indigenem Material wie Papier aus Baumrinde und Pflanzenfarben zusammen mit den aus Europa bekannten Materialien. Geklärt wird, inwieweit neben den bekanntesten Farbstoffen wie Cochenille, Mayablau oder Mischungen mit Tonmineralen auch mineralische Pigmente zum Einsatz kamen.
Vorgestellt werden die auf Tafel 36 in den "Vues des Cordillères et Monuments des Peuples Indigènes de l`Amerique, Voyage de Humboldt et Bonpland" abgebildeten Fragmente. Die hier von Humboldt vorgenommene Zusammenstellung wird mit der Farbpalette der in Berlin archivierten originalen Schriftstücke verglichen. Die Interpretation der Ergebnisse gibt einen Hinweis auf die Zuordnung oder auch Zusammengehörigkeit dieser einzigartigen Dokumente amerikanischer Geschichte. Hierbei wird die Frage aufgeworfen, inwiefern davon auszugehen ist, dass diese mit weiteren Fragmenten in Verbindung gebracht werden können, was für die Beleuchtung der kulturhistorischen Zusammenhänge von großer Bedeutung ist.
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.
Summary: A screening test for potential emissions of volatile organic compounds (VOC) was run on different thermoplastic filaments used for 3D printing. The method of direct thermal desorption was used to simulate the high temperatures during the 3D printing process and to identify the main compounds emitted from the filaments. A large number of unexpected compounds were detected that might affect the user’s health and have an impact on indoor air chemistry.
Introduction: The use of desktop 3D printers is increasing. Compared to other devices with known emissions, e.g. laser printers, there is still a lack of information on possible emissions of VOC and ultrafine particles during operation and the effect on indoor air quality. Most of the commercially available desktop 3D printers operate with a molten polymer deposition. For this process a solid thermoplastic filament is heated in an extrusion nozzle. Most filaments for desktop 3D printers use either acrylonitrile butadiene styrene (ABS) or polylactic acid (PLA) as filament. Alternatives are polyvinyl alcohol (PVA) or polycarbonate (PC).
Method: Eight different thermoplastic filaments for 3D printers were analysed by direct thermal desorption followed by GC-MS identification of the emitted substances. Direct thermal desorption was done by desorbing 5 mg of the feedstock for 1 minute at a temperature of 210°C. This is an average temperature for 3D printing with thermoplastic filaments.
Results and conclusions: The comparison of the 4 different filament groups showed the highest overall emissions from ABS, followed by PLA, PC and PVA. Filament ABS 2 emitted mainly SVOCs and triphenyl phosphate, the latter has the highest emission for a single compound from all evaluated filaments.
Thermoplastic filaments are a new source of VOC emissions due to the high temperatures associated with 3D printing, which can reach up to 270°C. Some of the detected compounds like lactic acid, lactide and bisphenol A have never been described before in the indoor environment. Additionally some of the main substances could not be identified and some others might have the potential to affect the indoor air chemistry.
The appearance of some newly detected compounds raises concerns about potential health effects for the users of 3D printers at home.
Wasserzeichen und Papierstrukturen können einen wesentlichen Beitrag bei der Analyse von Kunstobjekten auf Papier darstellen. Ausgangspunkt hierfür bildet die korrekte Dokumentation mit entsprechender Bildaufnahme und der richtigen Erfassung und Interpretation der Phänomene. An Fallbeispielen aus Forschungsprojekten zu niederländischen Zeichnungen am Kupferstich-Kabinett Dresden und der Grafischen Sammlung Weimar sollen die Möglichkeiten der Papier- und Wasserzeichenforschung als historische Hilfswissenschaft demonstriert werden. Dieser Abendvortrag dient zugleich als Einführung in die Technologie der (Hand-)Papierherstellung, Wasserzeichenerfassung und –recherche.
In addition to previously reported results on the simulated aging of polystyrene samples (PS) containing 1 wt. % hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene (PP)-samples containing 0.1 wt. % BDE-209. All studied polymer samples were exposed to a defined weathering schedule in a climate chamber in accordance to regulation EN ISO 4892-3:2006.For the determination of BDE-209 in the collected rain water samples derived from the used climate chamber, the samples were prepared in accordance with a validated protocol. Before the analyses, each sample was spiked with 2 µL of isotopically labeled BDE-209 (13C10-BDE-209) to serve as internal standard (ISTD) in the performed stable isotope dilution analysis. Subsequently the samples were extracted with isooctane, the obtained aliquots of the extracts were concentrated to 200 µL and 2 µL of the resulting solution were injected to the GC/MS for quantification.
Additionally, the total bromine contents are monitored for the aged and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) as well as X-ray fluorescence analysis (XRF) as non-destructive and rapid method. Furthermore, results from surface analysis using environmental scanning electron microscopy (ESEM) for morphological characterization of the aged and untreated samples were presented and discussed. In general, the resulting data from the accelerated aging will be compared to those from the natural weathering experiments (“atmospheric exposure”, in soil).
The atmospheric exposure was performed by placing the samples on a weathering rack, which is aligned in SW direction (in a 45° angle to the horizon). The weathering data were regularly recorded by Deutscher Wetterdienst at this site. The surfaces of the test specimens (aged and stored references) were analyzed by ESEM as well as by LA-ICP-MS and by XRF. The surface of PS and PP specimens aged outdoors present the aging under real conditions and allow the comparison to the accelerated aged specimens by means of the weathering chamber. This way, we explore the efficiency of the accelerated aging procedure, which provides the advantage of well-defined and reproducible conditions compared to natural weathering, as a tool for testing different plastic materials.
Additionally “in soil” experiments were conducted in-door in a well characterized testing soil. The soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining concrete basin inside of an air-conditioned room. In this manner, TOC, water capacity and humidity are recorded parameters. To assure a washing out process from the samples by the raining water, the target water content is calculated to 8%. The actual humidity is measured by a tensiometer, assuring the duration of the raining period. The water content is additionally monitored by weight of the basin, capturing water from raining periods. The correct humidity is a fundamental parameter for biological activity. Samples of PS resp. PP were of dimension 10x1cm and 5 specimens were placed up to the half in the soil per basin. Microbial activity of the soil, monitored by the reference polyurethane, sets HBCD resp. BDE-209 of the samples free and will be leached from the samples by raining water. Thereafter these will be captured by passive samplers placed in a distinct distance to the samples in the soil. The “in soil” experiments are complementary to the weathering experiments due to the biological activity in the soil. These experiments simulate the fate of the brominated flame retardants in the biosphere.
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.