TY - CONF A1 - Horn, Wolfgang A1 - Richter, Matthias A1 - Wilke, Olaf T1 - Volatile organic compounds from building products - Results from seven proficiency tests with emission test chambers conducted between 2008 and 2021 N2 - Emission testing of volatile organic compounds (VOC) from materials and products is commonly based on emission test chamber measurements. To ensure the comparability of results from different testing laboratories their measurement performance must be verified. For this purpose, Bundesanstalt für Materialforschung und -prüfung (BAM) organizes an international proficiency test every two years using well-characterised test materials (one sealant, one furniture board and four times a lacquer) with defined VOC emissions. The materials fulfilled the requirements of homogeneity, reproducibility, and stability. Altogether, 41 VOCs were included of which 37 gave test chamber air concentrations between 10 and 98 µg/m³. This is the typical concentration range to be expected and to be quantified when performing chamber tests. Four compounds had higher concentrations between 250 and 1105 µg/m³. The relative standard deviations (RSD) of BAM proficiency tests since 2008 are compared and the improvement of the comparability of the emission chamber testing is shown by the decrease of the mean RSD down to 23% in 2021. In contrast, the first large European interlaboratory comparison in 1999 showed a mean RSD of 51%. T2 - Proficiency Testing in Analytical Chemistry, Microbiology and Laboratory Medicine CY - Windsor, United Kingdom DA - 25.09.2023 KW - Proficiency Test KW - VOC-Emission KW - Chamber-test PY - 2023 AN - OPUS4-59694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian A1 - Köppen, Robert A1 - Becker, Roland A1 - Bücker, Michael A1 - Ostermann, Markus A1 - Traub, Heike T1 - Weathering scenarios – Changes in polymer surface morphologies and leaching of brominated flame retardants N2 - 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. T2 - Umwelt 2018 CY - Münster, Germany DA - 09.09.2018 KW - BFR KW - Weathering KW - PP KW - PS PY - 2018 AN - OPUS4-47029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonnerot, Olivier A1 - Del Mastro, G. A1 - Hammerstaedt, J. A1 - Mocella, V. A1 - Rabin, Ira T1 - XRF Ink analysis of selected fragments from the Herculaneum collection N2 - Hundreds of papyrus rolls, carbonized during the 79CE eruption of Mount Vesuvius, were discovered in 1754 at Herculaneum. Sophisticated mechanical methods for unrolling the best-preserved scrolls have been applied, with varying success. However, such processes have been abandoned, to prevent risk from irremediable damage or loss and to preserve the integrity of the extremely fragile rolls. Following the development of X-ray based non-invasive techniques, attempts to virtually unroll the scrolls were made. The most common ink in Antiquity was carbon-based, and the main element of carbonized papyrus is carbon, making these investigations difficult. However, some attempts with synchrotron X-ray phase-contrast tomography (XPCT) were successful. Recently, the identification of antique inks containing metals raised hope that if some of the inks contain metal the rolls can be virtually unrolled using conventional CT- technique. We investigated the inks of a selection of partially unrolled fragments stored at the Biblioteca Nazionale di Napoli with X-ray fluorescence in order to select the best candidates for tomography. Despite the many difficulties (analysis of several layers sticking together, letters barely visible, difficulty to separate contribution from the ink and from the papyrus, inhomogeneity of the support, fragility of the fragments…), encouraging results were found, with a number of inks from Greek fragments found to contain additions to the soot (Fe, Pb, Cu P). T2 - International Symposium on Archaeometry CY - Online meeting DA - 16.05.2022 KW - XRF KW - Ink KW - Herculaneum KW - Papyrus PY - 2022 AN - OPUS4-54892 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strzelczyk, Rebecca A1 - Horn, Wolfgang A1 - Matthias, Richter A1 - Christoph, Grimmer T1 - Zeolites loaded with VOCs as reference for material emissions testing N2 - Nowadays, people spend most of their time indoors. Thus, a good indoor air quality is important. Emissions of volatile organic compounds (VOCs) from furniture and building materials can cause health complaints1. Quantitative VOC-emission testing is carried out under standardized conditions in emission test chambers. In the presented project an emission reference material (ERM) is developed that emits a defined mixture of VOCs which is required for quality assurance and -control (QA/QC) measures. Porous materials (e.g zeolites, activated carbons, MOFs or aerogels) are used as reservoir materials and impregnated with VOC. The porous materials are selected, among others, by their pore size, pore size distribution, polarity and availability. Due to their regular pore structure zeolites are tested at first. For a prediction of the emission profile, the ERM is supposed to exhibit a constant emission rate over time. The aim is a stability of ≤ 10 % change in the emission rate over a minimum of 14 days. Method For impregnation, the material is placed into an autoclave inside a rotatable basket. The VOC is added and the autoclave is closed. Afterwards, CO2 is inserted. The closed system is then heated to the supercritical point of CO2 (31 °C, 73.75 bar). In this state, the CO2 acts as solvent for the VOC. By rotating the basket, the distribution of the VOC is ensured. After a few minutes, the pressure is decreased slowly and the CO2 is released. For the determination of the emission profile, the impregnated sample is placed into an emission test chamber. These chambers can be operated either with dry or humid air (50 ± 5 % rel. humidity). Every second to third day, air samples are taken and analyzed by gas chromatography. For an ideal impregnation, several different pressures and temperatures as well as impregnation times are tested. Results Two zeolite materials tested in dry air conditions reach emission profiles with a decrease of less than 10 % over 14 days (heptane and toluene, respectively). Further it was discovered that smaller pellets of the same zeolite show better results than bigger particles. When the pore size of a zeolite is too small, e.g. 0.3 nm, the VOC cannot be absorbed sufficiently. The main disadvantage of zeolites is their hygroscopicity because it has a large impact on the release of VOC when they are used in emission test chambers under standardized test conditions (23 °C, 50 % rel. humidity). Activated carbons have emission profiles with a larger change over 14 days. However, the high hydrophobicity allows measurements in humid air conditions which was not possible with the before mentioned hygroscopic zeolites. It is possible to impregnate powdered materials as well, and thus powdered non-hygroscopic (n.h.) zeolites were impregnated. Their emission profiles are comparable to those of the activated carbons. The use of methylated hygroscopic zeolites with a decrease in hygroscopicity did not yield successful emission measurements. The change over 14 days is calculated only for the stable phase (~250–300 h). The desired stability of ≤ 10 % change of the emission rate over 14 days could already be reached under dry testing conditions. Further investigations under humid conditions show that zeolites with high Si/Al-ratios are non-hygroscopic and comparable to activated carbons (20–30 % change). The next step is to reduce the change in the emission rate of these materials to the aimed ≤ 10 % over 14 days. T2 - Deutsche Zeolithtagung CY - Jena, Germany DA - 28.02.2024 KW - VOC KW - Emission KW - Quality assurance KW - Reference material KW - Zeolite PY - 2024 AN - OPUS4-59843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -