4 Material und Umwelt
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Museumsvitrinen sollen Kunst- und Kulturgut „ins rechte Licht“ setzen und vor Diebstahl oder Vandalismus schützen. Vergleicht man historische Schauvitrinen, die zumeist aus einfachen Glasscheiben in Holzrahmungen bestehen, mit heutigen Konstruktionen, lässt sich eine Entwicklung zu hochtechnisierten Gebilden ablesen, die deutlich mehr Ansprüchen genügen müssen als in der Vergangenheit.
Zahlreiche Beispiele verdeutlichen, dass Kunstwerke nicht nur außerhalb, sondern auch innerhalb von Museen oder Archiven ungünstigen Umwelteinflüssen ausgesetzt sind. So können Einbauten bzw. Dekorationen in Ausstellungsräumen, Aufbewahrungsbehältnisse in Depoträumen oder Ausstellungsvitrinen flüchtige Substanzen, sogenannte VOCs (Volatile Organic Compounds) freisetzen, die zu irreversiblen Veränderungen an den Objekten führen und diese schädigen. Hierzu zählen organische Säuren, wie Ameisen- oder Essigsäure, aber auch Verbindungen, die Sulfide enthalten. Hier wird die an der BAM entwickelte BEMMA-Bewertungsmethode vorgestellt, die von Museen verwendet werden kann Materialien mit einem geringeren Emissionspotential auszusuchen.
Metagenomic datasets of air samples collected during episodes of severe smoke-haze in Malaysia
(2021)
Transboundary emissions of smoke-haze from land and forest fires have recurred annually during the dry period (June to October, over the past few decades) in South East Asia. Hazardous air quality has been recorded in Malaysia during these episodes. Agricultural practices such as slash-and-burn of biomass and peat fires particularly in Sumatera and Kalimantan, Indonesia, have been implicated as the major causes of the haze. Past findings have shown that a diversity of microbes can thrive in air including in smoke-haze polluted air. In this study, metagenomic data were generated to reveal the diversity of microorganisms in air during days with and without haze. Air samples were collected during non-haze (2013A01) and two haze (2013A04 and 2013A05) periods in the month of June 2013. DNA was extracted from the samples, subjected to Multiple Displacement Amplification and whole genome sequencing (Next Generation Sequencing) using the HiSeq 2000 Platform. Extensive bio-informatic analyses of the raw sequence data then followed. Raw reads from these six air samples were deposited in the NCBI SRA databases under Bioproject PRJNA662021 with accession numbers SRX9087478, SRX9087479 and SRX9087480.
We present how mesoporosity can be engineered in transition metal phosphate (TMPs) materials in a template-free manner. The method involves the transformation of a precursor metal phosphate phase, called M-struvite (NH4MPO4·6H2O, M = Mg2+, Ni2+, Co2+, NixCo1−x2+). It relies on the thermal decomposition of crystalline M-struvite precursors to an amorphous and simultaneously mesoporous phase, which forms during degassing of NH3 and H2O. The temporal evolution of mesoporous frameworks and the response of the metal coordination environment were followed by in situ and ex situ scattering and diffraction, as well as X-ray spectroscopy. Despite sharing the same precursor struvite structure, different amorphous and mesoporous structures were obtained depending on the involved transition metal. We highlight the systematic differences in absolute surface area, pore shape, pore size, and phase transitions depending on the metal cation present in the analogous M-struvites. The amorphous structures of thermally decomposed Mg-, Ni- and NixCo1−x-struvites exhibit high surface areas and pore volumes (240 m2 g−1 and 0.32 cm−3 g−1 for Mg and 90 m2 g−1 and 0.13 cm−3 g−1 for Ni). We propose that the low-cost, environmentally friendly M-struvites could be obtained as recycling products from industrial and agricultural wastewaters. These waste products could be then upcycled into mesoporous TMPs through a simple thermal treatment for further application, for instance in (electro)catalysis.
Industrial and agricultural waste streams (waste water, sludges, tailings, etc.) which contain high concentrations of NH4+, PO43–, and transition metals are environmentally harmful and toxic pollutants. At the same time, phosphorous and transition metals constitute highly valuable resources. Typically, separate pathways have been considered to extract hazardous transition metals or phosphate independently from each other. Investigations on the simultaneous removal of multiple components have been carried out only to a limited extent. Here, we report the synthesis routes for Ni- and Co-struvites (NH4MPO4·6H2O, M = Ni2+ and Co2+), which allow for P, ammonia, and metal co-precipitation. By evaluating different reaction parameters, the phase and stability of transition metal struvites as well as their crystal morphologies and sizes could be optimized. Ni-struvite is stable in a wide reactant concentration range and at different metal/phosphorus (M/P) ratios, whereas Co-struvite only forms at low M/P ratios. Detailed investigations of the precipitation process using ex situ and in situ techniques provided insights into the crystallization mechanisms/crystal engineering of these materials. M-struvites crystallize via intermediate colloidal amorphous nanophases, which subsequently aggregate and condense to final crystals after extended reaction times. However, the exact reaction kinetics of the formation of a final crystalline product varies significantly depending on the involved metal cation in the precipitation process: several seconds (Mg) to minutes (Ni) to hours (Co). The achieved level of control over the morphology and size makes precipitation of transition metal struvites a promising method for direct metal recovery and binding them in the form of valuable phosphate raw materials. Under this paradigm, the crystals can be potentially up-cycled as precursor powders for electrochemical or (electro)catalytic applications, which require transition metal phosphates.
The physical and chemical analysis of aerosols using reliable and physically traceable methods is important for the thorough investigation of airborne particles to support a better understanding of their origin as well as their health and climate impacts. Within the European Metrology Research AeroMet project,the aim of hysikalisch–Technische Bundesanstalt’s (PTB) X-ray spectrometry group is to develop and establish traceable and reliable X-ray methods to measure the elemental mass deposition per unit area, the elemental composition,and the chemical binding state of particulate matter supported by a flat substrate. This approach can substantially contribute to support quantitative analytical methods during on-site measurement campaigns where portable Instrumentation is employed by qualifying suitable calibration samples for commercial analytical X-ray instruments and by investigating samples collected during the field campaign.
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.
BAM is currently building up a platform of novel nanoRMs relying on iron oxide nanoparticles of different shape, size and surface chemistry. Iron oxide was chosen as a core material because of its relevance to the material and life sciences.
As a first candidate of this series, we present cubic iron oxide nanoparticles with a nominal edge length of 8 nm. These particles were synthesized by thermal decomposition of iron oleate in high boiling organic solvents adapting well-known literature procedures. After dilution to a concentration suitable for electron microscopy (TEM and SEM) as well as for small-angle X-ray scattering (SAXS) measurements, the candidate nanoRM was bottled and assessed for homogeneity and stability by both methods following the guidelines of ISO 17034 and ISO Guide 35.
The particle sizes obtained by both STEM-in-SEM and TEM are in excellent agreement with a minimum Feret of 8.3 nm ± 0.7 nm. The aspect ratio (AR) of the iron oxide cubes were extracted from the images as the ratio of minimum Feret to Feret resulting in an AR of 1.18 for TEM to 1.25 for SEM. Alternatively, a rectangular bounding box was fitted originating from the minimum Feret and the longest distance through the particle in perpendicular direction. This led to AR values of 1.05 for TEM and 1.12 for SEM, respectively. The results confirm the almost ideal cubic shape.
Reliable measurement of the size of polydisperse, complex-shaped commercial nanopowders is a difficult but necessary task, e.g., for regulatory requirements and toxicity risk assessment. Suitable methods exist for the accurate characterization of the size of non-aggregated, stabilized, spherical and monodisperse nanoparticles. In contrast, industrial nanoscale powders usually require dedicated sample preparation procedures developed for the analysis method of choice. These nano-powders tend to agglomerate and/or aggregate, a behavior which in combination with an innate broad particle size distribution and irregular shape often significantly alters the achievable accuracy of the measured size parameters. The present study systematically tests two commercially available nanoscale powders using different sample preparation methods for correlative analysis by scanning electron microscopy, dynamic light scattering, Brunauer–Emmet–Teller method and differential mobility analysis. One focus was set on the sample preparation by embedding nanoparticles in carbon-based hot-mounting resin. Literature on this topic is scarce and the accuracy of the data extracted from cross sections of these particles is unclearly stated. In this paper systematic simulations on the deviation of the size parameters of well-defined series of nanoparticles with different shapes from the nominal value were carried out and the contributing factors are discussed.
The objective of this study is to find out, to what extent the geochemical characteristics of lapis lazuli can be utilized in respect to its provenance. A wide range of variables is taken into consideration depending on the quantity of samples analysed from a specific geological region and the methods applied. In order to provide evidence, a multi-technique analytical approach using µXRF, ESEM, PGAA and PIXE is applied to samples from the most famous deposits of lapis lazuli. Special elements determined as fingerprints are compared in relation to the forming conditions obvious in textural features. The results and statistical output allow a differentiation that enables an optimized local classification of the blue stone. An absolute requirement for all geo-tracing performed on blue colored cultural objects of unknown provenance is awareness of the limits of analysis. The possible sources of lapis lazuli are tested by analysing the blue pigment used as paint on murals and ink on manuscripts from the Silk Road.
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.
Natural building materials for interior fitting and refurbishment - What about indoor emissions?
(2021)
Indoor air quality can be adversely affected by emissions from building materials, consequently having a negative impact on human health and well-being. In this study, more than 30 natural building materials (earth dry boards and plasters, bio-based insulation materials, and boards made of wood, flax, reed, straw, etc.) used for interior works were investigated as to their emissions of (semi-) volatile organic compounds ((S)VOC), formaldehyde, and radon. The study focused on the emissions from complete wall build-ups as they can be used for internal Partition walls and the internal insulation of external walls. Test chambers were designed, allowing the compounds to release only from the surface of the material facing indoors under testing Parameters that were chosen to simulate model room conditions. The emission test results were evaluated using the AgBB evaluation scheme, a procedure for the health-related evaluation of construction products and currently applied for the approval of specific groups of building materials in Germany.
Seventeen out of 19 sample build-ups tested in this study would have passed this scheme since they generally proved to be low-emitting and although the combined emissions of multiple materials were tested, 50% of the measurements could be terminated before half of the total testing time.
The reliable measurement of very volatile organic compounds (VVOC) in indoor air by use of thermal desorption gas chromatography (TD-GC) in order to include them into evaluation schemes for building products even nowadays is a great challenge. For capturing these small molecules with carbon numbers ranging from C 1 –C 6 , strong adsorbents are needed. In the present study, recovery rates of nine suitable adsorbents of the groups of porous polymers, graphitised carbon blacks (GCB) and carbon molecular sieves (CMS) are tested against a complex test gas standard containing 29 VVOC. By consideration of the recovery and the relative humidity (50% RH), combinations of the GCB Carbograph 5TD, the two CMS Carboxen 1003 and Carbosieve SII as well as the porous polymer Tenax® GR were identified to be potentially suitable for sampling the majority of the VVOC out of the gas mix. The results reveal a better performance of the adsorbents in combination than being used alone, particularly under humid sampling conditions. The recovery rates of the chosen compounds on each adsorbent should be in the range of 80–120%.
3D-printing or additive manufacturing has many promising and unique advantages. Especially low cost molten polymer Deposition Printers are increasingly populär in the private and educational sector.
Their environmental friendliness can be questioned due to recently reported ultrafine particle and suspected VOC emissions, To further investigate 3D-printing as a potential indoor air pollution source we characterized fine and ultrafine particle emissions from a molten polymer deposition printer producing a 3D object with ten marketable polymer filament materials under controlled conditions in a test chamber. VOC emissions from the filaments have also been compared. Using a straightforward emission model time dependent and averaged particle emission rates were determined. The results indicate that under comparable conditions some filament materials produce mainly ultrafine particles up to an average rate of 1013 per minute. This value is in the upper ränge of typical indoor ultrafine particle sources (e.g. Smoking, frying, candle light, laser printer). The observed material-specific rates differ by five Orders of magnitude. Filament-specific gaseous emissions of organic compounds such as bisphenol A, styrene and others were also detected.
Our results suggest a detailed evaluation of related risks and considering protective measures such as housing and filtering.
Quantitative chemical analysis of airborne particulate matter (PM) is vital for the understanding of health effects in indoor and outdoor environments, as well as for enforcing EU air quality regulations. Typically, airborne particles are sampled over long time periods on filters, followed by lab-based analysis, e.g., with inductively coupled plasma mass spectrometry (ICP-MS). During the EURAMET EMPIR AEROMET project, cascade impactor aerosol sampling is combined for the first time with on-site total reflection X-ray fluorescence (TXRF) spectroscopy to develop a tool for quantifying particle element compositions within short time intervals and even on-site. This makes variations of aerosol chemistry observable with time resolution only a few hours and with good size resolution in the PM10 range. The study investigates the proof of principles of this methodological approach. Acrylic discs and silicon wafers are shown to be suitable impactor carriers with sufficiently smooth and clean surfaces, and a non-destructive elemental mass concentration measurement with a lower limit of detection around 10 pg/m3 could be achieved. We demonstrate the traceability of field TXRF measurements to a radiometrically calibrated TXRF reference, and the results from both analytical methods correspond satisfactorily.
Today glass is broadly used in modern architecture. For indoor applications it is possible to produce decorated glass by using enamel colours and glass painting techniques without any problems. However, this is more limited for applications out of doors. Humidity and environmental pollution attack the surface of the coating and can damage it. There are only a few colours on the market which are resistant towards acids and bases until now. Additionally, most of those colours are opaque. To extend the colour palette, chemically resistant low melting coloured glasses are being developed which are transparent and intensively toned even in thin coating thicknesses. To achieve such an ambitious aim, many parameters have to combine and act in a complex manner. New compositions of lead borosilicate, zinc borosilicate and lead-zinc borosilicate glasses were produced and milled as powder. The thermal properties as well as the environmental stability were analysed. The influence of PbO and ZnO on the thermal properties and the environmental stability were investigated. Evaluation of the fusing results shows that the production and mixture of transparent vitreous enamels for the exterior side of glasses is possible. The tests made it clear that the original materials for making the vitreous enamels must be excellently ground and prepared to achieve a satisfactory result. The method to produce durable vitreous enamels for exterior application also seems to allow the production of glass colours.
Cellulose ethers, like methyl cellulose (MC) or hydroxypropyl cellulose (HPC), are widely used in conservation. They also occur as additives and rheology modifiers in various products like dispersions or gels. Do such products release harmful volatile organic compounds (VOC) during their accelerated aging? A mass testing series utilizing the Oddy test of 60 commercial cellulose ethers ranks the products in safe for permanent use (P, no corrosion), only for temporary use (T, slight corrosion), and unsuitable at all (F, heavy corrosion). Results show that 55% of the products passed the test whereas 33% are for temporary use as slight corrosion occurred on at least one metal coupon and only 11% failed the Oddy test. Raman measurements of the corrosion products identified oxides like massicot, litharge, cuprite, and tenorite among carbonates (hydrocerussite, plumbonacrite), and acetates like basic lead acetate, lead acetate trihydrate as well as lead formate as main phases. For example, commercial, industrial Klucel® G (HPC) scored a T rating through slight corrosion on the lead coupon. Basic lead acetate among other phases indicates the presence of acetic acid. Additional measurements of the sample with thermal desorption GC–MS utilizing the BEMMA scheme confirm the high acetic acid outgassing and reveal the presence of a small amount of formaldehyde.
The diversity of fused filament fabrication (FFF) filaments continues to grow rapidly as the popularity of FFF-3D desktop printers for the use as home fabrication devices has been greatly increased in the past decade. Potential harmful emissions and associated health risks when operating indoors have induced many emission studies. However, the lack of standardization of measurements impeded an objectifiable comparison of research findings. Therefore, we designed a chamber-based standard method, i.e., the strand printing method (SPM), which provides a standardized printing procedure and quantifies systematically the particle emission released from individual FFF-3D filaments under controlled conditions. Forty-four marketable filament products were tested. The total number of emitted particles (TP) varied by approximately four orders of magnitude (1E9 ≤ TP ≤ 1E13), indicating that origin of polymers, manufacturer-specific additives, and undeclared impurities have a strong influence. Our results suggest that TP characterizes an individual filament product and particle emissions cannot be categorized by the polymer type (e.g., PLA or ABS) alone. The user's choice of a filament product is therefore decisive for the exposure to released particles during operation. Thus, choosing a filament product awarded for low emissions seems to be an easily achievable preemptive measure to prevent health hazards.
Gegenstand dieser Arbeit ist die Untersuchung eines bestehenden pyrometallurgischen Prozesses zur Rückgewinnung von Tantal und Niob aus metallurgischen Reststoffen mit vorwiegend niedriger Wertstoffkonzentration.
Zur näheren Erforschung der im vorliegenden Stoffsystem ablaufenden Reduktionsprozesse wurden in einem Elektrolichtbogenofen Schmelzversuche im Pilotmaßstab durchgeführt. Als Reduktionsmittel diente Koks, welcher mithilfe einer Argon-gespülten Eisenlanze in die flüssige mineralische Schmelze eingebracht wurde. Während der Reduktionsbehandlung werden Refraktärmetalle wie Tantal und Niob in ihre Carbide überführt und anschließend in der erschmolzenen eisenbasierten Metallphase am Boden des Reaktors angereichert. Neben Tantal und Niob gelangt auch ein Teil des im Einsatzmaterial enthaltenen Titans als unerwünschtes Begleitelement in die Metallphase.
Sein Großteil verbleibt jedoch als Oxid in der Schlacke und wird dort hauptsächlich im Mineral Perowskit (CaTiO3) gebunden. Die erstarrten Schlackeproben wurden mit verschiedenen Methoden wie Röntgenfluoreszensanalyse, Röntgenbeugung und Rasterelektronenmikroskopie mit gekoppelter energiedispersiver Röntgenanalyse untersucht, um die Bildung tantalhaltiger Mineralphasen zu verschiedenen Stadien des Reduktionsprozesses zu verfolgen.
Die hier gewonnenen Erkenntnisse zeigen, dass weniger die durch das Einblasen von Koks verursachte Reduktionsreaktion, sondern das Absinken der tantalreichen Eisentröpfchen in der flüssigen mineralischen Schmelze, gefolgt von ihrer Anreicherung in die Metallphase, für die Kinetik ausschlaggebend ist.
The development of traceable new methodologies to quantify elemental air pollutants in particulate matter (PM) supports modernization of methods used in air quality monitoring networks in Europe. In the framework of the EURAMET EMPIR AEROMET II project, the combination of cascade impactor aerosol sampling and total reflection X-ray fluorescence elemental spectroscopy (TXRF) was investigated. This technique requires a traceable calibration based on reference samples. This paper describes a new, simple and effective method to produce such reference samples using flexible, reusable, and low-cost parylene C shadow masks, fabricated by photolithographic steps. These shadow masks can be used to produce reference samples that mimic the Dekati cascade impactor’s deposition patterns by applying as-prepared micro stencils to 30 mm acrylic substrates and evaporating a reference material (Ti) in arrangements of thin circular dots. The highly flexible direct patterning of acrylic discs with reference material, otherwise impossible with conventional photolithography, allows multiple reusing of the same micro stencils. The aspect ratios of the dots could be repeated with an error less than 4 %. A first set of standard reference samples for the 13 stages of the Dekati cascade impactor was produced and preliminary TXRF measurements of the deposited Ti masses were performed. The centricity of the deposition patterns turned out to be an important parameter for the quality of the TXRF results. The parylene mask technology for the production of reference samples turns out to be a promising new approach for the traceable calibration of TXRF spectrometers for the quantification of element concentrations in environmental aerosol samples but, due to its great versatility, it could be used for several other micropatterning applications on conventional and unconventional substrates.
Nonporous corundum powder, known as an abrasive material in the industry, was functionalized covalently with protein binders to isolate and enrich specific proteins from complex matrices. The materials based on corundum were characterized by TEM, ESEM, BET, DLS, EDS, and zeta potential measurements. The strong Al-O-P bonds between the corundum surface and amino phosphonic acids were used to introduce functional groups for further conjugations. The common crosslinker glutaraldehyde was compared with a hyperbranched polyglycerol (PG) of around 10 kDa. The latter was oxidized with periodate to generate aldehyde groups that can covalently react with the amines of the surface and the amino groups from the protein via a reductive amination process. The amount of bound protein was quantified via aromatic amino acid analysis (AAAA). This work shows that oxidized polyglycerol can be used as an alternative to glutaraldehyde. With polyglycerol, more of the model protein bovine serum albumin (BSA) could be attached to the surface under the same conditions, and lower non-specific binding (NSB) was observed. As a proof of concept, IgG was extracted with protein A from crude human plasma. The purity of the product was examined by sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). A binding capacity of 1.8 mg IgG per gram of corundum powder was achieved. The advantages of corundum include the very low price, extremely high physical and chemical stability, pressure resistance, favorable binding kinetics, convenient handling, and flexible application.