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Micro-(nano-)encapsulation technology involves building of a barrier between the core and the environment and offers a number of benefits to preserve the functional and physicochemical properties of core material. Tremendous progress has been made in synthesizing well-defined capsules to achieve desired properties such as particle size, chemical composition, and controlled release of the payload.
Encapsulation of volatile organic compounds (VOCs) that could evaporate with a defined rate is of immense interest for application in emission reference materials (ERM). These are urgently needed for quality assurance and quality control purposes (QA/QC) required by test standards for the determination of chemical emissions of construction and other materials for interior use. As such ERMs are hardly available on the market, the EU-funded EMPIR project MetrIAQ [1] was started to fill this gap by developing a material with temporally constant emission of VOCs typically found in indoor air.
Different capsules in a size range between 5 and 50 μm were synthesized through an interfacial polyaddition/polycondensation reaction in direct (water-in-oil) system. As VOC several types of hydrophobic liquid materials were used. After synthesis, the morphology and physicochemical properties of capsules were characterized by electron microscopy, FTIR and DSC/TGA. An encapsulation efficiency up to 90% could be reached. The emission kinetic of volatile agents was studied in emission test chambers at 23 °C and 50% RH for 14 days. First results indicate that variation of the cross-linking grade of the shell material is one important parameter to adjust the desired emission rate. The overall aim is to achieve a consistent emission profile that decreases by less than 10 % over a target period of at least 14 days.
Micro-(nano-)encapsulation technology involves building a barrier between the core and the environment and offers several benefits to preserve the functional and physicochemical properties of core material. Tremendous progress has been made in synthesizing well-defined capsules to achieve desired properties such as particle size, chemical composition, and controlled release of loaded compounds.
Encapsulation of volatile organic compounds (VOCs) that could evaporate with a defined rate is of immense interest for application in emission reference materials (ERM). These are urgently needed for quality assurance and quality control purposes (QA/QC) required by test standards for the determination of chemical emissions of construction and other materials for interior use. As such ERMs are hardly available on the market, the EU-funded EMPIR project MetrIAQ was started to fill this gap by developing a material with temporally constant emission of VOCs typically found in indoor air.
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.
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.
Laser Powder Bed Fusion (L-PBF) is a promising additive manufacturing (AM) technology for metal part production especially for complex and lightweight structures or functional designs. In L PBF processes several by-products including welding plume and its condensates, spatter and ejected powder are generated during laser exposure. Investigations of micro- and nano-sized by-products have received little attention in literature. This study focuses on the analysis of particle emissions in L PBF of 316L stainless steel using a scattered light aerosol spectrometer and a fast mobility particle sizer spectrometer during the process which allows for in-situ analysis of particle sizes in the range of 6 nm to 100 µm. A distinct correlation of emission signals to part position can be revealed. In addition, a significant influence of laser scanning vector directions on emission signals is presented. Furthermore, differing powder layer thicknesses can be recognised by deviations in emission signals.
Laser Powder Bed Fusion (L-PBF) is a promising additive manufacturing (AM) technology for metal part production especially for complex and lightweight structures or functional designs. In L PBF processes several by-products including welding plume and its condensates, spatter and ejected powder are generated during laser exposure. Investigations of micro- and nano-sized by-products have received little attention in literature. This study focuses on the analysis of particle emissions in L PBF of 316L stainless steel using a scattered light aerosol spectrometer and a fast mobility particle sizer spectrometer during the process which allows for in-situ analysis of particle sizes in the range of 6 nm to 100 µm. A distinct correlation of emission signals to part position can be revealed. In addition, a significant influence of laser scanning vector directions on emission signals is presented. Furthermore, differing powder layer thicknesses can be recognised by deviations in emission signals.
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.
The new OECD test guideline will address the following four main steps in the determination of the length and width distributions of fibers: sample preparation, image acquisition, data evaluation and uncertainty analysis. As the sample preparation has to be optimized for each material, general quality criteria will be given in the protocol. For full visibility of a fiber the appropriate resolution has to be chosen. In the data evaluation the length and diameter of each fiber will be determined concurrently to allow for application of different regulatory definitions. The quality of the results critically depends on the sample preparation as well as the data evaluation. In this step the classification rules have to be formulated and followed accurately in order to optimize reproducibility of the method. The SOP will be validated in an international round robin test, which is planned for 2018/2019.
The new OECD test guideline will address the following four main steps in the determination of the length and width distributions of fibers: sample preparation, image acquisition, data evaluation and uncertainty analysis. As the sample preparation has to be optimized for each material, general quality criteria will be given in the protocol. For full visibility of a fiber the appropriate resolution has to be chosen. In the data evaluation the length and diameter of each fiber will be determined concurrently to allow for application of different regulatory definitions. The quality of the results critically depends on the sample preparation as well as the data evaluation. In this step the classification rules have to be formulated and followed accurately in order to optimize reproducibility of the method. The SOP will be validated in an international round robin test, which is planned for 2018/2019.
The particle size distribution is considered the most relevant information for nanoscale property identification and material characterization. The current OECD test guideline on particle size and size distribution (TG 110) is not applicable to ‘nano-sized’ objects. In this project we thus develop a new OECD test guideline for the measurement of the size and size distribution of particles and fibers with at least one dimension in the nanoscale. A fiber is defined as an object having an aspect ratio of length/diameter l/d >3. The width and length of each fiber should be measured concurrently.
In order to measure the particle size distributions, many techniques are available. 9 methods for particles and 2 methods for fibres have been tested in a prevalidation study and appropriate methods will be compared in an interlaboratory round robin test starting in February 2019.
Vorstellung der Ergebnisse bei der Entwicklung einer neuen OECD Prüfrichtlinie zur Bestimmung der Partikelgröße und Anzahlgrößenverteilung von Nanomaterialien. (Projektteil Fasern.)
Ergebnisse:
Abweichungen zwischen SEM and TEM insbesondere bei langen Fasern
Die Anwendung von TEM auf kurze Fasern < 5 µm beschränkt
Für SEM wurde keine signifikante Abhängigkeit der Bestimmung der Faserdurchmesser von der Pixelgröße der Aufnahmen festgestellt
Für TEM wurde eine Abhängigkeit der Bestimmung der Faserdurchmesser von der Pixelgröße festgestellt
Der Einfluss der Bildauswertenden auf die Varianz der Ergebnisse ist klein im Vergleich zu der gesamten Varianz.
Nanofasern können mit TEM und SEM bestimmt werden!
The particle size distribution is considered the most relevant information for nanoscale property identification and material characterization. The current OECD test guideline on particle size and size distribution (TG 110) is not applicable to ‘nano-sized’ objects. In this project we thus develop a new OECD test guideline for the measurement of the size and size distribution of particles and fibers with at least one dimension in the range of 1 - 1000 nm. A fiber is defined as an object having an aspect ratio of length/diameter l/d >3. The width and length of each fiber should be measured concurrently.
In order to measure the particle size distributions, many techniques are available. 9 methods for particles and 2 methods for fibres have been tested in a prevalidation study and appropriate methods will be compared in an interlaboratory round robin test starting in February 2019.
The particle size distribution is considered the most relevant information for nanoscale property identification and material characterization. The current OECD test guideline on particle size and size distribution (TG 110) is not applicable to ‘nano-sized’ objects. In this project we thus develop a new OECD test guideline for the measurement of the size and size distribution of particles and fibers with at least one dimension in the range of 1 - 1000 nm. A fiber is defined as an object having an aspect ratio of length/diameter l/d >3. The width and length of each fiber should be measured concurrently.
In order to measure the particle size distributions, many techniques are available. 9 methods for particles and 2 methods for fibres have been tested in a prevalidation study and appropriate methods will be compared in an interlaboratory round robin test starting in February 2019.
AbstractThe correlation between altered extracellular pH and various pathological conditions, including cancer, inflammation and metabolic disorders, is well known. Bulk pH measurements cannot report the extracellular pH value at the cell surface. However, there is a limited number of suitable tools for measuring the extracellular pH of cells with high spatial resolution, and none of them are commonly used in laboratories around the world. In this study, a versatile ratiometric nanosensor for the measurement of extracellular pH was developed. The nanosensor consists of biocompatible polystyrene nanoparticles loaded with the pH-inert reference dye Nile red and is surface functionalized with a pH-responsive fluorescein dye. Equipped with a targeting moiety, the nanosensor can adhere to cell membranes, allowing direct measurement of extracellular pH at the cell surface. The nanosensor exhibits a sensitive ratiometric pH response within the range of 5.5–9.0, with a calculated pKa of 7.47. This range optimally covers the extracellular pH (pHe) of most healthy cells and cells in which the pHe is abnormal, such as cancer cells. In combination with the nanosensors ability to target cell membranes, its high robustness, reversibility and its biocompatibility, the pHe nanosensor proves to be well suited for in-situ measurement of extracellular pH, even over extended time periods. This pH nanosensor has the potential to advance biomedical research by improving our understanding of cellular microenvironments, where extracellular pH plays an important role.
The European building sector is moving towards more complex and high-tech building approaches. While focusing on energy efficiency, aspects e.g. occupant health, sustainability and life cycle costing are often neglected. This study highlights the potential of earthen plasters in combination with natural ventilation for low-tech solutions.
The EU funded project [H]house established the outstanding performance of earthen materials in light of hygrothermal and air purifying properties, which were further supported by experimental data from monitoring of naturally ventilated pilot buildings in Berlin. Additionally, [H]house demonstrated through LCC an increased cost efficiency of earth based low-tech solutions in comparison to conventional constructions relying on mechanical ventilation.
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.
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.
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.
Der Mensch verbringt die überwiegende Zeit des Tages in Innenräumen von Gebäuden. Der Aufenthalt in Innenräumen umfasst das Wohnen, Bürotätigkeiten oder auch Nutzung öffentlicher Gebäude wie Kindertagesstätten, Schulen, Sporthallen und Bibliotheken. Um Innenräume von Gebäuden ohne Gefährdung für die menschliche Gesundheit nutzen zu können, müssen diese bei ihrer Errichtung und Verwendung dauerhaft die an sie gestellten hohen Anforderungen zu Gesundheit und Hygiene erfüllen. Die Innenraumluftqualität und ihre Wahrnehmung durch die Raumnutzer spielt für das individuelle Wohlbefinden und die Gesundheit eine entscheidende Rolle.
Dieses Buch richtet sich bevorzugt an Bauplaner, Architekten, Bauingenieure und Bauherren aber auch an Bauproduktehersteller. Ihnen allen fällt die wichtige Aufgabe zu, Aufenthaltsräume von Gebäuden durch eine gezielte Bauproduktverwendung zu gestalten und dauerhaft nutzbar zu machen. Die Frage, ob der Aufenthalt in Gebäuden den Menschen gesundheitlich beeinträchtigen oder sogar krank machen kann, hängt wesentlich von der qualitativen und quantitativen Zusammensetzung der Raumluft ab.
„Innenraumluftqualität und Bauprodukte“ enthält Angaben über wichtige Inhaltsstoffe der Raumluft und damit verbundene Einflussfaktoren, und geht im Besonderen auf Emissionen aus Bauprodukten ein. So vermögen Bauprodukte oftmals als großflächige Emissionsquellen die Innenraumluft mit verschiedenartigen Stoffen und Stoffgemischen anzureichern, mit der Folge, dass Raumnutzer diesen dauerhaft und teilweise intensiv ausgesetzt sind.
Das Buch vermittelt wichtige Erkenntnisse über flüchtige organische Verbindungen (VOC) aus Bauprodukten sowie deren Verhalten in der Raumluft etwa in Bezug auf Emissionsdauer, Hausstaubdeposition und Sekundärquellenbildung. Auf spezifische VOC-Einzelstoffemissionen – sehr flüchtige (VVOC) bis hin zu schwerflüchtigen (SVOC) – und einzelne chemische Stoffgruppen in Zusammenhang mit ihrem Vorkommen in Bauprodukten wird eingegangen.
Die wesentlichen Voraussetzungen und die Bedeutung einzelner VOC und VOC-Stoffgemische für die Expositionssituation und die Gesundheit von Raumnutzern werden in einem eigenen Kapitel beschrieben. Wichtige Kenntnisse über gesundheitliche Stoffwirkungen werden transparent erläutert. Angesprochen werden der inhalative Aufnahmepfad, Effekte durch Reizstoffe an den Atemwegen, andere toxische Wirkungen und die Auswirkungen von geruchsintensiven und -belästigenden Stoffen.Das Kapitel „Bewertung der Innenraumluftqualität“ vermittelt die allgemein anerkannte Vorgehensweise zur Beurteilung der Luftqualität und erstreckt sich auf chemische Stoffe, Geruchseinwirkungen sowie auf das Edelgas Radon. Bauplaner, Architekten, Bauingenieure und Bauherren werden in die Lage versetzt, die Bedeutung und Anwendung verschiedener Beurteilungsparameter und ihre Beurteilungswerte anschaulich nachzuvollziehen und deren Verwendung in Beurteilungen und Prüfberichten gezielt einzuordnen. Im Detail wird die notwendige Abgrenzung der Verwendung der Begrifflichkeiten „Grenzwerte“ und „toxikologisch begründete Innenraumluftrichtwerte des Ausschusses für Innenraumrichtwerte (AIR)“ mit den dazugehörigen aktuellen Richtwerten (RW II bzw. RW I) erklärt. Auch die Bedeutung und der Anwendungsbereich internationaler Beurteilungen der WHO und der europäischen Chemikalienbewertung (REACH) werden erläutert. Das Buch liefert Informationen über die Ermittlung und Verwendung statistisch abgeleiteter Beurteilungswerte, die als Referenzwerte definiert sind.
Die Ergebnisse aktueller Referenzwertstudien zum Vorkommen einzelner VOC und von VOC-Stoffgemischen als Summe aller nachgewiesenen VOC (TVOC-Wert) in Wohnräumen, Büros und auch öffentlichen Gebäuden wie Schulen – einschließlich ihrer Methodik und Analytik – werden erläutert und diskutiert. Der Verwendungszweck eines Bauproduktes in Gebäuden zwingt dazu, bereits vor dessen Einbau mittels konkretisierten Produktanforderungen eine Beurteilung des Gesundheitsschutzniveaus für die späteren Raumnutzer zu gewährleisten. Daher sind alle am Bau beteiligten Personen wie Bauplaner, Architekten, Bauingenieure und Bauproduktehersteller gefordert. Zwar treten in den Bauproduktemissionen viele VOC in eher geringeren Konzentrationen auf, jedoch zeigen einige nachweisbare Einzelstoffe sowohl Reizeffekte oder andere toxische Wirkungen als auch erhebliche Geruchsintensitäten auf.
„Innenraumluftqualität und Bauprodukte“ geht aus diesem Grund zwei bedeutsamen Fragen nach: Wie lässt sich das Gefährdungspotenzial der emittierten VOC aus Bauprodukten bevorzugt bewerten und wie lassen sich die Anforderungen an den Aufenthaltsraum zum Gesundheitsschutzniveau in Bezug auf Bauproduktemissionen prüfen, beurteilen und letztlich gewährleisten?
Hierzu gibt das Buch aktuelle Informationen zum anerkannten Prüf- und Bewertungsverfahren vom Ausschuss zur gesundheitlichen Bewertung von Bauprodukten (AgBB). Über das breit etablierte AgBB-Schema zur gesundheitlichen Beurteilung von Emissionen flüchtiger organischer Verbindungen (VVOC, VOC, SVOC) aus innenraumrelevanten Bauprodukten wird im Detail nachvollziehbar berichtet. Im Fokus steht die Anwendung des AgBB-Schemas in der Praxis. In einem umfangreichen Kapitel wird auf die Durchführung von Materialemissionsmessungen sowie Bewertungen der Geruchsemissionen und die dafür notwendigen Voraussetzungen eingegangen. Abbildungen und Messberichte geben einen weitreichenden Einblick zum Verständnis einer Prüfkammeruntersuchung auf flüchtige organische Verbindungen (VVOC, VOC, SVOC). Zur Verdeutlichung werden beispielhaft Messdaten angeführt zu unterschiedlichen Bauprodukten, wie Bodenbelägen, Bodenbelagsklebstoffen, Holz und Holzwerkstoffen, Lacken und Farben,
Kunstharzfertigputzen und Dichtstoffen. Das Buch bietet tabellarische Übersichten über das Vorkommen und die Konzentration ermittelter VOC-Emissionen aus Bauprodukten verschiedener Produktgruppen und zeigt Möglichkeiten auf, wie in der Praxis bestimmte SVOC-Emissionen, etwa Flammschutzmittel und Biozide, sowie Sekundäremissionen aus Bauprodukten analysiert und quantifiziert werden können. Darüber hinaus gibt es einen Überblick über die geltenden baurechtlichen Anforderungen in Bezug auf Hygiene und Gesundheit. Öffentlich-rechtliche Mindestforderungen zur Sicherstellung des Gesundheitsschutzniveaus für in Innenräume von Gebäuden eingebrachte Bauprodukte werden mit den zugrunde zu legenden Bestimmungen der Musterbauordnung (MBO) und ihrer neuen Muster-Verwaltungsvorschrift Technische Baubestimmungen (MVV TB) beschrieben.
Eigens wird ein Einblick in rechtliche Regelungen – in Bezug auf die gesundheitsbezogenen Anforderungen an bauliche Anlagen, die über die „Anforderungen an bauliche Anlagen bezüglich des Gesundheitsschutzes (ABG)“ konkretisiert sind – gegeben. Es wird ersichtlich, dass die Anforderungen für Emissionen flüchtiger organischer Verbindungen (VVOC, VOC, SVOC) aus Bauprodukten mindestens denen des AgBB entsprechen. Die in Europa noch lückenhafte und unvollständige Harmonisierung der Normen zum Gesundheitsschutz wird dargelegt. Das Buch leistet so Hilfestellung, um trotzdem gemäß den MBO- bzw. MVV TB-Anforderungen gesundheitsbezogene Angaben zu Produktleistungen zu ermöglichen.