The volume-specific surface area (VSSA) of a particulate material is one of two apparently very different metrics recommended by the European Commission for a definition of “nanomaterial” for regulatory purposes: specifically, the VSSA metric may classify nanomaterials and non-nanomaterials differently than the median size in number metrics, depending on the chemical composition, size, polydispersity, shape, porosity, and aggregation of the particles in the powder. Here we evaluate the extent of agreement between classification by electron microscopy (EM) and classification by VSSA on a large set of diverse particulate substances that represent all the anticipated challenges except mixtures of different substances. EM and VSSA are determined in multiple labs to assess also the level of reproducibility. Based on the results obtained on highly characterized benchmark materials from the NanoDefine EU FP7 project, we derive a tiered screening strategy for the purpose of implementing the definition of nanomaterials. We finally apply the screening strategy to further industrial materials, which were classified correctly and left only borderline cases for EM. On platelet-shaped nanomaterials, VSSA is essential to prevent false-negative classification by EM. On porous materials, approaches involving extended adsorption isotherms prevent false positive classification by VSSA. We find no false negatives by VSSA, neither in Tier 1 nor in Tier 2, despite real-world industrial polydispersity and diverse composition, shape, and coatings. The VSSA screening strategy is recommended for inclusion in a technical guidance for the implementation of the definition. Graphical abstractWe evaluate the extent of agreement between classification by electron microscopy (EM) and classification by Volume-Specific Surface Area (VSSA) on a large set of diverse particulate substances. These represent the challenges anticipated for identification of nanomaterials by the European Commission recommendation for a definition of nanomaterials for regulatory purposes. Electronic supplementary materialThe online version of this article (doi:10.1007/s11051-017-3741-x) contains supplementary material, which is available to authorized users.
New applications of low‐temperature co‐fired ceramics (LTCC), such as pressure sensors or integrated functional layers, require materials that possess higher coefficients of thermal expansion (CTE). To fabricate LTCC with elevated CTE, two methods of material design are examined: firstly, glass ceramic composites (GCC), which consist of >50 vol% glass in the starting powder, and, secondly, glass‐bonded ceramics (GBC), where glass is added as a sintering aid only. The CTE of GBC is mainly determined by the crystalline component. For GCC, the CTE can be well predicted, if CTE and elastic data of each phase in the microstructure are known. A nonlinear characteristic of the CTE versus phase composition was found with increasing Ecrystals/Eglass ratio and absolute CTE difference between the components. The glass composition and glass amount can be used to compensate the fixed properties of a crystalline material in a desired way. However, because the CTE and permittivity of a glass cannot be chosen independently, an optimum glass composition has to be found. For a given LTCC, it is possible to control the devitrification by shifting the glass composition. In this way, the resulting CTE values can be predicted more exactly and tailoring becomes possible. Different LTCC materials, based on the crystalline compounds Ba(La,Nd)2Ti4O12, ZrO2 (Y‐TZP), SiO2 (quartz), and specially developed glasses, possessing an elevated CTE of around 10 × 10−6 K−1 while showing permittivity ɛr between 6 and 63, are introduced.
Macrophages play a pivotal role in tissue reaction and immune response. They recognize, phagocytose particles and generate cytokines to influence local cellular reactions. Friction and wear of implant components usually generates microparticles (MP) in a size range of 1-10 mum and nanoparticles (NP) in the range of 10-1000 nm. To investigate the possible impact of MP or NP on cellular reactions, we exposed murine macrophages (RAW264.7) to corundum MP and NP. The same mass was used in both NP and MP cell culture solutions, i.e. there were more NP than MP per identical volumes of culture solution. After 4, 24, 48, 72, and 96 h aliquots of cell culture supernatants were tested for different cytokines, growth factors and nitric oxide. Macrophages were stained with MGG (May-Grünwald Giemsa), counted and morphologically characterized by scanning electron microscopy and transmission electron microscopy. Particles were attached to cell surfaces and phagocytosed within cells. Cells stimulated with particles or lipopolysaccharides for positive controls showed surface modifications indicating enhanced function. Although only marginal differences between negative controls and particle-stimulated cells were observed in respect to cytokine production, exposure to corundum particles led to a decrease in the number of vital macrophages and to an increase in the number of giant cells. Corundum NP formed micron-sized aggregates in the cell culture medium and led to the production of more giant cells than MP. Sodiumdodecylsulfate polyacrylamide gel electrophoresis of the cell culture medium with particles proved the adsorption of proteins to particles.
The aim of this work was to select and characterize model particles, which correspond to real wear products from artificial hip joints, and to investigate the dispersing behavior of these powders. Commercially available nano and microparticles of corundum, graphite, and chromium oxide were selected or alternatively self-produced by milling. These powders were characterized regarding density, specific surface area, crystalline phases, particle size distributions and shape. Volume-based particle size distributions Q(3)(d) were measured after dispersing in water, water with dispersant, Ringers solution, and cell culture solution (Dulbecco's Modified Eagle's Medium (DMEM)) by laser diffraction and ultrasonic spectroscopy. Nanopowders formed agglomerates in the micrometer range in cell culture solutions. The micropowders showed only a marginal agglomeration. The median diameters of the dispersed nanopowders were even bigger than those of micropowders. Calculations of the number-based size distribution Q(0)(d) showed that in spite of the agglomeration the predominant number of the nano and microparticles is in the sub micrometer range, with only one exception, the micrographite powder.
Presented are results of an inter‐laboratory study (ILS) for measurements of the particle size distribution of fine powders in wet dispersion by laser diffraction. In this proficiency test 32 participants from four countries took part. They utilized 13 different devices from 7 manufacturers. Three commercial powders (glass spheres and two silicon carbide powders) showing a median diameter of about 30, 10 and 1 μm (volume distribution), respectively, were chosen for the procedure. A homogeneity study was carried out after the units had been separated and bottled. All participants received their test samples including a description of the standard operating procedures based on ISO 13320:2009 – to ensure that experiments were performed in a consistent manner. Results were calculated using the Mie Theory. The general means and the precision of the results were estimated in accordance with ISO 5725‐2:2002. The evaluation showed excellent values of repeatability standard deviation. Values of 4 to 21 % of the reproducibility standard deviation of the results were found in the particle size range above 1 μm. Much larger deviation between the labs was detected in the case of smaller particles. Differences in the design of the analyzers were unambiguously identified as the main reason for the large deviations.
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