The increasing demand of analytical information related to inorganic engineered nanomaterials requires the adaptation of existing techniques and methods, or the development of new ones.The challenge for the analytical sciences has been to consider the nanoparticles as a new sort of analytes, involving both chemical (composition, mass and number concentration) and physical information (e.g. size, shape, aggregation). Moreover, information about the species derived from the nanoparticles themselves and their transformations must also be supplied. Whereas techniques commonly used for nanoparticle characterization, such as light scattering techniques, show serious limitations when applied to complex samples, other well-established techniques, like electron microscopy and atomic spectrometry, can provide useful information in most cases. Furthermore, separation techniques, including flow field flow fractionation, capillary electrophoresis and hydrodynamic chromatography, are moving to the nano domain, mostly hyphenated to inductively coupled plasma mass spectrometry as element specific detector.Emerging techniques based on the detection of single nanoparticles by using ICP-MS, but also coulometry, are in their way to gain a position. Chemical sensors selective to nanoparticles are in their early stages, but they are very promising considering their portability and simplicity.Although the field is in continuous evolution, at this moment it is moving from proofs-of-2 concept in simple matrices to methods dealing with matrices of higher complexity and relevant analyte concentrations. To achieve this goal, sample preparation methods are essential to manage such complex situations. Apart from size fractionation methods, matrix digestion, extraction and concentration methods capable of preserving the nature of the nanoparticles are being developed. This review presents and discusses the state-of-the-art analytical techniques and sample preparation methods suitable for dealing with complex samples. Single-and multimethod approaches applied to solve the nanometrological challenges posed by a variety of stakeholders are also presented.
Luster is a decorative metallic film that was applied on the surface of medieval glazed pottery. It can be obtained via the low-temperature (ϳ650°C), controlled reduction of copper and silver compounds. In this paper, we show that luster is a thin layered film (200 -500 nm thick) that contains metallic spherical nanocrystals dispersed in a silicon-rich matrix and has a metal-free outermost glassy layer that is 10 -20 nm thick. Silver nanocrystals seem to be separated from those of copper, forming aggregates 5-100 m in diameter. This composite structure exhibits optical properties that are dependent on both the particle size and the matrix. Luster is indeed the first reproducible nanostructured thin metallic film that was made by humans.
The discovery of the workshop`Les Olleries Xiques' in Paterna has provided a unique opportunity to analyse the raw materials, and in particular the recipes used in the production of the lustre decorations. Chemical and phase analyses of lustre raw materials and of lustre decorations belonging to the workshop pottery are shown. A comparison with existing ancient documentation on lustre recipes is also presented.
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