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Organisationseinheit der BAM
Results are reported from a pilot study under the Consultative Committee for Amount of Substance (CCQM) to compare measurements of and resolve any relevant measurement issues in, the amount of thermal SiO2 oxide on (100) and (111) orientation Si wafer substrates in the thickness range 1.5 - 8 nm. As a result of the invitation to participate in this activity, 45 sets of measurements have been made in different laboratories using 10 analytical methods: medium-energy ion scattering spectrometry (MEIS), nuclear reaction analysis (NRA), RBS, elastic backscattering spectrometry (EBS), XPS, SIMS, ellipsometry, grazing-incidence x-ray reflectrometry (GIXRR), neutron reflectometry and transmission electron microscopy (TEM). The measurements are made on separate sets of 10 carefully prepared samples, all of which have been characterised by a combination of ellipsometry and XPS using carefully established reference conditions and reference parameters.
The results have been assessed against the National Physical Laboratory (NPL) data and all show excellent linearity. The remaining data sets correlate with the NPL data with average root-mean-square scatters of 0.15 nm, half being better than 0.1 nm and a few at or better than 0.05 nm. Each set of data allows a relative scaling constant and a zero thickness offset to be determined. Each method has an inherent zero thickness offset between 0 nm and 1 nm and it is these offsets, measured here for the first time, that have caused many problems in the past. There are three basic classes of offset: water and carbonadeous contamination equivalent to ~1 nm as seen by ellipsometry; adsorbed oxygen mainly from water at an equivalent thickness of 0.5 nm as seen by MEIS, NRA, RBS and possibly GIXRR; and no offset as seen by XPS using the Si 2p peaks. Each technique has a different uncertainty for the scaling constant and consistent results have been achieved. X-Ray photoelectron spectroscopy has large uncertainties for the scaling constant but a high precision and, critically, if used correctly, has zero offset. Thus, a combination of XPS and the other methods allows the XPS scaling constant to be determined with low uncertainty, traceable via the other methods. XPS laboratories returning results early were invited to test a new reference procedure. All showed very significant improvements. The reference attenuation lengths thus need scaling by 0.986 ± 0.009 (at an expansion factor of 2) deduced from the data for the other methods. Several other methods have small offsets and, to the extent that these can be shown to be constant or measurable, then these methods will also show low uncertainty. Recommendations are provided for parameters for XPS, MEIS, RBS and NRA to improve their accuracy.
The fluorolytic sol–gel synthesis is applied with the intention to obtain two different types of core–shell nanoparticles, namely, SrF2–CaF2 and CaF2–SrF2. In two separate fluorination steps for core and shell formation, the corresponding metal lactates are reacted with anhydrous HF in ethylene glycol. Scanning transmission electron microscopy (STEM) and dynamic light scattering (DLS) confirm the formation of particles with mean dimensions between 6.4 and 11.5 nm. The overall chemical composition of the particles during the different reaction steps is monitored by quantitative Al Kα excitation X-ray photoelectron spectroscopy (XPS). Here, the formation of stoichiometric metal fluorides (MF2) is confirmed, both for the core and the final core–shell particles. Furthermore, an in-depth analysis by synchrotron radiation XPS (SR-XPS) with tunable excitation energy is performed to confirm the core–Shell character of the nanoparticles. Additionally, Ca2p/Sr3d XPS intensity ratio in-Depth profiles are simulated using the software Simulation of Electron Spectra for Surface Analysis (SESSA). In principle, core–shell like particle morphologies are formed but without a sharp interface between calcium and strontium containing phases.
Surprisingly, the in-depth chemical distribution of the two types of nanoparticles is equal within the error of the experiment. Both comprise a SrF2-rich core domain and CaF2-rich shell domain with an intermixing zone between them. Consequently, the internal morphology of the final nanoparticles seems to be independent from the synthesis chronology.
Im ersten Teil dieses Aufsatzes wurde gezeigt, dass nur ein Teil der für den Deponiebau wesentlichen technischen Eigenschaften in den europäisch harmonisierten Bauproduktnormen DIN EN 13252 und DIN EN 13257, die der CE-Kennzeichnung der Geotextilien (GTX) und geotextilverwandten Produkte (GTP) zugrunde liegen, erfasst werden. Um eine im Wesentlichen vorhandene Gleichwertigkeit der Produkteigenschaften überhaupt abwägen zu können, müssen aber sämtliche relevanten Eigenschaften bekannt sein. Dies erfordert für CE-gekennzeichnete Produkte zusätzliche Prüfungen auf der Grundlage der DepV-Liste der Kriterien und Einwirkmechanismen (Anhang 1, Nummer 2.1.1, DepV). In diesem Teil werden die Tabellen C1 und C2 sowie die Tabelle D aus dem ersten Teil, in denen die Eigenschaften der harmonisierten europäischen Normen (hEN) den Anforderungen der DepV gegenübergestellt wurden, in technischer Hinsicht näher erläutert.
In absehbarer Zeit werden CE-gekennzeichnete Geovliesstoffe, Geogewebe, geosynthetische Dränelemente und Geogitter aus Kunststoff erhältlich sein, bei denen die CE-Leistungserklärung den Hinweis enthält 'dauerhaft für bis zu 100 Jahre' oder sogar 'dauerhaft für mindestens 100 Jahre'. Hersteller, Bauherren, Planer und zuständige Behörden werden sich daher die Frage stellen, ob diese Produkte auf der Grundlage von Anhang 1 Nummer 2.1 Satz 7 Ziffer 1 der Deponieverordnung (DepV) im Deponiebau auch ohne Zulassung verwendet werden dürfen. Ein Vergleich der europäisch harmonisierten Bauproduktnormen DIN EN 13252 und DIN EN 13257, die der CE-Kennzeichnung der Geotextilien und geotextilverwandten Produkte zugrunde liegen, mit den Anforderungen der DepV zeigt nun aber, dass nur ein Teil der für den Deponiebau wesentlichen technischen Eigenschaften in diesen Normen erfasst werden. Daher sind für CE gekennzeichnete Produkte zusätzliche Prüfungen auf der Grundlage der DepV-Liste der Kriterien und Einwirkmechanismen erforderlich. Die in den Produktnormen beschriebene Qualitätssicherung ist nach Anhang 1 Nummer 2 Satz 14 ff der DepV ebenfalls für die Gleichwertigkeit nicht ausreichend. Eine CE-Kennzeichnung ist deshalb noch kein Nachweis, dass die Produkte dem Stand der Technik nach der DepV entsprechen und die Eigenschaften der Produkte den geforderten Eigenschaften im Wesentlichen gleichwertig sind, auch wenn mit Bezug auf den Anhang B der genannten Normen deren Dauerhaftigkeit für 100 Jahre vom Hersteller deklariert wird.----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
In the near future, CE-marked woven and nonwoven geotextiles, geocomposite drains and geogrids will be available on the market, whose declaration of performance will contain the qualification 'predicted service life up to 100 years' or even 'predicted service life minimum 100 years'. Manufacturer, principals and their design engineers as well as the responsible authorities will have to deal with the question, whether such products can be used on the basis of Annex 1, no. 2.1, sentence 7, cipher 1 of the German landfill ordinance (DepV) as components of landfill liner and capping systems. A comparison of the harmonized European standards hEN 13252 and 13257, on which the CE-marking of geotextiles and geotextile-related products is based, with the DepV, shows that only a few of the essential technical characteristics actually relevant for landfill constructions are considered in these standards. Therefore, additional tests based on the DepV-list of criteria and mechanisms of action are necessary for CE-marked products. Requirements on quality managements in the hEN are likewise not adequate for essential equivalence with respect to annex 1, No. 2.1, sentence 14 ff, DepV. Therefore, CE-marking is actually no proof of the fulfilment of the state of the techno logy according to the DepV and of the essential equivalence of product properties to the required properties, albeit the declaration of performance indicates a predicted service life of 100 years.
Accurate and reproducible measurement of the structure and properties of high-value nanoparticles is extremely important for their commercialization. A significant proportion of engineered nanoparticle systems consist of some form of nominally core-shell structure, whether by design or unintentionally. Often, these do not form an ideal core-shell structure, with typical deviations including polydispersity of the core or shell, uneven or incomplete shells, noncentral cores, and others. Such systems may be created with or without intent, and in either case an understanding of the conditions for formation of such particles is desirable. Precise determination of the structure, composition, size, and shell thickness of such particles can prove challenging without the use of a suitable range of characterization techniques. Here, the authors present two such polymer core-shell nanoparticle systems, consisting of polytetrafluoroethylene cores coated with a range of thicknesses of either polymethylmethacrylate or polystyrene. By consideration of surface energy, it is shown that these particles are expected to possess distinctly differing coating structures, with the polystyrene coating being incomplete. A comprehensive characterization of these systems is demonstrated, using a selection of complementary techniques including scanning electron microscopy, scanning transmission electron microscopy, thermogravimetric analysis, dynamic light scattering, differential centrifugal sedimentation, and X-ray photoelectron spectroscopy. By combining the results provided by these techniques, it is possible to achieve superior characterization and understanding of the particle structure than could be obtained by considering results separately.
This is a corrigendum to the original article "Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy" that was published in "The journal of physical chemistry C", vol. 123 (2019), no. 49 pp. 29765-29775.
An approach to achieve 'zero leakage' is discussed with respect to experience in Germany, where strict regulations for landfill lining and capping Systems have been developed and issued because of large environmental Problems related to landfills that accumulated in the 1970s and 1980s. Using a thick, high-quality high-density Polyethylene (HDPE) geomembrane (GM) that is installed free of residual waves and wrinkles in intimate contact with a compacted clay liner or geosynthetic clay liner of very low permeability, by a qualified, experienced, well-equipped and properly third-party-controlled installer, and which is protected by heavy protection layers designed with respect to the long-term performance of the GM may result in a liner or capping system of practically no leakage. This is demonstrated by analysing results of measurements obtained from permanently installed leak-detection Systems in combination with HDPE GMs. The survey was based on 32 German landfills with 1.276.500 m² of installed GMs.
Designing the performance of geogrids in reinforce soil constructions usually does not consider long-term behavior and possible failure modes of junctions between longitudinal and transverse ribs. How could behavior of junctions be included? To which extend is it necessary? On the conference Geo-Chicago 2016, Swan and Yuan presented an ultimate limit state equation for the short-term material resistance of junctions. We discuss limitations and suggest improvements to include long-term behavior of junctions. Nevertheless, the approach applies only to a specific mode of shear-tensile failure of junctions and only to strictly rigid geogrids. A new design concept presented in the same year by Jacobs on the conference GeoAmerica for the special case of the anchorage of geogrids, which reinforce capping system on long and steep slopes of landfills, tried to overcome these drawbacks. We discuss the aspects of this concept related to the long-term behavior
of junctions and the interplay between the load applied to junctions and the flexibility of longitudinal ribs. This interplay and the long-term junction strength determine the long-term behavior of geogrids.