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Organisationseinheit der BAM
Ultra-short pulse laser seeding techniques for silicon crystallite growth on amorphous substrates
(1999)
African cement inffastructure is quite complex. Apart from Northern Africa and South Africa in particular, cement plants are scarce resulting in highly unstable cement pricing. Clinker and cement are imported from overseas, e.g. from Portugal, Turkey, Pakistan, Indonesia, and China. Imports are typically determined by the lowest price, and as a result the countries of origin of products vaiy regularly yielding large scatter of properties. Quality control and a good quality infrastructure are thus of utmost importance for the safety of the popuiace, an issue, which is actually often neglected. With funding of the German Metrology Institute (PTB) and Support of the SPIN project, a proficiency testing scheme for cement testing according to EN 196 was set up for African laboratories. Proficiency testing schemes, also called round robins. are interlaboratory performance comparisons allowing participants to evaluate themselves against pre-established criteria. Thev are a powerful tool to help laboratories improve their performance as well as demonstrate their competences to accreditation bodies or Customers. 26 laboratories from 20 nations, 18 of which from Africa, participated. The BAM Federal Institute for Materials Research and Testing acted as coordinator and provider of the scheme. The aim of the round robin was to interpret the submitted data further beyond the pure statistic analyses. The data provided a positive picture of the performance of the participants in general, but it also exhibited a number of technical fields that need improvement. The paper provides the general results of the scheme and analyses identified strengths and weak points based on the submitted and non submitted data as well as on discrepancies from the EN 196 procedures during measurements. The application of EN Standards for material testing is critically discussed and since quality infrastructure is also always an issue between industrial and political stakeholders, suggestions for the mitigation of the identified shared problems are given.
When it comes to higher accuracies, new technologies and real applications in additive manufacturing, there is one topic which cannot be avoided: The material response on the chosen processing parameters and its agreement and correspondence with literature data of the wrought material grade counterpart. In industrial Additive Manufacturing (AM) standards in terms of printing parameters, protection gas atmospheres or powder handling instructions are not obligatory. Therefore, the question must be answered whether the AM process is reproducible and reliable over different printing companies. This was the motivation to realize a round robin test between 8 European printing companies and academic partners. The consortium had printed and tested fatigue and tensile testing bars under plant-specific conditions. A commonly used cast aluminum alloy, AlSi10Mg, was chosen as test material for the PBF-LB/M process. Differences of the results between the partners and the scatter itself were discussed in detail.
Advances in scanning electron microscopy (SEM) enable the high-resolution imaging of single nanoparticles (NPs) with sizes well below 10 nm. The SEM analysis in transmission mode (T-SEM) of NPs on thin film supports has many benefits when compared to the analysis of NPs on bulk substrates. The enhanced material (mass - thickness) contrast of the T-SEM imaging mode is well suited for in-depth and, particularly valuable, to very accurate, traceable, lateral dimensional measurements of NPs. Compared to samples prepared on bulk substrates, T-SEM with energy dispersive X-ray spectroscopy (EDS) achieves a drastically improved spatial resolution of the emitted X-rays. The poor signal-to-noise ratio of the X-ray spectra emitted by a single nanoparticle (NP) can be improved by the use of high-sensitivity (high collection solid angle) silicon drift (SDD), energy-dispersive X-ray spectrometers (EDS). The EDS spectral imaging of a single NP with a spatial resolution below 10 nm has become possible. This is demonstrated by means of various examples of nanostructures. Advanced data processing of T-SEM/EDS results sets the stage for the automated classification of NPs by feature analysis. This method combines the detection of morphological structures of interest by image processing of T-SEM micrographs with the chemical classification by EDS.
The properties of nanomaterials are influenced not only by their chemical composition but also by physical properties (such as size, geometry and crystal structure). For the reliable determination and assessment of behaviour and effects of nanomaterials as well as for the determination of the exposure of humans and environment a comprehensive physical-chemical characterization of nanomaterials is essential. This is an important prerequisite to identify them as nanomaterials and to interpret and compare test results and - in future – to forecast interaction and effects of nanomaterials.
In 2006, the OECD launched a sponsorship program for the testing of nanomaterials in which 11 nanomaterials were thoroughly investigated using a variety of methods. The aim of the project was, among other things, to find out where problems occur and where there are gaps in the measurement and test procedures and where are changes required. An important outcome of the sponsorship program was the finding that the OECD Test Guidelines should in several cases be extended to the specific needs in testing of nanomaterials. The existing standardized test methods of the OECD for physical-chemical characterization have not been developed for nanomaterials in particular. A high demand for an extension of the test guidelines was identified. Germany complied with the OECD's request in 2017 and has agreed to extend the “Test Guideline on Particle Size Distribution / Fiber Length and Diameter Distributions Test Guideline” for Manufactured Nanomaterials (MN). UBA commissioned BAM and BAuA with the preparation of the Test Guideline. The aim of the project is the development of a harmonized test protocol for a valid and reproducible determination of particle size and size distribution which is one of the most relevant physical-chemical properties for MNs.
Different measuring methods provide different results for the size distribution of the particles. This is caused by the different measuring principles of the methods. Each method measures a specific parameter that ultimately determines particle size. First, the measured quantity differs for each method (Scattered light intensity, 2D image / projection, electric mobility, etc.). Second, the calculated diameters of the MN may differ (Feret Diameter, Area Projection, Mobility Diameter, Aerodynamic Diameter, Hydrodynamic Diameter). Third, a measuring method provides a size distribution which is measured either mass-based, surface-based or number-based. A conversion between the results requires additional parameters and thus possibly increases the measurement error.
In addition to the technical differences, the individual parameters are strongly influenced by the structure and material of the nanoparticles. For example, a surface functionalization can lead to very different results in the size distribution. The suitability of measurement methods differs with the material of the MN. As a result, two very different results can be measured for the particle size distribution using two different methods, which are nevertheless both correct. Several large projects in recent years therefore concluded that nanomaterials should be characterized by at least two complementary method. Imaging techniques are regarded as one of these methods for the characterization, the complementary methods are supposed to be statistical methods.
The different results for the size distribution of nanomaterials become problematic for the registration of new MN. A comparable and reproducible size distribution is a prerequisite for a standardized registration. In the future, the particle size distribution in the EU will also decide on the classification of a substance as a nanomaterial or as a non-nanomaterial. Especially in borderline cases, a standardized and comparable measurement methodology is therefore essential.
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 OECD test guidelines (TGs) for testing chemicals have been widely used for regulatory purposes all over the world since the establishment of the Mutual Acceptance of Data (MAD) principle in 1984. This MAD principle ensures that, if a chemical is tested under the Good Laboratory Practice (GLP) conditions accordingly to an OECD TG, the data should be accepted in all OECD countries. The TGs have been developed, harmonized, internationally validated (round robin tests) and adopted by OECD countries to be used for the physical-chemical characterisation, fate estimation, and hazard identification for risk assessment of various chemicals. In addition to the TGs, OECD Guidance Documents (GDs) usually provide guidance on how to use TGs and how to interpret the results. These GDs do not have to be fully experimentally validated, and hence they are not under MAD, but they are based on relevant published scientific research.
But are the existing TGs and the related GDs applicable and adequate for the regulatory testing of nanomaterials? In general, for nanomaterials it is accepted that most of the "endpoints" or more precisely measurement variables are applicable. However, for some endpoints new or amended TGs are needed. In addition, several GDs are needed to give more precise advice on the test performance in order to gain regulatory relevant data on nanomaterials.
Deflagrationsrohrsicherungen sind Sicherheitseinrichtungen, die den Durchfluss von brennbaren Gasen und Dämpfen brennbarer Flüssigkeiten ermöglichen, den Flammendurchschlag und eine weitere Explosionsausbreitung nach der Zündung von explosionsfähigen Gas-/Dampf-Luftgemischen jedoch verhindern sollen. Die Einbaubedingungen sind dabei von besonderer Bedeutung für die Wirksamkeit der Deflagrationsrohrsicherungen. Oft lassen sich aus betrieblichen bzw. verfahrenstechnischen Gründen entsprechende Einbaubedingungen nur schwer oder nicht realisieren. So können beispielsweise Rohrleitungsverzweigungen zusätzliche Turbulenzen induzieren und dadurch zu erhöhten Flammenausbreitungsgeschwindigkeiten und Explosionsdrücken und ggf. zum Versagen der Deflagrationsrohrsicherung führen. Neben den „klassischen“ Untersuchungsmethoden dieser Belastungssituationen von Deflagrationsrohrsicherungen, wie die Erfassung des Explosionsdruckes und der Flammenausbreitungsgeschwindigkeiten, werden in diesem Beitrag die Ergebnisse der visuellen Beobachtungen des Reaktionsverlaufes sowie die Belastungen der Flammendurchschlagsicherung bei unterschiedlichen Einbaubedingungen in den Vordergrund gestellt. Gegenübergestellt wird die Belastungssituation der Flammensperre in einer geraden und einer verzweigten Rohrleitung. Verwendet wurde dafür eine speziell gefertigte Deflagrationsrohrsicherung, die eine Beobachtung des Reaktionsverlaufs im Bereich der spiralförmig gewickelten Metallbändern erlaubt. Zusätzlich wurde im geschützten Bereich in der Rohrleitung eine Kamera installiert, die die Belastungssituation bei den einzelnen Versuchen dokumentierte.
Die Ergebnisse bestätigen sehr eindrucksvoll, dass die Belastungssituation der Deflagrationsrohrsicherung sich in Abhängigkeit von der Konfiguration der Rohrleitung entscheidend ändert