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Final Draft of the OECD Test Guideline for Particle Size and Particle Size Distribution of Nanomaterials.
The OECD Working Party on Manufactured Nanomaterials (WPMN) has actively worked towards understanding possible safety issues for manufactured nanomaterials and has contributed significantly to resolving these by developing Test Guidelines, Guidance Documents, Test Reports and other publications with the aim of a safe use of manufactured nanomaterials. The OECD website (www.oecd.org/science/nanosafety) and the referenced publications contain more background information.
Among others, the OECD Test Guideline “Particle Size Distribution/Fibre Length and Diameter Distributions” (TG 110, adopted in 1981) was identified to require an update to address the specific needs of manufactured nanomaterials as the TG 110 is currently only valid for particles and fibres with sizes above 250 nm. The WPMN prioritised to either update TG 110 to be applicable also to particles at the nanoscale or draft a new nanomaterial specific Test Guideline (TG). Eventually, it was decided to develop a new TG for particle size and particle size distribution measurements of nanomaterials covering the size range from 1 nm to 1000 nm for further justification. This TG overlaps with TG 110 in the size range from 250 nm to 1000 nm. When measuring particulate or fibrous materials, the appropriate TG should be selected depending on the size range of particles tested. In line with TG 110, the new TG for nanomaterials includes separate parts for particles and fibres. For the part of this TG which addresses particles, several methods applicable to nanomaterials were reviewed and included to take into account developments since 1981 when the TG110 was adopted. This TG includes the following methods: Atomic Force Microscopy (AFM), Centrifugal Liquid Sedimentation (CLS)/Analytical Ultracentrifugation (AUC), Dynamic Light Scattering (DLS), Differential Mobility Analysis System (DMAS), (Nano)Particle Tracking Analysis (PTA/NTA), Small Angle X-Ray Scattering (SAXS), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM).
For measuring the diameter and length of fibres, analysing images captured with electron microscopy is currently the only method available. This TG includes Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM).
To test the validity of this TG, an ILC was performed. Test materials were chosen to reflect a broad 68 range of nanomaterial classes, e.g. metals, metal oxides, polymers and carbon materials. Where possible, well-characterised test materials were used. Additionally, the test materials were chosen, so that they reflect a broad range of sizes representing the size range 1 nm to 1000 nm and finally,
for fibres only, aspect ratios from length/diameter of 3 to > 50.
With a growing percentage of elderly people in the population and, correspondingly, an increasing rate of fractures of the proximal femur, the question how to stabilize medial femoral-neck fractures is gaining increasing importance. Especially in Hungary and Scandinavian countries, femoral-head-preserving surgery is advocated. However, the main problems of this procedure are re-dislocation and necrosis of the femoral head. Encouraged by two theoretical mathematical considerations, a biomechanical experiment was performed to investigate two different methods of screw fixation of medial femoral-neck fractures. The results showed that a head-preserving internal fixation with two cranial screws and a three-point supported screw at the bottom of the neck had distinct biomechanical advantages compared to conventional screw fixation. This has encouraged us to more frequently perform this minimally invasive and head-preserving surgery in Pauwels I and II medial fractures of the femoral head.
Ultra-short pulse laser seeding techniques for silicon crystallite growth on amorphous substrates
(1999)
Studienziel: Bei der zunehmenden Überalterung der Bevölkerung und der zunehmenden Inzidenz an hüftgelenknahen Oberschenkelfrakturen nimmt die Frage der Versorgung der medialen Schenkelhalsfraktur eine zunehmende Rolle ein. Vor allem aus Ungarn und den skandinavischen Ländern wird die kopferhaltende Therapie propagiert. Das Redislozieren dieser Frakturen und die Hüftkopfnekrose sind jedoch dagegenstehende Probleme. Methode: Ermutigt durch zwei theoretische mathematische Überlegungen wurden in einem biomechanischen Experiment zwei verschiedene Möglichkeiten der Verschraubung der medialen Schenkelhalsfraktur erprobt. Ergebnisse: Als Ergebnis zeigte sich, dass eine kopferhaltende Versorgung mit 2 kranial liegenden Schrauben und einer dreipunktabgestützten Schraube am Adam'schen Bogen deutliche biomechanische Vorteile hat gegenüber der herkömmlichen Verschraubung. Schlussfolgerung: Dies ermutigt uns, zunehmend die minimalinvasive und kopferhaltende Versorgung der medialen Schenkelhalsfraktur insbesondere bei Pauwels-I- und II-Verletzungen einzusetzen.
Despite their inherent instability, 4n π systems have recently received significant attention due to their unique optical and electronic properties. In dibenzopentalene (DBP), benzanellation stabilizes the highly antiaromatic pentalene core, without compromising its amphoteric redox behavior or small HOMO−LUMO energy gap. However, incorporating such molecules in organic devices as discrete small molecules or amorphous polymers can limit the performance (e.g., due to solubility in the battery electrolyte solution or low internal surface area). Covalent organic frameworks (COFs), on the contrary, are highly ordered, porous, and crystalline materials that can provide a platform to align molecules with specific properties in a well-defined, ordered environment. We synthesized the first antiaromatic framework materials and obtained a series of three highly crystalline and porous COFs based on DBP. Potential applications of such antiaromatic bulk materials were explored: COF films show a conductivity of 4 × 10−8 S cm−1 upon doping and exhibit photoconductivity upon irradiation with visible light. Application as positive electrode materials in Li-organic batteries demonstrates a significant enhancement of performance when the antiaromaticity of the DBP unit in the COF is exploited in its redox activity with a discharge capacity of 26 mA h g−1 at a potential of 3.9 V vs. Li/Li+ . This work showcases antiaromaticity as a new design principle for functional framework materials.
This guideline is intended to be used as an aid to laboratories when they are managing the
use of software and computers with respect to the requirements of ISO/IEC 17025. The
working group consisted of representatives from accreditation bodies and conformity assessment
operators, specifically laboratory organisations, but also included certification
bodies, inspection bodies and metrology institutes.
This paper presents the results of an interlaboratory study of the rheological properties of cement paste and ultrasound gel as reference substance. The goal was to quantify the comparability and reproducibility of measurements of the Bingham parameters yield stress and plastic viscosity when measured on one specific paste composition and one particular ultrasound gel in different laboratories using different rheometers and measurement geometries.
The procedures for both in preparing the cement paste and carrying out the rheological measurements on cement paste and ultrasound gel were carefully defined for all of the study’s participants. Different conversion schemes for comparing the results obtained with the different measurement setups are presented here and critically discussed. The procedure proposed in this paper ensured a reasonable comparability of the results with a coefficient of variation for the yield stress of 27% and for the plastic viscosity of 24%, despite the individual measurement series’ having been performed in different labs with different rheometers and measurement geometries.
A great number of Central Asian wall paintings, archeological materials, architectural fragments, and textiles, as well as painting fragments on silk and paper, make up the so called Turfan Collection at the Asian Art Museum in Berlin. The largest part of the collection comes from the Kucha region, a very important cultural center in the third to ninth centuries. Between 1902 and 1914, four German expeditions traveled along the northern Silk Road. During these expeditions, wall paintings were detached from their original settings in Buddhist cave complexes. This paper reports a technical study of a wall painting, existing in eight fragments, from the Buddhist cave no. 40 (Ritterhöhle). Its original painted surface is soot blackened and largely illegible. Grünwedel, leader of the first and third expeditions, described the almost complete destruction of the rediscovered temple complex and evidence of fire damage. The aim of this case study is to identify the materials used for the wall paintings. Furthermore, soot deposits as well as materials from conservation interventions were of interest. Non-invasive analyses were preferred but a limited number of samples were taken to provide more precise information on the painting technique. By employing optical and scanning electron microscopy, energy dispersive X-ray spectroscopy, micro X-ray fluorescence spectroscopy, X-ray diffraction analysis, and Raman spectroscopy, a layer sequence of earthen render, a ground layer made of gypsum, and a paint layer containing a variety of inorganic pigments were identified.
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.
Need for large-area EDS detectors for imaging nanoparticles in a SEM operating in transmission mode
(2014)
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.
Iron can form numerous oxides, hydroxides, and oxide−hydroxides. Despite their relevance, many of the transformation processes between these phases are still poorly understood. In particular the crystallization of quasi-amorphous hydroxides and oxide−hydroxides is difficult to assess, since typical diffraction and scattering methods provide only sampleaveraged information about the crystallized phases. We report a new approach for the investigation of the crystallization of oxide−hydroxides. The approach relies on model-type films that comprise a defined homogeneous nanostructure. The nanostructure allows quantitative linking of Information obtained by bulk-averaging diffraction techniques (XRD, SAXS) with locally resolved information, i.e., Domain sizes (SEM, TEM, LEEM) and phase composition (SAED). Using time-resolved imaging and diffraction we deduce mechanism and kinetics for the crystallization of ferrihydrite into hematite. Hematite forms via nucleation of hematite domains and subsequent Domain growth that terminates only upon complete transformation. A Johnson−Mehl−Avrami−Kolmogorov model describes the kinetics over a wide temperature range. The derived understanding enables the first synthesis of ferrihydrite films with ordered mesoporosity and quantitative control over the films’ hematite and ferrihydrite content.
Towards the standardization of biochar analysis: the COST action TD1107 interlaboratory comparison
(2016)
Biochar produced by pyrolysis of organic residues is increasingly used for soil amendment and many other applications. However, analytical methods for its physical and chemical characterization are yet far from being specifically adapted, optimized, and standardized. Therefore, COST Action TD1107 conducted an interlaboratory comparison in which 22 laboratories from 12 countries analyzed three different types of biochar for 38 physical–chemical parameters (macro- and microelements, heavy metals, polycyclic aromatic hydrocarbons, pH, electrical conductivity, and specific surface area) with their preferential methods. The data were evaluated in detail using professional interlaboratory testing software. Whereas intralaboratory repeatability was generally good or at least acceptable, interlaboratory reproducibility was mostly not (20% < mean reproducibility standard deviation < 460%). This paper contributes to better comparability of biochar data published already and provides recommendations to improve and harmonize specific methods for biochar analysis in the future.
Chapter 6: Case studies
(2023)
Phage display biopanning with Illumina next-generation sequencing (NGS) is applied to reveal insights into peptide-based adhesion domains for polypropylene (PP). One biopanning round followed by NGS selects robust PP-binding peptides that are not evident by Sanger sequencing. NGS provides a significant statistical base that enables motif analysis, statistics on positional residue depletion/enrichment, and data analysis to suppress false-positive sequences from amplification bias. The selected sequences are employed as water-based primers for PP-metal adhesion to condition PP surfaces and increase adhesive strength by 100% relative to nonprimed PP.
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.
African cement infrastructure 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 vary regularly yielding large scatter of properties. Quality control and a good quality infrastructure are thus of utmost importance for the safety of the populace, 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 inter-laboratory performance comparisons allowing participants to evaluate themselves against pre-established criteria. They 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.