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XUV- and X-ray free-electron-lasers (FEL) combine short wavelength, ultrashort pulse duration, spatial coherence and high intensity. This unique combination of properties opens up new possibilities to study the dynamics of non-reversible phenomena with ultrafast temporal and nano- to atomic-scale spatial resolution. In this contribution we wish to present results of time-resolved experiments performed at the XUV-FEL FLASH (HASYLAB/Hamburg) aimed to investigate the nano-scale structural dynamics of laser-irradiated materials. Thin films and fabricated nano-structures, deposited on Si3N4-membranes, have been excited with ultrashort optical laser pulses. The dynamics of the non-reversible structural evolution of the irradiated samples during laser-induced melting and ablation has been studied in an optical pump - XUV-probe configuration by means of single-shot coherent scattering techniques (i.e. diffraction imaging [1]). In a first set of experiments we investigated the formation of laser induced periodic surface structures (LIPSS) on the surface of thin Si-films (thickness 100 nm). In a simplified view LIPPS are generated as a result of interference between the incident laser pulse and surface scattered waves which leads to a periodically modulated energy deposition. Time-resolved scattering using femtosecond XUV-pulses (with a wavelength of 13.5 nm and 7 nm) allowed us to directly follow LIPSS evolution on an ultrafast time-scale and with better than 40 nm spatial resolution. The observed scattering patterns show almost quantitative agreement with theoretical predictions [2] and reveal that the LIPSS start to form already during the 12 ps pump pulse. In the second set of measurements we studied picosecond and femtosecond laser induced ablation and disintegration of fabricated nano-structures. Correlations of coherent diffraction patterns measured at various time delays to the pattern of the undisturbed object show that order in the structure is progressively lost starting from short length scales. This structural rearrangement progresses at close to the speed of sound in the material. Under certain circumstances (e.g. adequate sampling) it became also possible to reconstruct real-space images of the object as it evolves over time [3]. The possibility of femtosecond single-shot imaging of ultrafast dynamic processes with nanoscale resolution provides yet more details of the physical processes involved. [1] H. N. Chapman et al. Nature Phys. 2, 839 (2006). [2] J. F. Young et al., Phys. Rev. B 27, 1155 (1983). [3] A. Barty et al. Nature Phot. 2, 415 (2008).
Crystal structures of four different di-aryl-1,3,4-oxadiazole compounds (aryl = 2-pyridyl-, 3-pyridyl-, 2-aminophenyl-, 3-aminophenyl-) are determined. Crystallization of di(2-pyridyl)-1,3,4-oxadiazole yielded monoclinic and triclinic polymorphs. The structures are characterized by the occurrence of ππ interactions. Additionally, in case of the aminophenyl compounds intra- as well as intermolecular hydrogen bonds are found that influence the packing motif as well. Since these molecules are often used as ligands in metalorganic complexes similarities and differences of the molecular conformation between the molecules in the pure crystals and that of the ligands in the complexes are discussed.
Amphiphilic amino acids represent promising scaffolds for biologically active soft matter. In order to understand the bulk self-assembly of amphiphilic amino acids into thermotropic liquid crystalline phases and their biological properties a series of tyrosine ionic liquid crystals (ILCs) was synthesized, carrying a benzoate unit with 0–3 alkoxy chains at the tyrosine unit and a cationic guanidinium head group. Investigation of the mesomorphic properties by polarizing optical microscopy (POM), differential scanning calorimetry (DSC) and X-ray diffraction (WAXS, SAXS) revealed smectic A bilayers (SmAd) for ILCs with 4-alkoxy- and 3,4-dialkoxybenzoates, whereas ILCs with 3,4,5-trisalkoxybenzoates showed hexagonal columnar mesophases (Colh ), while different counterions had only a minor influence. Dielectric measurements revealed a slightly higher dipole moment of non-mesomorphic tyrosine-benzoates as compared to their mesomorphic counterparts. The absence of lipophilic side chains on the benzoate unit was important for the biological activity. Thus, non-mesomorphic tyrosine benzoates and crown ether benzoates devoid of additional side chains at the benzoate unit displayed the highest cytotoxicities (against L929 mouse fibroblast cell line) and antimicrobial activity (against Escherichia coli DTolC and Staphylococcus aureus) and promising selectivity ratio in favour of antimicrobial activity.
In this paper we present results of our recent efforts to understand the mechanical interface behaviour of single-walled carbon nanotubes (CNTs) embedded in metal matrices. We conducted experimental pull-out tests of CNTs embedded in Pd or Au and found Maximum forces in the range 10 - 102 nN. These values are in good agreement with forces obtained from molecular Dynamics simulations taking into account surface functional Groups (SFGs) covalently linked to the CNT material. The dominant failure mode in experiment is a CNT rupture, which can be explained with the presence of SFGs. To qualify the existence of SFGs on our used CNT material, we pursue investigations by means of fluorescence labeling of surface species in combination with Raman imaging. We also report of a tensile test system to perform pull-out tests inside a transmission electron microscope to obtain in situ images of CNT-metal interfaces under mechanical loads at the atomic scale.
This key comparison was performed to demonstrate the capability of NMIs to analyse the purity of methane for use as a source gas in the preparation of standard gas mixtures. This capability is an essential requirement for the preparation of accurate standards of natural gas and some other fuels.
Since it is difficult to carry out a comparison with individual samples of pure gas, the sample for this comparison was a synthetic mixture of high purity methane with selected added impurities of nitrogen, argon, carbon dioxide and ethane. These mixtures were prepared by a gas company as a batch of 10 cylinders and their homogeneity and stability were evaluated by NMIJ.
The KCRVs for the four different analytes in this key comparison are based on a consensus of values reported by participants. The uncertainties in the degrees of equivalence were calculated by combining the reported uncertainties with the homogeneity of the samples and the uncertainty of the KCRV. The results submitted are generally consistent with the KCRV within the estimated uncertainties.
Finally, this comparison demonstrates that the analysis of nitrogen, argon, carbon dioxide and ethane in methane at amount fractions of 1 µmol/mol to 5 µmol/mol is generally possible with an uncertainty of 5% to 10%.
Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/.
The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA).
DatesIssue 1A (Technical Supplement 2012)
This pilot study compares the performance of participants in analyzing gas mixtures of nitrogen dioxide in nitrogen by comparison with in-house gravimetric standards using Fourier transformed infrared spectroscopy (FT-IR). In this study the same gas mixtures were used as in the key comparison CCQM-K74, which was designed to evaluate the level of comparability of National Metrology Institutes' measurement capabilities for nitrogen dioxide (NO2) at a nominal mole fraction of 10 µmol/mol. In the comparison CCQM-K74 most of the participants used chemiluminescence, with a small number using UV absorption or FT-IR spectroscopy, and thus it is of interest to improve understanding of the comparative performance of these techniques because they do not exhibit any cross-sensitivity to nitric acid (HNO3), which was known to be present in the mixtures used for the comparison.
The results of this pilot study indicate good consistency and a level of agreement similar to that reported in the comparison CCQM-K74, demonstrating that FT-IR can be operated as a comparison method when calibrated with appropriate gas standards and can achieve similar measurement uncertainties to chemiluminescence and UV absorption techniques.
An additional pilot study, CCQM-P110-B2, was conducted on the same gas mixtures in parallel with this pilot study. The second study addressed FT-IR spectroscopy when used to measure the gas mixtures with respect to reference spectra. The results of this second study will be reported elsewhere.
Main text. To reach the main text of this paper, click on Final Report.
The final report has been peer-reviewed and approved for publication by the CCQM-GAWG.
DatesIssue 1A (Technical Supplement 2012)
Laboratory test results are of vital importance for correctly classifying and labelling chemicals as “hazardous” as defined in the UN Globally Harmonized System (GHS) / EC CLP Regulation or as “dangerous goods” as defined in the UN Recommendations on the Transport of Dangerous Goods. Interlaboratory tests play a decisive role in assessing the reliability of laboratory test results. Interlaboratory tests performed over the last 10 years have examined different laboratory test methods. After analysing the results of these interlaboratory tests, the following conclusions can be drawn:
1. There is a need for improvement and validation for all laboratory test methods examined.
2. To avoid any discrepancy concerning the classification and labelling of chemicals, the use of validated laboratory test methods should be state of the art, with the results accompanied by the measurement uncertainty and (if applicable) the probability of incorrect classification.
This paper addresses the probability of correct/incorrect classification (for example, as dangerous goods) on the basis of the measurement deviation obtained from interlaboratory tests performed by the Centre for quality assurance for testing of dangerous goods and hazardous substances (CEQAT-DGHS) to validate laboratory test methods. This paper outlines typical results (e.g. so-called “Shark profiles” – the probability of incorrect classification as a function of the true value estimated from interlaboratory test data) as well as general conclusions and steps to be taken to guarantee that laboratory test results are fit for purpose and of high quality.
CEQAT-DGHS Interlaboratory Test Programme for Chemical Safety - Need of Test Methods Validation
(2019)
Safety experts, manufacturers, suppliers, importers, employers or consumers must be able to rely on the validity of safety-related test methods and on correct test results and assessments in the laboratory. Via the eChemPortal lots of data from the REACH registration dossiers are available. However, the quality and correctness of the information remains in the responsibility of the data submitter. Unfortunately, we found more or less appropriate information on physicochemical properties and concluded that more quality or adequacy of any data submitted will be needed.
Interlaboratory tests play a decisive role in assessing the reliability of test results. Interlaboratory tests on different test methods have been performed by Bundesanstalt für Materialforschung und –prüfung (BAM) and Physikalisch-Technische Bundesanstalt (PTB) in collaboration with the QuoData GmbH during the last 10 years. Significant differences between the results of the participating laboratories were observed in all interlaboratory tests. The deviations of the test results were not caused only by laboratory faults but also by deficiencies of the test method.
In view of the interlaboratory test results the following conclusions can be drawn:
• To avoid any discrepancy on classification and labelling of chemicals it should become state of the art to use validated test methods and the results accompanied by the measurement uncertainty.
• A need for improvement is demonstrated for all examined test methods. Thus, interlaboratory tests shall initially aim at the development, improvement and validation of the test methods and not on proficiency tests.
• The laboratory management and the practical execution of the tests need to be improved in many laboratories.
• The term "experience of the examiner" must be seen critically: A "long experience with many tests" is not necessarily a guarantee for correct results.