TY - JOUR A1 - Fittschen, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Böttger, S. A1 - Rosenberg, D. A1 - Menzel, M. A1 - Jensen, W. A1 - Busker, M. A1 - Gotlib, Z. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Wobrauschek, P. A1 - Streli, C. ED - de Oliveira Guilherme Buzanich, Ana T1 - A setup for synchrotron-radiation-induced total reflection X-ray fluorescence and X-ray absorption near-edge structure recently commissioned at BESSY II BAMline N2 - An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml⁻¹ to μg ml⁻¹). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NISTwater 1640. Low limits of detection of less than 100 fg absolute (10 pg ml⁻¹) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state. KW - TXRF KW - TXRF-XANES KW - Sample changer KW - BAMline KW - Re-XANES PY - 2016 DO - https://doi.org/10.1107/S1600577516001995 SN - 1600-5775 VL - 23 IS - 3 SP - 820 EP - 824 PB - International Union of Crystallography AN - OPUS4-38656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Kabelitz, Anke A1 - Gorelik, T. E. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Kolb, U. A1 - Rademann, K. A1 - Emmerling, Franziska T1 - The crystallisation of copper(II) phenylphosphonates N2 - The crystal structures and syntheses of four different copper(II) phenylphosphonates, the monophenylphosphonates α-, β-, and γ-Cu(O3PC6H5)·H2O (α-CuPhPmH (1) β-CuPhPmH (2) and γ-CuPhPmH (3)), and the diphosphonate Cu(HO3PC6H5)2·H2O (CuPhP2mH (4)), are presented. The compounds were synthesized from solution at room temperature, at elevated temperature, under hydrothermal conditions, and mechanochemical conditions. The structures of α-CuPhPmH (1) and CuPhP2mH (4) were solved from powder X-ray diffraction data. The structure of β-CuPhPmH (2) was solved by single crystal X-ray analysis. The structures were validated by extended X-ray absorption fine structure (EXAFS) and DTA analyses. Disorder of the crystal structure was elucidated by electron diffraction. The relationship between the compounds and their reaction pathways were investigated by in situ synchrotron measurements. KW - Mechanochemistry KW - Metal phosphonate KW - In situ PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-384217 DO - https://doi.org/10.1039/C6DT02904C SN - 1477-9226 SN - 1477-9234 VL - 45 IS - 43 SP - 17453 EP - 17463 PB - The Royal Society of Chemistry AN - OPUS4-38421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - The structure and in situ synthesis investigation of isomorphic mononuclear molecular metal phenylphosphonates N2 - We describe a fast and effective synthesis for molecular metal phosphonates. Isomorphic compounds [M(II)(HO₃PPh)₂(H₂O₃PPh)₂(H₂O)₂] (M = Mn (1), Co (2), Ni (3); Ph = C₆H₅) were obtained by grinding. The complexes are mononuclear compounds containing neutral and monodeprotonated phenylphosphonic acid and water as ligands. The crystal structures were determined using powder X-ray diffraction (PXRD) data and validated by extended X-ray absorption fine structure (EXAFS) data. Combined synchrotron XRD measurements and Raman spectroscopy were conducted for investigating the reactions in situ. Based on these data, the intermediates were characterized and the formation mechanism was derived. KW - Mechanochemistry KW - Metal phosphonate KW - In situ KW - XRD PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-363944 DO - https://doi.org/10.1039/c6dt00787b SN - 1477-9226 SN - 1477-9234 SN - 1364-5447 VL - 45 IS - 23 SP - 9460 EP - 9467 AN - OPUS4-36394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska T1 - Time- & spatial-resolved X-ray absorption fine structure (XAFS) spectroscopy in a single-shot – new analytical possibilities for in situ material characterization N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ-2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 µm is achieved. KW - Time resolution KW - Single-shot XAFS PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-370892 DO - https://doi.org/10.1107/S1600577516003969 SN - 1600-5775 IS - 23 SP - 769 EP - 776 PB - International Union of Crystallography CY - Chester, UK AN - OPUS4-37089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hachmöller, O. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Aichler, M. A1 - Radtke, Martin A1 - Dietrich, D. A1 - Schwamborn, K. A1 - Lutz, L. A1 - Werner, M. A1 - Sperling, M. A1 - Walch, A. A1 - Karst, U. T1 - Elemental bioimaging and speciation analysis for the investigation of Wilsons disease using μXRF and XANES N2 - A liver biopsy specimen from a Wilson’s disease (WD) patient was analyzed by means of micro-X-ray fluorescence (mXRF) spectroscopy to determine the elemental distribution. First, bench-top mXRF was utilized for a coarse scan of the sample under laboratory conditions. The resulting distribution maps of copper and iron enabled the determination of a region of interest (ROI) for further analysis. In order to obtain more detailed elemental information, this ROI was analyzed by synchrotron radiation (SR)-based mXRF with a beam size of 4 mm offering a resolution at the cellular level. Distribution maps of additional elements to copper and iron like zinc and manganese were obtained due to a higher sensitivity of SR-mXRF. In addition to this, X-ray absorption near edge structure spectroscopy (XANES) was performed to identify the oxidation states of copper in WD. This speciation analysis indicated a mixture of copper(I) and copper(II) within the WD liver tissue. KW - progressive hepatolenticular degeneration KW - mXRF Micro-X-ray fluorescence spectroscopy KW - XANES X-ray absorption near edge structure spectroscopy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-360811 DO - https://doi.org/10.1039/C6MT00001K SN - 1756-5901 SN - 1756-591X PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-36081 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Hübert, Thomas A1 - Tiebe, Carlo A1 - Banach, Ulrich ED - Rodriguez Mendez, M. T1 - Electronic Noses for the Quality Control of Spices N2 - The chapter describes the application of electronic noses (multigas sensors) for the quality control of spices and spice mixtures. Electronic noses were successfully applied for headspace analysis of spices. It was demonstrated in many investigations that electronic noses can contribute to the characterization of spices and spice mixtures in order to distinguish spices and spice mixtures, differentiate by origin, growth seasons,and processing,indicate adulteration from original, detect mold infestation. Electronic noses can be used as a fast screening method to provide information about the product quality. However, it needs samples and methods for reference, careful training, and complex calibration to consider influencing and disturbing effects as well as the possible limitations of the instrumentation. The correlation to classical chemical analysis methods is always advisable. Machined olfaction methods are capable to support the sensory analysis; however, they cannot yet substitute them. KW - Spice KW - Electronic Nose KW - Multigas sensor KW - Quality control PY - 2016 SN - 978-0-12-800243-8 DO - https://doi.org/10.1016/B978-0-12-800243-8.00012-3 SP - Chapter 12, 115 EP - 124 PB - Academic Press CY - Oxford AN - OPUS4-35443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Gawlitza, Kornelia T1 - Gas standards for the calibration of novel fluorescence sensors for ammonia N2 - Ammonia and its conversion product ammonium have a strong negative impact on human health and ecosystems. Most ammonia measurements in ambient air are performed in the molar fraction range (0.5 to 500) nmol/mol. There is a need for reliable traceable ammonia gas standards as well as in situ analytical procedures for the monitoring of ammonia in ambient air. The permeation method is an effective tool for dynamically generating precise gas standards with a low uncertainty in the concentration range of a few nmol/mol to several µmol/mol in an inert carrier gas, e. g. pure nitrogen or purified ambient air. Here, we present our ammonia gas standard generator as well as results of the characterisation of its individual components supporting the uncertainty assessment according to GUM for stable gas concentrations in this range. In order to detect ammonia in the nmol/mol-range, a suitable sensor has to be developed. In this contribution, we therefore additionally present first approaches on the development of such a sensor using optical fluorescence as transduction mechanism due to its intrinsically high sensitivity and high spatial resolution. Incorporation of a fluorescent dye, which shows fluorescence enhancement in the presence of ammonia, into a polymer matrix allows to reversibly recognize low amounts of ammonia. It can be concluded that fluorescence sensor is a robust tool for measurements of ammonia; however it needs calibration for the planed use. T2 - MetNH3-workshop on the progress in ammonia metrology CY - Braunschweig, Germany DA - 24.02.2016 KW - Ammonia KW - Fluorescence sensor KW - Permeation KW - Test gas generation PY - 2016 AN - OPUS4-35810 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sieg, H. T1 - Artificial digestion of aluminium-containing nanomaterials and their effects on the gastrointestinal tract in vitro N2 - Although aluminium is one of the most common elements in the biosphere, up to now little is known about its impact on human health. aluminium and its chemical derivatives are highly abundant in food, food contact materials and consumer products. Humans are exposed to aluminium via the gastrointestinal tract (GI tract). Exposition can change substantially due to consumer behavior since aluminium is also a compound of numerous food additives. Recently, aluminium exposition is increasingly considered to cohere with cancer and neurodegenerative disorders. Lately, due to an increasing attentiveness on this topic, limiting values for food additives have been tightened by the EFSA. However, cellular effects of aluminium and especially aluminium-containing nanomaterials, that represent a significant part of chemicals found in food products, are widely unknown and in the focus of our research activities, for example in the bilateral SolNanoTOX project. We established an in vitro simulation system of the GI tract, where nanomaterials undergo the different physiological, chemical and proteinbiochemical conditions of saliva, gastric juice and the intestine. The artificially digested nanomaterials, as well as soluble aluminium chloride as ionic control substance, were subjected to several analytical and biochemical methods to characterize their change of appearance and their cytotoxic effects on intestinal cellular models. We observed the fate of the nanomaterials during typical pH-values of saliva, gastric and intestinal juice with Dynamic light scattering measurements and ICP-MS in the single particle mode. After observable disappearance at pH 2 the particles recovered in the simulated intestinal fluid. The simulation of the GI tract, mainly the change of pH settings, can lead to a certain chemical activation of aluminium that can increase bioavailability in the intestine after oral uptake of aluminium-containing food products. In vitro assays like CTB, MTT and cellular impedance measurements showed that there were no acute cytotoxic effects measurable after a period up to 48h after incubation, comparable to undigested particles. In contrast, high amounts of aluminium ions showed synergistic effects on cell viability compared to non-digested aluminium ions. Although toxicological potential of Al ions to healthy tissue appears to be low, increased hazardous potential cannot be ruled out to pre-damaged tissue and can have a relevance in risk assessment for special consumer groups with for example chronical intestinal inflammation or dietary eating behavior combined with high exposure to Al-containing food products. T2 - 82nd Annual Meeting of the German Society for Experimental and Clinical Pharmacology and Toxicology CY - Berlin, Germany DA - 29.02.2016 KW - Nanoparticles KW - Digestion KW - SAXS KW - Cytotoxicity PY - 2016 AN - OPUS4-36026 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kästner, Claudia T1 - Aggregation and deaggregation of silver nanoparticles - what does your gut say? N2 - Due to the increasing utilization of silver nanoparticles in consumer related products, many studies focus on investigations regarding their toxicological potential. This includes investigations concerning uptake, distribution and excretion of the particles. So far, little attention was paid to changes of physical and chemical properties in the human body. During processes like digestion, the question arises whether they can pass this barrier in a nanoscale form. In this study we analytically monitored the changes in the size distribution of silver nanoparticles during an artificial digestion process with the help of small angle x-ray scattering (SAXS). Therefore, we synthesized polyacrylic acid stabilized ultra-small silver nanoparticles with a radius of 3 nm and a size distribution width of 18%. The artificial digestion process mimics the gastro-intestinal passage and simulates the oral, gastric and small intestinal conditions. Additionally, food components like oil, starch, glucose and skimmed milk powder are used to provide a preferably realistic environment. In absence of any food components the low pH initiates aggregation of the particles in the stomach. However, the particles unexpectedly stabilize in a defined cluster form with a mean radius of 12 nm. By the use of the food components oil and starch we observed that the particles are dispersed again. Now we found a bimodal size distribution of primary particles and aggregates. In contrast to that, with skimmed milk powder only a slight aggregation occurs in the stomach. In the gastric tract the particle distribution is stabilized at a mean volume weighted radius of 5 nm. Hence, skimmed milk powder acts as a colloidal stabilizer. For comparison we also used silver nitrate as a control substance. Surprisingly, we observed a formation of nanoparticles already in the saliva. During the digestion process the distribution narrows and finally in the intestine it shows a stable distribution with a mean volume weighted radius of 3 nm and a small fraction of aggregates. These results indicate that the silver nanoparticles can pass the biological barriers of the digestion process in a nanoscale form but undergo a transformation in the size distribution. However, even from pure silver nitrate nanoparticle formation can be observed. This sketches a complex mechanism in which not only food components but also silver ions cause changes in nanoparticle size and aggregation. T2 - 11th International Conference on Biological Barriers CY - Saarbrücken, Germany DA - 07.03.2016 KW - digestion KW - small-angle X-ray scattering KW - silver nanoparticles PY - 2016 AN - OPUS4-35539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brieger, C. A1 - Melke, J. A1 - van der Bosch, N. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - de Oliveira Guilherme Buzanich, Ana A1 - Krishna Kayarkatte, M. A1 - Schoeckel, A. A1 - Roth, C. T1 - A combined in-situ XAS-DRIFTS study unraveling adsorbate induced changes on the Pt nanoparticle structure N2 - The adsorption behavior of Platinum nanoparticles was studied for the as-received catalyst (under inert gas), under hydrogen and CO atmosphere using our newly designed in-situ cell. X-ray Absorption Spectroscopy (XAS) and Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) experiments were performed simultaneously with high data quality. Structural information and the type of adsorbate could be revealed via Extended X-ray Absorption Fine Structure (EXAFS) analysis, Dl X-ray Absorption Near Edge Structure analysis (Dl XANES) and in-situ DRIFTS. The as-received catalyst showed sub-surface oxygen and O(n-fold). Under CO atmosphere only CO(atop) was found. Reversible adsorbate induced changes of the Pt nanoparticle structure were derived from changes in the PtAPt coordination number and the corresponding bond distance. Under reducing conditions (H2, CO) a significant increase in both values occurred. Temperature dependent desorption of CO revealed a gradual shift from PtACO to PtAO. Reoxidation was clearly assigned to strong metal support interaction from the SiO2 support. KW - X-ray absorption spectroscopy KW - DRIFTS KW - XANES KW - CO adsorption KW - Platinum KW - Strong metal support interaction KW - Silica support KW - Adsorbates KW - Infrared spectroscopy PY - 2016 DO - https://doi.org/10.1016/j.jcat.2016.03.034 IS - 339 SP - 57 EP - 67 PB - Elsevier Inc. CY - Philadelphia, Pennsylvania, USA AN - OPUS4-35815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Beiranvand, Z. A1 - Kakanejadifard, A. A1 - Donskyi, Ievgen A1 - Faghani, A. A1 - Tu, Z. A1 - Lippitz, Andreas A1 - Sasanpour, P. A1 - Maschietto, F. A1 - Paulus, B. A1 - Haag, R. A1 - Adeli, M. T1 - Functionalization of fullerene at room temperature: toward new carbon vectors with improved physicochemical properties N2 - In this work, fullerene has been functionalized with cyanuric Chloride at room temperature by a nitrene mediated [2 + 1] cycloaddition reaction. The adduct after functionalization is inherently in the form of azafulleroid and shows broad UV absorption in the wavelength range of 200–800 nm, as well as photothermal conversion and fluorescence with a high quantum yield. KW - Functionalization of fullerenes KW - XPS KW - NEXAFS PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-387076 DO - https://doi.org/10.1039/c6ra23419d SN - 2046-2069 VL - 6 IS - 114 SP - 112771 EP - 112775 PB - Royal Society of Chemistry (RSC) AN - OPUS4-38707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mielke, Johannes A1 - Dohányosová, P. A1 - Lopez, S. A1 - Hodoroaba, Vasile-Dan T1 - Electrospray deposition of nanoparticles on TEM grids N2 - The authors have tested the prototype of an electrospray deposition system developed by the company RAMEM under its trademark IONER. To test the prototype and assess its performance, several materials have been sprayed onto TEM grids and the resulting particle distributions were compared to more traditional sample preparation strategies like the “drop on grid” method. Operation parameters such as the sample flow-rate, capillary – substrate distance, electric field strength and sampling period length have been optimized. It was found that the particles deposited by electrospray generally show a much more homogeneous spatial distribution on the substrate and a substantial increase of the number of single particles, which are much better suited to an automatic image evaluation procedure than the agglomerated particles observed otherwise. The applicability of the technique to a broad range of materials is demonstrated by various examples, but also the influence of the substrate, the choice of the particular TEM grid, on the obtained spatial particle distribution is assessed. KW - Electrspray deposition KW - Electron microscopy KW - Nanoparticles KW - Sample preparation PY - 2016 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/electrospray-deposition-of-nanoparticles-on-tem-grids/459E634B7F74D474A19E15E69DA82E5D DO - https://doi.org/10.1017/S1431927616010072 SN - 1431-9276 SN - 1435-8115 VL - 22 IS - Suppl 3 SP - 1846 EP - 1847 PB - Cambridge AN - OPUS4-38436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mielke, Johannes T1 - Evaluation of particle sizing techniques for the implementation of the EC definition of a nanomaterial N2 - What is a nanomaterial? Beyond a pure academic interest, this question has substantial im-plications for consumer protection and regulatory purposes. The European Commission has recommended a definition of nanomaterial (2011/696/EU), which states that a given material is considered a nanomaterial if more than 50 % of the particles in the number size distribution have a smallest dimension between 1 and 100 nm. Although several well established particle sizing techniques exist, the implementation of this definition for any particulate material remains a metrological challenge. The European research project NanoDefine (http://www.nanodefine.eu) has the aim of pro-viding help for the implementation of the definition. One central task is the performance evaluation of the available particle sizing techniques. For this purpose, a wide variety of real world materials has been selected. All available sizing techniques, including imaging, mobility-based and static scattering techniques, independent whether being counting, fractionating, spectroscopic or integrally sizing, will be applied to all of the projects materials to test the techniques performance and to establish their ranges of applicability. Because most of the techniques do not measure in number metrics as required in the nanomaterial definition, the quality of the conversion to the number based particle size distribution is assessed as well. Special care is taken on suitable sample preparation procedures as one of the most chal-lenging issues towards reaching a highly accurate result. Within this contribution, first results of the performance testing of state of the art characterisation techniques on the unique set of NanoDefine real world materials are going to be presented. From these results, first conclu-sions about the material dependent ranges of applicability for the considered particle sizing techniques can be drawn. The technique specific advantages and shortcomings with respect to the application of the EC definition as well as the analytical challenges encountered will be highlighted. Acknowledgements: The research leading to these results has received funding from the European Community's Seventh Framework Programme (FP7/2007-2013) under grant agreement n° 604347. T2 - PARTEC CY - Nürnberg, Germany DA - 19.04.2016 KW - Nanomaterial PY - 2016 AN - OPUS4-35802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Procop, Mathias A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Berger, D. T1 - Determination of the Effective Detector Area of an Energy-Dispersive X-Ray Spectrometer at the Scanning Electron Microscope Using Experimental and Theoretical X-Ray Emission Yields N2 - A method is proposed to determine the effective detector area for energy-dispersive X-ray spectrometers (EDS). Nowadays, detectors are available for a wide range of nominal areas ranging from 10 up to 150mm2. However, it remains in most cases unknown whether this nominal area coincides with the “net active sensor area” that should be given according to the related standard ISO 15632, or with any other area of the detector device. Moreover, the specific geometry of EDS installation may further reduce a given detector area. The proposed method can be applied to most scanning electron microscope/EDS configurations. The basic idea consists in a comparison of the measured count rate with the count rate resulting from known X-ray yields of copper, titanium, or silicon. The method was successfully tested on three detectors with known effective area and applied further to seven spectrometers from different manufacturers. In most cases the method gave an effective area smaller than the area given in the detector description. KW - Energy-dispersive X-ray spectrometer (EDS) KW - EDX KW - Effective area KW - X-ray emission yield KW - Geometrical collection efficiency PY - 2016 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/div-classtitledetermination-of-the-effective-detector-area-of-an-energy-dispersive-x-ray-spectrometer-at-the-scanning-electron-microscope-using-experimental-and-theoretical-x-ray-emission-yieldsdiv/E15B2E67C349201CF323E778EB9C6D94 DO - https://doi.org/10.1017/S1431927616011788 VL - 22 IS - 6 SP - 1360 EP - 1368 PB - Cambridge University Press CY - New York, NY, USA AN - OPUS4-38858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Can today’s methods afford to easily and reliably classify nanomaterials? N2 - In the contribution the NanoDefine sizing techniques are discussed after their systematic evaluation on NanoDefine materials. The results of the comparative study BET versus electron microscopy are also discussed. Furthermore, recommendations for application of the gained knowledge are given. T2 - NanoDefine Workshop Analytical Challenges and Industry Needs CY - Frankfurt, Germany DA - 08.02.2016 KW - Nanomaterial PY - 2016 AN - OPUS4-35924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Method evaluation and selection N2 - In this contribution the particle sizing techniques evaluated in NanoDefine are presented together with recommendations for their application/implementation on real-world materials. The experimental evaluation is discussed based on examples on NanoDefine materials. A systematic study on volume specific surface area as derived from BET measurements versus electron microscopy on powdered materials is also presented. T2 - NanoDefine NSC Synergy workshop CY - Brussels, Belgium DA - 02.02.2016 KW - nanomaterial PY - 2016 AN - OPUS4-35923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - From k-values to elemental composition by EMPA (EDX & WDX) N2 - k-values (k-ratio, K-value) is defined as ratio of the X-ray photon intensity I measured for a particular characteristic peak from the unknown sample to the value measured for the same X-ray peak from a reference material of known composition under identical conditions of beam energy, spectrometer efficiency and electron dose. T2 - CCQM - Surface and Micro/Nano Analysis Working Group (SAWG) Meeting for 2016 CY - Paris, France DA - 19.04.2016 KW - k-values KW - EPMA KW - EDX KW - WDX PY - 2016 AN - OPUS4-35794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Proposal of an inter-laboratory comparison on shape of bipyramidal TiO2 nanoparticles by TEM N2 - A proposal of an inter-laboratory study (ILC) on determination of size and shape distribution of TiO2 nanoparticles (NPs) by transmission electron microscopy is presented. The anatase NPs synthesized in a controllable fashion within the EU/FP7 project SETNanoMetro can be considered as shape-defined (bipyramidal) and are offered to complete the list of case studies already in progress within ISO/TC229/JWG2. The main points of the measurement procedure are presented as well as a proposed procedure to evaluate the size and shape according to the standard operation procedure already developed within SETNanoMetro is discussed. Potential ILC participants and a plan with next step to be carried out are proposed. T2 - Joint Meeting IEC TC 113 'Nanotechnology for electrotechnical products and systems' and ISO/TC229/JWG2 'Nanotechnologies'/'Measurement and characterization' CY - Lowell, MA, USA DA - 09.05.2016 KW - Nanoparticles KW - TiO2 KW - TEM KW - Shape KW - Inter-laboratory comparison KW - ISO PY - 2016 AN - OPUS4-38900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mielke, Johannes A1 - Babick, F. A1 - Uusimäki, T. A1 - Müller, P. A1 - Verleysen, E. A1 - Hodoroaba, Vasile-Dan T1 - Evaluation of electron microscopy techniques for the purpose of classification of nanomaterials N2 - Electron microscopy techniques such as TEM, STEM, SEM or TSEM (transmission in SEM) are capable of assessing the size of individual nanoparticles accurately. Nevertheless, the challenging aspect is sample preparation from powder or liquid form on the substrate, so that a homogeneous distribution of well-separated (deagglomerated) particles is attained. The systematic study in this work shows examples where the extraction of the critical, smallest particle dimension - as the decisive particle parameter for the classification as a NM - is possible by analysing the sample after ist simple, dry preparation. The consequences of additional typical issues like loss of information due to screening of smaller particles by larger ones or the (in)ability to access the constituent particles in aggregates are discussed. KW - Nanomaterial KW - Electron microscopy KW - Particle size distribution KW - Classification PY - 2016 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/evaluation-of-electron-microscopy-techniques-for-the-purpose-of-classification-of-nanomaterials/0B66A25EA7F7A5A3622C02A359C8304F DO - https://doi.org/10.1017/S1431927616005523 SN - 1431-9276 SN - 1435-8115 VL - 22 IS - Suppl. 3 SP - 936 EP - 937 PB - Cambridge AN - OPUS4-38445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kim, K. J. A1 - Kim, A. S. A1 - Jang, J. S. A1 - Suh, J. K. A1 - Wirth, Thomas A1 - Hodoroaba, Vasile-Dan A1 - Unger, Wolfgang A1 - Araujo, J. R. A1 - Archanjo, B. S. A1 - Galhardo, C. E. A1 - Damasceno, J. A1 - Achete, C. A. A1 - Wang, H. A1 - Wang, M. A1 - Bennett, J. A1 - Simons, D. A1 - Kurokawa, A. A1 - Terauchi, S. A1 - Fujimoto, T. A1 - Streeck, C. A1 - Beckhoff, B. A1 - Spencer, S. A1 - Shard, A. T1 - Measurement of mole fractions of Cu, In, Ga and Se in Cu(In,Ga)Se2 films N2 - CCQM key comparison K-129 for the quantitative analysis of Cu(In,Ga)Se2 (CIGS) films has been performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The objective of this key comparison is to compare the equivalency of the National Metrology Institutes (NMIs) and Designated Institutes (DIs) for the measurement of mole fractions of Cu, In, Ga and Se in a thin CIGS film. The measurand of this key comparison is the average mole fractions of Cu, In, Ga and Se of a test CIGS alloy film in the unit of mole fraction (mol/mol). Mole fraction with the metrological unit of mol/mol can be practically converted to atomic fraction with the unit of at%. In this key comparison, a CIGS film with certified mole fractions was supplied as a reference specimen to determine the relative sensitivity factors (RSFs) of Cu, In, Ga and Se. The mole fractions of the reference specimen were certified by isotope dilution - inductively coupled plasma/mass spectrometry (ID-ICP/MS) and are traceable to the SI. A total number counting (TNC) method was recommended as a method to determine the signal intensities of the constituent elements acquired in the depth profiles by Secondary Ion Mass Spectrometry (SIMS), X-ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES). Seven NMIs and one DI participated in this key comparison. The mole fractions of the CIGS films were measured by depth profiling based-SIMS, AES and XPS. The mole fractions were also measured by non-destructive X-Ray Fluorescence (XRF) Analysis and Electron Probe Micro Analysis (EPMA) with Energy Dispersive X-ray Spectrometry (EDX). In this key comparison, the average degrees of equivalence uncertainties for Cu, In, Ga and Se are 0.0093 mol/mol, 0.0123 mol/mol, 0.0047 mol/mol and 0.0228 mol/mol, respectively. These values are much smaller than that of Fe in a Fe-Ni alloy film in CCQM K-67 (0.0330 mol/mol). This means that the quantification of multi-element alloy films is possible by depth profiling analysis using the TNC method. KW - CIGS KW - Key comparison KW - CCQM KW - SIMS KW - XPS KW - AES KW - XRF KW - EPMA PY - 2016 UR - http://iopscience.iop.org/article/10.1088/0026-1394/53/1A/08011 DO - https://doi.org/10.1088/0026-1394/53/1A/08011 SN - 0026-1394 SN - 1681-7575 VL - 53, Technical Supplement SP - Article 08011, 1 EP - 19 PB - IOP Publishing AN - OPUS4-38110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -