TY - JOUR A1 - Wolf, S. E. A1 - Müller, L. A1 - Barrea, R. A1 - Kampf, C.J. A1 - Leiterer, Jork A1 - Panne, Ulrich A1 - Hoffmann, T. A1 - Emmerling, Franziska A1 - Tremel, W. T1 - Carbonate-coordinated metal complexes precede the formation of liquid amorphous mineral emulsions of divalent metal carbonates JF - Nanoscale N2 - During the mineralisation of metal carbonates MCO3 (M = Ca, Sr, Ba, Mn, Cd, Pb) liquid-like amorphous intermediates emerge. These intermediates that form via a liquid/liquid phase separation behave like a classical emulsion and are stabilized electrostatically. The occurrence of these intermediates is attributed to the formation of highly hydrated networks whose stability is mainly based on weak interactions and the variability of the metal-containing pre-critical clusters. Their existence and compositional freedom are evidenced by electrospray ionization mass spectrometry (ESI-MS). Liquid intermediates in non-classical crystallisation pathways seem to be more common than assumed. PY - 2011 DO - https://doi.org/10.1039/c0nr00761g SN - 2040-3364 SN - 2040-3372 IS - 3 SP - 1158 EP - 1165 PB - RSC Publ. CY - Cambridge AN - OPUS4-23355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Knappe, Patrick A1 - Panne, Ulrich T1 - MALDI-TOF imaging mass spectrometry of artifacts in 'dried droplet' polymer samples JF - Analytical and bioanalytical chemistry N2 - Matrix-assisted laser desorption/ionization-timeof-flight (MALDI-TOF) imaging of polystyrenes with various molecular masses was applied to study spatial molecular mass distribution of polymers in sample spots prepared by the 'dried droplet' method. When different solvents and target surfaces were examined, a segregation of single homologous polymers was observed depending upon the evaporation rate of the solvent. For the observed Patterns left by the evaporating droplet, a hypothesis is offered taking into account different hydrodynamic interactions and diffusion. The results illustrate that spot preparation using the conventionally 'dried droplet' method is prone to artifacts and should be avoided for reliable and reproducible MALDI mass spectrometry experiments with regards to the Determination of molecular masses and mass distributions. KW - MALDI KW - Mass spectrometry imaging KW - Polymer KW - Droplet PY - 2011 DO - https://doi.org/10.1007/s00216-011-4773-1 SN - 1618-2642 SN - 1618-2650 VL - 401 IS - 1 SP - 127 EP - 134 PB - Springer CY - Berlin AN - OPUS4-24538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Walter, Astrid A1 - Panne, Ulrich A1 - Weller, Michael G. T1 - A novel immunoreagent for the specific and sensitive detection of the explosive triacetone triperoxide (TATP) JF - Biosensors N2 - Triacetone triperoxide (TATP) is a primary explosive, which was used in various terrorist attacks in the past. For the development of biosensors, immunochemical µ-TAS, electronic noses, immunological test kits, or test strips, the availability of antibodies of high quality is crucial. Recently, we presented the successful immunization of mice, based on the design, synthesis, and conjugation of a novel TATP derivative. Here, the long-term immunization of rabbits is shown, which resulted in antibodies of extreme selectivity and more than 1,000 times better affinity in relation to the antibodies from mice. Detection limits below 10 ng L-1 (water) were achieved. The working range covers more than four decades, calculated from a precision profile. The cross-reactivity tests revealed an extraordinary selectivity of the antibodies—not a single compound could be identified as a relevant cross-reactant. The presented immunoreagent might be a major step for the development of highly sensitive and selective TATP detectors particularly for security applications. KW - Organic peroxides KW - Terrorism KW - Biosensor development PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-240291 UR - http://www.mdpi.com/2079-6374/1/3/93 DO - https://doi.org/10.3390/bios1030093 SN - 2079-6374 VL - 1 IS - 3 SP - 93 EP - 106 PB - MDPI CY - Basel AN - OPUS4-24029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Deciphering the sulfate attack of cementitious materials by high-resolution micro-x-ray diffraction JF - Analytical chemistry N2 - The durability of cementitious materials depends, among others, on their resistance against chemical attack during the service life of a building. Here, we present an approach to analyze changes in the phase composition due to chemical attack in the form of sulfate ingress within the microstructure. Micro-X-ray (µX-ray) diffraction using synchrotron radiation in Debye–Scherrer (transmission) geometry allowed a spatial resolution of 10 µm. Phase transformations in the wake of damaging processes were observed in a detailed high-resolution imaging study. In comparison, samples containing supplementary cementitious materials were investigated and used to reconstruct the influence of different degeneration processes in detail. Additionally, reaction fronts within the bulk were localized by micro-X-ray fluorescence analysis. The experimental setup provided the possibility for analyzing the phase assemblage of a given sample without destroying the microstructure. The specimens for phase analysis are thick sections of the primary material and can be used for further microscopic analysis of the microstructure and microchemistry, e.g., scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM–EDX) or Raman spectroscopy. PY - 2011 DO - https://doi.org/10.1021/ac200181g SN - 0003-2700 SN - 1520-6882 VL - 83 IS - 10 SP - 3744 EP - 3749 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudtsch, S. A1 - Gusarova, Tamara A1 - Aulich, A. A1 - Fahr, M. A1 - Fischer, J. A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Procedure for the impurity-related correction at the indium fixed-point JF - International Journal of Thermophysics N2 - Determining the influence of impurities on the fixed-point emperatures of the ITS-90 requires the completion of several tasks. In this paper, the Progress made at Physikalisch-Technische Bundesanstalt (PTB) and BAMFederal Institute for Materials Research and Testing is presented and remaining questions are discussed. The projected characterization procedure at PTB, which is based on the established SIE method (sum of the individual estimates), using a new indium fixed-point cell is described as an example. This procedure includes an SI-traceable chemical Analysis of the material in the fixed-point cell with sufficiently low uncertainties, the individual experimental determination of the influence of the quantified impurities on the fixed-point temperature, and the establishment of direct links to the phase-transition temperatures of the national standard and of an assumed material of ideal purity. A characteristic difference to the common practice is the chemical analysis of the fixed-point metal being done after determining the cell’s freezing temperature. This allows for the detection and consideration of contamination and purification effects due to the filling process, or due to the contact with the carbon crucible and other parts of the fixed-point cell. A chemical analysis of an indium fixed-point was carried out by BAM with relative measurement uncertainties below 30 % which have not been previously achieved. The results provide evidence for the precipitation of some impurities, which is apparently inconsistent with the corresponding binary phase diagrams, but was explained in a recent publication. Implications for the use of the SIE method shall be described briefly at the end. KW - Chemical analysis KW - Fixed-points KW - Impurities KW - ITS-90 PY - 2011 DO - https://doi.org/10.1007/s10765-011-0915-0 SN - 0195-928X SN - 1572-9567 VL - 32 IS - 1-2 SP - 293 EP - 302 PB - Springer CY - Dordrecht AN - OPUS4-23373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, Vanessa A1 - Procop, M. A1 - Bjeoumikhova, S. A1 - Panne, Ulrich A1 - Hodoroaba, Vasile-Dan T1 - A routine procedure for the characterisation of polycapillary X-ray semi-lenses in prallelising mode with SEM/EDS JF - Journal of analytical atomic spectrometry N2 - The accurate knowledge of the properties of polycapillary X-ray semi-lenses has a significant influence on the quantitative results in a widespread field of applications involving microfocus X-ray beams. A routine procedure for the characterisation of a polycapillary X-ray semi-lens with a scanning electron microscope (SEM) having attached an energy dispersive spectrometer (EDS) is presented in this paper. A key issue of the procedure consists of fitting the semi-lens in front of the EDS for spectra acquisition. Relevant semi-lens parameters such as focal distance, full width at half maximum (FWHM) of the acceptance area, and transmission are determined in parallelising mode of the semi-lens. Special attention has been paid to the calculation of the transmission. KW - Polycapillary X-ray optics KW - Semi-lens KW - Parallelising mode KW - SEM KW - EDS KW - Acceptance area KW - FWHM KW - Transmission KW - Focal distance KW - XRF PY - 2011 DO - https://doi.org/10.1039/c0ja00135j SN - 0267-9477 SN - 1364-5544 VL - 26 IS - 3 SP - 499 EP - 504 PB - Royal Society of Chemistry CY - London AN - OPUS4-23555 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moreno-Gordaliza, E. A1 - Giesen, Charlotte A1 - Lázaro, A. A1 - Esteban-Fernández, D. A1 - Humanes, B. A1 - Canas, B. A1 - Panne, Ulrich A1 - Tejedor, A. A1 - Jakubowski, Norbert A1 - Gómez-Gómez, M.M. T1 - Elemental bioimaging in kidney by LA-ICP-MS as a tool to study nephrotoxicity and renal protective strategies in cisplatin therapies JF - Analytical chemistry N2 - A laser ablation inductively coupled plasma mass spectrometry (LA–ICP–MS)-based methodology is presented for Pt, Cu, and Zn bioimaging on whole kidney 3 µm sagittal sections from rats treated with pharmacological doses of cisplatin, which were sacrificed once renal damage had taken place. Pt turned out to accumulate in the kidney cortex and corticomedullary junction, corresponding to areas where the proximal tubule S3 segments (the most sensitive cells to cisplatin nephrotoxicity) are located. This demonstrates the connection between platinum accumulation and renal damage proved by histological examination of HE-stained sections and evaluation of serum and urine biochemical parameters. Cu and Zn distribution maps revealed a significant displacement in cells by Pt, as compared to control tissues. A dramatic decrease in the Pt accumulation in the cortex was observed when cilastatin was coadministered with cisplatin, which can be related to its nephroprotective effect. Excellent imaging reproducibility, sensitivity (LOD 50 fg), and resolution (down to 8 µm) were achieved, demonstrating that LA–ICP–MS can be applied as a microscopic metal detector at cellular level in certain tissues. A simple and quick approach for the estimation of Pt tissue levels was proposed, based on tissue spiking. PY - 2011 DO - https://doi.org/10.1021/ac201933x SN - 0003-2700 SN - 1520-6882 VL - 83 IS - 20 SP - 7933 EP - 7940 PB - American Chemical Society CY - Washington, DC AN - OPUS4-24965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Merk, Virginia A1 - Schulte, Franziska A1 - Rooch, Heidemarie A1 - Feldmann, Ines A1 - Dörfel, Ilona A1 - Österle, Werner A1 - Panne, Ulrich A1 - Kneipp, Janina T1 - Surface-enhanced Raman scattering with silver nanostructures generated in situ in a sporopollenin biopolymer matrix JF - Chemical communications N2 - Silver nanoparticles were generated based on citrate reduction in the ultrastructure of the sporopollenin biopolymer of Ambrosia artemisiifolia (ragweed) and Secale cereale (rye). The nanoparticles enable the acquisition of SERS spectra and thereby a vibrational characterization of the local molecular structure of sporopollenin. PY - 2011 DO - https://doi.org/10.1039/c0cc05326k SN - 0022-4936 SN - 0009-241x SN - 1359-7345 SN - 1364-548x N1 - Geburtsname von Merk, Virginia: Joseph, V. - Birth name of Merk, Virginia: Joseph, V. VL - 47 IS - 11 SP - 3236 EP - 3238 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-23482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Merk, Sven A1 - Shabanov, Sergej V. A1 - Gornushkin, Igor B. A1 - Panne, Ulrich T1 - Laser-induced plasma tomography by the Radon transform JF - Journal of analytical atomic spectrometry N2 - The Radon transform is tested as a method for reconstruction of the emissivity distribution of asymmetric laser induced plasmas. Two types of experiments were carried out. First, the plasma asymmetry is introduced via focusing the laser by a cylindrical lens to create plasma plumes elongated along the symmetry axis of the lens. Second, an asymmetric power distribution across the laser beam is created by reflecting the latter from a damaged mirror. Various effects on the quality of the plasma emissivity reconstructed by the Radon tomography method are investigated. The understanding of these effects appears to be essential to design a proper experimental setup to study LIBS plasmas by the Radon tomography method. It is demonstrated that the Radon tomography can successfully be used for experimental studies of asymmetric LIBS plasmas. KW - Radon transform KW - Laser induced plasma KW - LIBS KW - Plasma tomography PY - 2011 DO - https://doi.org/10.1039/c1ja10187k SN - 0267-9477 SN - 1364-5544 VL - 26 SP - 2483 EP - 2492 PB - Royal Society of Chemistry CY - London AN - OPUS4-24889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matiaske, Anna-Maria A1 - Gornushkin, Igor B. A1 - Panne, Ulrich T1 - Double-pulse laser-induced breakdown spectroscopy for analysis of molten glass JF - Analytical and bioanalytical chemistry N2 - A mobile double-pulse laser-induced breakdown spectroscopy system for industrial environments is presented. Its capabilities as a process analytical technique for the recovery of metals from molten inorganic wastes are investigated. Using low-melting glass doped with different amounts of additives as a model system for recycling slags, the optimum number of shots, laser inter-pulse and acquisition delay times are optimized for solid and liquid (1200 °C) glass. Limits of detection from 7 ppm (Mn) to 194 ppm (Zn) are achieved working at a distance of 75 cm from the sample. To simplify the quantification of molten samples in an industrial furnace, the possibility is examined of using solid standards for analysis of molten material. KW - Laser-induced breakdown spectroscopy KW - LIBS KW - Double-pulse LIBS KW - Molten glass KW - Recycling PY - 2011 DO - https://doi.org/10.1007/s00216-011-5165-2 SN - 1618-2642 SN - 1618-2650 VL - 402 IS - 8 SP - 2597 EP - 2606 PB - Springer CY - Berlin AN - OPUS4-23950 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -