TY - JOUR A1 - Herwig, Nadine A1 - Stephan, Kristin A1 - Panne, Ulrich A1 - Pritzkow, Wolfgang A1 - Vogl, Jochen T1 - Multi-element screening in milk and feed by SF-ICP-MS N2 - In this study, an analytical procedure for multi-element screening of 40 elements in milk and feed samples was developed. Three different digestion and two different calibration methods were tested for the best suitability. The analytical procedure for the quantification of minor and trace elements is based on sector field ICP-MS (SF-ICP-MS). The method validation revealed good agreement between the determined elemental mass fractions and the certified values of two milk and three feed reference materials. Milk samples of dairy cows at different feeding regimes were collected from two different farms. The results of our study showed significant differences of nine elemental mass fractions (Li, P, Mn, Co, Cu, Rb, Sr, Br, I) between milk from the two locations. Further, a correlation between the elemental mass fractions of milk and the ingested feed and water was observed. KW - Multi-element screening KW - SF-ICP-MS KW - Dairy cows KW - Milk KW - Feed KW - Water PY - 2011 DO - https://doi.org/10.1016/j.foodchem.2010.07.050 SN - 0308-8146 VL - 124 IS - 3 SP - 1223 EP - 1230 PB - Elsevier Ltd. CY - Amsterdam [u.a.] ; Jena AN - OPUS4-22042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Spectrochemical Analysis: Tools and Toys!? T2 - GDCH-Vortrag, Wintersemester, Universtät Essen-Duisburg CY - Essen, Germany DA - 2011-02-02 PY - 2011 AN - OPUS4-22140 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Höhse, Marek A1 - Gornushkin, Igor B. A1 - Merk, Sven A1 - Panne, Ulrich T1 - Assessment of suitability of diode pumped solid state lasers for laser induced breakdown and Raman spectroscopy N2 - The potential of a diode pumped solid state (DPSS) laser for laser induced breakdown spectroscopy (LIBS) and Raman spectroscopy was investigated. The DPSS laser operating at repetition rates of 1 Hz–200 kHz, pulse energy of ~1 mJ, and pulse duration of ~20 ns was added to a conventional LIBS system equipped with the flashlamp-pumped Nd:YAG laser (10 Hz, 400 mJ, 6 ns) to directly compare the two laser systems. Despite the lower mass ablated per laser pulse (~several nanograms) and a weaker plasma, the total mass ablated per measurement interval (~1 s) and total emission signal were significantly higher than those obtained with the flashlamp pumped Nd:YAG laser. This resulted in the improved signal-to-noise ratio and better limits of detection (LOD). The best LODs were obtained for Cu, Cr and Ni in ultrapure standard iron samples, 0.7 ppm, 1 ppm and 5 ppm, correspondingly. The plasma from the DPSS laser was characterized in terms of its radiative properties, temperature, and shockwave propagation speed. The suitability of this laser for LIBS-Raman was demonstrated by mapping the elemental and molecular composition of a mineral sample. The results strongly imply that DPSS lasers are the promising source for LIBS, Raman, or combined LIBS-Raman spectroscopy. PY - 2011 DO - https://doi.org/10.1039/c0ja00038h SN - 0267-9477 SN - 1364-5544 VL - 26 IS - 2 SP - 414 EP - 424 PB - Royal Society of Chemistry CY - London AN - OPUS4-22943 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 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 - 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 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 - CONF A1 - Panne, Ulrich T1 - Hyphenated Techniques for New Insights in Polymer Analysis: 2dim LC and MALDI T2 - 4. Workshop Möglichkeiten und Grenzen der HPLC in den Lebenswissenschaften CY - Dresden, Germany DA - 2011-03-30 PY - 2011 AN - OPUS4-23460 LA - deu 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 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 - Behnke, Thomas A1 - Würth, Christian A1 - Hoffmann, Katrin A1 - Hübner, Martin A1 - Panne, Ulrich A1 - Resch-Genger, Ute T1 - Encapsulation of hydrophobic dyes in polystyrene micro- and nanoparticles via swelling procedures N2 - Aiming at the derivation of a generalized procedure for the straightforward preparation of particles fluorescing in the visible and near-infrared (NIR) spectral region, different swelling procedures for the loading of the hydrophobic polarity-probe Nile Red into nano- and micrometer sized polystyrene particles were studied and compared with respect to the optical properties of the resulting particles. The effect of the amount of incorporated dye on the spectroscopic properties of the particles was investigated for differently sized beads with different surface chemistries, i.e., non-functionalized, aminomodified and PEG-grafted surfaces. Moreover, photostability and leaking studies were performed. The main criterion for the optimization of the dye loading procedures was a high and thermally and photochemically stable fluorescence output of the particles for the future application of these systems as fluorescent labels. KW - Fluorescence KW - Nile red KW - Polystyrene KW - Nanoparticles KW - Microparticles KW - Encapsulation KW - Swelling PY - 2011 DO - https://doi.org/10.1007/s10895-010-0632-2 SN - 1053-0509 SN - 1573-4994 VL - 21 IS - 3 SP - 937 EP - 944 PB - Plenum Publ. Corp. CY - New York, NY AN - OPUS4-22692 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leiterer, Jork A1 - Panne, Ulrich A1 - Thünemann, Andreas A1 - Weidner, Steffen T1 - Container-less polymerization in acoustically levitated droplets: an analytical study by GPC and MALDI-TOF mass spectrometry N2 - Molecular masses and end groups of polystyrene (PS) formed in a novel container-less polymerization strategy, based on levitated droplets in an acoustic trap, were determined by Gel Permeation Chromatography (GPC) and Matrix-assisted Laser Desorption/Ionization Time of Flight Mass spectrometry (MALDI-TOF MS). KW - Ultraschallfalle KW - MALDI Massenspektrometrie KW - Polymerisation PY - 2011 DO - https://doi.org/10.1039/c0ay00390e SN - 1759-9660 SN - 1759-9679 VL - 3 IS - 1 SP - 70 EP - 73 PB - RSC Publ. CY - Cambridge AN - OPUS4-23655 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 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 - Weidner, Steffen A1 - Knappe, Patrick A1 - Panne, Ulrich T1 - MALDI-TOF imaging mass spectrometry of artifacts in 'dried droplet' polymer samples 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 - Kühn, Andreas A1 - Scharf, Oliver A1 - Ordavo, I. A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Radtke, Martin A1 - Berger, Achim A1 - Ostermann, Markus A1 - Panne, Ulrich T1 - Pushing the limits for fast spatially resolved elemental distribution patterns N2 - A new setup for fast spatially resolved measurements of elemental trace amounts under total reflection conditions using a new colour X-ray camera is described. Samples prepared on conventional total reflection X-ray fluorescence (TXRF) reflectors were measured at BESSY II synchrotron. A spatial resolution of 50 × 50 µm² was obtained, while the required time for the investigation of a 10 × 10 mm² sample is 30 seconds. The set-up is up to 350 times faster than conventional X-ray fluorescence systems for elemental traces. The major components of the X-ray camera are polycapillary optics and a pn-CCD chip with an active area of 13 × 13 mm². This area is divided into 264 × 264 pixels of 48 × 48 µm². A full X-ray spectrum with a resolution of 152 eV @ 5.9 keV and a chip temperature of 246 K is recorded for each pixel. The chip has a read-out rate of 400 Hz. PY - 2011 DO - https://doi.org/10.1039/c1ja10069f SN - 0267-9477 SN - 1364-5544 VL - 26 SP - 1986 EP - 1989 PB - Royal Society of Chemistry CY - London AN - OPUS4-24386 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 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 - 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) 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 - Bahlmann, Arnold A1 - Falkenhagen, Jana A1 - Weller, Michael G. A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - Cetirizine as pH-dependent cross-reactant in a carbamazepine-specific immunoassay N2 - High performance liquid chromatography (HPLC) was hyphenated with a previously reported carbamazepine-specific enzyme-linked immunosorbent assay (ELISA) as a screening approach to water analysis in order to identify possible interferences from transformation products. Treated wastewater was analysed and three substances were recognized by the antibody besides carbamazepine: the metabolites 10,11-dihydro-10,11-epoxycarbamazepine and 2-hydroxycarbamazepine plus the structurally not obviously related antihistamine cetirizine. The molar cross-reactivity against cetirizine was found to be pH-dependent and assessed to be 400% at pH 4.5 and 22% at pH 10.5. Performing the ELISA at pH 10.5 greatly improved the accuracy when carbamazepine was determined in surface and wastewater samples. KW - Immunoassay KW - ELISA KW - Cetirizin KW - Carbamazepin KW - pH-Abhängigkeit KW - Kreuzreaktivität PY - 2011 DO - https://doi.org/10.1039/c0an00928h SN - 0003-2654 SN - 1364-5528 VL - 136 IS - 7 SP - 1357 EP - 1364 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-23546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -