TY - JOUR A1 - Knobbe, N. A1 - Vogl, Jochen A1 - Pritzkow, Wolfgang A1 - Panne, Ulrich A1 - Fry, H. A1 - Lochotzke, H.M. A1 - Preiss-Weigert, A. T1 - C and N stable isotope variation in urine and milk of cattle depending on the diet N2 - The stable carbon and nitrogen isotopic composition of urine and milk samples from cattle under different feeding regimes were analysed over a period of six months. The isotope ratios were measured with isotope ratio mass spectrometry (IRMS). The δ13C values of milk and urine were dependent on different feeding regimes based on C3 or C4 plants. The δ13C values are more negative under grass feeding than under maize feeding. The δ13C values of milk are more negative compared to urine and independent of the feeding regime. Under grass feeding the analysed milk and urine samples are enriched in 13C relative to the feed, whereas under maize feeding the 13C/12C ratio of urine is in the same range and milk is depleted in 13C relative to the diet. The difference between the 15N/14N ratios for the two feeding regimes is less pronounced than the 13C/12C ratios. The δ15N values in urine require more time to reach the new equilibrium, whereas the milk samples show no significant differences between the two feeding regimes. KW - Cattle KW - Urine KW - Milk KW - Feeding regime KW - Stable isotope PY - 2006 U6 - https://doi.org/10.1007/s00216-006-0644-6 SN - 1618-2642 SN - 1618-2650 VL - 386 IS - 1 SP - 104 EP - 108 PB - Springer CY - Berlin AN - OPUS4-12746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leiterer, Jork A1 - Leitenberger, W. A1 - Emmerling, Franziska A1 - Thünemann, Andreas A1 - Panne, Ulrich T1 - The use of an acoustic levitator to follow crystallization in small droplets by energy-dispersive X-ray diffraction N2 - For the investigation of small sample volumes, the use of an acoustic levitator was tested as a `sample holder' for hovering droplets in a synchrotron beam. It might be advantageous to use levitated droplets instead of samples confined in solid holders, especially for the study of crystallization processes where the influence of containing walls has to be minimized. In a first experiment, the crystallization of sodium chloride in a small droplet of aqueous solution has been followed with a time resolution of 30 s. The collected diffraction peaks are compared with data in the ICSD database. KW - EDXD KW - Noncontact measurement technique KW - X-ray-scattering KW - Synchrotron-radiation KW - Acoustic levitation PY - 2006 U6 - https://doi.org/10.1107/S0021889806024915 SN - 0021-8898 SN - 1600-5767 VL - 39 IS - 5 SP - 771 EP - 773 PB - Blackwell CY - Oxford AN - OPUS4-13516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krause, Benjamin Christoph A1 - Seifert, Stephan A1 - Panne, Ulrich A1 - Kneipp, Janina A1 - Weidner, Steffen T1 - Matrix-assisted laser desorption/ionization mass spectrometric investigation of pollen and their classification by multivariate statistics N2 - RATIONALE A fast and reliable online identification of pollen is not yet available. The identification of pollen is based mainly on the evaluation of morphological data obtained by microscopic methods. METHODS Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-TOF MS) was applied to the analysis of extracts and milled pollen samples. The obtained MALDI data were explored for characteristic peak patterns which could be subjected to a multivariate statistical analysis. RESULTS Two sample preparation methods are presented, which require only minimal or no chemical extraction of the pollen. MALDI pollen spectra could be recorded showing various peak patterns. A multivariate statistics approach allowed the classification of pollen into clusters indicating similarities and differences between various species. CONCLUSIONS These results demonstrate the potential and the reliability of MALDI-TOF MS for the identification and, in combination with multivariate statistics, also for the classification of pollen. KW - MALDI TOF mass spectrometry KW - Pollen KW - Multivariate statistics PY - 2012 U6 - https://doi.org/10.1002/rcm.6202 SN - 0951-4198 SN - 1097-0231 VL - 26 IS - 9 SP - 1032 EP - 1038 PB - Wiley CY - Chichester AN - OPUS4-25648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - González, M.G. A1 - Niessner, R. A1 - Panne, Ulrich A1 - Haisch, C. A1 - Resch-Genger, Ute T1 - Determination of the absolute fluorescence quantum yield of rhodamine 6G with optical and photoacoustic methods - providing the basis for fluorescence quantum yield standards N2 - To establish the methodical basis for the development and certification of fluorescence quantum yield standards, we determined the fluorescence quantum yield Φf of rhodamine 6G (R6G) with two absolute methods with complementary measurement principles, here optical spectroscopy using an integrating sphere setup and pulsed laser photoacoustic spectroscopy (PAS). For the assessment of aggregation- and reabsorption-induced distortions of measured fluorescence quantum yields and procedures for the reliable consideration of such effects, this systematic comparison was performed in ethanol and in water employing different concentrations of R6G. In addition, the relative and absolute fluorescence quantum yields of these solutions were obtained with a calibrated spectrofluorometer and a commercialized integrating sphere setup. Based upon this systematic comparison, experimental advantages and systematic sources of variation were identified for both methods. KW - Fluorescence KW - Photoluminescence KW - Quantum yield KW - Photoacoustic spectroscopy KW - Absolute quantum yield KW - Integrating sphere KW - Rhodamine 6G KW - Aggregation KW - Reabsorption PY - 2012 U6 - https://doi.org/10.1016/j.talanta.2011.12.051 SN - 0039-9140 VL - 90 SP - 30 EP - 37 PB - Elsevier CY - Amsterdam AN - OPUS4-25710 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schenk, Jonas A1 - Batzdorf, Lisa A1 - Emmerling, Franziska A1 - Kneipp, Janina A1 - Panne, Ulrich A1 - Buurman, Merwe T1 - Simultaneous UV/Vis spectroscopy and surface enhanced raman scattering of nanoparticle formation and aggregation in levitated droplets N2 - The formation and growth of hydroxylamine reduced silver nanoparticles were investigated by simultaneous Raman and UV/Vis spectroscopy coupled to an acoustic levitator as a sample holder. Based on the UV/Vis spectra, a two step particle formation mechanism with fast initial formation and adjacent coalescence can be proposed for the reduction of silver nitrate with hydroxylamine. The presence of the analyte adenine during particle formation resulted in differences in the adenine SERS signature compared to experiments, where adenine was added after particle synthesis. It was possible to monitor the adenine and sodium chloride induced aggregation of the nanoparticles and its dynamics based on both the extinction spectra and the SERS data. Correlating the information from the extinction spectra with the SERS intensity, the maximum SERS signals were observed at maximum extinction of the aggregated nanoparticle solution at the Raman excitation wavelength. PY - 2012 U6 - https://doi.org/10.1039/c2ay05744a SN - 1759-9660 SN - 1759-9679 N1 - Geburtsname von Batzdorf, Lisa: Tröbs, L. - Birth name of Batzdorf, Lisa: Tröbs, L. N1 - Geburtsname von Buurman, Merwe: Albrecht, M. - Birth name of Buurman, Merwe: Albrecht, M. VL - 4 IS - 5 SP - 1252 EP - 1258 PB - RSC Publ. CY - Cambridge AN - OPUS4-25742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bahlmann, Arnold A1 - Carvalho, José Joao A1 - Weller, Michael G. A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - Immunoassays as high-throughput tools: monitoring spatial and temporal variations of carbamazepine, caffeine and cetirizine in surface and wastewaters N2 - Carbamazepine (CBZ), caffeine and cetirizine were monitored by enzyme-linked immunosorbent assays (ELISAs) in surface and wastewaters from Berlin, Germany. This fast and cost-efficient method enabled to assess the spatial and temporal variation of these anthropogenic markers in a high-throughput screening. CBZ and cetirizine were detected by the same antibody, which selectively discriminates between both compounds depending on the pH value used in the incubation step. To our best knowledge, this is the first dual-analyte immunoassay working with a single antibody. The frequent sampling with 487 samples being processed allowed for the repeated detection of unusually high concentrations of CBZ and caffeine. ELISA results correlate well with the ones obtained by liquid chromatography tandem mass spectrometry (LC-MS/MS). Caffeine concentrations found in surface waters were elevated by combined sewer overflows after stormwater events. During the hay fever season, the concentrations of the antihistamine drug cetirizine increased in both surface and wastewaters. Caffeine was almost completely removed during wastewater treatment, while CBZ and cetirizine were found to be more persistent. The maximum concentrations of caffeine, CBZ and cetirizine found in influent wastewater by LC–MS/MS were 470, 5.0 and 0.49 µg L-1, while in effluent wastewater the concentrations were 0.22, 4.5 and 0.51 µg L-1, respectively. For surface waters, concentrations up to 3.3, 4.5 and 0.72 µg L-1 were found, respectively. KW - ELISA KW - Carbamazepine KW - Caffeine KW - Cetirizine KW - Environmental monitoring KW - Anthropogenic markers PY - 2012 U6 - https://doi.org/10.1016/j.chemosphere.2012.05.020 SN - 0045-6535 SN - 0366-7111 VL - 89 IS - 11 SP - 1278 EP - 1286 PB - Elsevier Science CY - Kidlington, Oxford AN - OPUS4-26187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lindner, Uwe A1 - Lingott, Jana A1 - Richter, Silke A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Speciation of gadolinium in surface water samples and plants by hydrophilic interaction chromatography hyphenated with inductively coupled plasma mass spectrometry N2 - Hydrophilic interaction chromatography (HILIC) coupled with inductively coupled plasma mass spectrometry (ICP-MS) was optimized for speciation analysis of gadolinium-based contrast agents in environmental samples, in particular surface river waters and plants. Surface water samples from the Teltow channel, near Berlin, were investigated over a distance of 5 km downstream from the influx of a wastewater treatment plant. The total concentration of gadolinium increased significantly from 50 to 990 ngL-1 due to the influx of the contrast agents. After complete mixing with the river water, the concentration remained constant over a distance of at least 4 km. Two main substances [Dotarem® (Gd-DOTA) and Gadovist® (Gd-BT-DO3A)] have been identified in the river water using standards. A gadolinium-based contrast agent, possibly Gd-DOTA (Dotarem®), was also detected in water plant samples taken from the Teltow channel. Therefore, uptake of contrast agents [Gadovist® (Gd-BTDO3A), Magnevist® (Gd-DTPA), Omniscan® (Gd-DTPA-BMA), Dotarem® (Gd-DOTA), and Multihance® (Gd-BOPTA)] by plants was investigated in a model experiment using Lepidium sativum (cress plants). HILIC–ICP-MS was used for identification of different contrast agents, and a first approach for quantification using aqueous standard solutions was tested. For speciation analysis, all investigated contrast agents could be extracted from the plant tissues with a recovery of about 54 % for Multihance® (Gd-BOPTA) up to 106 % for Gadovist® (Gd-BT-DO3A). These experiments demonstrate that all contrast agents investigated are transported from the roots to the leaves where the highest content was measured. KW - Gadolinium-based contrast agents KW - Hydrophilic interaction chromatography (HILIC) KW - Speciation KW - Inductively coupled plasma mass spectrometry (ICP-MS) KW - Plants KW - Surface water PY - 2013 U6 - https://doi.org/10.1007/s00216-012-6643-x SN - 1618-2642 SN - 1618-2650 VL - 405 IS - 6 SP - 1865 EP - 1873 PB - Springer CY - Berlin AN - OPUS4-27929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gopala, Anil A1 - Mahn, S. A1 - Panne, Ulrich A1 - Kipphardt, Heinrich T1 - In situ vacuum thermal mass spectroscopy for the selection of an environmentally friendly, energy saving catalytic additive and optimization of the process by a novel ignition mechanism N2 - We report herein the utilization of vacuum thermal mass spectrometry (VTMS) for the selection of an environmentally friendly, energy saving catalytic additive and a novel ignition mechanism, which is complementary to catalysis for the reduction of zinc oxide with carbon. PY - 2013 U6 - https://doi.org/10.1039/c3ra40223a SN - 2046-2069 VL - 3 IS - 25 SP - 9677 EP - 9680 PB - RSC Publishing CY - London AN - OPUS4-28659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhu, Shengchao A1 - Panne, Ulrich A1 - Rurack, Knut T1 - A rapid method for the assessment of the surface group density of carboxylic acid-functionalized polystyrene microparticles N2 - Particle-based assays are becoming versatile analytical tools due to their cost-effectiveness, speed, straightforward and diverse functionalization chemistries, especially when polystyrene particles are used. The introduction of functional groups (–COOH, –NH2, etc.) to the surface of such polystyrene particles promotes their application in bioanalytics. However, the traditional method to determine the amount of surface carboxylate groups is conductivity titration, which is usually time- and resources-consuming and discontinuous. Here, we synthesized polystyrene microparticles with different contents of carboxylate groups, and then investigated a simpler and potentially continuous approach to determine the amount of surface carboxylate groups by Zeta potential measurements. The results were compared to the traditional titration method and to actual coupling efficiencies of the functionalized particles with a model oligonucleotide probe as determined by flow cytometry. All quantification methods revealed good agreement. KW - Konduktometrische Titration KW - Mikropartikel KW - Oberflächenfunktionalisierung KW - Polystyrol KW - Zeta-Potential PY - 2013 U6 - https://doi.org/10.1039/c3an36578f SN - 0003-2654 SN - 1364-5528 VL - 138 IS - 10 SP - 2924 EP - 2930 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-28660 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 U6 - 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 - Carvalho, José Joao A1 - Walter, Astrid A1 - Baermann, Yvonne A1 - Weller, Michael G. A1 - Panne, Ulrich A1 - Schenk, J.A. A1 - Schneider, Rudolf T1 - Non-invasive monitoring of immunization progress in mice via IgG from feces N2 - A non-invasive method to monitor the humoral immune response in mice after immunization is described. From fecal pellets of an individual mouse, a sufficient amount of active immunoglobulins or their fragments can be extracted to perform a regular examination of the status of the immune response by immunoassay. Hapten-specific antibodies from the feces of mice from three immunization trials showed very similar characteristics to those obtained from serum at a given date. Therefore, it can be suspected that some serum IgG enters the intestinal lumen and ends up in the feces, where they appear to be considerably stable. Hapten-specific IgAs were not found in the feces. Being able to analyze antibody titers in feces could be an interesting animal welfare refinement to standard practice that does not entail repeated blood sampling. KW - Immunization monitoring KW - IgG KW - Coproantibodies KW - Feces KW - Animal welfare KW - 3R concept PY - 2012 UR - http://iv.iiarjournals.org/content/26/1/63.full.pdf+html SN - 0258-851x VL - 26 IS - 1 SP - 63 EP - 70 PB - In vivo CY - Athens AN - OPUS4-25283 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 U6 - 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 - Merk, Sven A1 - Shabanov, Sergej V. A1 - Gornushkin, Igor B. A1 - Panne, Ulrich T1 - Laser-induced plasma tomography by the Radon transform 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 U6 - 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 - Gusarova, Tamara A1 - Methven, B. A1 - Kipphardt, Heinrich A1 - Sturgeon, R. A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Calibration of double focusing glow discharge mass spectrometry instruments with pin-shaped synthetic standards N2 - Calibration of two commercially available glow discharge double focusing mass spectrometers, the VG 9000 and Element GD, is described using synthetic pin standards pressed from solution doped copper and zinc matrices. A special pressing die was developed for this purpose and optimal results were obtained with the highest possible pressures, i.e., 95 kN·cm- 2. This calibration approach permits the determination of trace element mass fractions down to µg·kg- 1 with small uncertainties and additionally provides traceability of the GD-MS results in the most direct manner to the SI (International System of Units). Results were validated by concurrent measurements of a number of compact copper and zinc certified reference materials. The impact of the sample pin cross-section (circular or square) was investigated with the use of a new pin-sample holder system for the Element GD. The pin-sample holder was designed by the manufacturer for pin-samples having circular cross-section; however, samples with square pin cross-section were also shown to provide acceptable results. Relative Sensitivity Factors for some 50 analytes in copper (VG 9000, Element GD) and zinc matrices (VG 9000) are presented. The field of applicability of GD-MS may be considerably extended via analysis of pin geometry samples based on their ease of preparation, especially with respect to the accuracy and traceability of the results and the enhanced number of analytes which can be reliably calibrated using such samples. KW - Glow discharge KW - Pin sample KW - Calibration PY - 2011 U6 - https://doi.org/10.1016/j.sab.2011.12.001 SN - 0584-8547 SN - 0038-6987 VL - 66 IS - 11-12 SP - 847 EP - 854 PB - Elsevier CY - Amsterdam AN - OPUS4-25346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Giesen, Charlotte A1 - Müller, Larissa A1 - Mairinger, T. A1 - Drescher, Daniela A1 - Kneipp, Janina A1 - Roos, P.H. A1 - Panne, Ulrich A1 - Jakubowski, Norbert T1 - Iodine as an elemental marker for imaging of single cells and tissue sections by laser ablation inductively coupled plasma mass spectrometry N2 - A new laser ablation (LA)-ICP-MS method for single cell and cell nucleus imaging was developed. Therein, iodine was employed as an elemental dye for fibroblast cells and for thin tissue sections. At an incubation time of 60 s, iodine is located mainly within the cell nuclei. This effect was illustrated in fibroblast cells, and iodine signal within the cell nucleus was as high as 5 × 104 cps at 4 µm laser spot size. The surrounding cytoplasm was iodinated as well, but to a lesser extent. The spatial resolution attained was sufficient to detect even smaller cell nuclei within a liver biopsy tissue. Furthermore, iodine was successfully employed for biomolecule labeling and we demonstrated that iodine signal increased with increasing thickness of a palatine tonsil tissue. Thus, the use of iodine as an internal standard to correct for tissue inhomogeneities in LA-ICP-MS was investigated for the simultaneous detection of two tumor markers (Her 2 and CK 7) in breast cancer tissue. Additionally, lanthanide background resulting from glass ablation can be corrected for by Eu standardization. PY - 2011 U6 - https://doi.org/10.1039/c1ja10227c SN - 0267-9477 SN - 1364-5544 N1 - Geburtsname von Müller, Larissa: Wäntig, L. - Birth name of Müller, Larissa: Wäntig, L. VL - 26 IS - 11 SP - 2160 EP - 2165 PB - Royal Society of Chemistry CY - London AN - OPUS4-24964 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 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 U6 - 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 - Giesen, Charlotte A1 - Mairinger, T. A1 - Khoury, L. A1 - Müller, Larissa A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Multiplexed immunohistochemical detection of tumor markers in breast cancer tissue using laser ablation inductively coupled plasma mass spectrometry N2 - We optimized multiplexed immunohistochemistry (IHC) on breast cancer tissue. Up to 20 tumor markers are routinely evaluated for one patient, and thus, a common analysis results in a series of time consuming staining procedures. As an alternative, we used lanthanides for labeling of primary antibodies, which are applied in IHC. Laser ablation (LA) ICPMS was elaborated as a detection tool for multiplexed IHC of tissue sections. In this study, we optimized sample preparation steps and LA ICPMS parameters to achieve a sufficient signal-to-background ratio. The results prove the high selectivity of applied antibodies, which was sustained after labeling. Up to three tumor markers (Her 2, CK 7, and MUC 1) were detected simultaneously in a single multiplex analysis of a 5 µm thin breast cancer tissue at a laser spot size of 200 µm. Furthermore, the LA ICPMS results indicate a significantly higher expression level of MUC 1 compared to Her 2 and CK 7, which was not obvious from the conventionally stained tissue sections. PY - 2011 U6 - https://doi.org/10.1021/ac2016823 SN - 0003-2700 SN - 1520-6882 N1 - Geburtsname von Müller, Larissa: Wäntig, L. - Birth name of Müller, Larissa: Wäntig, L. VL - 83 IS - 21 SP - 8177 EP - 8183 PB - American Chemical Society CY - Washington, DC AN - OPUS4-24966 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Merk, Sven A1 - Demidov, Alexandr A1 - Panne, Ulrich A1 - Shabanov, Sergej V. A1 - Smith, B.W. A1 - Omenetto, N. T1 - Tomography of single and double pulse laser-induced plasma using Radon transform technique N2 - The Radon transform tomography is used for reconstruction of the emissivity distribution in single- (SP) and double-pulse (DP) laser induced plasmas in orthogonal geometry. The orthogonal DP plasma is intrinsically asymmetric and thus suitable for the Radon reconstruction. The DP plasma consists of two plasmas separated by a short time interval of ~ 1 µs. The first plasma is created in air near the surface of a Si wafer and is followed (pre-ablation mode) or preceded (post-ablation mode) by the second plasma induced on this surface. A spectrometer moves in a semi-circular path around the plasma keeping the plasma in the rotation center. The optical detection is arranged so that a thin plasma layer parallel to the target surface is monitored. The axial symmetry of the SP plasma is investigated by comparing data from the Abel inversion taken at different angles and Radon reconstruction. The multi-angle measurements are used to estimate errors of the Abel reconstruction due to asymmetries of the plasma. Time-resolved Radon reconstruction in white light is performed for the DP plasma in both pre- and post-ablation modes. In the former case, the effect of ablated aerosol on the formation of the air plasma is monitored. In the latter case, a formation of an asymmetric compression shock created by the target plasma inside the air plasma is visualized. This observation is supported by computer simulations. An interaction of the two plasmas is studied by spectrally resolved Radon reconstruction revealing a complex distribution of target and ambient species inside the plasma at all studied delay times. Overall, it is demonstrated that Radon-based tomography is an informative tool to study transient asymmetric laser induced plasmas. KW - Radon transform tomography of SP KW - DP laser induced plasma KW - LIBS KW - Orthogonal double pulse plasma PY - 2012 U6 - https://doi.org/10.1016/j.sab.2012.06.033 SN - 0584-8547 SN - 0038-6987 VL - 76 SP - 203 EP - 213 PB - Elsevier CY - Amsterdam AN - OPUS4-27438 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Drescher, Daniela A1 - Giesen, Charlotte A1 - Traub, Heike A1 - Panne, Ulrich A1 - Kneipp, Janina A1 - Jakubowski, Norbert T1 - Quantitative imaging of gold and silver nanoparticles in single eukaryotic cells by laser ablation ICP-MS N2 - Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was utilized for spatially resolved bioimaging of the distribution of silver and gold nanoparticles in individual fibroblast cells upon different incubation experiments. High spatial resolution was achieved by optimization of scan speed, ablation frequency, and laser energy. Nanoparticles are visualized with respect to cellular substructures and are found to accumulate in the perinuclear region with increasing incubation time. On the basis of matrix-matched calibration, we developed a method for quantification of the number of metal nanoparticles at the single-cell level. The results provide insight into nanoparticle/cell interactions and have implications for the development of analytical methods in tissue diagnostics and therapeutics. KW - Imaging KW - Cell KW - Nanoparticles KW - Laser ablation KW - ICP-MS PY - 2012 U6 - https://doi.org/10.1021/ac302639c SN - 0003-2700 SN - 1520-6882 VL - 84 IS - 22 SP - 9684 EP - 9688 PB - American Chemical Society CY - Washington, DC AN - OPUS4-27440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schenk, Jonas A1 - Panne, Ulrich A1 - Buurman, Merwe T1 - Interaction of levitated ionic liquid droplets with water N2 - The influence of a humid or dry atmosphere on acoustically levitated ionic liquid droplets was studied by volumetric analysis and vibrational spectroscopy. Imidazolium-based ionic liquids with two types of anions, fluorinated (BF4 and PF6) and alkylsulfate anions, were investigated. The amount of absorbed water was correlated with structural differences of the ionic liquids and analyzed in terms of equilibrium mole fraction as well as absorption rate. The type of anion had the most significant influence on the amount of adsorbed water from the atmosphere. Furthermore, spectral changes in the in situ Raman spectra due to absorbed water were studied for all investigated ionic liquids. For 1-ethyl-3-methylimidazolium ethylsulfate, an exemplary detailed analysis of the intermolecular interactions between cations, anions and water was carried out based on the spectroscopic data. The observed band shifts were explained with a hydrogen bond between the anion and water. KW - Ionic liquids KW - Levitated droplets KW - Raman spectroscopy PY - 2012 U6 - https://doi.org/10.1021/jp309661p SN - 1520-6106 SN - 1520-5207 SN - 1089-5647 N1 - Geburtsname von Buurman, Merwe: Albrecht, M. - Birth name of Buurman, Merwe: Albrecht, M. VL - 116 IS - 48 SP - 14171 EP - 14177 PB - Soc. CY - Washington, DC AN - OPUS4-27427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stindt, Arne A1 - Buurman, Merwe A1 - Panne, Ulrich A1 - Riedel, Jens T1 - CO2 laser ionization of acoustically levitated droplets N2 - For many analytical purposes, direct laser ionization of liquids is desirable. Several studies on supported droplets, free liquid jets, and ballistically dispensed microdroplets have been conducted, yet detailed knowledge of the underlying mechanistics in ion formation is still missing. This contribution introduces a simple combination of IR-MALDI mass spectrometry and an acoustical levitation device for contactless confinement of the liquid sample. The homebuilt ultrasonic levitator supports droplets of several millimeters in diameter. These droplets are vaporized by a carbon dioxide laser in the vicinity of the atmospheric pressure interface of a time of flight mass spectrometer. The evaporation process is studied by high repetition rate shadowgraphy experiments elucidating the ballistic evaporation of the sample and revealing strong confinement of the vapor by the ultrasonic field of the trap. Finally, typical mass spectra for pure glycerol/water matrix and lysine as an analyte are presented with and without the addition of trifluoracetic acid, and the ionization mechanism is briefly discussed. The technique is a promising candidate for a reproducible mass spectrometric detection scheme for the field of microfluidics. KW - Ambient mass spectrometry KW - Levitated droplets KW - IR-MALDI PY - 2012 UR - http://link.springer.com/content/pdf/10.1007%2Fs00216-012-6500-y U6 - https://doi.org/10.1007/s00216-012-6500-y SN - 1618-2642 SN - 1618-2650 N1 - Geburtsname von Buurman, Merwe: Albrecht, M. - Birth name of Buurman, Merwe: Albrecht, M. SP - 1 EP - 6(?) PB - Springer CY - Berlin AN - OPUS4-27429 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Giesen, C. A1 - Müller, Larissa A1 - Panne, Ulrich A1 - Jakubowski, Norbert T1 - History of inductively coupled plasma mass spectrometry-based immunoassays N2 - The analysis of biomolecules requires highly sensitive and selective detection methods capable of tolerating a complex, biological matrix. First applications of biomolecule detection by ICP-MS relied on the use of heteroelements as a label for quantification. However, the combination of immunoassays and ICP-MS facilitates multiparametric analyses through elemental tagging, and provides a powerful alternative to common bioanalytical methods. This approach extends the detection of biomarkers in clinical diagnosis, and has the potential to provide a deeper understanding of the investigated biological system. The results might lead to the detection of diseases at an early stage, or guide treatment plans. Immunoassays are well accepted and established for diagnostic purposes, albeit ICP-MS is scarcely applied for the detection of immune-based assays. However, the screening of biomarkers demands high throughput and multiplex/multiparametric techniques, considering the variety of analytes to be queried. Finally, quantitative information on the expression level of biomarkers is highly desirable to identify abnormalities in a given organism. Thus, it is the aim of this review to introduce the fundamentals, and to discuss the enormous strength of ICP-MS for the detection of different immunoassays on the basis of selected applications, with a special focus on LA-ICP-MS. KW - ICP-MS KW - LA-ICP-MS KW - Immunoassay KW - Elemental tagging KW - Multiplexing PY - 2012 U6 - https://doi.org/10.1016/j.sab.2012.06.009 SN - 0584-8547 SN - 0038-6987 N1 - Geburtsname von Müller, Larissa: Wäntig, L. - Birth name of Müller, Larissa: Wäntig, L. VL - 76 SP - 27 EP - 39 PB - Elsevier CY - Amsterdam AN - OPUS4-27686 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sarfraz, Adnan A1 - Simo, A. A1 - Fenger, R. A1 - Christen, W. A1 - Rademann, K. A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Morphological diversity of caffeine on surfaces: needles and hexagons N2 - A systematic crystal morphology study on the pharmaceutical model compound caffeine has been conducted on different surfaces: silicon, silver, soda lime glass, and silver subsurface ion-exchanged soda-lime silicate (SIMO) glasses. The morphology of the solid caffeine deposits has been investigated using environmental scanning electron microscopy (ESEM), atomic force microscopy (AFM), and X-ray diffraction (XRD). Needle-shaped caffeine crystals have been observed by drop-casting and also by applying the rapid expansion of supercritical solutions (RESS) technique using supercritical carbon dioxide. The aspect ratio of the crystalline needles typically vary between 10 and 100, but have been observed as large as 500. The XRD data of the RESS products indicate unambiguously the presence of the thermodynamically most stable polymorph of caffeine known as the β-form. Under defined conditions we observe a unique, surface-mediated morphology for caffeine crystals with nearly perfect hexagonal shape. The relative fraction of the hexagons was seen to strongly increase especially when SIMO glasses were used. These hexagons have a distinct upper size limit depending on the solvent and substrate being used. The size distribution analysis of the hexagons yielded an average perimeter of typically 10 µm. The mechanism of the formation process of this new hexagonal motif is explained in terms of the spinodal dewetting of the thin film of caffeine solution on the surface. KW - Caffeine KW - Silicon KW - Silver KW - Ion exchanged soda lime silicate glass KW - ESEM KW - AFM KW - X-ray diffraction KW - RESS KW - Carbon dioxide KW - Supercritical fluids PY - 2012 U6 - https://doi.org/10.1021/cg101358q SN - 1528-7483 VL - 12 IS - 2 SP - 583 EP - 588 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-25457 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Wenzel, Klaus-Jürgen A1 - Sarfraz, Adnan A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - A wall-free climate unit for acoustic levitators N2 - Acoustic levitation represents the physical background of trapping a sample in a standing acoustic wave with no contact to the wave generating device. For the last three decades, sample holders based on this effect have been commonly used for contact free handling of samples coupled with a number of analytical techniques. In this study, a wall-free climate unit is presented, which allows the control of the environmental conditions of suspended samples. The insulation is based on a continuous cold/hot gas flow around the sample and thus does not require any additional isolation material. This provides a direct access to the levitated sample and circumvents any influence of the climate unit material to the running analyses. KW - Acoustic levition PY - 2012 U6 - https://doi.org/10.1063/1.4705968 SN - 0034-6748 SN - 1089-7623 VL - 83 IS - 5 SP - 055101-1 - 055101-3 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-25881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Sarfraz, Adnan A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - First seconds in a building's life - In situ synchrotron X-ray diffraction study of cement hydration on the millisecond timescale N2 - Setting cement: Highly dynamic hydration processes that occur during the first seconds of cement hydration were studied by time-resolved synchrotron X-ray diffraction. Polycarboxylate ether additives were found to influence the formation of the initial crystalline hydration products on a molecular level. KW - Cement hydration KW - Colloidal suspensions KW - In situ analysis KW - X-ray diffraction KW - SyXRD KW - High resolution KW - In-situ PY - 2012 U6 - https://doi.org/10.1002/anie.201200993 SN - 1433-7851 SN - 1521-3773 SN - 0570-0833 VL - 51 IS - 20 SP - 4993 EP - 4996 PB - Wiley-VCH CY - Weinheim AN - OPUS4-26287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, Vanessa A1 - Panne, Ulrich A1 - Hodoroaba, Vasile-Dan T1 - Calculation of X-ray tube spectra by means of photon generation yields and a modified Kramers background for side-window X-ray tubes N2 - Popular X-ray tube models available in the literature, i.e. 'Pella', 'Ebel', and 'Finkelshtein and Pavlova', are systematically evaluated with the focus on the estimation of the associated uncertainties. Also taken in consideration and compared is our recent semi-empirical own approach already employed in our lab. This has been working for the common target elements rhodium, molybdenum and tungsten and was further extended in the present work for the target elements copper, chromium and vanadium. By using a modern scanning electron microscope/energy dispersive spectroscopy (SEM/EDS) system this time, higher performances such as stability of the beam current and especially the better energy resolution of the EDS have enabled the reliable extension of our own X-ray tube spectrum approach into the low-energy range, due to increasing interest. Hence, also the more challenging X-ray lines of copper, chromium and vanadium L-series lying in the energy range below 1–2?keV are included into the model. Such low-energy L-lines or, e.g. M-lines of tungsten, are not treated explicitly by the other existing popular algorithms for the nowadays widely used geometries of side-window tubes, offering a unique virtue to our present, modern approach. With our own model, a measurement uncertainty of the X-ray tube spectra (considering the uncertainties associated with the SEM beam current, the detector acceptance solid angle and efficiency of the spectrometer) within 15% has been estimated. The validation of the approach is demonstrated with metrological measurements with a calibrated SEM/EDS system geometrically configured as a side-window X-ray tube. KW - X-ray tube spectra KW - Side-window X-ray tube KW - Reference-free XRF KW - Photon generation yield KW - Kramers background KW - Calibrated SEM/EDS PY - 2012 U6 - https://doi.org/10.1002/xrs.2391 SN - 0049-8246 VL - 41 IS - 4 SP - 264 EP - 272 PB - Wiley CY - Chichester AN - OPUS4-26239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ivleva, N.P. A1 - Niessner, R. A1 - Panne, Ulrich T1 - Characterization and discrimination of pollen by Raman microscopy N2 - The chemical characterization and discrimination of allergy-relevant pollen (common ragweed (Ambrosia artemisiifolia), white birch (Betula pendula), English oak (Quercus robur), and European linden (Tilia cordata)) has been studied by Raman microscopy. Spectra were obtained at different excitation wavelengths (514, 633, and 780 nm) and various methods were examined to minimize the strong fluorescence background. The use of a He–Ne laser (633 nm) for excitation yields high-quality single pollen Raman spectra, which contain multiple bands due to pollen components such as carotenoids, proteins, nucleic acids, carbohydrates, and lipids. Multivariate classification, i.e. principal component analysis (PCA) and hierarchical cluster analysis, demonstrated the validity of the approach for discrimination between different pollen species. KW - Raman spectroscopy KW - Pollen KW - Multivariate classification PY - 2005 U6 - https://doi.org/10.1007/s00216-004-2942-1 SN - 1618-2642 SN - 1618-2650 VL - 381 IS - 1 SP - 261 EP - 267 PB - Springer CY - Berlin AN - OPUS4-7185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prestel, H. A1 - Schott, L. A1 - Niessner, R. A1 - Panne, Ulrich T1 - Characterization of sewage plant hydrocolloids using asymmetrical flow field-flow fractionation and ICP-mass spectrometry N2 - Asymmetrical flow field-flow fractionation (AF4) was applied to characterize aquatic colloids from biological sewage plants and to infer information of colloidal loads, sources, and sinks within the plants, resp. the colloidal interaction with the aqueous phase and the sewage sludge. To characterize the colloids further, especially the distributions of colloid associated heavy metals, the AF4 system was coupled to an inductively coupled plasma mass spectrometer (ICP-MS). The size distribution is determined by AF4 with UV absorbance and fluorescence detection after a calibration by monodisperse polystyrene sulfonate standards (PSS). Samples from different sewage plants and from different depths and locations within a plant were compared. The fulvic/humic acid fraction with a particle diameter dp < 10 nm appeared to be comparable in all samples and decreases only slightly along the plants, whereas larger colloids with dp > 10 nm almost completely passed into the sewage sludge. The concentrations of the initial colloidal heavy metals decreased along the plants. KW - Humic colloids KW - Biological sewage plants KW - Asymmetrical flow field-flow fractionation (AF4) KW - Inductively coupled plasma mass spectrometry (ICP-MS) PY - 2005 SN - 0043-1354 VL - 39 IS - 15 SP - 3541 EP - 3552 PB - Elsevier CY - Amsterdam AN - OPUS4-10887 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Metrology in chemistry - a rocky road N2 - The application of metrology in chemical analysis is today hampered by psychological and practical barriers. The argumentation is based on the differences in physical and chemical metrology, which arises mainly from the objects of the measurements. The term “measurement” is discussed in the realm of analytical chemistry with a special focus on the inherent relation between chemical identification and determination as well as the consequent use of the concept of traceability and uncertainty. KW - Metrology in chemistry KW - Chemical analysis KW - Traceability KW - Uncertainty PY - 2008 U6 - https://doi.org/10.1007/s00604-007-0909-6 SN - 0026-3672 SN - 1436-5073 VL - 162 IS - 1-2 SP - 35 EP - 41 PB - Springer CY - Wien AN - OPUS4-17727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulte, Franziska A1 - Brzezinka, K.-W. A1 - Lutzenberger, K. A1 - Stege, H. A1 - Panne, Ulrich T1 - Raman spectroscopy of synthetic organic pigments used in 20th century works of art N2 - Raman microscopy allows a non-destructive characterisation of inorganic and organic painting materials such as pigments and organic dyestuffs. The objectives of this study are the more recent organic pigments typically present in paintings and other art works from the 20th century. More than 20 organic synthetic pigments from different chemical classes could be identified by Raman spectroscopy using different excitation wavelengths (457.9, 476.5, 487.9, 514.5, 632.8, and 1064 nm). To evaluate the performance for real paint samples, varying paint mixtures of the Hansa Yellow pigment PY 3 and the binding medium Mowilith, a polyvinyl acetate (PVAC) compound, were characterised; PY 3 was determined at a 1 wt% level in the binder. In addition, commercial tube paints containing the quinacridone violet PV 19 were studied. The pigment was clearly identified in all of these more complex oil and acrylic paints. Finally, alizarin (PR 83) and a green copper phthalocyanine pigment (PG 7) could unambiguously be identified by Raman microscopy in the painting Woman with mandolin in yellow and red of Max Beckmann dating 1950. The discovery of a red naphthol AS pigment by Raman spectroscopy in a sample from the Three field workers by Georg Baselitz (1964/1965) demonstrated that in some cases complementary chromatographic methods are needed for a comprehensive identification of the organic pigments. KW - Raman microscopy KW - FT-Raman spectroscopy KW - Synthetic organic pigments KW - Modern art PY - 2008 U6 - https://doi.org/10.1002/jrs.2021 SN - 0377-0486 SN - 1097-4555 VL - 39 IS - 10 SP - 1455 EP - 1463 PB - Wiley CY - Chichester AN - OPUS4-18401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Maike A1 - Gornushkin, Igor B. A1 - Florek, S. A1 - Mory, D. A1 - Panne, Ulrich T1 - Approach to Detection in Laser-Induced Breakdown Spectroscopy N2 - Gated detection with intensified detectors, e.g., ICCDs, is today the accepted approach for detection of plasma emission in laser-induced breakdown spectroscopy (LIBS). However, these systems are more cost-intensive and less robust than nonintensified CCDs. The objective of this paper is to compare, both theoretically and experimentally, the performance of an intensified (ICCD) and nonintensified (CCD) detectors for detection of plasma emission in LIBS. The CCD is used in combination with a mechanical chopper, which blocks the early continuum radiation from the plasma. The detectors are attached sequentially to an echelle spectrometer under the same experimental conditions. The laser plasma is induced on a series of steel samples under atmospheric conditions. Our results indicate that there is no substantial difference in the performance of the CCD and ICCD. Signal-to-noise ratios and limits of detection achieved with the CCD for Si, Ni, Cr, Mo, Cu, and V in steel are comparable or even better than those obtained with the ICCD. This result is further confirmed by simulation of the plasma emission signal and the corresponding response of the detectors in the limit of quantum (photon) noise. KW - LIBS KW - Detektorvergleich KW - ICCD CCD PY - 2007 U6 - https://doi.org/10.1021/ac0621470 SN - 0003-2700 SN - 1520-6882 VL - 79 IS - 12 SP - 4419 EP - 4426 PB - American Chemical Society CY - Washington, DC AN - OPUS4-15044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tognoni, E. A1 - Cristoforetti, G. A1 - Legnaioli, S. A1 - Palleschi, V. A1 - Salvetti, A. A1 - Müller, Maike A1 - Panne, Ulrich A1 - Gomushkin, I. T1 - A numerical study of expected accuracy and precision in Calibration-Free Laser-Induced Breakdown Spectroscopy in the assumption of ideal analytical plasma N2 - Calibration-Free Laser-Induced Breakdown Spectroscopy (CF-LIBS) has been proposed several years ago as an approach for quantitative analysis of Laser-Induced Breakdown Spectroscopy spectra. Recently developed refinement of the spectral processing method is described in the present work. Accurate quantitative results have been demonstrated for several metallic alloys. However, the degree of accuracy that can be achieved with Calibration-Free Laser-Induced Breakdown Spectroscopy analysis of generic samples still needs to be thoroughly investigated. The authors have undertaken a systematic study of errors and biasing factors affecting the calculation in the Calibration-Free Laser-Induced Breakdown Spectroscopy spectra processing. These factors may be classified in three main groups: 1) experimental aberrations (intensity fluctuations and inaccuracy in the correction for spectral efficiency of a detection system), 2) inaccuracy in theoretical parameters used for calculations (Stark broadening coefficients and partition functions) and 3) plasma non-ideality (departure from thermal equilibrium, spatial and temporal inhomogeneities, optical thickness, etc.). In this study, the effects of experimental aberrations and accuracy of spectral data were investigated, assuming that the analytical plasma is ideal. Departure of the plasma conditions from ideality will be the object of future work. The current study was based on numerical simulation. Two kinds of metallic alloys, iron-based and aluminum-based, were studied. The relative weight of the error contributions was found to depend on the sample composition. For the here-investigated samples, the experimental aberrations contribute to the overall uncertainty on the quantitative results more than theoretical parameters. The described simulation method can be applied to the Calibration-Free Laser-Induced Breakdown Spectroscopy analysis of any other kind of sample. KW - LIBS KW - Quantitative analysis KW - Standard-less analysis KW - Accuracy KW - Precision PY - 2007 U6 - https://doi.org/10.1016/j.sab.2007.10.005 SN - 0584-8547 SN - 0038-6987 VL - 62 IS - 12 SP - 1287 EP - 1302 PB - Elsevier CY - Amsterdam AN - OPUS4-16566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, Britta A1 - Recknagel, Sebastian A1 - Czerwensky, Michael A1 - Matschat, Ralf A1 - Michaelis, Matthias A1 - Peplinski, Burkhard A1 - Panne, Ulrich T1 - Analysis of pure copper - a comparison of analytical mehods KW - Pure copper KW - Elemental analytical mehtods KW - Reference material KW - Sample dissolution PY - 2008 U6 - https://doi.org/10.1007/s00604-007-0849-1 SN - 0026-3672 SN - 1436-5073 VL - 160 SP - 97 EP - 107 PB - Springer CY - Wien AN - OPUS4-17565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bremser, Wolfram A1 - Becker, Roland A1 - Kipphardt, Heinrich A1 - Lehnik-Habrink, Petra A1 - Panne, Ulrich A1 - Töpfer, Antje T1 - Stability testing in an integrated scheme N2 - ISO Guide 35 deals with RM stability issues and scrutinizes the evaluation of stability testing results under the assumption that either there is no trend at all (a rather rare situation), or any observed deterministic change is insignificant and thus can be neglected. However, market demands for reliable reference materials are obviously not limited to stable or at least seemingly stable materials. In many analytical applications, analytes and measurands under consideration are known, or at least suspected, to be unstable on time scales that may vary widely from measurand to measurand. The Federal Institute for Materials Research and Testing (BAM) has developed (and successfully uses) an integrated approach in its certification practice. The approach is based on an initial stability study and subsequent post-certification monitoring. Data evaluation is model-based and takes advantage of all information collected in the stability testing scheme(s). It thus allows one to deal with any kind of instability observed, to assess limiting time intervals at any stress condition in the range tested, to estimate a final expiry date for materials with detected instabilities or the maximum admissible re-testing interval for seemingly stable materials, and to assess maximum admissible stress loads during delivery of the material to the customer. The article describes (and exemplifies) typical study layout, the model selection, and the integrated data assessment. KW - Certified reference materials KW - Stability KW - Shelf life KW - Arrhenius model KW - ERM PY - 2006 U6 - https://doi.org/10.1007/s00769-006-0152-6 SN - 0949-1775 SN - 1432-0517 VL - 11 IS - 10 SP - 489 EP - 495 PB - Springer CY - Berlin AN - OPUS4-14063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leiterer, Jork A1 - Grabolle, Markus A1 - Rurack, Knut A1 - Resch-Genger, Ute A1 - Ziegler, J. A1 - Nann, T. A1 - Panne, Ulrich T1 - Acoustically Levitated Droplets - A Contactless Sampling Method for Fluorescence Studies N2 - Acoustic levitation is used as a newtool to study concentration-dependent processes influorescence spectroscopy. With this technique, small amounts of liquid and solid samples can be measured without the need for sample supports or containers, which often limits signal acquisition and can even alter sample properties due to interactions with the support material. We demonstrate that, because of the small sample volume, fluorescence measurements at high concentrations of an organic dye are possible without the limitation of inner-filter effects, which hamper such experiments in conventional, cuvette-based measurements. Furthermore, we show that acoustic levitation of liquid samples provides an experimentally simple way to study distance-dependent fluorescence modulations in semiconductor nanocrystals. The evaporation of the solvent during levitation leads to a continuous increase of solute concentration and can easily be monitored by laser-induced fluorescence. KW - Acoustic levitation KW - Dyes KW - Energy transfer KW - Fluorescence KW - Quantum dots KW - Nanocrystals KW - Ultrasonic trap PY - 2008 U6 - https://doi.org/10.1196/annals.1430.039 SN - 0077-8923 SN - 1749-6632 SN - 0094-8500 VL - 1130 SP - 78 EP - 84 PB - New York Academy of Sciences CY - New York, NY AN - OPUS4-17658 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leiterer, Jork A1 - Emmerling, Franziska A1 - Panne, Ulrich A1 - Christen, W. A1 - Rademann, K. T1 - Tracing Coffee Tabletop Traces N2 - Crystallization processes under different conditions are of fundamental interest in chemistry, pharmacy, and medicine. Therefore, we have studied the formation of micro- and nanosized crystals using water-caffeine (1,3,7-trimethyl-1H-purine-2,6(3H,7H)-dione) solutions under ambient conditions as a relevant model system. When droplets of an aqueous caffeine solution evaporate and eventually dry on surfaces (glass, polystyrene, and polyester), stable “coffee tabletop” rings with a perimeter of typically 3 mm are formed after 20 to 50 min. Using a micro focus X-ray beam available at the BESSY µSpot-beamline, the fine structure of different caffeine needles can be distinguished. Unexpectedly, both crystal modifications (α- and β-caffeine) are present, but locally separated in these rings. Furthermore, AFM studies reveal the presence of even smaller particles on a nanometer length scale. To eliminate influences of surface irregularities from the crystallization process, acoustic levitation of liquid samples was employed. Such levitated droplets are trapped in a stable position and only surrounded by air. The solvent in an ultrasonically levitated drop evaporates completely, and the resulting crystallization of caffeine was followed in situ by synchrotron X-ray diffraction. In this case, the diffraction pattern is in accordance with pure α-caffeine and does not indicate the formation of the room temperature polymorph β-caffeine. Hence, our investigations open new vistas that may lead to a controlled formation of cocrystals and novel polymorphs of micro- and nanocrystalline materials, which are of relevance for fundamental studies as well as for pharmaceutical and medical applications. KW - Polymorphism KW - Crystallization KW - Acoustic levitation KW - Evaporation of droplets KW - µSpot KW - Micro spot KW - Synchrotron radiation PY - 2008 U6 - https://doi.org/10.1021/la800768v SN - 0743-7463 SN - 1520-5827 VL - 24 IS - 15 SP - 7970 EP - 7978 PB - American Chemical Society CY - Washington, DC AN - OPUS4-17818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eichelbaum, M. A1 - Kneipp, Janina A1 - Schmidt, B.E. A1 - Panne, Ulrich A1 - Rademann, K. T1 - SERS and Multiphoton-Induced Luminescence of Gold Micro- and Nanostructures Fabricated by NIR Femtosecond-Laser Irradiation KW - Gold KW - Luminescence KW - Multiphoton fabrication KW - Sol-gel processes KW - Surface-enhanced Raman scattering PY - 2008 U6 - https://doi.org/10.1002/cphc.200800417 SN - 1439-4235 SN - 1439-7641 VL - 9 IS - 15 SP - 2163 EP - 2167 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-18233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulte, Franziska A1 - Lingott, J. A1 - Panne, Ulrich A1 - Kneipp, Janina T1 - Chemical characterization and classification of Pollen N2 - We report on the in situ characterization of tree pollen molecular composition based on Raman spectroscopy. Different from purification-based analysis, the nondestructive approach allows (i) to analyze various classes of molecules simultaneously at microscopic resolution and (ii) to acquire fingerprint-like chemical information that was used for the classification of pollen from different species. Hierarchical cluster analysis of spectra from fresh pollen samples of 15 species partly related at the genus level and family level indicates separation of species based on the complete Raman spectral signature and yields classification in accord with biological systematics. The results have implications for the further elucidation of pollen biochemistry and also for the development of chemistry-based online pollen identification methods. PY - 2008 U6 - https://doi.org/10.1021/ac801791a SN - 0003-2700 SN - 1520-6882 SP - 1 EP - 12 PB - American Chemical Society CY - Washington, DC AN - OPUS4-18234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kneipp, Janina A1 - Li, X. A1 - Sherwood, M. A1 - Panne, Ulrich A1 - Kneipp, H. A1 - Stockman, M.I. A1 - Kneipp, K. T1 - Gold Nanolenses Generated by Laser Ablation-Efficient Enhancing Structure for Surface Enhanced Raman Scattering Analytics and Sensing N2 - Nanoaggregates formed by metal spheres of different radii and interparticle distances represent finite, deterministic, self-similar systems that efficiently concentrate optical fields and act as “nanolenses”. Here we verify experimentally the theoretical concept of nanolenses and explore their potential as enhancing nanostructures in surface enhanced Raman scattering (SERS). Self-similar structures formed by gold nanospheres of different sizes are generated by laser ablation from solid gold into water. These nanolenses exhibit SERS enhancement factors on the order of 109. The “chemically clean” preparation process provides several advantages over chemically prepared nanoaggregates and makes the stable and biocompatible gold nanolenses potent enhancing structures for various analytical and sensing applications. KW - SERS KW - Ablation KW - Gold-Nanopartikel PY - 2008 U6 - https://doi.org/10.1021/ac8002215 SN - 0003-2700 SN - 1520-6882 VL - 80 IS - 11 SP - 4247 EP - 4251 PB - American Chemical Society CY - Washington, DC AN - OPUS4-18231 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, Vanessa A1 - Ostermann, Markus A1 - Panne, Ulrich A1 - Hodoroaba, Vasile-Dan T1 - Performance of mu-XRF with SEM/EDS for trace analysis on the example of RoHS relevant elements - measurement, optimisation and predivtion of the detection limits N2 - For ten years µ-XRF (micro-focus X-ray fluorescence) analysis has been performed with SEM/EDS (scanning electron microscope with an energy dispersive X-ray detector) so that non-destructive analysis of elements at trace level concentrations below 100 µg g-1 becomes possible. This can be considered as a valuable completion of the classical electron probe microanalysis by EDS, an analytical method 'suffering' from rather poor limits of detection in the range of one to two orders of magnitude higher than those of µ-XRF. Based on a representative actual application, namely analysis of RoHS relevant elements at trace concentration levels, the performance of the rather new analytical method with respect to its limits of detection is systematically evaluated. CRMs (certified reference materials) specially prepared to support the quantitative XRF analysis of RoHS relevant elements were employed. On the other side, based on calculations of µ-XRF spectra according to a recently developed physical model the optimization of the analytical performance is also successfully undertaken. KW - RoHS KW - XRF KW - muXRF KW - SEM/EDS KW - Detection limits KW - Trace elements KW - Modelling PY - 2013 U6 - https://doi.org/10.1039/c3ja50064k SN - 0267-9477 SN - 1364-5544 VL - 28 IS - 9 SP - 1466 EP - 1474 PB - Royal Society of Chemistry CY - London AN - OPUS4-29045 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Müller, Urs A1 - Malaga, Katarina A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Spatially resolved investigation of complex multi-phase systems using muXRF, SEM-EDX and high resolution SyXRD N2 - Spatially resolved analysis of complex multi-phase systems can be validated through different analytical methods. This study compares investigations by scanning electron microscopy coupled with energy dispersive X-ray fluorescence analysis and high resolution X-ray diffraction. The studied sulfate attacked cement paste containing fly ashes consists of different interacting crystalline and amorphous phases. The complementary methods revealed in detail changes in phase composition due to the chemical attack. The advantages and disadvantages of both methods are discussed and suggestions are given for combining them with additional methods to maximize the information content. KW - EDX-SEM KW - SyXRD KW - Spatial investigations KW - Comparison KW - High resolution KW - Cement paste KW - Sulfate attack KW - Damaging mechanism PY - 2013 U6 - https://doi.org/10.1016/j.cemconcomp.2012.08.018 SN - 0958-9465 SN - 1873-393X VL - 37 SP - 241 EP - 245 PB - Elsevier Ltd. CY - Barking, Essex AN - OPUS4-29111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, Vanessa A1 - Warrikhoff, A. A1 - Panne, Ulrich A1 - Hodoroaba, Vasile-Dan T1 - Determination of the efficiency of an energy dispersive X-ray spectrometer up to 50 keV with a SEM N2 - Both electron and polychromatic photon excitations (micro-focus X-ray source) at a scanning electron microscope (SEM) are used to determine the efficiency of an energy dispersive X-ray spectrometer up to 50 keV by means of a calibrated X-ray spectrometer and reference materials (RM) specially selected for this purpose. KW - Detector efficiency KW - Calibration KW - XRF KW - EDS KW - SEM KW - EDS-TM001 KW - Scattering PY - 2009 U6 - https://doi.org/10.1039/b907815k SN - 0267-9477 SN - 1364-5544 VL - 24 SP - 1034 EP - 1036 PB - Royal Society of Chemistry CY - London AN - OPUS4-19714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Höhse, Marek A1 - Mory, D. A1 - Florek, S. A1 - Weritz, Friederike A1 - Gornushkin, Igor B. A1 - Panne, Ulrich T1 - A combined laser-induced breakdown and Raman spectroscopy Echelle system for elemental and molecular microanalysis N2 - Raman and laser-induced breakdown spectroscopy is integrated into a single system for molecular and elemental microanalyses. Both analyses are performed on the same ~ 0.002 mm² sample spot allowing the assessment of sample heterogeneity on a micrometric scale through mapping and scanning. The core of the spectrometer system is a novel high resolution dual arm Echelle spectrograph utilized for both techniques. In contrast to scanning Raman spectroscopy systems, the Echelle-Raman spectrograph provides a high resolution spectrum in a broad spectral range of 200-6000 cm- 1 without moving the dispersive element. The system displays comparable or better sensitivity and spectral resolution in comparison to a state-of-the-art scanning Raman microscope and allows short analysis times for both Raman and laser induced breakdown spectroscopy. The laser-induced breakdown spectroscopy performance of the system is characterized by ppm detection limits, high spectral resolving power (15,000), and broad spectral range (290-945 nm). The capability of the system is demonstrated with the mapping of heterogeneous mineral samples and layer by layer analysis of pigments revealing the advantages of combining the techniques in a single unified set-up. KW - LIBS KW - Raman KW - Echelle KW - Laser-induced breakdown spectroscopy KW - Hyphenated technique PY - 2009 U6 - https://doi.org/10.1016/j.sab.2009.09.004 SN - 0584-8547 SN - 0038-6987 VL - 64 IS - 11-12 SP - 1219 EP - 1227 PB - Elsevier CY - Amsterdam AN - OPUS4-20493 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gopala, Anil A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Use of mass spectrometric detection as a versatile process monitoring tool: reduction patterns in a milled ZnO/Al mixture N2 - Mass spectrometric detection can play a prominent role in the assessment of different reactions occurring at varied temperatures in a milled ZnO/Al mixture. This is the first time that online mass spectrometric information was used as a tool for monitoring and understanding the chemical reduction process mechanism. We have observed four different types of reaction taking place: (1) distillation of Zn metal, (2) reduction of ZnO by activated Al, (3) melting of Al and finally (4) reduction of ZnO by inactivated Al. The experimental conditions and results observed by QMS were supported with literature data and physical measurement data from X-Ray Diffraction (XRD) which gave us an idea about the complex reaction cascade which occurred during the formation of the zinc metal. PY - 2010 U6 - https://doi.org/10.1039/c0ay00057d SN - 1759-9660 SN - 1759-9679 VL - 2 SP - 451 EP - 454 PB - RSC Publ. CY - Cambridge AN - OPUS4-21291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gusarova, Tamara A1 - Hofmann, T. A1 - Kipphardt, Heinrich A1 - Venzago, C. A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Comparison of different calibration strategies for the analysis of zinc and other pure metals by using the GD-MS instruments VG 9000 and element GD N2 - Synthetic pressed metal powder standards doped with standard solutions were used for the calibration of both commercially available high resolution GD-MS instruments Element GD and VG 9000 for zinc matrix. Different quantification procedures (IBR, Standard RSF, matrix matched RSF from the calibration with CRMs and use of doped synthetic standards) are compared using zinc matrix as an example, whereas the calibration with doped pellets turned out to be the best quantification technique for high-purity materials. The applicability of the Standard RSF concept is scrutinised. In this context, RSF values for several Matrices (Co, Cu, Fe, In and Zn) are reported additionally. PY - 2010 U6 - https://doi.org/10.1039/b921649a SN - 0267-9477 SN - 1364-5544 VL - 25 SP - 314 EP - 321 PB - Royal Society of Chemistry CY - London AN - OPUS4-22376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Giesen, Charlotte A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Weller, Michael G. T1 - Comparison of ICP-MS and photometric detection of an immunoassay for the determination of ochratoxin A in wine N2 - An immunoassay was developed for ochratoxin A (OTA) detection in wine and two completely different detection methods were compared: ICP-MS and photometry. For labelling, we applied secondary antibodies conjugated with gold nanoparticles for ICP-MS and with horseradish peroxidase for photometric detection, respectively. Detection limits of the assay were determined as 0.003 µg L-1 for both detection methods. OTA in wine was determined below the EU limit value of 2 µg kg-1. The measurement range was between 0.01 and 1 µg L-1 for ICP-MS and photometric detection. Assay precision detected by ICP-MS and photometry were similar showing that precision of the detection method has only a minor effect on total assay precision. By using BSA as a buffer additive to minimize nonspecific binding, we could also confirm that OTA strongly binds to BSA. In a comparison study of several additives, casein was found to be preferable. PY - 2010 U6 - https://doi.org/10.1039/c0ja00009d SN - 0267-9477 SN - 1364-5544 VL - 25 IS - 10 SP - 1567 EP - 1572 PB - Royal Society of Chemistry CY - London AN - OPUS4-22704 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 U6 - 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 - 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 U6 - 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 - 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 U6 - 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 - TY - JOUR A1 - Gornushkin, Igor B. A1 - Panne, Ulrich A1 - Winefordner, J. D. T1 - Linear correlation for identification of materials by laser induced breakdown spectroscopy: Improvement via spectral filtering and masking N2 - The purpose of this work is to improve the performance of a linear correlation method used for material identification in laser induced breakdown spectroscopy. The improved correlation procedure is proposed based on the selection and use of only essential spectral information and ignoring empty spectral fragments. The method is tested on glass samples of forensic interest. The 100% identification capability of the new method is demonstrated in contrast to the traditional approach where the identification rate falls below 100% for many samples. KW - Correlation analysis KW - Linear correlation KW - Material identification KW - Laser induced plasma KW - LIBS PY - 2009 U6 - https://doi.org/10.1016/j.sab.2009.07.038 SN - 0584-8547 SN - 0038-6987 VL - 64 IS - 10 SP - 1040 EP - 1047 PB - Elsevier CY - Amsterdam AN - OPUS4-20621 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chinthalapati, Siva Kesava Raju A1 - Cossmer, Antje A1 - Scharf, Holger A1 - Panne, Ulrich A1 - Lück, Detlef T1 - Speciation of gadolinium based MRI contrast agents in environmental water samples using hydrophilic interaction chromatography hyphenated with inductively coupled plasma mass spectrometry KW - HPLC-ICP-MS KW - HILIC chromatography KW - Speciation KW - Gadolinium KW - MRI contrast agent PY - 2010 U6 - https://doi.org/10.1039/b919959d SN - 0267-9477 SN - 1364-5544 VL - 25 SP - 55 EP - 61 PB - Royal Society of Chemistry CY - London AN - OPUS4-20705 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Development of SI traceable standards for element determination N2 - In Germany a system of primary amount of substance standards for elemental analysis is being developed, which forms the material´s basis for the National Standards for element determination. The metrological concept and technical approach is briefly described. The objective of traceability in chemistry, in this case for elemental determination, is illustrated on the example of copper. KW - Copper KW - Element determination KW - Metrology KW - Primary standards KW - Traceability PY - 2009 U6 - https://doi.org/10.2533/chimia.2009.637 SN - 0009-4293 VL - 63 IS - 10 SP - 637 EP - 639 PB - Schweizerische Chemische Gesellschaft CY - Basel AN - OPUS4-20727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bahlmann, Arnold A1 - Weller, Michael G. A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - Monitoring carbamazepine in surface and wastewaters by an immunoassay based on a monoclonal antibody N2 - The pharmaceutical compound carbamazepine (CBZ) is an emerging pollutant in the aquatic environment and may potentially be used as a wastewater marker. In this work, an enzyme-linked immunosorbent assay (ELISA) for the detection of carbamazepine in surface and sewage waters has been developed. The heterogeneous immunoassay is based on a commercially available monoclonal antibody and a novel enzyme conjugate (tracer) that links the hapten via a hydrophilic peptide (triglycine) spacer to horseradish peroxidase. The assay achieves a limit of detection of 24 ng/L and a quantitation range of 0.05-50 µg/L. The analytical performance and figure of merits were compared to liquid chromatography-tandem mass spectrometry after solid-phase extraction. For nine Berlin surface water samples and one wastewater sample, a close correlation of results was observed. A constant overestimation relative to the CBZ concentration of approximately 30% by ELISA is probably caused by the presence of 10,11-epoxy-CBZ and 2-hydroxy-CBZ in the samples. The ELISA displayed cross-reactivities for these compounds of 83% and 14%, respectively. In a first screening of 27 surface water samples, CBZ was detected in every sample with concentrations between 0.05 and 3.2 µg/L. Since no sample cleanup is required, the assay allowed for the determination of carbamazepine with high sensitivity at low costs and with much higher throughput than with conventional methods. KW - Carbamazepine KW - ELISA KW - Antibody KW - Immunoassay KW - Surface water KW - LC-MS/MS KW - Pharmaceuticals PY - 2009 U6 - https://doi.org/10.1007/s00216-009-2958-7 SN - 1618-2642 SN - 1618-2650 VL - 395 IS - 6 SP - 1809 EP - 1820 PB - Springer CY - Berlin AN - OPUS4-20927 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traub, Heike A1 - Czerwensky, Michael A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Panne, Ulrich T1 - Different calibration strategies for the analysis of pure copper metal by nanosecond laser ablation inductively coupled plasma mass spectrometry N2 - In this work, different calibration strategies for the determination of trace elements in pure copper metal by nanosecond laser ablation ICP-MS were investigated. In addition to certified reference materials (CRMs), pellets of doped copper powder were used for calibration. The micro homogeneity of the CRMs as well as the solution-doped pellets was sufficient to use them as calibration samples in combination with a laser spot size of 200 µm. In contrast, pellets doped with analytes in solid form showed a significant heterogeneity. For most of the investigated analytes and copper CRMs the measured mass fractions were within ± 20% of their certified values when other copper CRMs were used as calibration samples. When solution-doped powder pellets were used as calibration samples a systematic trend towards mass fractions below the certified values was observed for nearly all elements determined in the analysed CRMs. Thermal fractionation effects during the ablation of the solution-doped pellets were suspected as the extent of the fractionation depends on the irradiance, whereas fractionation is reduced at higher irradiance. PY - 2010 U6 - https://doi.org/10.1039/b915564c SN - 0267-9477 SN - 1364-5544 VL - 25 IS - 5 SP - 690 EP - 696 PB - Royal Society of Chemistry CY - London AN - OPUS4-21195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulte, Franziska A1 - Panne, Ulrich A1 - Kneipp, Janina T1 - Molecular changes during pollen germination can be monitored by Raman microspectroscopy N2 - The processes associated with pollen germination were studied in vitro for two tree species, Salix caprea and Fraxinus excelsior under different nutrient conditions. The results provide evidence of changes in chemical composition of the pollen grains during germination. From the comparison of spectra of the pollen grain body and the growing pollen tube, it can be concluded that there are major chemical differences between these two morphological units. Comparison of germinated and ungerminated pollen grains reveals alterations in the metabolism. Composition of the germinating pollen grain and its morphological units depends on the plant species, but also on the nutrient conditions. The results suggest species-specific utilization of metabolite storage, and potential alterations of the pollen outer coat. Furthermore, discharge of molecules into the nutrient medium may depend on the nutrient conditions in the germination experiments. This has implications for further experiments on dynamic processes in pollen and related plant materials. KW - Pollen germination KW - Raman microspectroscopy KW - Imaging KW - Coumaric acid KW - Pollen tube KW - Sporopollenin PY - 2010 U6 - https://doi.org/10.1002/jbio.201000031 SN - 1864-063X VL - 3 IS - 8-9 SP - 542 EP - 547 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-23211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Carvalho, José Joao A1 - Weller, Michael G. A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - Monitoring caffeine in human saliva using a newly developed ELISA N2 - Caffeine is a useful indicator to quickly assess liver function. High-throughput tests are needed for single-point caffeine measurements, with low cross-reactivity toward its major metabolite, paraxanthine. A newly developed ELISA was compared with an LC-MS/MS reference method, using 60 saliva samples from 10 individuals, before and after caffeine intake. Bland-Altman plot, Student t-test and F-test were used to compare the two methods. Proteins were precipitated using organic solvent and the caffeine recoveries compared with those obtained using sample microfiltration. The antibody, with a low cross-reactivity toward paraxanthine (0.08%), allows quantification of caffeine in saliva samples from 2.5 µg/L to 125 µg/L with high precision and the ELISA shows comparable results to those obtained by LC-MS/MS. A one-step protein precipitation using an organic solvent provides comparable results to a more costly and time-consuming microfiltration pre-treatment of samples. The new ELISA is a fit-for-purpose method to accurately and precisely determine caffeine in saliva samples. KW - Caffeine KW - Cytochrome P450 CYP1A2 KW - Enzyme-linked immunosorbent assay KW - LC-MS/MS KW - Liver function tests KW - Saliva PY - 2012 U6 - https://doi.org/10.1080/00032719.2012.696226 SN - 0003-2719 SN - 1532-236X VL - 45 IS - 17 SP - 2549 EP - 2561 PB - Taylor & Francis CY - Philadelphia, Pa. AN - OPUS4-27267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoehse, M. A1 - Paul, Andrea A1 - Gornushkin, Igor B. A1 - Panne, Ulrich T1 - Multivariate classification of pigments and inks using combined Raman spectroscopy and LIBS N2 - The authenticity of objects and artifacts is often the focus of forensic analytic chemistry. In document fraud cases, the most important objective is to determine the origin of a particular ink. Here, we introduce a new approach which utilizes the combination of two analytical methods, namely Raman spectroscopy and laser-induced breakdown spectroscopy (LIBS). The methods provide complementary information on both molecular and elemental composition of samples. The potential of this hyphenation of spectroscopic methods is demonstrated for ten blue and black ink samples on white paper. LIBS and Raman spectra from different inks were fused into a single data matrix, and the number of different groups of inks was determined through multivariate analysis, i.e., principal component analysis, soft independent modelling of class analogy, partial least-squares discriminant analysis, and support vector machine. In all cases, the results obtained with the combined LIBS and Raman spectra were found to be superior to those obtained with the individual Raman or LIBS data sets. KW - Pigments KW - Raman KW - LIBS KW - Chemometrics PY - 2012 U6 - https://doi.org/10.1007/s00216-011-5287-6 SN - 1618-2642 SN - 1618-2650 VL - 402 IS - 4 SP - 1443 EP - 1450 PB - Springer CY - Berlin AN - OPUS4-25440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Shabanov, Sergej V. A1 - Panne, Ulrich T1 - Abel inversion applied to a transient laser induced plasma: implications from plasma modeling N2 - We test the effects of non-uniformity, non-transparency, and non-stationarity of a laser-induced plasma on the results obtained by the Abel inversion method. The method is commonly used for obtaining spatially resolved emissivity of axially symmetric non-homogeneous radiating objects. Besides the axial symmetry, the plasma is assumed to be optically thin. As the method addresses a certain plasma state, the plasma is required to be stationary during measurements. It is difficult to satisfy the aforementioned conditions for transient laser induced plasmas. As such the plasmas are not stationary; they have steep gradients of thermodynamic parameters that rapidly vary during the plasma evolution. Therefore, any conclusion based on time-integrated measurements and the corresponding data processing should account for these effects. In this work, we use the collision-dominated plasma model to generate time- and spatially resolved synthetic spectra. The spectra are processed by executing the Abel inversion using two numerical algorithms. Thus obtained spatially resolved plasma parameters (emissivity, temperature, and number density) are compared with the exact parameters used to set up the model. In doing so, the accuracy of the Abel inversion method is assessed. Special attention is paid to the dynamic aspect of the expanding plasma and possible errors which result from time-integrated measurements. PY - 2011 U6 - https://doi.org/10.1039/c1ja10044k SN - 0267-9477 SN - 1364-5544 VL - 26 IS - 7 SP - 1457 EP - 1465 PB - Royal Society of Chemistry CY - London AN - OPUS4-25824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balski, Matthias A1 - Kipphardt, Heinrich A1 - Berger, Achim A1 - Meyer, S. A1 - Panne, Ulrich T1 - Determination of impurities in solar grade silicon by inductively coupled plasma sector field mass spectrometry (ICP-SFMS) subsequent to matrix evaporation N2 - A method for the determination of 22 trace impurities in solar grade silicon after dissolution in a mixture of HF and HNO3 and subsequent matrix evaporation is reported. The presented method involves a simple, inexpensive, one-vessel sample preparation apparatus design. The recoveries of B, Na, Mg, Al, P, K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Mo, Sb, W, and Tl at 250 µg kg-1 level are in the range of 93 to 108%. After careful selection of monitored isotopes and their respective resolutions, a sector field mass spectrometer has been used to carry out the measurements. Limits of determination down to 120 ng kg-1 have been obtained using a calibration by three-point standard addition. The method was tested on diluted NIST SRM 57b silicon powder as well as on synthetic test samples and also applied successfully on raw solar grade silicon samples in an interlaboratory comparison including NAA. KW - Solar grade silicon KW - Matrix separation KW - Sector field mass spectrometry PY - 2014 U6 - https://doi.org/10.1039/C3AY41213J SN - 1759-9660 SN - 1759-9679 VL - 6 IS - 1 SP - 77 EP - 85 PB - RSC Publ. CY - Cambridge AN - OPUS4-29893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shigeta, K. A1 - Traub, Heike A1 - Panne, Ulrich A1 - Okino, A. A1 - Rottmann, L. A1 - Jakubowski, Norbert T1 - Application of a micro-droplet generator for an ICP-sector field mass spectrometer - optimization and analytical characterization N2 - A micro-droplet generator (µDG) sample introduction system was coupled to a sector field ICP-MS instrument to investigate the analytical figures of merit with respect to single cell analysis. The sector field instrument was operated for the first time in a fast scanning mode (E-scan) with the shortest time resolution of 100 µs to measure the single droplet time resolved and using the original detector in a pulse counting mode without modification of the existing electronics. For reduction of the droplet diameter a triple pulse mode of the droplet generator was applied and a droplet diameter down to 23 µm has been achieved for this investigation with a 100% transport efficiency of droplets. Signal duration times of single droplets of less than 500 µs have been measured. Overall detection efficiencies in the range of 10-3 counts per atom have been achieved and absolute limits of detection range between 120 ag for Fe and 1.1 ag for Mg as a mean value from 1000 droplet events. PY - 2013 U6 - https://doi.org/10.1039/c2ja30207a SN - 0267-9477 SN - 1364-5544 VL - 28 IS - 5 SP - 646 EP - 656 PB - Royal Society of Chemistry CY - London AN - OPUS4-29447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shigeta, K. A1 - Koellensperger, G. A1 - Rampler, E. A1 - Traub, Heike A1 - Rottmann, L. A1 - Panne, Ulrich A1 - Okino, A. A1 - Jakubowski, Norbert T1 - Sample introduction of single selenized yeast cells (Saccharomyces cerevisiae) by micro droplet generation into an ICP-sector field mass spectrometer for label-free detection of trace elements N2 - We have applied a micro droplet generator (µDG) for sample introduction of single selenized yeast cells into a sector field ICP-MS, which was operated in a fast scanning mode with sampling rates of up to 10 kHz, to measure single cells time resolved with 100 µs integration time. Selenized yeast cells have been used as a model system for preliminary investigation. The single cells to be measured have been embedded into droplets and it will be shown that the time duration of a single cell event always is about 400 to 500 µs, and thus comparable to the time duration of a droplet without a cell. A fixed droplet generation rate of 50 Hz produced equidistant signals in time of each droplet event and was advantageous to separate contribution from background and blank from the analytical signal. Open vessel digestion and a multielement analysis were performed with washed yeast cells and absolute amounts per single cell were determined for Na (0.91 fg), Mg (9.4 fg), Fe (5.9 fg), Cu (0.54 fg), Zn (1.2 fg) and Se (72 fg). Signal intensities from single cells have been measured for the elements Cu, Zn and Se, and histograms were calculated for about 1000 cell events. The mean elemental sensitivities measured here range from 0.7 counts per ag (Se) to 10 counts per ag (Zn) with RSD's from 49% (Zn) to 69% (Se) for about 1000 cell events. PY - 2013 U6 - https://doi.org/10.1039/c3ja30370e SN - 0267-9477 SN - 1364-5544 VL - 28 IS - 5 SP - 637 EP - 645 PB - Royal Society of Chemistry CY - London AN - OPUS4-29448 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosenkranz, D. A1 - Kriegel, F. L. A1 - Mavrakis, E. A1 - Pergantis, S. A. A1 - Reichardt, P. A1 - Tentschert, J. A1 - Jakubowski, N. A1 - Laux, P. A1 - Panne, Ulrich A1 - Luch, A. T1 - Versatile dual-inlet sample introduction system for multi-mode single particle inductively coupled plasma mass spectrometry N2 - Metal-containing nanoparticles (NP) can be characterized with inductively coupled plasma mass spectrometers (ICP-MS) in terms of their size and number concentration by using the single-particle mode of the instrument (spICP-MS). The accuracy of measurement depends on the setup, operational conditions of the instrument and specific parameters that are set by the user. The transport efficiency of the ICP-MS is crucial for the quantification of the NP and usually requires a reference material with homogenous size distribution and a known particle number concentration. Currently, NP reference materials are available for only a few metals and in limited sizes. If particles are characterized without a reference standard, the results of both size and particle number may be biased. Therefore, a dual-inlet Setup for characterizing nanoparticles with spICP-MS was developed to overcome this problem. This setup is based on a conventional introduction system consisting of a pneumatic nebulizer (PN) for nanoparticle solutions and a microdroplet Generator (μDG) for ionic calibration solutions. A new and flexible interface was developed to facilitate the coupling of μDG, PN and the ICP-MS system. The interface consists of available laboratory components and allows for the calibration, nanoparticle (NP) characterization and cleaning of the arrangement, while the ICP-MS instrument is still running. Three independent analysis modes are available for determining particle size and number concentration. Each mode is based on a different calibration principle. While mode I (counting) and mode III (μDG) are known from the literature, mode II (sensitivity), is used to determine the transport efficiency by inorganic ionic Standard solutions only. It is independent of NP reference materials. The μDG based inlet system described here guarantees superior analyte sensitivities and, therefore, lower detection limits (LOD). The size dependent LODs achieved are less than 15 nm for all NP (Au, Ag, CeO2) investigated. KW - Spectrometer KW - Reference KW - Calibration PY - 2020 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-536121 SN - 1940-087X IS - 163 SP - 1 EP - 19 PB - MyJoVE Corporation CY - Cambridge, MA, USA AN - OPUS4-53612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winckelmann, Alexander A1 - Nowak, S. A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Riedel, Jens A1 - Vogl, Jochen A1 - Panne, Ulrich A1 - Abad Andrade, Carlos Enrique T1 - High-Resolution Atomic Absorption Spectrometry Combined With Machine Learning Data Processing for Isotope Amount Ratio Analysis of Lithium N2 - An alternative method for lithium isotope amount ratio analysis based on a combination of high-resolution atomic absorption spectrometry and spectral data analysis by machine learning (ML) is proposed herein. It is based on the well-known isotope shift of approximately 15 pm for the electronic transition 22P←22S at around the wavelength of 670.8 nm, which can be measured by the state-of-the-art high-resolution continuum source graphite furnace atomic absorption spectrometry. For isotope amount ratio analysis, a scalable tree boosting ML algorithm (XGBoost) was employed and calibrated using a set of samples with 6Li isotope amount fractions, ranging from 0.06 to 0.99 mol mol–1, previously determined by a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS). The calibration ML model was validated with two certified reference materials (LSVEC and IRMM-016). The procedure was applied toward the isotope amount ratio determination of a set of stock chemicals (Li2CO3, LiNO3, LiCl, and LiOH) and a BAM candidate reference material NMC111 (LiNi1/3Mn1/3Co1/3O2), a Li-battery cathode material. The results of these determinations were compared with those obtained by MC-ICP-MS and found to be metrologically comparable and compatible. The residual bias was −1.8‰, and the precision obtained ranged from 1.9 to 6.2‰. This precision was sufficient to resolve naturally occurring variations, as demonstrated for samples ranging from approximately −3 to +15‰. To assess its suitability to technical applications, the NMC111 cathode candidate reference material was analyzed using high-resolution continuum source atomic absorption spectrometry with and without matrix purification. The results obtained were metrologically compatible with each other. KW - Lithium KW - Isotope KW - Machine learning KW - Algorithms KW - Reference material KW - AAS KW - Atomic Absorption Spectrometry PY - 2021 U6 - https://doi.org/10.1021/acs.analchem.1c00206 SN - 1520-6882 VL - 93 IS - 29 SP - 10022 EP - 10030 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-53028 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abad Andrade, Carlos Enrique A1 - Mimus, S. A1 - Recknagel, Sebastian A1 - Jakubowski, N. A1 - Panne, Ulrich A1 - Becker-Ross, H. A1 - Huang, M.-D. T1 - Determination of organic chlorine in water via AlCl derivatization and detection by high-resolution continuum source graphite furnace molecular absorption spectrometry N2 - High-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GF-MAS) was employed for determining adsorbable organic chlorine (AOCl) in water. Organic chlorine was indirectly quantified by monitoring the molecular absorption of the transient aluminum monochloride molecule (AlCl) around a wavelength of 261.42 nm in a graphite furnace. An aluminum solution was used as the molecularforming modifier. A zirconium coated graphite furnace, as well as Sr and Ag solutions were applied as modifiers for a maximal enhancement of the absorption signal. The pyrolysis and vaporization temperatures were 600 °C and 2300 °C, respectively. Non-spectral interferences were observed with F, Br, and I at concentrations higher than 6 mg L-1, 50 mg L-1, and 100 mg L-1, respectively. Calibration curves with NaCl, 4-chlorophenol, and trichlorophenol present the same slope and dynamic range, which indicates the chlorine atom specificity of the method. This method was evaluated and validated using synthetic water samples, following the current standard DIN EN ISO 9562:2004 for the determination of the sum parameter adsorbable organic halides (AOX) for water quality. These samples contain 4-chlorophenol as the chlorinated organic standard in an inorganic chloride matrix. Prior to analysis, organic chlorine was extracted from the inorganic matrix via solid-phase extraction with a recovery rate >95%. There were no statistically significant differences observed between measured and known values and for a t-test a confidence level of 95% was achieved. The limits of detection and characteristic mass were found to be 48 and 22 pg, respectively. The calibration curve was linear in the range 0.1–2.5 ng with a correlation coefficient R2 = 0.9986. KW - Chlorides KW - Chlorine KW - Graphite furnace KW - Spectrometry KW - Diatomic molecule KW - Water KW - AlCl PY - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-534426 SN - 1759-9660 VL - 13 IS - 33 SP - 3724 EP - 3730 PB - The Royal Society of Chemistry CY - London, UK AN - OPUS4-53442 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Phukphatthanachai, P. A1 - Panne, Ulrich A1 - Traub, Heike A1 - Pfeifer, Jens A1 - Vogl, Jochen T1 - Quantification of sulphur in copper and copper alloys by GDMS and LA-ICP-MS, demonstrating metrological traceability to the international system of units N2 - The quantification of the sulphur mass fraction in pure copper and copper alloys by GDMS and LA-ICP-MS revealed a lack of traceability mainly due to a lack of suitable certified reference materials for calibrating the instruments. Within this study GDMS and LA-ICP-MS were applied as routine analytical tools to quantify sulphur in copper samples by applying reference materials as calibrators, which were characterized for their sulphur mass fraction by IDMS beforehand. Different external calibration strategies were applied including a matrix cross type calibration. Both techniques with all calibration strategies were validated by using certified reference materials (others than those used for calibration) and good agreement with the reference values was achieved except for the matrix cross type calibration, for which the agreement was slightly worse. All measurement results were accompanied by an uncertainty statement. For GDMS, the relative expanded (k = 2) measurement uncertainty ranged from 3% to 7%, while for LA-ICP-MS it ranged from 11% to 33% when applying matrix-matched calibration in the sulphur mass fraction range between 25 mg kg-1 and 1300 mg kg-1. For cross-type calibration the relative expanded (k = 2) measurement uncertainty need to be increased to at least 12% for GDMS and to at least 54% for LA-ICP-MS to yield metrological compatibility with the reference values. The so obtained measurement results are traceable to the international system of units (SI) via IDMS reference values, which is clearly illustrated by the unbroken chain of calibrations in the metrological traceability scheme. KW - Sulfur KW - Copper KW - GDMS KW - LA-ICP-MS KW - Uncertainty KW - Traceability KW - SI PY - 2021 U6 - https://doi.org/10.1039/d1ja00137j SN - 0267-9477 VL - 36 IS - 11 SP - 2404 EP - 2414 PB - Royal Society of Chemistry AN - OPUS4-53412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winckelmann, Alexander A1 - Morcillo Garcia-Morato, Dalia A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Riedel, Jens A1 - Vogl, Jochen A1 - Panne, Ulrich A1 - Abad Andrade, Carlos Enrique T1 - Determination of lithium in human serum by isotope dilution atomic absorption spectrometry N2 - The therapeutic dose of lithium (Li) compounds, which are widely used for the treatment of psychiatric and hematologic disorders, is close to its toxic level; therefore, drug monitoring protocols are mandatory. Herein, we propose a fast, simple, and low-cost analytical procedure for the traceable determination of Li concentration in human serum, based on the monitoring of the Li isotope dilution through the partially resolved isotope shift in its electronic transition around 670.80 nm using a commercially available high-resolution continuum source graphite furnace atomic absorption spectrometer. With this technique, serum samples only require acidic digestion before analysis. The procedure requires three measurements—an enriched 6Li spike, a mixture of a certified standard solution and spike, and a mixture of the sample and spike with a nominal 7Li/6Li ratio of 0.82. Lanthanum has been used as an internal spectral standard for wavelength correction. The spectra are described as the linear superposition of the contributions of the respective isotopes, each consisting of a spin-orbit doublet, which can be expressed as Gaussian components with constant spectral position and width and different relative intensity, reflecting the isotope ratio in the sample. Both the spectral constants and the correlation between isotope ratio and relative band intensity have been experimentally obtained using commercially available materials enriched with Li isotopes. The Li characteristic mass (mc) obtained corresponds to 0.6 pg. The procedure has been validated using five human serum certified reference materials. The results are metrologically comparable and compatible to the certified values. The measurement uncertainties are comparable to those obtained by the more complex and expensive technique, isotope dilution mass spectrometry. KW - Lithium KW - Human serum KW - Isotope dilution KW - Atomic absorption spectrometry KW - High-resolution continuum source graphite furnace atomic absorption spectrometry PY - 2021 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-532446 VL - 414 IS - 1 SP - 251 EP - 256 PB - Springer CY - Berlin AN - OPUS4-53244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Michalik-Onichimowska, Aleksandra A1 - Beitz, T. A1 - Panne, Ulrich A1 - Löhmannsröben, H.-G. A1 - Riedel, Jens T1 - Microsecond mid-infrared laser pulses for atmospheric pressure laser ablation/ionization of liquid samples N2 - In many laser based ionization techniques with a subsequent drift time separation, the laser pulse generating the ions is considered as the start time t0. Therefore, an accurate temporal definition of this event is crucial for the resolution of the experiments. In this contribution, the laser induced plume dynamics of liquids evaporating into atmospheric pressure are visualized for two distinctively different laser pulse widths, Δt = 6 nanoseconds and Δτ = 280 microseconds. For ns-pulses the expansion of the generated vapour against atmospheric pressure is found to lead to turbulences inside the gas phase. This results in spatial and temporal broadening of the nascent clouds. A more equilibrated expansion, without artificial smearing of the temporal resolution can, in contrast, be observed to follow μs-pulse excitation. This leads to the counterintuitive finding that longer laser pulses results in an increased temporal vapour formation definition. To examine if this fume expansion also eventually results in a better definition of ion formation, the nascent vapour plumes were expanded into a linear drift tube ion mobility spectrometer (IMS). This time resolved detection of ion formation corroborates the temporal broadening caused by collisional impeding of the supersonic expansion at atmospheric pressure and the overall better defined ion formation by evaporation with long laser pulses. A direct comparison of the observed results strongly suggests the coexistence of two individual ion formation mechanisms that can be specifically addressed by the use of appropriate laser sources. KW - Plume KW - Laser ablation KW - Ion mobility spectrometry KW - Pulse duration KW - Ionization PY - 2017 U6 - https://doi.org/10.1016/j.snb.2016.06.155 VL - 238 SP - 298 EP - 305 PB - Elsevier CY - Amsterdam, NL AN - OPUS4-37158 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nietzold, Carolin A1 - Dietrich, Paul A1 - Lippitz, Andreas A1 - Panne, Ulrich A1 - Unger, Wolfgang T1 - Cyclodextrin – ferrocene host – guest complexes on silicon oxide surfaces N2 - Research on carbohydrate based interactions with proteins, nucleic acids or antibodies has gained increased interest in the last years especially in clinical diagnosis or drug development. The efficiency of diagnostic interfaces depends upon the number of probe molecules, e.g. carbohydrates. The control of surface parameters as density and distribution of immobilized carbohydrates is essential for a reliable interaction with protein analytes. A controlled production of biomolecular interfaces can be reached by a stepwise quality control during buildup of these biointerfaces. Here, ß-amino-cyclodextrin molecules were attached to amine-reactive silicon oxide surfaces via click chemistry to construct a model biosensor surface. The amount of surface bound carbohydrates was determined indirectly after chemical derivatization with 4-(trifluoromethyl)-benzylamine (TFMBA). Moreover, these surfaces were used to form host-guest complexes of ferrocene (guest) and β-cyclodextrin (host) moieties to mimic the target binding (sensing) of the model biosensor. Surface chemical analysis of all steps during biosensor construction was performed using X-ray photoelectron spectroscopy (XPS) and near-edge X-ray absorption fine structure spectroscopy (NEXAFS). Our approach widens the possibilities to generate switchable surfaces based on ß-Cyclodextrin surfaces for biosensor applications. KW - ß-amino-cyclodextrin KW - Ferrocene KW - Guest complexe KW - XPS KW - NEXAFS PY - 2016 U6 - https://doi.org/10.1002/sia.5958 SN - 0142-2421 SN - 1096-9918 VL - 48 IS - 7 SP - 606 EP - 610 PB - Wiley AN - OPUS4-36856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nadejde, C. A1 - Neamtu, M. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Ababei, G. A1 - Panne, Ulrich T1 - Hybrid iron-based core-shell magnetic catalysts for fast degradation of bisphenol A in aqueous systems N2 - Three types of hybrid modified magnetite (Fe₃O₄) nanoparticles, functionalized with either chitosan, chitosan/iron (II) oxalate or chitosan/iron (III) citrate, were synthesized by chemical precipitation method. The obtained nanomaterials were characterized by energy dispersive X-ray spectroscopy, X-ray diffraction, Brunauer–Emmett–Teller analysis, scanning and Transmission electron microscopy, Fourier transform infrared spectroscopy and vibrating sample magnetometry. The prepared composites were further tested as magnetic catalysts for the removal of bisphenol A (BPA) in aqueous media. The kinetic Degradation experiments were performed at laboratory scale, while the best operational parameters for all three materials were established: 1.00 g L⁻¹ of catalyst, 10 mmol L⁻¹ H₂O₂, under simulated solar light irradiation. After 15 min of UVA irradiation under the experimental conditions mentioned above, it was possible to decompose up to 99% of the micropollutant over all catalysts. Fe₃O₄/chitosan/iron oxalate catalyst showed the highest and fastest catalytic activity in BPA removal. Catalytic wet peroxide oxidation of non-biodegradable micropollutants on such iron-based hybrid nanoparticles can be a suitable pre-treatment method for wastewater decontamination, as an environment-friendly simplified Approach for water clean-up. KW - Katalysator KW - Bisphenol A KW - Nano KW - Fenton KW - Magnetische Nanopartikel PY - 2016 U6 - https://doi.org/10.1016/j.cej.2016.05.090 SN - 1385-8947 VL - 302 SP - 587 EP - 594 PB - Elsevier CY - Amsterdam AN - OPUS4-37126 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, Holger A1 - Baldofski, Stefanie A1 - Hoffmann, Kristin A1 - Flemig, Sabine A1 - Silva, C. P. A1 - Esteves, V. I. A1 - Emmerling, Franziska A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - Structural considerations on the selectivity of an immunoassay for sulfamethoxazole N2 - Sulfamethoxazol (SMX),a sulfonamide, is a widely used bacteriostatic antibiotic and therefore a promising marker for the entry of anthropogenic Pollution in the environment. SMX is frequently found in wastewater and surface water. This study presents the production of high affinity and selective polyclonal antibodies for SMX and the development and Evaluation of a direct competitive enzyme-linked immunosorbent assay(ELISA)for the quantification of SMX in environmental watersamples. The crystal structures of the cross-reacting compounds sulfamethizole, N4-acetyl-SMX andsuccinimidyl-SMX were determined by x-ray diffraction aiming to explain their high cross-reactivity. These crystal structures are described for the first time. The quantification range of the ELISA is 0.82–63 µg/L. To verify our results, the SMX concentration in 20 environmental samples,including wastewater and surfacewater,was determined by ELISA and tandem mass spectrometry(MS/MS).A good Agreement of the measured SMX concentrations was found with average recoveries of 97–113%for the results of ELISA compared to LC-MS/MS. KW - X-Ray diffraction KW - Sulfamethoxazole KW - ELISA KW - LC-MS/MS PY - 2016 U6 - https://doi.org/10.1016/j.talanta.2016.05.049 SN - 0039-9140 SN - 1873-3573 IS - 158 SP - 198 EP - 207 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-36676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lingott, Jana A1 - Lindner, Uwe A1 - Telgmann, Lena A1 - Esteban-Fernández, Diego A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Gadolinium-uptake by aquatic and terrestrial organisms-distribution determined by laser ablation inductively coupled plasma mass spectrometry N2 - The uptake of gadolinium containing chelates by plants and animals grown in exposed water or on soil irrigated with exposed water was investigated. Gd contrast agents was studied by monitoring the elemental distribution with laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). KW - Gadolinium-uptake KW - Speciation KW - HILIC KW - ICP-MS PY - 2016 U6 - https://doi.org/10.1039/c5em00533g SN - 2050-7887 VL - 18 IS - 2 SP - 200 EP - 207 PB - Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-36281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Janine A1 - Fettig, I. A1 - Philipp, Rosemarie A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Fisicaro, P. A1 - Alasonati, E. T1 - Determination of tributyltin in whole water matrices under the European water framework directive N2 - Monitoring of water quality is important to control water pollution. Contamination of the aquatic systemhas a large effect on human health and the environment. Under the European Water Framework Directive(WFD) 2000/60/EC and the related directive on environmental quality standards (EQS) in the field of waterpolicy 2008/105/EC, the need for sensitive reference methods was highlighted. Since tributyltin (TBT) isone of the WFD listed priority substances a method was developed which is capable to qualify and quantifythe pollutant at the required low WFD EQS of 0.2 ng L⁻¹ in whole water bodies, i.e. in non-filtered watersamples with dissolved organic carbon and suspended particulate matter. Therefore special attention waspaid on the interaction of TBT with the suspended particulate matter and humic substances to obtain acomplete representation of the pollution in surface waters. Different water samples were investigatedvarying the content of organic dissolved and suspended matter. Quantification was performed usingspecies-specific isotope dilution (SSID) and gas chromatography with inductively coupled plasma massspectrometry (GC-ICP-MS). Different sample treatment strategies were evaluated and compared. Theprocess of internal standard addition was investigated and optimized, hence the equilibrium betweeninternal standards and matrix is of primary importance to perform accurate SSID. Samples spiked at EQSlevel were analyzed with a recovery between 95 and 105 %. Additionally real surface water samples wereinvestigated and the TBT concentration for the whole water body was determined and compared withconventional routine analysis method. KW - Tributyltin (TBT) KW - Environmental quality standard (EQS) KW - Isotope dilution KW - Humic acid KW - Surface water KW - Suspended particulate matter PY - 2016 U6 - https://doi.org/10.1016/j.chroma.2016.06.068 SN - 0021-9673 VL - 1459 SP - 112 EP - 119 AN - OPUS4-36930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Porizka, Pavel A1 - Klessen, Benjamin A1 - Kaiser, J. A1 - Gornushkin, Igor B. A1 - Panne, Ulrich A1 - Riedel, Jens T1 - High repetition rate laser-induced breakdown spectroscopy using acousto-optically gated detection N2 - This contribution introduces a new type of setup for fast sample analysis using laser-induced breakdown spectroscopy (LIBS). The novel design combines a high repetition rate laser (up to 50 kHz) as excitation source and an acousto-optical modulator (AOM) as a fast switch for temporally gating the detection of the emitted light. The plasma radiation is led through the active medium of the AOM where it is diffracted on the transient ultrasonic Bragg grid. The diffracted radiation is detected by a compact Czerny-Turner spectrometer equipped with a CCD line detector. Utilizing the new combination of high repetition rate lasers and AOM gated detection, rapid measurements with total integration times of only 10 ms resulted in a limit of detection (LOD) of 0.13 wt.% for magnesium in aluminum alloys. This short integration time corresponds to 100 analyses/s. Temporal gating of LIP radiation results in improved LODs and consecutively higher sensitivity of the LIBS setup. Therefore, an AOM could be beneficially utilized to temporally detect plasmas induced by high repetition rate lasers. The AOM in combination with miniaturized Czerny-Turner spectrometers equipped with CCD line detectors and small footprint diode pumped solid state lasers results in temporally gateable compact LIBS setups. KW - Laser Induced Breakdown Spectroscopy KW - LIBS KW - Aluminium KW - Charge coupled devices KW - Magnesium KW - Light diffraction PY - 2014 U6 - https://doi.org/10.1063/1.4890337 SN - 0034-6748 SN - 1089-7623 VL - 85 IS - 7 SP - 073104-1 - 073104-8 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-31358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gabriel, Stefan A1 - Pfeifer, Dietmar A1 - Schwarzinger, C. A1 - Panne, Ulrich A1 - Weidner, Steffen T1 - Matrix-assisted laser desorption/ionization time-of-flight mass spectrometric imaging of synthetic polymer sample spots prepared using ionic liquid matrices N2 - RATIONALE Polymer sample spots for matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) prepared by the dried-droplet method often reveal ring formation accompanied by possible segregation of matrix and sample molecules as well as of the polymer homologs itself. Since the majority of sample spots are prepared by this simple and fast method, a matrix or sample preparation method that excludes such segregation has to be found. METHODS Three different ionic liquid matrices based on conventionally used aromatic compounds for MALDI-TOF MS were prepared. The formation of ionic liquids was proven by 1H NMR spectroscopy. MALDI-Imaging mass spectrometry was applied to monitor the homogeneity. RESULTS Our results show a superior sample spot homogeneity using ionic liquid matrices. Spots could be sampled several times without visible differences in the mass spectra. A frequently observed loss of matrix in the mass spectrometer vacuum was not observed. The necessary laser irradiance was reduced, which resulted in less polymer fragmentation. CONCLUSIONS Ionic liquid matrices can be used to overcome segregation, a typical drawback of conventional MALDI dried-droplet preparations. Homogeneous sample spots are easy to prepare, stable in the MS vacuum and, thereby, improve the reproducibility of MALDI. PY - 2014 U6 - https://doi.org/10.1002/rcm.6810 SN - 0951-4198 SN - 1097-0231 VL - 28 IS - 5 SP - 489 EP - 498 PB - Wiley CY - Chichester AN - OPUS4-30267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balski, Matthias A1 - Emmerling, Franziska A1 - Kipphardt, Heinrich A1 - Panne, Ulrich T1 - Determination of boron in silicon without use of additional complexing agents N2 - Methods for the determination of boron in various matrices described in the literature usually employ complexing agents like mannitol to retain the volatile boron species during matrix evaporation steps. However, also relatively high boron recoveries from silicon containing samples have been reported when no complexing agents were added to the digestion acids. The mechanism behind this matrix-dependant recovery has been investigated by studying the boron recovery in the analysis of solar grade silicon. It was found that the NH4+ ion formed by the reduction of nitric acid during sample digestion is responsible for the higher recovery of boron, which leads to a possible analysis method without the use of complexing agents if the sample preparation procedure is carefully optimized. KW - Boron KW - Complexing agents KW - Matrix evaporation KW - Sample enrichment PY - 2014 U6 - https://doi.org/10.1039/c4ay00410h SN - 1759-9660 SN - 1759-9679 VL - 6 IS - 12 SP - 4003 EP - 4008 PB - RSC Publ. CY - Cambridge AN - OPUS4-30956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gusarova, Tamara A1 - Hodoroaba, Vasile-Dan A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Panne, Ulrich T1 - Exploitation of the hollow cathode effect for sensitivity enhancement of Grimm-type DC glow discharge optical emission spectroscopy N2 - The hollow cathode (HC) effect was investigated in non-cooled 15 mm deep drilled flat metallic analytical samples that were easy to prepare. The deep cavity used ("complete HC" in contrast to "recessed HC" with 2-3 mm deep cavity) intensified the HC effect notably and therefore distinctly improved the detection power of the common GD-OES with planar cathodes. A signal enhancement of up to a factor of 150, not reported earlier, in comparison with flat conventional samples was achieved. A better separation of the analytical lines from spectral interferences was observed when the HC assembly was applied. Additionally, an effect of strongly enhanced intensities of atomic lines and somewhat decreased intensities of ionic lines was detected in the case of HC in comparison to usual planar cathodes. The investigations were carried out with samples of copper, steel and zinc matrices using both the same and individually optimised glow discharge (GD) electrical parameters. KW - Hollow cathode KW - Grimm type glow discharge KW - Emission spectroscopy KW - GD-OES KW - Sensitivity PY - 2009 U6 - https://doi.org/10.1039/b814977a SN - 0267-9477 SN - 1364-5544 VL - 24 SP - 680 EP - 684 PB - Royal Society of Chemistry CY - London AN - OPUS4-19600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gopala, Anil A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Mass spectrometry insight of the process mechanism during the vacuum distillation of zinc N2 - Detection and monitoring of volatile elements released during the preparation of ultra high purity zinc by vacuum distillation (VD) is reported using online quadrupole gas source mass spectrometry (QMS). The theoretically calculated vapour pressures (pv) for the volatile impurity elements using Dushman constants and the practically observed mass spectra were found to be consistent (S. Dushman and J. M. Lafferty, Scienific Foundations of Vacuum Technique, 2nd ed., Wiley, New York, 1962). This is the first time that the potential ability of an online mass spectrometer was used for monitoring and understanding the process mechanism during the purification of metals (Zn) using VD. We here also illustrate our findings with the results from high resolution glow discharge mass spectrometer (HR-GDMS) analysis before and after the purification of Zn. PY - 2009 U6 - https://doi.org/10.1039/b904133h SN - 0267-9477 SN - 1364-5544 VL - 24 SP - 887 EP - 890 PB - Royal Society of Chemistry CY - London AN - OPUS4-19595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 U6 - 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 - JOUR A1 - Chinthalapati, Siva Kesava Raju A1 - Lück, Detlef A1 - Scharf, Holger A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - A novel solid phase extraction method for pre-concentration of gadolinium and gadolinium based MRI contrast agents from the environment N2 - An efficient solid phase extraction (SPE) method using bis-(2-ethylhexyl)-phosphate (HDEHP) coated reverse phase C18 support has been developed for the pre-concentration of Gadolinium (Gd) and Gd contrast agents widely used in magnetic resonance imaging (MRI). Enrichment of Gd in the ionic form has been compared with strong cation exchange material Chromabond SA (SCX), weak ion exchange material Chelex-100 and also with lanthanide specific HDEHP modified reverse phase C18. The determination of Gd and its complexes after enrichment were performed using inductively coupled plasma mass spectrometry (ICP-MS) and on the basis of 158Gd. Among the three SPE materials, HDEHP coated reverse phase C18 SPE has been found to be most efficient, yielding a hundredfold Gd enrichment with > 95% recovery for linear and cyclic contrast agents like Gd-DTPA (Magnevist), Gd-DOTA (Dotarem), Gd-BOPTA (Multihance), and Gd-BT-DO3A (Gadovist). The developed SPE method has been successfully applied to the surface water and waste water samples originated from different places in Berlin, Germany. The results were in good agreement with the results obtained with direct measurement with ICP-MS. The developed pre-concentration method can be efficiently used for the determination of trace levels of gadolinium in the environment even with less sensitive analytical techniques. KW - Solid phase extraction KW - Magnetic resonance imaging KW - Gadolinium KW - Gd based contrast agents KW - Chelex-100 KW - HDEHP KW - Speciation PY - 2010 U6 - https://doi.org/10.1039/c003251d SN - 0267-9477 SN - 1364-5544 VL - 25 IS - 10 SP - 1573 EP - 1580 PB - Royal Society of Chemistry CY - London AN - OPUS4-21985 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Shabanov, Sergej V. A1 - Merk, Sven A1 - Tognoni, E. A1 - Panne, Ulrich T1 - Effects of non-uniformity of laser induced plasma on plasma temperature and concentrations determined by the Boltzmann plot method: implications from plasma modeling PY - 2010 U6 - https://doi.org/10.1039/C0JA00016G SN - 0267-9477 SN - 1364-5544 VL - 25 SP - 1643 EP - 1653 PB - Royal Society of Chemistry CY - London AN - OPUS4-22942 LA - eng 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 U6 - 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 - Traub, Heike A1 - Wälle, M. A1 - Koch, J. A1 - Panne, Ulrich A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Günther, D. T1 - Evaluation of different calibration strategies for the analysis of pure copper and zinc samples using femtosecond laser ablation ICP-MS N2 - Solution-doped metal powder pellets as well as aspirated liquids were used as calibration samples to analyze pure copper and zinc certified reference materials (CRMs) by femtosecond laser ablation ICP-MS. It was demonstrated that calibration by copper pellets resulted in relative deviations up to 20%, whereas fs-LA-ICP-MS among copper-based CRMs led to inaccuracies in the same range unless nominal mass fractions were chosen to be <3 mg/kg. Calibration by zinc pellets generally provided better accuracy. Depending on the analyte considered, deviations below 10% were obtained even for mass fractions close to the limit of quantification. Our data, therefore, indicate solution-doped metal powder pellets to be suitable as calibration samples for fs-LA-ICP-MS of metals. Furthermore, the utilization of liquid standards for calibration was found to result in stronger deviations of up to 50% for both copper and zinc samples which, in addition, turned out to be dependent on the plasma conditions. KW - Laser ablation KW - ICP-MS KW - Calibration KW - Copper KW - Zinc KW - Metal PY - 2009 U6 - https://doi.org/10.1007/s00216-009-3061-9 SN - 1618-2642 SN - 1618-2650 VL - 395 IS - 5 SP - 1471 EP - 1480 PB - Springer CY - Berlin AN - OPUS4-20402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gopala, Anil A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Process methodology for the small scale production of m6N5 purity zinc using a resistance heated vacuum distillation system N2 - Ultra high purity Zn (m6N5) was obtained through triple vacuum distillation using an m4N5 Zn as input material. High-volatile impurities were removed from the zinc matrix by vacuum evaporation, while traces having lower volatility than the matrix remained in the residual material after finishing of the entire purification process. The time required for the removal of the main high-volatile impurity (Cd) was monitored using a connected gas source mass spectrometer. During distillation the Zn vapor of the distillate was condensed on the cap of a glassy carbon crucible which was water cooled by a movable copper block. The temperatures were optimized for the removal of the volatiles and for the distillation process using vapor pressure data. High resolution glow discharge mass spectrometry was applied for the analysis and purity evaluation of the distilled and input zinc. The analysis confirmed the reduction of the metallic impurities from 43 mg kg-1 to 0.5 mg kg-1 (m6N5) after three consecutive vacuum distillations. An increase in the grain size and a decrease in the micro-hardness were observed for the purified Zn material. KW - Ultra high purity KW - Vacuum distillation KW - High resolution glow discharge mass KW - Spectrometry KW - Micro-hardness KW - Zinc KW - Purification PY - 2010 U6 - https://doi.org/10.1016/j.matchemphys.2010.02.080 SN - 0254-0584 VL - 122 IS - 1 SP - 151 EP - 155 PB - Elsevier CY - Amsterdam AN - OPUS4-21127 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gopala, Anil A1 - Zellmann, M. A1 - Kipphardt, Heinrich A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Mass spectrometric study of the impurity profile in Zn during reduction-distillation of ZnO with activated and inactivated Al N2 - In this work, we report on the application of hyphenated gas source mass spectrometry to study and understand the mechanism of the reduction-distillation of ZnO using Al powder as reductant in its activated and inactivated form. The experiments revealed that the purity of the Zn metal produced were superior using activated Al with respect to inactivated Al, i.e., m5N8 (99.9998% metallic based) versus m5N3. The achieved purity levels of Zn and the absence of high volatile Cd, Mg, and Sb impurities in the gas phase and the material collected were explained with respect to the impurity elements free-energy values, vapor pressure data, and an observed scavenging effect of the Ta crucible, which was supported by the on-line observed mass spectrometric profiles of the residual gas. PY - 2010 U6 - https://doi.org/10.1016/j.jasms.2010.04.009 SN - 1044-0305 VL - 21 IS - 9 SP - 1620 EP - 1623 PB - Elsevier CY - New York, NY AN - OPUS4-21910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gopala, Anil A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Kipphardt, Heinrich T1 - Real time monitoring of chemical transformations during catalytic reduction using gas source mass spectrometry: carbon/zinc carbonate hydroxide N2 - We report herein the utilization of a vacuum reduction distillation system (VRDS) coupled with mass spectrometry (MS) to characterize chemical transformations in thermal analysis. The system initially designed to monitor metal purification by distillation is applied for the first time to the catalytic reaction of in situ formed nickel oxide during the carbothermic reduction of zinc oxide. PY - 2010 U6 - https://doi.org/10.1039/c004179c SN - 0267-9477 SN - 1364-5544 VL - 25 SP - 1378 EP - 1380 PB - Royal Society of Chemistry CY - London AN - OPUS4-21911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Walter, Astrid A1 - Pfeifer, Dietmar A1 - Kraus, Werner A1 - Emmerling, Franziska A1 - Schneider, Rudolf A1 - Panne, Ulrich A1 - Weller, Michael G. T1 - Triacetone Triperoxide (TATP): Hapten design and development of antibodies N2 - Triacetone triperoxide (TATP), an improvised explosive, is a potential security threat because of its cost-efficient synthesis and the difficulty in detecting it. A highly selective antibody could provide the necessary specificity to the detection process. To obtain antibodies, a hapten made from acetone, hydrogen peroxide, and 7-oxooctanoic acid has been designed, synthesized, and confirmed by NMR that displays the utmost similarity to the analyte. The single-crystal X-ray structures of the solvated species TATP·methanol (1:1) and the TATP derivate were determined. In both compounds, the molecules exhibit D3 symmetry and adopt a twisted boat-chair conformation. The hapten was coupled to bovine serum albumin, and mice were immunized. An immune response against TATP was elicited, and selective antibodies were detected in the mouse serum, which should be very useful for the development of a TATP biosensor system. An ELISA with a limit of detection for TATP of 65 µg L-1 is shown. KW - TATP KW - Triacetone triperoxide KW - Explosive KW - Antibody KW - Hapten immunoassay KW - Structure PY - 2010 U6 - https://doi.org/10.1021/la1018339 SN - 0743-7463 SN - 1520-5827 VL - 26 IS - 19 SP - 15418 EP - 15423 PB - American Chemical Society CY - Washington, DC AN - OPUS4-22469 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, Vanessa A1 - Warrikhoff, A. A1 - Panne, Ulrich A1 - Hodoroaba, Vasile-Dan T1 - Determination of emitted X-ray tube spectra by means of a calibrated instrumental setup KW - X-ray tube spectrum KW - XRF KW - SEM KW - EDS KW - Spectrometer efficiency PY - 2010 U6 - https://doi.org/10.1017/S1431927610054292 SN - 1431-9276 SN - 1435-8115 VL - 16 IS - Supplement S2 SP - 930 EP - 931 PB - Cambridge University Press CY - New York, NY AN - OPUS4-22471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Carvalho, José Joao A1 - Weller, Michael G. A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - A highly sensitive caffeine immunoassay based on a monoclonal antibody KW - Caffeine KW - ELISA KW - Antibody KW - LC–MS–MS KW - Water KW - Wastewater marker PY - 2010 U6 - https://doi.org/10.1007/s00216-010-3506-1 SN - 1618-2642 SN - 1618-2650 VL - 396 IS - 7 SP - 2617 EP - 2628 PB - Springer CY - Berlin AN - OPUS4-22651 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 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-240291 UR - http://www.mdpi.com/2079-6374/1/3/93 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 - Matiaske, Anna-Maria A1 - Gornushkin, Igor B. A1 - Panne, Ulrich T1 - Double-pulse laser-induced breakdown spectroscopy for analysis of molten glass 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 U6 - 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 - TY - JOUR A1 - Gornushkin, Igor B. A1 - Panne, Ulrich T1 - Radiative models of laser-induced plasma and pump-probe diagnostics relevant to laser-induced breakdown spectroscopy N2 - The paper describes past and present efforts in modeling of laser-induced plasma and overviews plasma diagnostics carried out by pump-probe techniques. Besides general information on existing plasma models, the emphasis is given to models relevant to spectrochemical analysis, i.e. models of radiating plasma. Special attention is paid to collisional-radiative (CR) and collisional-dominated (CD) plasma models where radiative processes play an important role. Also, calibration-free (CF) models are considered which may endow with the possibility for standardless spectroscopic analysis. In the diagnostic part, only methods based on the use of additional diagnostic tools (auxiliary lasers, optics, and probes) are described omitting those based on plasma own radiation. A short review is provided on image-based diagnostics (shadowgraphy, schlieren, and interferometry), absorption and fluorescence, Langmuir probe, and less frequently used cavity ringdown and Thomson scattering methods. KW - Laser ablation KW - Modeling KW - Plasma diagnostics KW - Laser-induced breakdown spectroscopy PY - 2010 U6 - https://doi.org/10.1016/j.sab.2010.03.021 SN - 0584-8547 SN - 0038-6987 VL - 65 IS - 5 SP - 345 EP - 359 PB - Elsevier CY - Amsterdam AN - OPUS4-24003 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 U6 - 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 - 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 U6 - 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 - 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 U6 - 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 - 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 U6 - 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 - 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 U6 - 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 - Panne, Ulrich A1 - Bremser, Wolfram T1 - Considerations with regard to the calculation of key comparison reference values and uncertainties N2 - Much has been published over the last years on finding the best (consensus) reference value for a given set of key comparison data, and a suite of approaches proposed. In this paper, several aspects are highlighted which should be taken into account when deciding on key comparison strategies, protocols, and the best approach to reliable key comparison reference value and uncertainty. Some of these aspects are briefly discussed. The paper is intended to intensify discussions, and any comments and opinions are welcome. KW - Key comparison KW - Reference value KW - Reference value uncertainty KW - Equivalence PY - 2009 U6 - https://doi.org/10.1007/s00769-009-0515-x SN - 0949-1775 SN - 1432-0517 VL - 14 IS - 5 SP - 281 EP - 287 PB - Springer CY - Berlin AN - OPUS4-19460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wienold, Julia A1 - Traub, Heike A1 - Lange, Britta A1 - Giray, Thorsten A1 - Recknagel, Sebastian A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Elemental analysis of copper and magnesium alloy samples using IR-laser ablation in comparison with spark and glow discharge methods N2 - Three methods for direct solid sampling of bulk material namely IR laser ablation, glow discharge and spark OES, were compared with respect to analytical figures of merit obtained for elemental analysis with atomic spectrometry. Matrices investigated were copper, pressed doped copper powder, and magnesium alloys. For the vast majority of analytes, statistical equivalence regarding precision (usually ≤ 5%) and the performance of the calibrations between the compared methods was demonstrated. KW - LA-ICP-MS KW - GD-MS KW - Spark-OES KW - LA-ICP-OES KW - Copper KW - Magnesium PY - 2009 U6 - https://doi.org/10.1039/b903251g SN - 0267-9477 SN - 1364-5544 VL - 24 SP - 1570 EP - 1574 PB - Royal Society of Chemistry CY - London AN - OPUS4-20257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulte, Franziska A1 - Mäder, J. A1 - Kroh, L.W. A1 - Panne, Ulrich A1 - Kneipp, Janina T1 - Characterization of pollen carotenoids with in situ and high-performance thin-layer chromatography supported resonant Raman spectroscopy N2 - Raman signatures of the carotenoid component are studied in individual pollen grains from different species of trees. The information is obtained as differences in the strong pre-resonant Raman spectra measured before and after photodepletion of the carotenoid molecules. The results provide the first in situ evidence of interspecies differences in pollen carotenoid content, structure, and/or assembly between plant species without prior purification. The analysis of carotenoids in situ is confirmed by high-performance thin-layer chromatography (HPTLC)-supported resonance Raman data measured directly on the HPTLC plates after separation of carotenoids in pollen extracts. Utilization of the in situ, extraction-free procedure in carotenoid analysis will improve sensitivity and structural selectivity and provides insight into carotenoid structure and composition in single pollen grains. PY - 2009 U6 - https://doi.org/10.1021/ac901389p SN - 0003-2700 SN - 1520-6882 VL - 81 IS - 20 SP - 8426 EP - 8433 PB - American Chemical Society CY - Washington, DC AN - OPUS4-20260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klimakow, Maria A1 - Leiterer, Jork A1 - Kneipp, Janina A1 - Rössler, E. A1 - Panne, Ulrich A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Combined synchrotron XRD/Raman measurements: In situ identification of polymorphic transitions during crystallization processes N2 - A combination of two analytical methods, time-resolved X-ray diffraction (XRD) and Raman spectroscopy, is presented as a novel tool for crystallization studies. An acoustic levitator was employed as sample environment. This setup enables the acquisition of XRD and Raman data in situ simultaneously within a 20 s period and hence permits investigation of polymorphic phase transitions during the crystallization process in different solvents (methanol, ethanol, acetone, dichloromethane, acetonitrile). These real time measurements allow the determination of the phase content from the onset of the first crystalline molecular assemblies to the stable system. To evaluate the capability of this approach, the setup was applied to elucidate the crystallization process of the polymorphic compound nifedipine. The results indicate the existence of solvent-dependent transient phases during the crystallization process. The quality of the data allowed the assignment of the lattice constants of the hitherto unknown crystal structure of the β-polymorph. KW - Synchrotron radiation KW - XRD KW - Raman spectroscopy KW - Polymorphism KW - Crystallization KW - Acoustic levitation KW - Nifedipine PY - 2010 U6 - https://doi.org/10.1021/la100540q SN - 0743-7463 SN - 1520-5827 VL - 26 IS - 13 SP - 11233 EP - 11237 PB - American Chemical Society CY - Washington, DC AN - OPUS4-21396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -