TY - JOUR A1 - Trimpin, S. A1 - Lee, C. A1 - Weidner, Steffen A1 - El-Baba, T. A1 - Lutomski, C. A1 - Inutan, E. A1 - Foley, C. A1 - Ni, C.-K. A1 - McEwen, C. T1 - Unprecedented Ionization Processes in Mass SpectrometryProvide Missing Link between ESI and MALDI N2 - In the field of mass spectrometry,producing intact, highly-charged protein ions from surfaces is a conundrum with significant potential payoff in application areas ranging from bio-medical to clinical research. Here, we report on the ability to form intact, highly-charged protein ions on high vacuum time-of-flight mass spectrometers in the linear and reflectron modes achievable using experimental conditions that allow effective matrix removal from both the sample surfaces and from the charged clusters formed by the laser Ablation event. The charge states are the highest reported on high vacuum mass spectrometers, yet they remain at only around athird of the highest charge obtained using laser ablation with a suitable matrix at atmospheric pressure. Other than physical instrument modifications, the key to forming abundant and stable highly-charged ions appears to be the volatility of the matrix used. Cumulative results suggest mechanistic links between the ionization process reported here and traditional ionization methods of electrospray ionization and matrix-assisted laser desorp-tion/ionization. KW - MALDI KW - Electrospray KW - Mass spectrometry KW - Ionization PY - 2018 DO - https://doi.org/10.1002/cphc.201701246 SN - 1439-4235 SN - 1439-7641 VL - 19 IS - 5 SP - 581 EP - 589 PB - Wiley-VCH AN - OPUS4-44404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knabe, C. A1 - Stiller, M. A1 - Kampschulte, M. A1 - Wilbig, Janka A1 - Peleska, B. A1 - Günster, Jens A1 - Gildenhaar, R. A1 - Berger, G. A1 - Rack, A. A1 - Linow, U. A1 - Heiland, M. A1 - Rendenbach, C. A1 - Koerdt, S. A1 - Steffen, C. A1 - Houshmand, A. A1 - Xiang-Tischhauser, L. A1 - Adel-Khattab, D. T1 - A tissue engineered 3D printed calcium alkali phosphate bioceramic bone graft enables vascularization and regeneration of critical-size discontinuity bony defects in vivo N2 - Recently, efforts towards the development of patient-specific 3D printed scaffolds for bone tissue engineering from bioactive ceramics have continuously intensified. For reconstruction of segmental defects after subtotal mandibulectomy a suitable tissue engineered bioceramic bone graft needs to be endowed with homogenously distributed osteoblasts in order to mimic the advantageous features of vascularized autologous fibula grafts, which represent the standard of care, contain osteogenic cells and are transplanted with the respective blood vessel. Consequently, inducing vascularization early on is pivotal for bone tissue engineering. The current study explored an advanced bone tissue engineering approach combining an advanced 3D printing technique for bioactive resorbable ceramic scaffolds with a perfusion cell culture technique for pre-colonization with mesenchymal stem cells, and with an intrinsic angiogenesis technique for regenerating critical size, segmental discontinuity defects in vivo applying a rat model. To this end, the effect of differing Si-CAOP (silica containing calcium alkali orthophosphate) scaffold microarchitecture arising from 3D powder bed printing (RP) or the Schwarzwalder Somers (SSM) replica fabrication technique on vascularization and bone regeneration was analyzed in vivo. In 80 rats 6-mm segmental discontinuity defects were created in the left femur. KW - Additive Manufacturing KW - Bio active ceramic KW - In-vivo KW - Alcium alkali phosphate PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584555 DO - https://doi.org/10.3389/fbioe.2023.1221314 SN - 2296-4185 VL - 11 SP - 1 EP - 20 PB - Frontiers SA CY - Lausanne AN - OPUS4-58455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, C. A1 - Weidner, Steffen A1 - Falkenhagen, Jana A1 - Barner-Kowollik, C. T1 - In-depth LCCC-(GELC)-SEC characterization of ABA block copolymers generated by a mechanistic switch from RAFT to ROP N2 - A recently introduced procedure involving a mechanistic switch from reversible addition–fragmentation chain transfer (RAFT) polymerization to ring-opening polymerization (ROP) to form diblock copolymers is applied to synthesize ABA (star) block copolymers. The synthetic steps include the polymerization of styrene with R-group designed RAFT agents, the transformation of the thiocarbonyl thio end groups into OH functionalities, and their subsequent chain extension by ROP. The obtained linear ABA poly(ε-caprolactone)-block-poly(styrene)-block-poly(ε-caprolactone) (pCL-b-pS-b-pCL) (12 500 g mol¯¹ ≤ Mₙ ≤ 33 000 g mol¯¹) and the star-shaped poly(styrene)-block-poly(ε-caprolactone) (Mₙ = 36 000 g mol¯¹) copolymers were analyzed by size exclusion chromatography (SEC), nuclear magnetic resonance (NMR), infrared (IR) spectroscopy, and matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. The focus of the current study is on the detailed characterization of the ABA (star) block polymers via multidimensional chromatographic techniques specifically high performance liquid chromatography coupled to size exclusion chromatography (HPLC-SEC). In particular, we demonstrate the first time separation of poly(ε-caprolactone) (pCL) homopolymer and additionally poly(styrene) (pS) from the ABA poly(ε-caprolactone)-b-poly(styrene)-b-poly(ε-caprolactone) and star-shaped poly(styrene)-b-poly(ε-caprolactone) block copolymer utilizing critical conditions (CC) for pCL with concomitant gradient elution liquid chromatography (GELC). KW - Two-dimensional-liquid chromatography (2D-LC) KW - Liquid chromatography under critical conditions (LCCC) KW - Gradient elution liquid chromatography (GELC) KW - Soft ionization mass spectrometry (ESI, MALDI) KW - Reversible addition fragmentation chain transfer (RAFT) KW - Ring opening polymerization (ROP) PY - 2012 DO - https://doi.org/10.1021/ma2022452 SN - 0024-9297 SN - 1520-5835 VL - 45 IS - 1 SP - 87 EP - 99 PB - American Chemical Society CY - Washington, DC AN - OPUS4-25464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Trimpin, S. A1 - Inutan, E. A1 - Karki, S. A1 - Elia, E. A1 - Zhang, W. A1 - Weidner, Steffen A1 - Marshall, D. A1 - Hoang, K. A1 - Lee, C. A1 - Davis, E. A1 - Smith, V. A1 - Meher, A. A1 - Cornejo, M. A1 - Auner, G. A1 - McEwen, C. T1 - Fundamental studies of new ionization technologies and insights from IMS-MS N2 - Exceptional ion mobility spectrometry mass spectrometry (IMS-MS) developments by von Helden, Jarrold, and Clemmer provided technology that gives a view of chemical/biological compositions previously not achievable. The ionization method of choice used with IMS-MS has been electrospray ionization (ESI). In this Special issue contribution, we focus on fundamentals of heretofore unprecedented means for transferring volatile and nonvolatile compounds into gas-phase ions singly and multiply charged. These newer ionization processes frequently lead to different selectivity relative to ESI and, together with IMS-MS, may provide a more comprehensive view of chemical compositions directly from their original Environment such as surfaces, e.g., tissue. Similarities of results using solvent- and matrix-assisted ionization are highlighted, as are differences between ESI and the inlet ionization methods, especially with mixtures such as bacterial extracts. Selectivity using different matrices is discussed, as are results which add to our fundamental knowledge of inlet ionization as well as pose additional avenues for inquiry. IMS-MS provides an opportunity for comparison studies relative to ESI and will prove valuable using the new ionization technologies for direct analyses. Our hypothesis is that some ESI-IMS-MS applications will be replaced by the new ionization processes and by understanding mechanistic aspects to aid enhanced source and method developments this will be hastened. KW - Inlet ionization KW - Vacuum ionization KW - Matrices KW - Fundamentals KW - Ion mobility PY - 2019 DO - https://doi.org/10.1007/s13361-019-02194-7 SN - 1044-0305 SN - 1879-1123 VL - 30 IS - 6 SP - 1133 EP - 1147 PB - Springer AN - OPUS4-48011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lee, C. A1 - Inutan, E. D. A1 - Chen, J. L. A1 - Mukeku, M. M. A1 - Weidner, Steffen A1 - Trimpin, S. A1 - Ni, C.-K. T1 - Toward understanding the ionization mechanism of matrix‐assisted ionization using mass spectrometry experiment and theory N2 - Matrix‐assisted ionization (MAI) mass spectrometry does not require voltages, a laser beam, or added heat to initiate ionization, but it is strongly dependent on the choice of matrix and the vacuum conditions. High charge state distributions of nonvolatile analyte ions produced by MAI suggest that the ionization mechanism may be similar to that of electrospray ionization (ESI), but different from matrix‐assisted laser desorption/ionization (MALDI). While significant information is available for MAI using mass spectrometers operating at atmospheric and intermediate pressure, little is known about the mechanism at high vacuum. Eleven MAI matrices were studied on a high‐vacuum time‐of‐flight (TOF) mass spectrometer using a 266 nm pulsed laser beam under otherwise typical MALDI conditions. Detailed comparisons with the commonly used MALDI matrices and theoretical prediction were made for 3‐nitrobenzonitrile (3‐NBN), which is the only MAI matrix that works well in high vacuum when irradiated with a laser. Screening of MAI matrices with good absorption at 266 nm but with various degrees of volatility and laser energies suggests that volatility and absorption at the laser wavelength may be necessary, but not sufficient, criteria to explain the formation of multiply charged analyte ions. 3‐NBN produces intact, highly charged ions of nonvolatile analytes in high‐vacuum TOF with the use of a laser, demonstrating that ESI‐like ions can be produced in high vacuum. Theoretical calculations and mass spectra suggest that thermally induced proton transfer, which is the major ionization mechanism in MALDI, is not important with the 3‐NBN matrix at 266 nm laser wavelength. 3‐NBN:analyte crystal morphology is, however, important in ion generation in high vacuum. The 3‐NBN MAI matrix produces intact, highly charged ions of nonvolatile compounds in high‐vacuum TOF mass spectrometers with the aid of ablation and/or heating by laser irradiation, and shows a different ionization mechanism from that of typical MALDI matrices. KW - Ionization KW - MALDI-TOF MS KW - Mechanism PY - 2021 DO - https://doi.org/10.1002/rcm.8382 VL - 35 IS - 51 SP - e8382 PB - John Wiley & Sons AN - OPUS4-49209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cobet, C. A1 - Wollschläger, Nicole A1 - Esser, N. A1 - Richter, W. A1 - Baudach, Steffen A1 - Beck, Uwe A1 - Männ, Marion A1 - Brunn, S. A1 - Gruska, B. A1 - Richter, U. T1 - VUV-XUV-Ellipsometrie mit Synchrotronstrahlung T2 - 2. Workshop Ellipsometrie CY - Berlin, Deutschland DA - 2002-02-18 PY - 2002 AN - OPUS4-2282 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cortez, L. A1 - Squirrel, A. A1 - Boley, N. A1 - Garcia, C. A1 - van Berkel, P.M. A1 - Boisson, G. A1 - Foster, H. A1 - Papadakis, I. A1 - Steffen, Bernd T1 - How to interpret information from proficiency test exercises concerning the relative performance of accredited laboratories N2 - If the results from various proficiency tests are used to compare the performance of accredited and non-accredited laboratories, great care must be taken not to come to contradicting conclusions when interpreting them. This paper intends to draw the attention to various aspects that should be taken into account when trying to make conclusions from the relative performance of accredited laboratories in proficiency testing. KW - Proficiency test exercises KW - Accredited laboratories KW - Relative performance PY - 2003 DO - https://doi.org/10.1007/s00769-003-0674-0 SN - 0949-1775 SN - 1432-0517 VL - 8 IS - 11 SP - 511 EP - 513 PB - Springer CY - Berlin AN - OPUS4-1843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Frenz, Holger A1 - Gruhn, B. A1 - Dietrich, C. A1 - Lehmann, J. A1 - Krämer, E. A1 - Glaubitz, Steffen A1 - Wimmer, J. A1 - Rehmer, Birgit A1 - Kühn, Hans-Dieter A1 - Breitkreutz, Konrad A1 - Portella, Pedro Dolabella A1 - Hoffmann, E. A1 - Ziebs, Josef T1 - Sphäroguß als Werkstoff für Behälter zur Beförderung, Zwischen- und Endlagerung radioaktiver Stoffe; Untersuchung zu alternativen Eignungsnachweisen - Fachband 3: Werkstoffuntersuchungen, 1989 - 1992 N2 - Gußeisen mit Kugelgraphit und ferritischer bzw. ferritisch-perlitischer Matrix gehören zu einer Werkstoffgruppe, die ausreichende Festigkeiten mit hohen Duktilitäten verbindet. Mit der vorliegenden Arbeit wurden die Kenntnisse über die Zusammenhänge zwischen der chemischen Zusammensetzung, der Gefügeausbildung und den mechanischen Eigenschaften erweitert. Dabei wurden sowohl unterschiedliche Gießverfahren (Sand- und Kokillenguß) in der Herstellung, als auch die Auswirkungen von Umwandlungsprozessen im Gefüge infolge von Wärmebehandlungen diskutiert. Die statistische Auswertung von Einzelergebnissen aus der qualitätssichernden Begutachtung von Lager- und Transportbehältern für radioaktive Stoffe wurden durch mechanische und bruchmechanische Untersuchungen an 24 Werkstoffsorten aus Gußeisen mit Kugelgraphit ergänzt. KW - Eignungsnachweis KW - Endlagerung KW - Lagerbehälter KW - Radioaktiver Stoff KW - Sphäroguß (GGG-40) KW - Transportbehälter KW - Zwischenlagerung PY - 1992 N1 - Das Projekt wurde gefördert vom Bundesminister für Forschung und Technologie (BMFT); Förderkennzeichen: KWA 79052. SP - 1 EP - 178 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-59950 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brirmi, M A1 - Chabbah, T. A1 - Chatti, S. A1 - Schiets, F. A1 - Casabianca, H. A1 - Marestin, C. A1 - Mercier, R. A1 - Weidner, Steffen A1 - Errachid, A. A1 - Jaffrezic-Renault, N. A1 - Ben Romdhane, H. T1 - Effect of the pendent groups on biobased polymers, obtained from click chemistry suitable, for the adsorption of organic pollutants from water N2 - In this work, four triazole-based poly(ether-pyridine)s polymers were synthesized and used as an adsorbent for the removal of phenolic compounds from aqueous solutions. For this purpose, new fluoromonomers containing 1,2,3-triazole units were prepared by the Cu(I)-catalyzed 1,3-dipolar cycloaddition reaction and then used for the elaboration of novel poly(ether-pyridine-triazole)s (PEPTs) by direct polyconden-sation with isosorbide and bisphenol A. Chemical structure of fluorinated pyridinicmonomers as well as resulting polymers was confirmed by 1H and 19F NMR spectroscopic methods. The thermal behavior of the obtained PEPTs was characterized using differential scanning calorimetry and thermogravimetric analysis. Results of sorption showed that polymers can be effectively used as a sorbent for the removal of polarorganic pollutants. The isosorbide-based poly(ether-pyridine-triazole) which contains hydrophilic hydroxyl groups as pendants chains (P4) exhibited the highest sorption efficiencies (78%–100% after 1 h). In order to explain the results an adsorption mech-anism mainly based on π–π interactions and hydrogen bonding with the pendent groups is proposed. KW - Adsorption KW - Biobased polymers KW - Cycloaddition KW - Pentafluoropyridine KW - Phenolic compounds PY - 2022 DO - https://doi.org/10.1002/pat.5809 SN - 1042-7147 SP - 1 EP - 21 PB - Wiley online library AN - OPUS4-55389 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jlalia, I. A1 - Gomri, M. A1 - Chabbah, T. A1 - Chatti, S. A1 - Weidner, Steffen A1 - Abderrazak, H. A1 - Marestin, C. A1 - Mercier, R. A1 - Ben Halima, H. A1 - Lakard, B. A1 - Jaffrezic Renault, N. T1 - Design of Fluorinated Poly(Ether-Pyridine) Films for Impedimetric Detection of Heavy Metal Ions N2 - A series of fluorinated poly(ether-pyridine)s were synthesized via polycondensation of bis-perfluoropyridine with either bisphe-nol A (BPA) or isosorbide, a bio-sourced diol. The polymers were characterized using 1 H and 19 F NMR spectroscopy, and their molecular weights were determined using GPC. Thermal properties were assessed using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The presence of isosorbide in polymer P2 increases the glass transition temperature and results in a lower molecular weight and a higher hydrophilicity. On the other hand, polymer P3, based on BPA, shows the best thermal stability, the highest molecular weight, and the most pronounced hydrophobic character. Electrochemical impedance spectroscopy (EIS) was used to evaluate the modified gold electrodes for the selective detection of metal ions. Among the four target ions (Ni 2+, Cd 2+, Pb2+, and Hg 2+), defined by the European Water Framework Directive, Pb2+ was selectively detected on the hydrophilic polymer P2, while Cd 2+ was selectively detected on the hydrophobic polymer P3. The achieved detection limits were 5 × 10−11 M, corresponding to 10 ng/L for Pb2+ and 5.6 ng/L for Cd 2+, respectively. KW - Cadmium KW - Electrochemical impedance spectroscopy KW - Fluorinated polyether pyridines KW - Isosorbide KW - Lead PY - 2025 DO - https://doi.org/10.1002/pat.70038 SN - 1099-1581 VL - 36 IS - 1 SP - 1 EP - 14 PB - John Wiley & Sons Ltd. AN - OPUS4-62384 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -