TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, G. A1 - Emmerling, Franziska A1 - Kemnitz, E. T1 - Mechanochemical synthesis, characterization, and structure determination of new alkaline earth metal-tetrafluoroterephthalate frameworks: Ca(pBDC‑F4 )·4H2O, Sr(pBDC‑F4 )·4H2O, and Ba(pBDC‑F4 ) N2 - New fluorinated alkaline earth metal−organic frameworks were successfully synthesized by milling of metal hydroxides M(OH)2 with tetrafluoroterephthalic acid H2 pBDC-F4. Both calcium- and strontium-tetrafluoroterephthalates are tetrahydrated, while the barium tetrafluoroterephthalate is free of coordinating water molecules. The two isomorphic structures Ca(pBDC-F4)·4H2O and Sr(pBDC-F4)·4H2O were solved from the powder diffraction data by ab initio structure determination and subsequent Rietveld refinement. The products were thoroughly characterized by elemental analysis, thermal analysis, magicangle spinning NMR, Fourier transform infrared spectroscopy, scanning electron microscopy imaging, and Brunauer−Emmett−Teller measurements. Our findings suggest that the mechanochemical synthesis route is a promising approach for the preparation of new fluorinated alkaline earth metal−organic frameworks. KW - Mechanochemistry KW - MOFs KW - XRD PY - 2016 UR - http://pubs.acs.org/doi/abs/10.1021/acs.cgd.5b01457 DO - https://doi.org/10.1021/acs.cgd.5b01457 SN - 1528-7483 VL - 16/4 SP - 1923 EP - 1933 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-35940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bach, S. A1 - Panthöfer, M. A1 - Bienert, Ralf A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska A1 - Tremel, W. T1 - Role of water during crystallization of amorphous cobalt phosphate nanoparticles N2 - The transformation of amorphous precursors into crystalline solids and the associated mechanisms are still poorly understood. We illuminate the formation and reactivity of an amorphous cobalt phosphate hydrate precursor and the role of water for its crystallization process. Amorphous cobalt phosphate hydrate nanoparticles (ACP) with diameters of ∼20 nm were prepared in the absence of additives from aqueous solutions at low concentrations and with short reaction times. To avoid the kinetically controlled transformation of metastable ACP into crystalline Co₃(PO₄)₂ × 8H₂O (CPO) its separation must be fast. The crystallinity of ACP could be controlled through the temperature during precipitation. A second amorphous phase (HT-ACP) containing less water and anhydrous Co₃(PO₄)₂ was formed at higher temperature by the release of coordinating water. ACP contains approximately five molecules of structural water per formula unit as determined by thermal analysis (TGA) and quantitative IR spectroscopy. The Co²+ coordination in ACP is tetrahedral, as shown by XANES/EXAFS spectroscopy, but octahedral in crystalline CPO. ACP is stable in the absence of water even at 500 °C. In the wet state, the transformation of ACP to CPO is triggered by the diffusion and incorporation of water into the structure. Quantitative in situ IR analysis allowed monitoring the crystallization kinetics of ACP in the presence of water. KW - Fluorapatite-gelatin nanocomposites KW - Calcium-carbonate KW - Zinc phosphate KW - Crystal-growth KW - Nucleation KW - Polymorphism PY - 2016 DO - https://doi.org/10.1021/acs.cgd.6b00208 SN - 1528-7483 SN - 1528-7505 VL - 16 IS - 8 SP - 4232 EP - 4239 PB - ACS Publications AN - OPUS4-37616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ciornii, Dmitri A1 - Hodoroaba, Vasile-Dan A1 - Benismail, Nizar A1 - Altmann, Korinna T1 - Project 2: Interlaboratory Comparison on detection and quantitative assessment of microplastics by use of spectroscopic and thermo-analytical methods N2 - Validated and standardized methods in microplastic analysis are indispensable for robust monitoring and regulation. Alongside also reference materials are urgently needed. An interlaboratory comparison (ILC) offers a powerful tool to address both these challenges. The present study aimed to compare the precision and accuracy of various methods for the detection and quantification of microplastic in a water-soluble matrix. Additionally, it evaluated the suitability of the test materials (containing environmentally relevant plastic polymers) to serve as reference materials for the microplastic analysis. In this ILC several most used thermo-analytical and spectroscopic methods have been addressed: Pyrolysis-Gas Chromatography Mass Spectrometry (Py-GC/MS), Thermal Extraction-Desorption Gas Chromatography Mass Spectrometry (TED-GC/MS), micro-Fourier Transform Infrared Spectroscopy (µ-FTIR), and micro-Raman Spectroscopy and Laser Direct Infrared Spectroscopy (LDIR). Microplastic powders of polyethylene (PE) and polyethylene terephthalate (PET) were used to assess suitability of the test materials (microplastic tablets) for method validation and use in the ILCs. The participants were guided with a SOP how to dissolve the test samples and, depending on their selected method, either quantify the number of particles (by the spectroscopic methods) or determine the mass fraction of microplastic particles per sample (by the thermo-analytical methods). KW - ILC KW - Microplastic KW - FTIR KW - Raman KW - TED-GC/MS KW - Py-GC/MS PY - 2024 SP - 1 EP - 16 AN - OPUS4-60612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Zientek, Nicolai A1 - Rump, Doreen A1 - Fischer, Franziska A1 - Maiwald, Michael A1 - Emmerling, Franziska T1 - Make and break - Facile synthesis of cocrystals and comprehensive dissolution studies N2 - Mechanochemistry is increasingly used as a ‘green alternative’ for synthesizing various materials including pharmaceutical cocrystals. Herein, we present the mechanochemical synthesis of three new cocrystals containing the API carbamazepine (cocrystals CBZ:Indometacin 1:1, CBZ:Benzamide 1:1, and CBZ:Nifedipine 1:1). The mechanochemical reaction was investigated in situ documenting a fast and complete reaction within one minute. Online NMR spectroscopy proved the direct influence of the dissolution behaviour of the coformers to the dissolution behaviour of the API carbamazepine. The dissolution behaviour of the organic cocrystals is compared to the behaviour of the pure drug indicating a general applicability of this approach for detailed cocrystal dissolution studies. KW - Cocrystals KW - Carbamazepine KW - Mechanochemistry KW - Powder diffraction KW - Online NMR spectroscopy PY - 2017 DO - https://doi.org/10.1016/j.molstruc.2016.11.063 SN - 0022-2860 SN - 1872-8014 VL - 1133 SP - 18 EP - 23 AN - OPUS4-38664 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna A1 - Braun, U. T1 - Monitoring von Mikroplastik N2 - Der Vortrag gibt einen Überblick was bei der Analyse von Mikroplastik zu beachten ist und beschreibt die Vor- und Nachteile der TED-GC/MS. T2 - Abschlusstreffen MikroPlaTas CY - Online meeting DA - 23.06.2021 KW - Mikroplastik KW - TED-GC/MS KW - Mikroplastik-Analytik PY - 2021 AN - OPUS4-52916 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völzke, Jule L. A1 - Hodjat Shamami, Parya A1 - Gawlitza, Kornelia A1 - Feldmann, Ines A1 - Zimathies, Annett A1 - Meyer, Klas A1 - Weller, Michael G. T1 - High-purity corundum as support for affinity extractions from complex samples N2 - Nonporous corundum powder, known as an abrasive material in the industry, was functionalized covalently with protein binders to isolate and enrich specific proteins from complex matrices. The materials based on corundum were characterized by TEM, ESEM, BET, DLS, EDS, and zeta potential measurements. The strong Al-O-P bonds between the corundum surface and amino phosphonic acids were used to introduce functional groups for further conjugations. The common crosslinker glutaraldehyde was compared with a hyperbranched polyglycerol (PG) of around 10 kDa. The latter was oxidized with periodate to generate aldehyde groups that can covalently react with the amines of the surface and the amino groups from the protein via a reductive amination process. The amount of bound protein was quantified via aromatic amino acid analysis (AAAA). This work shows that oxidized polyglycerol can be used as an alternative to glutaraldehyde. With polyglycerol, more of the model protein bovine serum albumin (BSA) could be attached to the surface under the same conditions, and lower non-specific binding (NSB) was observed. As a proof of concept, IgG was extracted with protein A from crude human plasma. The purity of the product was examined by sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). A binding capacity of 1.8 mg IgG per gram of corundum powder was achieved. The advantages of corundum include the very low price, extremely high physical and chemical stability, pressure resistance, favorable binding kinetics, convenient handling, and flexible application. KW - Corundum KW - Sapphire KW - Affinity chromatography KW - Antibodies KW - Self-assembled monolayers (SAM) KW - Polyglycerol KW - Dendrimer KW - Nonspecific binding (NSB) KW - Purification KW - Solid-phase extraction (SPE) PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559342 DO - https://doi.org/10.3390/separations9090252 VL - 9 IS - 9 SP - 1 EP - 13 PB - MDPI CY - Basel AN - OPUS4-55934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kazlagić, Anera A1 - Russo, Francesco A1 - Vogl, Jochen A1 - Sturm, Patrick A1 - Stephan, D. A1 - Gluth, Gregor ED - Resch-Genger, Ute ED - Koch, Matthias ED - Meermann, Björn ED - Weller, Michael G. T1 - Development of a sample preparation procedure for Sr isotope analysis of Portland cements N2 - The 87Sr/86Sr isotope ratio can, in principle, be used for provenancing of cement. However, while commercial cements consist of multiple components, no detailed investigation into their individual 87Sr/86Sr isotope ratios or their influence on the integral 87Sr/86Sr isotope ratio of the resulting cement was conducted previously. Therefore, the present study aimed at determining and comparing the conventional 87Sr/86Sr isotope ratios of a diverse set of Portland cements and their corresponding Portland clinkers, the major component of these cements. Two approaches to remove the additives from the cements, i.e. to measure the conventional 87Sr/86Sr isotopic fingerprint of the clinker only, were tested, namely, treatment with a potassium hydroxide/sucrose solution and sieving on a 11-µm sieve. Dissolution in concentrated hydrochloric acid/nitric acid and in diluted nitric acid was employed to determine the 87Sr/86Sr isotope ratios of the cements and the individual clinkers. The aim was to find the most appropriate sample preparation procedure for cement provenancing, and the selection was realised by comparing the 87Sr/86Sr isotope ratios of differently treated cements with those of the corresponding clinkers. None of the methods to separate the clinkers from the cements proved to be satisfactory. However, it was found that the 87Sr/86Sr isotope ratios of clinker and cement generally corresponded, meaning that the latter can be used as a proxy for the clinker 87Sr/86Sr isotope ratio. Finally, the concentrated hydrochloric acid/nitric acid dissolution method was found to be the most suitable sample preparation method for the cements; it is thus recommended for 87Sr/86Sr isotope analyses for cement provenancing. KW - Cement KW - Provenancing KW - Sr isotopes KW - Portland clinker KW - Dissolution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542239 DO - https://doi.org/10.1007/s00216-021-03821-7 SN - 1618-2642 SN - 1618-2650 VL - 414 IS - 15 (Topical collection: Analytical methods and applications in the materials and life sciences) SP - 4379 EP - 4389 PB - Springer CY - Berlin AN - OPUS4-54223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Meermann, Björn A1 - Koch, Matthias A1 - Weller, Michael G. T1 - Editorial: Analytical methods and applications in materials and life sciences N2 - Current trends in materials and life sciences are flanked by the need to push detection limits to single molecules or single cells, enable the characterization of increasingly complex matrices or sophisticated nanostructures, speed up the time of analysis, reduce instrument complexity and costs, and improve the reliability of data. This requires suitable analytical tools such as spectroscopic, separation and imaging techniques, mass spectrometry, and hyphenated techniques as well as sensors and their adaptation to application-specific challenges in the environmental, food, consumer product, health sector, nanotechnology, and bioanalysis. Increasing concerns about health threatening known or emerging pollutants in drinking water, consumer products, and food and about the safety of nanomaterials led to a new awareness of the importance of analytical sciences. Another important driver in this direction is the increasing demand by legislation, particularly in view of the 17 sustainable development goals by the United Nations addressing clean energy, industry, and innovation, sustainable cities, clean water, and responsible consumption and production. In this respect, also the development of analytical methods that enable the characterization of material flows in production processes and support recycling concepts of precious raw materials becomes more and more relevant. In the future, this will provide the basis for greener production in the chemical industry utilizing recycled or sustainable starting materials. This makes analytical chemistry an essential player in terms of the circular economy helping to increase the sustainability of production processes. In the life sciences sector, products based on proteins, such as therapeutic and diagnostic antibodies, increase in importance. These increasingly biotechnologically produced functional biomolecules pose a high level of complexity of matrix and structural features that can be met only by highly advanced methods for separation, characterization, and detection. In addition, metrological traceability and target definition are still significant challenges for the future, particularly in the life sciences. However, innovative reference materials as required for the health and food sector and the characterization of advanced materials can only be developed when suitable analytical protocols are available. The so-called reproducibility crisis in sciences underlines the importance of improved measures of quality control for all kinds of measurements and material characterization. This calls for thorough method validation concepts, suitable reference materials, and regular interlaboratory comparisons of measurements as well as better training of scientists in analytical sciences. The important contribution of analytical sciences to these developments is highlighted by a broad collection of research papers, trend articles, and critical reviews from these different application fields. Special emphasis is dedicated to often-overlooked quality assurance and reference materials. T2 - 150 years BAM: Science with impact CY - Berlin, Germany DA - 01.01.2021 KW - Analysis KW - Life sciences KW - Analytical sciences KW - Quality assurance KW - Reference material KW - Fluorescence KW - Nanoparticle KW - Sensor KW - Material sciences KW - Pollutant KW - Environment KW - Method KW - Limit of detection KW - 150th anniversary KW - ABC KW - BAM KW - Collection KW - Editorial KW - Special issue KW - Bundesanstalt für Materialforschung und -prüfung KW - Jahrestag PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550720 DO - https://doi.org/10.1007/s00216-022-04082-8 SN - 1618-2642 SN - 1618-2650 VL - 414 IS - Topical collection: Analytical methods and applications in the materials and life sciences SP - 4267 EP - 4268 PB - Springer CY - Berlin AN - OPUS4-55072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schroeder, Barbara A1 - Le Xuan, Hoa A1 - Völzke, Jule L. A1 - Weller, Michael G. T1 - Preactivation Crosslinking - An Efficient Method for the Oriented Immobilization of Antibodies N2 - Crosslinking of proteins for their irreversible immobilization on surfaces is a proven and popular method. However, many protocols lead to random orientation and the formation of undefined or even inactive by-products. Most concepts to obtain a more targeted conjugation or immobilization requires the recombinant modification of at least one binding partner, which is often impractical or prohibitively expensive. Here a novel method is presented, which is based on the chemical preactivation of Protein A or G with selected conventional crosslinkers. In a second step, the antibody is added, which is subsequently crosslinked in the Fc part. This leads to an oriented and covalent immobilization of the immunoglobulin with a very high yield. Protocols for Protein A and Protein G with murine and human IgG are presented. This method may be useful for the preparation of columns for affinity chromatography, immunoprecipitation, antibodies conjugated to magnetic particles, permanent and oriented immobilization of antibodies in biosensor systems, microarrays, microtitration plates or any other system, where the loss of antibodies needs to be avoided, and maximum binding capacity is desired. This method is directly applicable even to antibodies in crude cell culture supernatants, raw sera or protein-stabilized antibody preparations without any purification nor enrichment of the IgG. This new method delivered much higher signals as a traditional method and, hence, seems to be preferable in many applications. KW - Antibody coating KW - Proximity-enhanced reaction KW - Immunoglobulins KW - IgG KW - Protein A KW - Protein G KW - Immunoprecipitation KW - Immunocapture KW - Regeneration KW - Biosensor KW - Immunosensor KW - Affinity chromatography KW - Immunoaffinity extraction KW - Oriented immobilization KW - Immunoassay KW - Bioconjugation PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479786 DO - https://doi.org/10.3390/mps2020035 SN - 2409-9279 VL - 2 IS - 2 SP - 1 EP - 14 PB - MDPI CY - Basel, Switzerland AN - OPUS4-47978 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Schroeder, Barbara A1 - Le Xuan, Hoa A1 - Völzke, Jule L. A1 - Weller, Michael G. T1 - Preactivation crosslinking – An efficient method for the oriented immobilization of antibodies N2 - Crosslinking of proteins for their irreversible immobilization on surfaces is a proven and popular method. However, many protocols lead to random orientation and the formation of undefined or even inactive by-products. Most concepts to obtain a more targeted conjugation or immobilization requires the recombinant modification of at least one binding partner, which is often impractical or prohibitively expensive. Here a novel method is presented, which is based on the chemical preactivation of Protein A or G with selected conventional crosslinkers. In a second step, the antibody is added, which is subsequently crosslinked in the Fc part. This leads to an oriented and covalent immobilization of the immunoglobulin with a very high yield. Protocols for Protein A and Protein G with murine and human IgG are presented. This method may be useful for the preparation of columns for affinity chromatography, immunoprecipitation, antibodies conjugated to magnetic particles, permanent and oriented immobilization of antibodies in biosensor systems, microarrays, microtitration plates or any other system, where the loss of antibodies needs to be avoided, and maximum binding capacity is desired. This method is directly applicable even to antibodies in crude cell culture supernatants, raw sera or protein-stabilized antibody preparations without any purification nor enrichment of the IgG. This new method delivered much higher signals as a traditional method and, hence, seems to be preferable in many applications. KW - Antibody coating KW - Proximity-enhanced reaction KW - Immunoglobulins KW - IgG KW - Protein G KW - Protein A KW - Immunoprecipitation KW - Immunocapture KW - Stabilization KW - Biosensor KW - Biochip KW - Microarray KW - ELISA KW - Immunoassay KW - Immunosensor KW - Crosslinker KW - Nanoparticles KW - Click chemistry KW - Herceptin KW - Trastuzumab PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-478797 DO - https://doi.org/10.20944/preprints201904.0205.v1 SN - 2310-287X SP - 1 EP - 17 PB - MDPI CY - Basel AN - OPUS4-47879 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -