TY - JOUR A1 - Usmani, Shirin M. A1 - Plarre, Rüdiger A1 - Hübert, Thomas A1 - Kemnitz, E. ED - Richter, K. ED - Van de Kulien, J.-W. T1 - Termite resistance of pine wood treated with nano metal fluorides N2 - Fluorides are well-known as wood preservatives. One of the limitations of fluoride-based wood preservatives is their high leachability. Alternative to current fluoride salts such as NaF used in wood protection are low water-soluble fluorides. However, impregnation of low water-soluble fluorides into wood poses a challenge. To address this challenge, low water-soluble fluorides like calcium fluoride (CaF2) and magnesium fluoride (MgF2) were synthesized as nanoparticles via the fluorolytic sol−gel synthesis and then impregnated into wood specimens. In this study, the toxicity of nano metal fluorides was assessed by termite mortality, mass loss and visual analysis of treated specimens after eight weeks of exposure to termites, Coptotermes formosanus. Nano metal fluorides with sol concentrations of 0.5 M and higher were found to be effective against termites resulting in 100% termite mortality and significantly inhibited termite feeding. Among the formulations tested, the least damage was found for specimens treated with combinations of CaF2 and MgF2 with an average mass loss less than 1% and visual rating of “1”. These results demonstrate the efficacy of low water-soluble nano metal fluorides to protect wood from termite attack. KW - Holzschutzmittel KW - Nanoparticles KW - Fluorides KW - Termites PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514325 DO - https://doi.org/10.1007/s00107-020-01522-z VL - 78 SP - 493 EP - 499 PB - Springer CY - Berlin AN - OPUS4-51432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bhuckory, S. A1 - Wegner, Karl David A1 - Qiu, X. A1 - Wu, Y.T. A1 - Jennings, T. L. A1 - Incamps, A. A1 - Hildebrandt, N. T1 - Triplexed CEA-NSE-PSA Immunoassay Using Time-Gated Terbium-to-Quantum Dot FRET N2 - Time-gated Förster resonance energy transfer (TG-FRET) between Tb complexes and luminescent semiconductor quantum dots (QDs) provides highly advantageous photophysical properties for multiplexed biosensing. Multiplexed Tb-to-QD FRET immunoassays possess a large potential for in vitro diagnostics, but their performance is often insufficient for their application under clinical conditions. Here, we developed a homogeneous TG-FRET immunoassay for the quantification of carcinoembryonic antigen (CEA), neuron-specific enolase (NSE), and prostatespecific antigen (PSA) from a single serum sample by multiplexed Tb-to-QD FRET. Tb–IgG antibody donor conjugates were combined with compact QD-F(ab’)2 antibody acceptor conjugates with three different QDs emitting at 605, 650, and 705 nm. Upon antibody–antigen–antibody Sandwich complex formation, the QD acceptors were sensitized via FRET from Tb, and the FRET ratios of QD and Tb TG luminescence intensities increased specifically with increasing antigen concentrations. Although limits of detection (LoDs: 3.6 ng/mL CEA, 3.5 ng/mL NSE, and 0.3 ng/mL PSA) for the triplexed assay were slightly higher compared to the single-antigen assays, they were still in a clinically relevant concentration range and could be quantified in 50 μL serum samples on a B·R·A·H·M·S KRYPTOR Compact PLUS clinical immunoassay plate reader. The simultaneous quantification of CEA, NSE, and PSA at different concentrations from the same serum sample demonstrated actual multiplexing Tb-to-QD FRET immunoassays and the potential of this technology for translation into clinical diagnostics. KW - Lanthanides KW - Nanoparticles KW - Biosensing KW - Multiplexing KW - FRET KW - Fluorescence KW - PSA KW - NSE KW - CEA PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512290 DO - https://doi.org/10.3390/molecules25163679 VL - 25 IS - 16 SP - 3679 PB - MDPI AN - OPUS4-51229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Tchipilov, Teodor A1 - Raysyan, Anna A1 - Weller, Michael G. T1 - Methods for the quantification of particle-bound protein – Application to reagents for lateral-flow immunoassays (LFIA) N2 - Protein immobilization for the functionalization of particles is used in various applications, including biosensors, lateral-flow immunoassays (LFIA), bead-based assays, and others. Common methods for the quantification of bound protein are measuring protein in the supernatant before and after coating and calculating the difference. This popular approach has the potential for a significant overestimation of the amount of immobilized protein since layers not directly bound to the surface (soft protein corona) are usually lost during washing and handling. Only the layer directly bound to the surface (hard corona) can be used in subsequent assays. A simplified amino acid analysis method based on acidic hydrolysis and RP-HPLC-FLD of tyrosine and phenylalanine (aromatic amino acid analysis, AAAA) is proposed to directly quantify protein bound to the surface of gold nano- and latex microparticles. The results are compared with indirect methods such as colorimetric protein assays, such as Bradford, bicinchoninic acid (BCA), as well as AAAA of the supernatant. For both particle types, these indirect quantification techniques show a protein overestimation of up to 1700% compared to the direct AAAA measurements. In addition, protein coating on latex particles was performed both passively through adsorption and covalently through EDC/sulfo-NHS chemistry. Our results showed no difference between the immobilization methodologies. This finding suggests that usual protein determination methods are no unambiguous proof of a covalent conjugation on particles or beads. KW - Soft protein corona KW - Hard protein corona KW - Gold particles KW - Nanoparticles KW - Mikroparticles KW - Antibody KW - Bioconjugation KW - Protein quantification KW - Supernatant KW - Sodium chloride method KW - Covalent conjugation KW - Latex particles KW - Lateral flow immunoassays PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545365 DO - https://doi.org/10.20944/preprints202203.0332.v1 SP - 1 EP - 8 PB - MDPI CY - Basel AN - OPUS4-54536 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von der Au, Marcus A1 - Faßbender, Sebastian A1 - Chronakis, Michail A1 - Vogl, Jochen A1 - Meermann, Björn T1 - Size determination of nanoparticles by ICP-ToF-MS using isotope dilution in microdroplets N2 - Within this work, the combination of a microdroplet generator and an ICP-ToF-MS for nanoparticle analysis is presented. For the size determination of platinum nanoparticles an on-line isotope dilution analysis approach was developed. The 194Pt/195Pt isotopic ratio was used for the characterization of the particles, while the 182W/183W isotopic ratio was monitored simultaneously for mass bias correction. The on-line ID-MDG-sp-ICP-ToF-MS approach was deployed for the size determination of three platinum nanoparticle samples (50 nm, 63 nm, 70 nm); for validation, complementary size characterization techniques (sp-ICP-ToF-MS and TEM) were used. The robustness of this technique was evidenced, by using sodium chloride concentrations up to 100 mg L−1 as a matrix component. Our new on-line ID MDG-sp-ICP-ToF-MS approach is a promising tool for the fast and reliable determination of nanoparticles' size in severe matrix concentrations, e.g., environmental samples. KW - ICP-ToF-MS KW - Nanoparticles KW - Isotope Dilution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552727 DO - https://doi.org/10.1039/D2JA00072E SN - 0267-9477 VL - 37 IS - 6 SP - 1203 EP - 1207 PB - Royal Society of Chemistry AN - OPUS4-55272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deumer, J. A1 - Pauw, Brian Richard A1 - Marguet, S. A1 - Skroblin, D. A1 - Taché, O. A1 - Krumrey, M. A1 - Gollwitzer, C. T1 - Small-angle X-ray scattering: characterization of cubic Au nanoparticles using Debye’s scattering formula N2 - A versatile software package in the form of a Python extension, named CDEF (computing Debye’s scattering formula for extraordinary form factors), is proposed to calculate approximate scattering profiles of arbitrarily shaped nanoparticles for small-angle X-ray scattering (SAXS). CDEF generates a quasi-randomly distributed point cloud in the desired particle shape and then applies the open-source software DEBYER for efficient evaluation of Debye’s scattering formula to calculate the SAXS pattern (https://github.com/j-from-b/CDEF). If self-correlation of the scattering signal is not omitted, the quasi-random distribution provides faster convergence compared with a true-random distribution of the scatterers, especially at higher momentum transfer. The usage of the software is demonstrated for the evaluation of scattering data of Au nanocubes with rounded edges, which were measured at the four-crystal monochromator beamline of PTB at the synchrotron radiation facility BESSY II in Berlin. The implementation is fast enough to run on a single desktop computer and perform model fits within minutes. The accuracy of the method was analyzed by comparison with analytically known form factors and verified with another implementation, the SPONGE, based on a similar principle with fewer approximations. Additionally, the SPONGE coupled to McSAS3 allows one to retrieve information on the uncertainty of the size distribution using a Monte Carlo uncertainty estimation algorithm. KW - X-ray scattering KW - SAXS KW - Non-spherical nanoparticles KW - Nanoparticles KW - Nanomaterials KW - Debye scattering equation KW - Simulation KW - Data fitting PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557652 DO - https://doi.org/10.1107/S160057672200499X VL - 55 IS - Pt 4 SP - 993 EP - 1001 PB - International Union of Crystallography CY - Chester, England AN - OPUS4-55765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chambers, M. S. A1 - Hunter, R. D. A1 - Hollamby, M. J. A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Snow, T. A1 - Danks, A. E. A1 - Schnepp, Z. T1 - In Situ and Ex Situ X‑ray Diffraction and Small-Angle X‑ray Scattering Investigations of the Sol−Gel Synthesis of Fe3N and Fe3C N2 - Iron nitride (Fe3N) and iron carbide (Fe3C) nanoparticles can be prepared via sol−gel synthesis. While sol−gel methods are simple, it can be difficult to control the crystalline composition, i.e., to achieve a Rietveld-pure product. In a previous in situ synchrotron study of the sol−gel synthesis of Fe3N/Fe3C, we showed that the reaction proceeds as follows: Fe3O4 → FeOx → Fe3N → Fe3C. There was considerable overlap between the different phases, but we were unable to ascertain whether this was due to the experimental setup (side-on heating of a quartz capillary which could lead to thermal gradients) or whether individual particle reactions proceed at different rates. In this paper, we use in situ wide- and small-angle X-ray scattering (wide-angle X-ray scattering (WAXS) and small-angle X-ray scattering (SAXS)) to demonstrate that the overlapping phases are indeed due to variable reaction rates. While the initial oxide nanoparticles have a small range of diameters, the size range expands considerably and very rapidly during the oxide−nitride transition. This has implications for the isolation of Rietveld-pure Fe3N, and in an extensive laboratory study, we were indeed unable to isolate phasepure Fe3N. However, we made the surprising discovery that Rietveld-pure Fe3C nanoparticles can be produced at 500 °C with a sufficient furnace dwell time. This is considerably lower than the previous reports of the sol−gel synthesis of Fe3C nanoparticles. KW - Small-angle X-ray Scattering KW - SAXS KW - Diffraction KW - XRD KW - Scattering KW - Sol-gel KW - Iron nitride KW - Nanoparticles KW - Iron carbide KW - Catalyst KW - In-situ KW - Ex-situ KW - Synthesis KW - Synchrotron PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548226 DO - https://doi.org/10.1021/acs.inorgchem.1c03442 VL - 61 IS - 18 SP - 6742 EP - 6749 PB - ACS Publications CY - Washington AN - OPUS4-54822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fernandez, L. A1 - Esteves, V. I. A1 - Cunha, A. A1 - Schneider, Rudolf A1 - Tome, J. P. C. T1 - Photodegradation of organic pollutants in water by immobilized porphyrins and phthalocyanines N2 - New methods for water treatment are required as a result from an increasing awareness in the reduction of the pollution impact in the environment. In the perspective of the photo-oxidation of organic pollutants present in water, the principal incentive for the preparation of heterogeneous photocatalysts is their easy recovery from the reaction mixture, which allows their reuse in successive runs, minimizing the loss of their original photocatalytic properties. Different types of supports can be used in the immobilization of photoactive species, such as porphyrins (Pors) and phthalocyanines (Pcs). This mini-review will consider the different methodologies for the immobilization of Pors and Pcs and their photocatalytic performance in the photodegradation of organic pollutants in water, addressing also their recycling ability in successive water treatments. KW - Porphyrins KW - Phthalocyanines KW - Water treatment KW - Organic pollutants KW - Advanced oxidation processes KW - Heterogeneous photocatalysis KW - TiO2 KW - Microporous KW - Nanoparticles PY - 2016 DO - https://doi.org/10.1142/S108842461630007X VL - 2016 IS - 20 SP - 150 EP - 166 PB - World Scientific Publishing AN - OPUS4-38503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Natte, Kishore A1 - Friedrich, Jörg Florian A1 - Wohlrab, Sebastian A1 - Lutzki, J. A1 - von Klitzing, R. A1 - Österle, Werner A1 - Orts-Gil, Guillermo T1 - Impact of polymer shell on the formation and time evolution of nanoparticle-protein corona N2 - The study of protein corona formation on nanoparticles (NPs) represents an actual main issue in colloidal, biomedical and toxicological sciences. However, little is known about the influence of polymer shells on the formation and time evolution of protein corona onto functionalized NPs. Therefore, silicapoly(ethylene glycol) core–shell nanohybrids (SNPs@PEG) with different polymer molecular weights (MW) were synthesized and exhaustively characterized. Bovine serum albumin (BSA) at different concentrations (0.1–6 wt%) was used as model protein to study protein corona formation and time evolution. For pristine SNPs and SNPs@PEG (MW = 350 g/mol), zeta potential at different incubation times show a dynamical evolution of the nanoparticle–protein corona. Oppositely, for SNPs@PEG with MW ≥2000 g/mol a significant suppression of corona formation and time evolution was observed. Furthermore, AFM investigations suggest a different orientation (side-chain or perpendicular) and Penetration depth of BSA toward PEGylated surfaces depending on the polymer length which may explain differences in protein corona evolution. KW - Nanoparticles KW - Silica KW - PEGylation KW - Protein corona KW - BSA KW - Biointerface PY - 2013 DO - https://doi.org/10.1016/j.colsurfb.2012.11.019 SN - 0927-7765 VL - 104 SP - 213 EP - 220 PB - Elsevier AN - OPUS4-38547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meiling, T. A1 - Cywinski, P. A1 - Bald, Ilko T1 - White carbon: Fluorescent carbon nanoparticles with tunable quantum yield in a reproducible green synthesis N2 - In this study, a new reliable, economic, and environmentally-friendly one-step synthesis is established to obtain carbon nanodots (CNDs) with well-defined and reproducible photoluminescence (PL) properties via the microwave-assisted hydrothermal treatment of starch and Tris-acetate-EDTA (TAE) buffer as carbon sources. Three kinds of CNDs are prepared using different sets of above mentioned starting materials. The as-synthesized CNDs: C-CND (starch only), N-CND 1 (starch in TAE) and N-CND 2 (TAE only) exhibit highly homogenous PL and are ready to use without need for further purification. The CNDs are stable over a long period of time (>1 year) either in solution or as freeze-dried powder. Depending on starting material, CNDs with PL quantum yield (PLQY) ranging from less than 1% up to 28% are obtained. The influence of the precursor concentration, reaction time and type of additives on the optical properties (UV-Vis absorption, PL emission spectrum and PLQY) is carefully investigated, providing insight into the chemical processes that occur during CND formation. Remarkably, upon freeze-drying the initially brown CND-solution turns into a non-fluorescent white/slightly Brown powder which recovers PL in aqueous solution and can potentially be applied as fluorescent marker in bio-imaging, as a reduction agent or as a photocatalyst. KW - Carbon dots KW - Quantum yield KW - Fluorescence KW - Nanoparticles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-367204 DO - https://doi.org/10.1038/srep28557 VL - 6 SP - Article 28557, 1 EP - 9 PB - Nature Publishing Group AN - OPUS4-36720 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kjaervik, Marit A1 - Müller, Anja A1 - Dietrich, P. A1 - Thissen, A. A1 - Bahr, S. A1 - Ritter, B. A1 - Kemnitz, E. A1 - Unger, Wolfgang T1 - Detection of suspended nanoparticles with near-ambient pressure x-ray photoelectron spectroscopy N2 - Two systems of suspended nanoparticles have been studied with near-ambient pressure x-ray photoelectron spectroscopy: silver nanoparticles in water and strontium fluoride—calcium fluoride core-shell nanoparticles in ethylene glycol. The corresponding dry samples were measured under ultra high vacuum for comparison. The results obtained under near-ambient pressure were overall comparable to those obtained under ultra high vacuum, although measuring silver nanoparticles in water requires a high pass energy and a long acquisition time. A shift towards higher binding energies was found for the silver nanoparticles in aqueous Suspension compared to the corresponding dry sample, which can be assigned to a change of surface potential at the water-nanoparticle interface. The shell-thickness of the core-shell nanoparticles was estimated based on simulated spectra from the National Institute of Standards and Technology database for simulation of electron spectra for surface analysis. With the instrumental set-up presented in this paper, nanoparticle suspensions in a suitable Container can be directly inserted into the analysis chamber and measured without prior sample preparation. KW - Nanoparticles KW - Suspensions KW - Core-shell nanoparticles KW - NAP-XPS PY - 2017 DO - https://doi.org/10.1088/1361-648X/aa8b9d SN - 1361-648X SN - 0953-8984 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. VL - 29 IS - 47 SP - 474002, 1 EP - 474002, 9 PB - IOP Publishing CY - UK AN - OPUS4-42951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja A1 - Schneider, Markus T1 - Surface chemical analysis of engineered nanoparticles by means of transmission x-ray microscopy and mass spectrometry N2 - PTFE/PS core-shell-nanoparticles were characterised by STXM, T-SEM, and ToF-SIMS. Shell-thicknesses were calculated and compared. Preliminary results from ToF-SIMS showed the capabilities of this method. T2 - BAM-BfR Seminar CY - Berlin, Germany DA - 15.02.2018 KW - STXM KW - NEXAFS KW - ToF-SIMS KW - SEM KW - Nanoparticles PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-44181 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pignatelli, Giuseppe T1 - Effects of nanoparticles on laser ablation N2 - Introduction: Laser Induced Breakdown Spectroscopy (LIBS) is an atomic emission analytical technique, wide spreading in laboratories and industries. One way to dramatically increase its analytical results is to deposit metal NPs on the sample surface, resulting in an better version called Nanoparticle Enhanced LIBS (NELIBS). In order to better know and use this technique, the evolution of the plasma has been studied with Tomography. T2 - CHESS 2017 CY - Florence, Italy DA - 27.11.2017 KW - LIBS KW - Nanoparticles PY - 2017 AN - OPUS4-43476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beyer, Sebastian T1 - Colloidal metalorganic frameworks as novel biofunctional nanoparticles for immunoassay applications N2 - Metal-organic framework (MOF) colloids have unique features that render them ideal signalling agents for realizing advanced immunoassay-based detection systems. MOFs are porous coordination polymers of metal nodes and organic linkers. The pore size of MOFs can be engineered and tailored to allow specific host (MOF) and guest (analyte) interactions. The particle sizes of the colloidal MOF can be tailored by employing methods from colloidal chemistry in wet synthesis. The adaption of established Layer-by-Layer polyelectrolyte coating protocols [1] allows equipping colloidal MOF particles with a nanometer thin polyelectrolyte membrane. This polyelectrolyte membrane serves as an interface for antibody binding. These biofunctional MOF nanoparticles have shown a strong immuno-binding that is sufficient for solid state immunoassays. Our current research addresses the design of luminescence encoded colloidal particle libraries by adjusting the ratios of e.g. Terbium (green) and Europium (red) metal nodes in mixed lanthanide based MOF-76. These mixed lanthanide MOF-76 particles are envisioned to allow multiplexed immuno-detection of endocrine disruptors such as bisphenol A. In addition we investigate the detection of analytes that do not allow the production of antibodies due to their inherent properties. Such “difficult analytes” have a strong hydrophobicity or are very small or highly toxic molecules. One example is the common plasticizer dioctylphthalate that is also a potent endocrine disruptor. MOF colloids can address this issue by specific host (MOF) : guest (analyte) interactions that result in analyte-specific colour change or exciplex-based fluorescence emission. Our overall aim is to develop methodologies that allow parallel sensing of two endocrine disruptors (e.g. bisphenol A & phthalates) by simultaneous immuno-detection and MOF:analyte specific interactions. T2 - BioSensor 2017 - 1st European and 10th German BioSensor Symposium CY - Potsdam, Germany DA - 20.03.2017 KW - MOFs KW - Immunoassay KW - Nanoparticles PY - 2017 AN - OPUS4-43522 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - Chemical characterisation of (core-shell) nanoparticles using PCA assisted ToF-SIMS and XPS N2 - The analysis of nanomaterials is currently an important task - especially in case of risk assessment – as the properties of these material class are not well understood. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surface’s chemical composition must be investigated to get a better understanding and prediction of the nanomaterials’ behavior. ToF-SIMS and XPS have proven to be powerful tools to determine the general chemical composition. The superior surface sensitivity of ToF-SIMS furthermore allows us to study mainly the utmost atomic layers and thus gives us an idea of the interactions involved. Here, we present initial data on the analysis of Hyflon®-polystyrene core-shell nanoparticles which can be used as a model system due to the known preparation and a rather good chemical as well as physical separation of core and shell. Furthermore, results on Au nanoparticles with and without an antibody shell are presented. Principle component analysis (PCA) will be used to detect the influence of sample preparation and for a better separation of different samples. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - 3rd NanoSafety Forum for Young Scientists CY - Valetta, Malta DA - 08.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS PY - 2018 AN - OPUS4-46248 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - Chemical characterisation and classification of (Core-Shell) nanoparticles using PCA assisted ToF-SIMS N2 - The analysis of nanomaterials is currently an important task - especially in case of risk assessment – as the properties of these material class are not well understood and their growing use in everyday life. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surface’s chemical composition must be investigated to get a better understanding and prediction of the nanomaterials’ behaviour. ToF-SIMS and XPS have proven to be powerful tools to determine the general chemical composition. The superior surface sensitivity of ToF-SIMS furthermore allows us to study mainly the utmost atomic layers and thus gives us an idea of possible interactions involved. Supported by multivariate data analysis such as principal component analysis (PCA), the method can also be used for sub-classification of different materials using slight differences in surface chemistry. Here, we present data of the analysis of Hyflon®-polystyrene core-shell nanoparticles which can be used as a model system due to the known preparation and a rather good chemical as well as physical separation of core and shell. Principle component analysis (PCA) will be used to detect the influence of sample preparation and for a better separation of different samples. This is achieved by measurement of a statistically relevant set of samples for every particle sample. We acquired surface spectra under static SIMS conditions with Bi32+ and analysed the resulting spectra by PCA. The carefully selected and refined peaks allow a reasonable categorization and further a reliable allocation of blank feeds. In detail, the fluorine containing, organic fragments are an indication for a heterogeneous shell that has errors. Furthermore, results on Au nanoparticles with and without an antibody shell are presented. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - SIMS-Europe CY - Münster, Germany DA - 16.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS KW - PCA KW - Titania KW - Core-Shell PY - 2018 AN - OPUS4-46249 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas A1 - Schneider, Markus A1 - Schäpe, Kaija T1 - Classification of engineered Titania nanomaterials via surface analysis using principal component analysis (PCA) assisted Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) N2 - Due to the growing number of engineered nanomaterials (NM) the need for a reliable risk assessment for these materials is today bigger than ever before. Especially the nanomaterial’s surface or shell directly interacts with its environment and therefore is a crucial factor for NM’ toxicity or functionality. Especially, titania is one of the NM with the greatest technological importance. It is used for a large number of applications and can be found in food, cosmetics, glasses, mirrors, paints to mention only a few. In 2012, experts estimate[d] the annual European nano-titania production or utilization at an amount of more than 10,000 t. Great progress has been achieved in the area of NM investigation and characterization during the past decade. A variety of publications provide information about technological innovation as well as hazard potential, which means the potential risk on human health and ecosystems. However, enhanced data harmonization and well-defined standards for nanomaterial analysis, could significantly improve the reliability of such studies which often suffers from varying methods, parameters and sample preparations. To develop a suitable approach for the NM’s risk assessment, the ACEnano project aims at establishing a toolbox of verified methods. The size of this well-structured European project allows to handle even those big challenges like data harmonization and standardization. Due to its powerful combination of superior surface sensitivity and lateral resolution down to the Nano regime, ToF-SIMS could become one of these toolbox methods. Supported by multivariate data analysis such as principal component analysis (PCA), the method can be used for sub-classification of nanomaterial families using slight differences in surface chemistry. Here, we show a PCA supported classification of titania nanoparticles from various sources (NIST, JRC, BAM) with ToF-SIMS. Parameters like size, shell, pre-preparation and crystal system cause variance in the data and allow us to distinguish the species from each other. Moreover, this variance in the data also occurs and can be used for investigation when we compare our measurements of particle ensembles with those of grown titania films. The carefully selected and refined peaks allow a reasonable particle categorization and further a reliable allocation of blank feeds, which introduces a promising approach for NM characterization in the context of NM risk assessment. T2 - SIMS-Europe CY - Münster, Germany DA - 16.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS KW - PCA KW - Titania PY - 2018 AN - OPUS4-46250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - Chemical Analysis of Core-Shell Nanoparticles using ToF-SIMS and XPS N2 - The analysis of nanomaterials is current an important task - especially in case of risk assessment, as the properties of these material class are not well understood currently. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surfaces chemical composition has to be investigated to get a better understanding and prediction of the nanomaterials' behavior. ToF-SIMS has proven as a powerful tool to determine said chemical composition. Its superior surface sensitivity allows us to study mainly the utmost atomic layer and therefore gives us an idea of the interactions involved. Here, we show first result from the validation of the method for the analysis of polystyrene and gold nanoparticles. ToF-SIMS will be compared to other methods like XPS, T-SEM or REM. Furthermore, principle component analysis (PCA) will be used to detect the influence of different sample preparation performed by an innovative microfluidic device. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - DPG-Frühjahrstagung der Sektion Kondensierte Materie gemeinsam mit der EPS CY - Berlin, Germany DA - 11.03.2018 KW - XPS KW - ToF-SIMS KW - Nanoparticles PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-44790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - Chemical Analysis of Core-Shell Nanoparticles using ToF-SIMS and XPS N2 - The analysis of nanomaterials is currently an important task - especially in case of risk assessment – as the properties of these material class are not well understood. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surface’s chemical composition must be investigated to get a better understanding and prediction of the nanomaterials’ behavior. ToF-SIMS and XPS have proven to be powerful tools to determine the general chemical composition. The superior surface sensitivity of ToF-SIMS furthermore allows us to study mainly the utmost atomic layer and thus gives us an idea of the interactions involved. Here, we present initial data on the analysis of Hyflon®-polystyrene core-shell nanoparticles which can be used as a model system due to the known preparation and a rather good chemical as well as physical separation of core and shell. Furthermore, principle component analysis (PCA) will be used to detect the influence of sample preparation and for a better separation of different samples. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - XPS KW - ToF-SIMS KW - Nanoparticles PY - 2018 AN - OPUS4-44795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmitt, Johannes T1 - Data Acquisition System for Single Particle Inductively Coupled Plasma Mass Spectrometry (spICP-MS) with Nanosecond Time Resolution N2 - This study presents our data acquisition system prototype for spICP-MS with nanosecond time resolution (nanoDAQ) and a matching data processing approach for nanosecond resolved single particle spICP-MS data. The system continuously samples the secondary electron multiplier (SEM) detector signal with a dwell time of approximately 2 ns and enables the detection of gold nanoparticles (AuNP) as small as 7.5 nm[1] with a commercial single quadrupole ICP-MS instrument. The acquired transient data is processed based on the temporal distance between detector events and the event density. It was shown that the inverse logarithm of the distance between detector events is proportional to the particle size and that the number of detector events corresponding to a particle signal distribution can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion.[1] The high data acquisition frequency of the systems allows recording of a statistically significant number of data points in 60 s or less, which leads to the main time limitation for analyses being merely the sample uptake time and rinsing step between analyte solutions. T2 - 55th Annual Conference of the German Society for Mass Spectrometry CY - Freising, Germany DA - 10.03.2024 KW - Nanoparticles KW - Mass Spectrometry KW - Instrumentation KW - spICP-MS PY - 2024 AN - OPUS4-62315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schardt, Annika A1 - Schmitt, Johannes A1 - Engelhard, Carsten T1 - Single particle inductively coupled plasma mass spectrometry with nanosecond time resolution N2 - In this proof-of-principle study, we present our contribution to single particle inductively coupled plasma mass spectrometry (spICP-MS) developments with a novel in-house built data acquisition system with nanosecond time resolution (nanoDAQ) and a matching data processing approach. The new system can continuously sample the secondary electron multiplier (SEM) detector signal and enables the detection of gold nanoparticles (AuNP) as small as 7.5 nm with the commercial single quadrupole ICP-MS instrument used in this study. Recording of the SEM signal by the nanoDAQ is performed with a dwell time of approximately 4 ns. A tailored method was developed to process this type of transient data, which is based on determining the temporal distance between detector events that is denoted as event gap (EG). We found that the inverse logarithm of EG is proportional to the particle size and that the number of detector events corresponding to a particle signal distribution can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. Due to the high data acquisition frequency, a statistically significant number of data points can be obtained in 60 s or less and the main time limitation for analyses is merely the sample uptake time and rinsing step between analyte solutions. At this stage, the data processing method provides average information on complete data sets only and will be adapted to enable particle-by-particle analysis with future hardware/software revision. KW - ICP-MS KW - Nanoparticles KW - Nanosecond time resolution KW - Single particle detection PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612706 DO - https://doi.org/10.1039/d3ja00373f SN - 1364-5544 SN - 0267-9477 VL - 39 IS - 2 SP - 389 EP - 400 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-61270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -