Filtern
Erscheinungsjahr
Dokumenttyp
- Zeitschriftenartikel (135)
- Vortrag (91)
- Posterpräsentation (55)
- Forschungsdatensatz (9)
- Beitrag zu einem Sammelband (8)
- Beitrag zu einem Tagungsband (7)
- Sonstiges (7)
- Forschungsbericht (6)
- Handbuch (4)
- Sammelband (Herausgeberschaft für den kompletten Band) (2)
Schlagworte
- Nanoparticles (326) (entfernen)
Organisationseinheit der BAM
- 6 Materialchemie (165)
- 6.1 Oberflächen- und Dünnschichtanalyse (130)
- 1 Analytische Chemie; Referenzmaterialien (35)
- 6.3 Strukturanalytik (20)
- 1.2 Biophotonik (16)
- 6.5 Synthese und Streuverfahren nanostrukturierter Materialien (16)
- 5 Werkstofftechnik (10)
- 6.6 Physik und chemische Analytik der Polymere (10)
- 1.1 Anorganische Spurenanalytik (9)
- 5.1 Mikrostruktur Design und Degradation (5)
Paper des Monats
- ja (2)
Eingeladener Vortrag
- nein (91)
The mechanism of action of zirconium permanent modifiers on graphite surfaces was investigated in order to understand its influence on the analytical signal in atomic and molecular absorption spectrometry (AAS/MAS). For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEMEDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. We propose here a mechanism, where ZrO2 acts as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. No evidence of the formation of zirconium carbide was found. Consequently, as the CaF formation is catalysed by a heterogeneous catalyst, surface modifications with ZrO2 nanoparticles and ZrO xerogels were investigated in order to increase the surface area. Their influence was evaluated in the molecule formation of CaF, CaCl, CaBr, and CaI. Graphite furnace modification with zirconium oxide nanoparticles proves to be the best choice for fluorine analysis with a signal enhancement of more than eleven times with respect a non-coated graphite furnace. However, the influence of zirconium modifications in the analytical signals of Cl, and I is lower than the F signals or even negative in case of the Br. Understanding zirconium modifiers as heterogeneous catalysts offers a new perspective to AAS and MAS, and reveals the potential of surface analytical methods for development of improved permanent modifiers and graphite furnace coatings.
We have applied laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) with subcellular resolution as an elemental mass microscope to investigate the distributions of Ag nanoparticles (NP) in a 3-dimentional multicellular spheroid (MCS) model. The production of MCS has been optimized by changing the seeding cell number (500 to 40,000 cells) and the growth period (1 to 10 days). Incubations of MCS with Ag nanoparticle suspensions were performed with a concentration of 5 µg mL-1 for 24 hours. Thin-sections of the Eosin stained MCS were analysed by elemental mass microscopy using LA-ICP-MS to image distributions of 109Ag, 31P, 63Cu, 66Zn and 79Br. A calibration using NP suspensions was applied to convert the measured Ag intensity into the number of particles being present in each measurement pixel. The numbers of NP determined ranged from 30 up to 4,000 particles in an enrichment zone. The particle distribution was clearly correlated to 31P, 66Zn and 79Br and was localized in an outer rim of proliferating cells (confirmed by DAPI) with a width of about two-single cell diameters. For the highest seeding cell number NPs were only detected in this outer rim, whereas small molecules as for instance 79Br and 109Ag ions were detected in the core of the MCS as well. Aniline blue staining demonstrated that this outer rim was rich in collagen structures in which fibroblast cells were embedded and a thin-membrane was visible which separated the core from the biological active cell layer functioning as biological barriers for NP transport. In this presentation, we will show the possibility using this 3-dimensional model for toxicological and medical applications.
The content of the paper is the assessment of the performance of (conventional) measurement techniques (MTs)with respect to the classification of disperse materials according to the EC recommendation for a definition of nanomaterial. This performance essentially refers to the accurate assessment of the number weighted median of (the constituent) particles. All data and conclusions are based on the analytical study conducted as real-world performance testing.
It comprised different types of MTs (imaging, counting, fractionating, spectroscopic and integral) as well as different types of materials. Beside reference materials with well-defined size distribution the study also included several commercial powders (variation of particle composition, morphology, coating, size range and polydispersity). In order to ensure comparability of measurement results, the participants were guided to use uniform protocols in sample preparation, conducting measurements, data analysis and in reporting results. Corresponding documents have been made public, in order to support the reviewing process of the paper, respectively to ensure the reproducibility of data by other users under the same conditions.
The scientific paper relies on a comprehensive set of revised measurement data reported in uniform templates, completely describes the experimental procedures and discusses the MTs’ performance for selected materials in detail. Even more, the study is summarised and evaluated, which leads to recommendations for the use of MTs within a tiered approach of NM characterisation. In addition, the paper critically examines the factors that may affect the outcome of such a comparison among different MTs.
A variety of methods used to prepare nano-objects for surface analysis are described along with information about when they might be best applied. Intrinsic properties of NPs which complicate their characterization and need to be considered when planning for surface or other analyses of NPs are identified, including challenges associated with reproducible synthesis and functionalization of the particles as well as their dynamic nature. The relevant information about the sample preparation processes, along with analysis details and data that need to be added to the collection of material provenance information is identified. Examples of protocols that have been successfully used for preparation of nano-objects for surface analysis are included in an annex.
Due to the recent widespread application of nanomaterials to biological systems, a careful consideration of their physiological impact is required. This demands an understanding of the complex processes at the bio–nano interface. Therefore, a comprehensive and accurate characterization of the material under physiological conditions is crucial to correlate the observed biological impact with defined colloidal properties. As promising candidates for biomedical applications, two SiO2-based nanomaterial systems were chosen for extensive size characterization to investigate the agglomeration behavior under physiological conditions. To combine the benefits of different characterization techniques and to compensate for their respective drawbacks, transmission electron microscopy, dynamic light scattering and asymmetric flow field-flow fractionation were applied. The investigated particle systems were (i) negatively charged silica particles and (ii) poly(organosiloxane) particles offering variable surface modification opportunities (positively charged, polymer coated). It is shown that the surface properties primarily determine the agglomeration state of the particles and therefore their effective size, especially under physiological conditions. Thus, the biological identity of a nanomaterial is clearly influenced by differentiating surface properties.
The main objective was to assess homogeneity of two bimodal gold materials, namely nPsize1 and nPSize2, containing approximately 1:1 and 10:1 particle number-based ratio of ~30nm and ~60nm particles. Particle number-based concentration within the two size fractions was determined with spICP-MS using the particle frequency method of calibration.
One aim of the EMPIR nPSize project 17NRM04 was to develop and validate three classes of candidate reference (test) materials (RTMs), with i) well-defined non-spherical shape, ii) relatively high polydispersity index, and iii) accurate particle concentrations.
To fulfil the requirements of the project, 11 different types of materials were prepared. Following the initial assessment of the materials suitability, nPSize5_PT_UNITO, nPSize6_AC_UNITO and nPSize7_GN_CEA materials were found unsuitable for the project, due to various reasons. PT material was deemed unsuitable due to its predominantly agglomerated nature. AC material contained relatively high amount of impurities (other particle forms). GN material was found too heterogeneous in both the length and width for the purpose of the project. The remaining 8 candidate RTMs were assessed for their homogeneity and stability and used for successful delivery of the associated activities within the nPSize project.
Nanometer- and micrometer-sized particles are of increasing importance for a wide range of applications in the material and life sciences. This includes carriers for, e.g., drugs as well as dye molecules for use as multichromophoric reporters for signal enhancement in optical assays, platforms for DNA sequencing, and the fabrication of nanosensors and targeted probes for bioimaging studies.
Application-relevant properties of such particles include their size (and size distribution), shape, colloidal stability, biocompatibility, and ease of subsequent functionalization, e.g., with linkers, sensor molecules, and targeting ligands. The latter requires knowledge of the number of groups effectively accessible for subsequent coupling reactions and hence, selective and sensitive methods of analysis, which can be ideally employed for the characterization of a broad variety of particle systems independent of their optical properties, i.e., scattering or the presence of encoding dyes. For product control, robust, reliable and fast methods performable with inexpensive equipment are prefered.
In this respect, we studied a variety of conventional labels for optical readout, utilizing changes in intensity and/or color of absorption and/or emission. In addition, we developed a platform of cleavable and multimodal labels for optical assays which consist of a cleavable linker and an optically active reporter moiety. In contrast to conventional reporters measured directly at the particle surface, which are prone to signal distortions by scattering and encoding dyes, these cleavable labels can be detected colorimetrically or fluorometrically both bound at the particle surface and after quantitative cleavage of the linker in the transparent supernatant. Moreover, they enable straightforward validation by method comparison with elemental analysis, ICP-OES or ICP-MS.
Here, we present representative examples of newly synthesized cleavable labels and their application for the quantification of amino, thiol and carboxy surface groups on different nanomaterials and compare these results with measurements using conventional optical labels.
Encapsulation of hydrophobic dyes in polystyrene micro- and nanoparticles via swelling procedures
(2011)
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.
A series of different nanoparticle suspensions (Gold, Latex, and SiO2 in varying concentrations) were microprinted onto TEM grids in a 4 x 4 array in the concentration range 7x10^8 to 1x10^11 NP/mL and imaged with SEM and TSEM. Concentrations and printing conditions (temperature, relative humidity) were varied in order to minimize the coffee ring effect.