Chemische Charakterisierung und Spurenanalytik
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Eingeladener Vortrag
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The transition from X-ray film to digital detectors in radiography is accompanied by an increase of unsharpness due to the larger inherent digital detector unsharpness in comparison to film. The basic spatial resolution of digital detectors (see EN ISO 17636-2) is used today to describe this unsharpness. The geometrical unsharpness of the radiographic projection of object structures onto the detector plane is determined by the focal spot size of the X-ray tube and the magnification. The focal spot size is measured today (see ASTM E 1165) from pin hole camera exposures or edge unsharpness (see ASTM E 2903). The final image unsharpness is a result of a convolution of the geometrical and inherent detector unsharpness function, divided by the magnification factor of the object onto the detector plane. Different approximations of this convolution result in ASTM E 1000 and ISO 17636-2 in different optimum values for the magnification factor for a given focal spot size of a X—ray tube and the basic spatial resolution of the detector. The higher contrast sensitivity, an advantage of digital radiography, compared to film radiography is furthermore improved when using higher X-ray voltages as used with film and smaller focal spots of the X-ray tubes. This allows a higher distance between object and detector resulting in reduced object scatter in the image. The interactions between all these parameters will be discussed and simple rules for practitioners will be derived in this contribution.
Nowadays, different nanoparticles have been developed for commercial applications. However, since data on toxicity are barely available, their increasing application in cosmetic products, food and their release in the environment might cause severe problems. An accurate separation, identification and characterization of nanoparticles becomes increasingly important1,2.
In this presentation, a two-dimensional separation approach based on AF4 and CE was showed and used to separate NPs with similar sizes but different coatings. Standard reference polystyrene NPs having comparable core sizes but different coatings were investigated. Different migration time and profiles were compared. Separation in either method resulted in non-baseline resolved or non-separated peaks. In contrast, two-dimensional coupling of AF4 and CE resulted in clearly separated regions in their 2 D plots in case of 20 and 50 nm particle mixtures, whereas the 100 nm NP mixture could not be separated. Various factors affecting the separation like hydrodynamic diameter or SDS concentration were discussed.
Future investigations will be focussed on inorganic NPs with differently charged coatings. There, AF4-CE coupling can be coupled with inductively coupled plasma mass spectrometry (ICP-MS) to enhance the sensitivity of this method.
Nowadays, different nanoparticles have been developed for commercial applications. However, since data on toxicity are barely available, their increasing application in cosmetic products, food and their release in the environment might cause severe problems. An accurate separation, identification and characterization of nanoparticles becomes increasingly important.
A common method for nanoparticle separation, which was introduced in 1976 by Giddings, represents asymmetrical field-flow fractionation (AF4). It is a flow based separation method, which can be theoretically used to separate particles range from 1 nm to 50 µm. However, when the particles are smaller than 10 nm, separation with AF4 will become difficult to perform. Because in this case strong separation force, which induces aggregation of particles, should be applied. This will decrease recoveries of analytes and limit its application in accurate quantitative analysis. Capillary electrophoresis (CE) is another well-developed separation technique, in which samples will be separated in relation to their electrophoretic mobility. In recent years, CE has been used to separate different kinds of nanoparticles like, gold colloids or CdSe Quantum dots. However, till now only separation of particles smaller than 50 nm was reported. Because large size distribution of bigger particles will result in strong peak broadening and long separation time.
A two-dimensional coupling of AF4 and CE might provide us a new separation method, which can extend the separation ranges of both methods and be a way to characterise particles with large size distributions.
Nowadays, different nanoparticles have been developed for commercial applications. However, since data on toxicity are barely available, their increasing application in cosmetic products, food and their release in the environment might cause severe problems. An accurate separation, identification and characterization of nanoparticles becomes increasingly important.
A common method for nanoparticle separation, which was introduced in 1976 by Giddings, represents asymmetrical field-flow fractionation (AF4). It is a flow based separation method, which can be theoretically used to separate particles range from 1 nm to 50 µm. However, when the particles are smaller than 10 nm, separation with AF4 will become difficult to perform. Because in this case strong separation force, which induces aggregation of particles, should be applied. This will decrease recoveries of analytes and limit its application in accurate quantitative analysis. Capillary electrophoresis (CE) is another well-developed separation technique, in which samples will be separated in relation to their electrophoretic mobility. In recent years, CE has been used to separate different kinds of nanoparticles like, gold colloids or CdSe Quantum dots. However, till now only separation of particles smaller than 50 nm was reported. Because large size distribution of bigger particles will result in strong peak broadening and long separation time.
A two-dimensional coupling of AF4 and CE might provide us a new separation method, which can extend the separation ranges of both methods and be a way to characterise particles with large size distributions.
The accumulation of plastics leaked into the environment achieve a high perception in the last years. It is uncontroversial that often an uncontrolled, high consumption of plastic products and a poor waste management resulted in plastic findings all over in the environment. However, less is known about the relevant pathways and fate of plastic in the environment. Especially plastic fragments smaller 5 mmm, so called microplastics, achieve a high attention, because their amount and risks arising from these fragments are still unknown. The basic mechanisms of plastic or more precise, of different polymer degradation processes are often not considered, resulting in unrealistic statements.
For generation of fundamental understanding of this problem we developed in the last years a fast thermoanalytical method for identification and mass quantification of microplastics in complex samples. The presentation will also give a short introduction about polymer degradation.
This presentation gives a short overview of isotope ratio measurements being carried out in the past few years at BAM in different fields such as plant metabolism, food web structures and archaeology. The corresponding isotope reference materials which have been certified at BAM in parallel are presented as well. Additionally an outlook is being provided on future iRM projects.
Environmental sustainability and –stability of Materials concerning the Migration of pollutants
(2018)
MaUS is an acronym for ”Material und Umweltsimulationen“. Plastics are in the focus of environmental politics due to their long-term behaviour and therefore to their persistence. Not only that they appear as visible contaminants in the sea and on the beach, but their unknown behaviour concerning their additives as well as the related transformation products are anxious. Therefore, we wish to establish a certified reference method to provide a method for testing plastics.
Aim of this project is the development of fast motion standard reference methods for testing plastics regarding to their environmental compatibility. To establish these testing methods, we use polystyrene (PS) and polypropylene (PP) with environmental relevant brominated flame retardants, known for their persistent bioaccumulative and toxic (PBT) properties. In case of PS the material contains 1 wt% of 1,2,5,6,9,10-hexabromocyclododecan (HBCD) and in case of PP 0.1 wt% bromodiphenylether (BDE-209), which is known as a substance of very high concern (SVHC). Furthermore, we use polycarbonate (PC), which is still used as material in baby flasks and releases Bisphenol A (BPA), an estrogenic active substance.
As an additional material PTFE is used for its importance as a source for two ubiquitous environmental substances (PFOS and PFOA), whose toxicological effects are still incompletely known.
The focus in this current work is set on the transfer of potential pollutants out of applied materials mentioned above into environmental compartments like water or soil. Here an accelerated aging concept should be developed to shortened time consuming natural processes. For these resulting simulations we use a programmable weathering chamber with dry and wet periods and with high and low temperatures. These programmes run for several weeks and according to a defined sampling schedule we take water samples, run a clean-up procedure by SPE (Molecular imprinted polymers (MiPs) resp. polymer-based cartridges (Waters Oasis HLB)) and analyse them by HPLC-UV resp. LC-MS/MS. Of most interest in case of flame retardants are photocatalytic transformation products. Therefore, we conduct a non-target-screening resp. a suspected target-screening by LC-MS/MS and HRMS.
The analysis of non-metals normally is carried out using elemental analysers which require reference material for calibration. In the lecture the CRM-program of BAM suitable for non-metal-analysis is presented. There are CRMs available with non-metal contents in the low ppm up to the high percent region.
Surface functionalization of nanomaterials is nowadays at the core of many applications of functional materials in the life and material sciences. Examples range from membranes and microarrays over bead-based assays, and next generation sequencing to nanometer-sized optical reporters, nanosensors, and magnetic and optical contrast agents. Typical function-nalization steps include silanization and grafting reactions with reactive monomers to introduce functional groups like amino or carboxylic acid groups or the attachment of ligands like polyethylene glycol (PEG) molecules and biomolecules. [1-3] This enables to tune e.g., dis-persibility, hydrophilicity and biocompatibility, minimize unspecific interactions, improve biofunctionalization efficiencies, and enhance blood circulation times and allows for the use of nanomaterials as reporters in assays or the design of targeted probes for bioimaging.
At the core of all functionalization strategies are reliable and validated methods for surface group and ligand quantification that can be preferably performed with routine laboratory instrumentation, require only small amounts of substances, and are suitable for many different types of nanomaterials. [3] There is meanwhile a considerable need to make these methods traceable. We present here versatile and simple concepts for the quantification of common functional groups, ligands, and biomolecules on different types of organic and inorganic nanomaterials, using conventional and newly developed cleavable and multimodal reporters, that can be detected with optical spectroscopy. [4-7] These reporters are chosen to enable method validation with the aid of method comparisons and mass balances. Also, strategies how to make these simple assays traceable to SI units using quantitative nuclear resonance spectroscopy (qNMR) and X-ray photoelectron spectroscopy (XPS) are derived.
Analytical Sciences has developed from Ostwald’s “unentbehrlichen Dienstmagd” to a chemical discipline at the core of many of today’s fundamental and applied scientific problems and innovations. An atomic or molecular understanding of basic processes in chemistry, soft matter physics, materials and life science is enabled only through new analytical methods and instrumentation. Similar observations can be found for pressing sociopolitical conflicts of the future: A rational discussion of global climate change or new energy sources is only possible with reliable analytical results. Progress in Analytical Sciences is only possible if the underlying interdisciplinary character is acknowledged and valued. The talk will illustrate the scope of modern Analytical Science through examples from process analysis relevant to modern process intensification and industry 4.0 to bioanalysis and the use of synchrotron radiation to elucidate fundamental reactions materials.
An improved algorithm for calibration-free laser induced breakdown spectroscopy (CF LIBS) will be presented which includes several novel features in comparison with previously proposed similar algorithms. In particular, it allows using spectral lines with arbitrary optical thickness for the construction of Saha-Boltzmann plots, retrieves the absorption path length (plasma diameter) directly from a spectrum, replaces the Lorentzian line profile function by the Voigt function, and allows for self-absorption correction using pre-calculated and tabulated data rather than approximating functions. The tabulated data embody the solutions of the radiative transfer equation for numerous combinations of optical thicknesses and line widths. The algorithm is thoroughly verified using synthetic spectra.
Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic, metal-organic, and inorganic compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms often remain unclear. In the last years, we have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy. A further development is the in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time. [5] Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. Based on these data, metastable polymorphs of cocrystals and coordination polymorphs could be isolated and struc-turally characterized. A multi-step diffusion mechanism was identified for most systems. Crystalline phases were obtained intermediately, suggesting that the synthesis is following Ostwald’s rules of stages. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses.
Neurodegenerative diseases are one of the major problems for our ageing society. Alzheimer’s disease (AD) as the most common neurodegenerative disorder affects over 46.8 million people worldwide and the number will increase as the population ages. The diagnosis of AD is challenging and only half of the patients are identified yet and often only in late stages. One reason is that existing assays for identification and quantification of AD biomarkers lack accuracy and are poorly comparable.
This study is part of the EU project “ReMiND” aiming to develop accurate, reliable and traceable methods for the detection and quantification of known and suspected AD biomarkers. Our target is the tau protein, as brain load and distribution of tau is highly correlated with the clinical progression of AD. We intend to develop a measurement method for the accurate quantification of tau by means of inductively coupled plasma mass spectrometry (ICP-MS).
ICP-MS is a powerful method for the matrix independent quantitative analysis of target elements. Developed for the use in inorganic trace analysis, ICP-MS is nowadays emerging as a valuable tool for bioanalytical questions. Especially the use of ICP-MS for quantitative proteomics by measuring heteroatoms is highly promising, considering that established quantification methods like organic mass spectrometry depend on the existence of matched protein and peptide standards or labelling of the target protein. In this work, we applied isotope dilution analysis (IDA) using ICP-MS to quantify proteins of known stoichiometry via their sulphur content. Sulphur is present in two amino acids, cysteine and methionine, and hence is omnipresent in nearly all proteins. A NIST standard bovine serum albumin (BSA) was quantified using sulfur IDA to optimize sample preparation and method parameters. Our goal is to employ the developed method in a proof of concept study for the quantification of the AD biomarker tau extracted from brains of a mouse model for AD.
Many current nanomaterials can serve as contrast agents in cellular or tissue imaging, drug delivery vehicles or therapeutics, whereas others can cause toxic effects. In order to evaluate nano-bio interactions, the number of nanoparticles (NPs) inside cells as well as their localisation within cellular substructures is of particular interest. The cellular uptake depends on the primary characteristics of the NPs (e.g. size, shape, surface coating) and on the cell type.
Laser ablation inductively coupled plasma mass spectrometry (LA‑ICP‑MS) is more and more used to study the NP pathway from uptake, via intracellular processing up to cell division. High-spatial resolution laser ablation at single cell level is achieved using novel low-dispersion LA chambers and by careful optimisation of laser energy, ablation frequency and scan speed at small laser spot sizes down to 1 µm. Different examples from BAM, Division 1.1 and cooperation partners using LA-ICP-MS to localize and quantify metal-containing nanoparticles are shown. The results demonstrate the potential of LA-ICP-MS providing insight into NP uptake, intracellular distribution and cell-to-cell variation.
qNMR provides the most universally applicable form of direct concentration or purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. The workshop presents basic terms of statistics and uncertainty analysis, which are the basis for qNMR spectroscopy and data analysis such as, e.g., standard deviations, linear regression, significance tests, etc. and gives typical examples of applications in qNMR spectroscopy.