Chemische Charakterisierung und Spurenanalytik
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Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (59)
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Eingeladener Vortrag
- nein (83)
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.
Gold ist eines der sieben schon im Altertum bekannten Metalle und wurde wg. seines Glanzes und seiner Seltenheit von alters her als Tauschmittel und zur Herstellung von Schmuck benutzt. Außerdem ist es einfach bearbeitbar und weitestgehend gegen chemische Einflüsse resistent. Die Untersuchungen von Gold mit synchrotronstrahlungsangeregter Röntgenfluoreszenzanalyse sind zerstörungsfrei und geben Auskunft über die in der untersuchten Probe vorhandenen chemischen Elemente. Bei den hier vorgestellten Untersuchungen an der BAMline stehen Fragestellungen wie Herkunft, Herstellungsverfahren und Zusammengehörigkeit von Goldfunden im Vordergrund. Die verschiedenen Fragestellungen werden an einer Reihe von Beispielen erläutert die vom Wikingerschatz aus Hiddensee über die Himmelsscheibe von Nebra bis hin zu Funden aus Ägypten langen. Zusätzlich werden die modernen Messmethoden vorgestellt, die am Synchrotron heutzutage zur Verfügung stehen.
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.
The Color X-ray Camera CXC or SLcam® is an energy-resolving X-ray camera capable of energy- and space-resolved measurements. It consists of a high-speed CCD detector coupled to a polycapil-lary optic that conducts the X-ray photons from the probe to distinct pixels onto the detector. The camera is capable of fast acquisition of spatially and energy resolved fluorescence images. A dedicated software enables the acquisition and the online processing of the spectral data for all 69696 pixels, leading to a real-time visualization of the elements distribution in a sample. It was developed in a joint project with BAM, IFG Berlin and PN Sensors. In this contribution we will mainly discuss the use of the CXC at our beamline, the BAMline at BESSY II and imaging applications of the CXC from different areas, like biology and archaeometry. Additionally new developments for the use of the detector without optics, like wavelength dispersive detection or 1shot-XANES, will be presented.
X-ray absorption fine structure spectroscopy (XAFS) is a frequently employed technique in order to investigate structural composition and change of chemical compounds such as catalytic species. These structural properties are essential (i) to understand underlying reaction mechanism and (ii) to further improve the design of efficient catalysts.
This investigation is based on a newly developed XAFS setup comprising both time- and lateral-resolved XAFS information simultaneously in a single-shot (S2XAFS). The primary broadband beam is generated by a filter/X-ray-mirror combination (bandpass). The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by an area sensitive detector with a theta to 2 theta geometry. This facile, stable and scanningless setup was tested at the BAMline @ BESSY-II (Berlin, Germany).
This contribution focuses on further experimental optimizations allowing the characterization of supported vanadium oxide (VOx) based catalysts at the lower hard X-ray regime (5 to 6 keV). First S2XAFS measurements of these catalysts are presented herein. Supported VOx catalysts show promising results in the oxidation of methane to formaldehyde.
S2XAFS allows determining the structural composition of the metal (i.e. vanadium) based on a fast and smart setup. It is therefore an ideal tool to identify crucial roles of chemical compounds in catalytic reactions.
XAFS@BAMline
(2018)
X-ray Absorption fine structure spectroscopy (XAFS) is a frequently employed technique in order to investigate structural composition and Change of chemical compounds such as catalytic species or corrosion processes. These structural properties are essential (i) to understand underlying reaction mechanism and (ii) to further improve the design of materials.
While XAFS measurements are usually performed with ionization Chambers or simple fluorescence detectors, we at BAMline specialize in measurements with innovative set-ups that meet Specialrequirements such as time resolution, (3D-) spatial Resolution or demanding sample environments.
This contribution presents various available XAFS configurations with their corresponding applications. In particular, these comprise single -shot XAFS for time- resolved measurements, grazing-exit XAFS with energy and a spatially resolved detector for the characterization of thin films and an in situ grazing incidence Setup for the characterization of corrosion layers.
Additionally,the possibility of analyzing Minute samples in total-reflection geometry is demonstrated.
To establish the SI traceability of the element content w(Hg) of a gravimetrically prepared 1 g/kg mercury solution, the latter was compared to a primary reference solution by means of high accuracy inductively coupled plasma optical emission spectrometry (ICP OES) measurements. For this purpose, the ICP OES bracketing method previously described [1] was improved to yield a relative expanded uncertainty of the mercury element content of Urel(w(Hg)) = 0.5 % (with k = 2) associated with the comparison of two monoelemental solutions. In case of mercury, such a small uncertainty was achieved for the first time. Before, in general, such small uncertainties were only reported applying isotope dilution methods performed with MC-ICP-MS. However, for mercury solutions at this concentration range, several dilution steps are necessary to prepare the samples for ID-MC-ICP-MS. The sum of the uncertainty contributions stemming from the dilution steps, as well as the intrinsic difficulties of measuring mercury at low concentrations, result in an overall uncertainty of the ICP-MS measurements, which is comparable to or even larger than those, achieved with the ICP OES method applied. We will present details of the sample preparation as well as of the dedicated ICP OES measurement approach, which were crucial to achieve such a small measurement uncertainty.
The newly developed method was successfully applied in the context of the development and production of elemental solution chemical reference standards (CRS), which are distributed by the EDQM. The CRS are intended to support measurements required by the European Pharmacopoeia, which has recently incorporated a new international guideline for the control of elemental impurities in medicinal products.
Analytical glow discharges with optical (GD-OES) and mass spectrometric (GD-MS) detection are able to obtain depth resolved information about the light elements hydrogen, carbon, nitrogen and oxygen in solid samples, where most of the other analytical techniques fail. However, the interpretation or even quantification of the measured signals is still very challenging. Problems arise due to physical effects (plasma processes such as the ‘Hydrogen effect’, the Doppler effect, self absorption or diffusion of hydrogen in the sample during sputtering) chemical effects(e.g. formation of compounds with argon or the matrix, poisoning of the sample or gettering) as well as instrumental difficulties (e.g. of the sensitivity, calibration and vacuum quality)..
The GD techniques are direct solid sampling methods and require reference materials for calibration. Unfortunately the list of available certified reference materials (CRM) suited for calibration of light elements in different matrix is relatively short Therefore, sintered materials doped with the analytes H2, O2 and N2 were produced at IFW Dresden and applied as calibration standards for hydrogen, oxygen and nitrogen. Due to the high analyte concentration added, it is very likely that the real concentration agree well with the added amount of light elements in the corresponding phases. The validation of the determination of the light element concentration in the sintered samples was possible in some cases only due to the lack of suitable techniques. This fact proves the need for the development of a reliable quantification of light elements by GDS.
A systematic dependence of the sputtering rate on the composition was found and can be explained by basic principles.
Using mixtures of TiH2 and ZrH2 with Cu the ratio of hydrogen and Cu lines has a good correlation with the corresponding concentration ratio. The hydrogen emission yield however decreases over 0.3 m% hydrogen and finally the hydrogen intensity may even decrease. This behaviour can be explained by a very similar quenching of the hydrogen and copper intensity caused by the hydrogen effect. First experiments with GD-MS show no saturation of the hydrogen ion current and thus confirm the quenching of the emission yield in GD-OES.
Sintered material for the oxygen calibration (Al2O3, CuO, Cu2O and MgO mixed with Cu, Al and Mg) confirmed the blue line shift effect at O I 130.22 nm, first time reported by Köster 2009 [1]. The effect is more pronounced at Mg than in Al and Cu, which due to line interference leads to a matrix dependent EY. This effect is negligible at O I 777.19 nm and the EY is matrix independent. Using GD-MS first promising results for the calibration of oxygen with these sintered samples could be obtained, when the sputtering rate was included in the evaluation.
More recently also sintered material for nitrogen calibration (AlN mixed with Al and Si3N4 mixed with Cu) was produced and points to a matrix independent emission yield of nitrogen
Reference materials are essential, when the accuracy and reliability of measurement results need to be guaranteed in order to generate confidence in the analysis.
These materials are frequently used for determining measurement uncertainty, for validation of methods, suitability testing and quality assurance. Especially direct solid sampling methods require reference materials for calibration.
They guarantee that measurement results can be compared to recognized reference values.
This presentation gives an overview about the use of GDMS in various certification procedures. Because it represents a fast, sensitive, multielement analyses technique without extensive sample preparation it plays a special role for the purity determination of high purity standards. Various calibration strategies and the preparation of traceable matrix matched calibration standards will be discussed.
For the certification of analyte content in matrix materials mainly techniques with solvent sample preparation are used. Here GD-MS is used to identify possible loss or contamination with analytes during the sample preparation step. Typically used acids to dissolve matrices lead to interferences in the ICP- mass spectrometric detection of various analytes and their quantification. Here GD-MS as direct method can also add an important contribution in the certification process.
Laser induced plasma (LIP) is a highly dynamic, short living event which presents significant difficulty for both diagnostics and modeling. The former requires precise spatially- and time-resolved measurements on a micron-nanosecond scale while the latter needs numerous descriptive parameters; many of them can only be obtained from experiment. Diagnostics and modeling should always complement each other for obtaining a truthful picture of LIP.
In this presentation, a newly developed collisional-dominated model will be presented. The model is based on the coupled Navier-Stokes, state, radiative transfer, material transport, and chemical equations. The model incorporates plasma chemistry through the equilibrium approach that relies on atomic and molecular partition functions. Several chemical systems are modeled including Si-C-Cl-N and B-H-Cl systems.
The model is used to study the equilibrium states of the systems as functions of the concentrations of plasma species and plasma temperature. The model also predicts the evolution of number densities of atomic and molecular species in the expanding plasma plume.
This course will provide an introduction to plasma diagnostic techniques. The major focus of the course will be on the discussions of the practical procedures as well as the underlying physical principles for the measurements of plasma fundamental characteristics (e.g., temperatures, thermodynamic properties, and electron number density). Particular emphasis will be placed on inductively coupled plasma–atomic emission spectrometry, but other analytical plasmas will also be used as examples when appropriate. Selected examples on how one can manipulate the operating conditions of the plasma source, based on the results of plasma diagnostic measurements, to improve its performance used for spectrochemical analysis will also be covered. Topics to be covered include thermal equilibrium, line profiles, temperatures, electron densities, excitation processes, microreactions, pump and probe diagnostics, tomography, temporal and spatial resolution. Basics of plasma computer modeling will be presented.
Generell ist es Ziel der Prozessführung, Reaktions- und Trennprozesse wirtschaftlich optimal zu betreiben. Hierzu werden in großen Anlagen modellbasiere Echtzeitoptimierungsverfahren (Real-time Optimization, RTO) eingesetzt. Die Qualität der Ergebnisse der Optimierung hängt dabei entscheidend von der Güte des verwendeten Modells ab. Die Entwicklung hochgenauer Modelle ist allerdings aufwändig, was für kleine Produktionsvolumina ein wesentliches Hindernis zur Nutzung solcher Methoden darstellt. Mit Hilfe der sogenannten Modifier-Adaptation ist eine iterative Betriebspunktoptimierung auch mit ungenauen Modellen möglich, wenn Messungen der für die Bewertung relevanten Größen (beispielsweise Produktkonzentrationen im Ausgangsstrom) verfügbar sein. Für eine Lithiierungsreaktion in einem bei INVITE kontinuierlich betriebenen Reaktor wurde im Rahmen des EU-Projekts CONSENS eine solche iterative Optimierung auf der Grundlage einer Messung der Zusammensetzung des Ausgangsstroms des Reaktors mit einem Online-NMR-Spektrometer realisiert. Das Spektrometer wurde an den Betrieb in einer explosionsgefährdeten Umgebung angepasst. Es konnte gezeigt werden, dass die Messdaten genau genug sind, um darauf eine Optimierung der Produktausbeute aufzubauen. Die iterative Optimierung führt den Prozess ausgehend vom mit dem Modell berechneten Betriebspunkt schrittweise zum wirtschaftlichen Optimum für die reale Anlage. Dabei reagiert die Optimierung auch auf unbekannte Abweichungen im Prozess (wie die Zusammensetzung des Feeds) und fährt iterativ den jeweils optimalen Betriebspunkt an.
Die Arbeiten wurden im Rahmen des EU-SPIRE-Projekts CONSENS, Förderkennzeichen 636942, durchgeführt.