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Eingeladener Vortrag
- nein (46)
LIBS matures to a quantitative method for elemental analysis rather than a qualitative diagnostic tool. Numerous real world applications for bulk and microanalysis profit from instrumental and methodical advances in the last decade. Today, recording of numerous spectra from samples can be done with low experimental efforts and low cost per spectrum. Not surprisingly, LIBS data, with a high spectral resolution and a broad spectral range, become “big data” and can be utilized in different ways beyond elemental analysis. But, what is the generic or best approach for quantitative LIBS analysis? What techniques can be employed to gain new insights into data? Emergent information can arise through data fusion of LIBS data with other data, i.e. orthogonal spectroscopic or other information related to the sample. But are fused data better than data from a single method?
This talk will provide an in-depth overview what chemometric tools can do for LIBS. For quantitative analysis, pre-processing tools are essential to improve precision, accuracy, and reproducibility but at the same time their application to data is still based on phenomenological criteria. Multivariate analysis seems to dominate LIBS, but are there drawbacks on using all information from spectra. For different data sets from real applications, the use of multivariate calibration and (un)supervised pattern recognition will be discussed in comparison with reference analytical methods and possible improvements through plasma diagnostics and modelling.
Der Vortrag gibt einen Überblick die deutsche Ressortforschung. Neben einer Einordnung in das deutsche Wissenschaftssystem werden in einem historischen Überblick die Besonderheiten der Ressortforschung diskutiert. Besonderes Augenmerk wird der Frage gewidmet „Was ist gute Ressortforschung“. Kritisch erscheint besonders die Vereinbarkeit von exzellenter Wissenschaft und seriöser und unabhängiger Politikberatung.
Previously applied methods for the quantification of sulphur in copper and other pure metals revealed a lack of SI-traceability and additionally showed inconsistent results, when different methods were compared.
Therefore, a reference procedure is required which allows SI-traceable values accompanied by a Sound uncertainty budget. In this study a procedure was developed for the quantification of total sulphur in copper at low concentration levels using inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS). The major part of the copper matrix was separated by adding ammonia which forms a complex with the copper while releasing the sulphur followed by chromatographic separation using a weak cation resin. After that the sulphur fraction was further purified by chromatographic means using first an anion exchange method and second a chelating resin. The developed procedure shows high performance, especially concerning high efficiency in matrix removal (>99.999%) while keeping the recovery of sulphur above 80%. Procedure blanks are in the order of 3–53 ng resulting in LOD and LOQ values of 0.2 mg g1 and 0.54 mg g1, respectively. The procedure is sufficient to facilitate value assignment of the total sulphur mass fraction in reference materials. Additionally, relative measurement uncertainties were calculated to be below 1% and the measurement results were traceable to the SI. The procedure reported in this study is a new reference procedure for sulphur measurement in copper, being fit for two major purposes, certification of reference materials and assignment of reference values for inter-laboratory comparison.
A simple metal staining procedure for identification and visualization of single cells by LA-ICP-MS
(2017)
High lateral resolution of metal detection in single cells by use of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) demands powerful staining methods. In this work different staining procedures for the single cell analysis with LA-ICP-MS were optimized. An iridium intercalator was utilized to stain the cell nuclei whereas the whole cell was stained by the use of maleimido-mono-amide-DOTA (mDOTA) complexing lanthanide(III) ions. The content of the artificially introduced metals per cell was quantified using a matrix matched calibration approach based on cellulose membranes onto which standards were spotted by a microarray spotter. Absolute metal stain amounts in the range of 2.34 to 9.81 femtomole per cell were determined. The metal staining procedures allow direct identification and visualization of single cells and their cell compartments by element microscopy without the use of bright field images of the sample.
Biomedical applications, including functional biomaterials, carbohydrate-arrays, and glycan-based biosensors.
The chemistry of glycan immobilization plays an essential role in the bioavailability and function of surface bound carbohydrate moieties. For biomedical applications the stability over time (shelf life) of glycan arrays is a crucial factor. Herein we report on approaches for surface and interface characterization relevant to the needs of production of glycan microarrays which were tested using model carbohydrate surfaces. For detailed characterization of glycan model surfaces we used a combination of X-ray photoelectron spectroscopy (XPS), near edge X-ray absorption fine structure spectroscopy (NEXAFS) and ToF SIMS which are complementary techniques of surface chemical analysis. Links to fluorescence spectroscopy often used for characterization in the microarray community were established as well. In detail, amine-reactive silicon oxide and glass surfaces were used for anchoring oligosaccharides with an amino linker. The amount of surface bound carbohydrates was estimated by X-ray photoelectron spectroscopy (XPS). Glycan immobilization was investigated using lectins, which are glycan-binding molecules. A shelf life study of model glycan microarrays on epoxy-coated glass surfaces was done over a period of 160 days under different storage conditions utilizing fluorescence, ToF-SIMS and XPS analysis. It was shown that glycan activity of the models used can be maintained at least for half a year of storage at 4 °C.
The identification of transformation products (TPs) of pesticides in food is a crucial task difficult to tackle, due to the lack of standards. In this work, we present a novel methodology to synthesize five main TP standards of the insecticide chlorpyrifos (CPF) and to investigate their occurrence in selected fruits and spices. TPs were electrochemically (EC) synthesized using a boron-doped diamond electrode (BDD) and identified by EC coupled online to mass spectrometry, LC-MS/MS, and high-resolution mass spectrometry. CPF and its TPs were analyzed in the food samples by LC-MS/MS on multiple reaction monitoring (MRM) after dispersive solid-phase extraction. A good recovery of 83–103% for CPF and 65–85% for TPs was obtained. Matrix effects, which cause signal suppression, ranged between 81 to 95% for all targeted analytes. The limit of detection and quantification for CPF were 1.6–1.9 and 4.9–5.7 μg/kg, respectively. Among investigated samples, CPF was determined in fresh lemon (104 μg/kg), fenugreek seed (40 μg/kg), and black pepper (31 μg/kg). CPF content in all samples was lower than the EU maximum residue level (MRL). The most frequently detected TPs were diethylthiophosphate and diethylphosphate. Other TPs, CPF oxon and trichloropyridinol, were also detected. Hence, EC is a versatile tool to synthesize TP standards which enables the determination of contaminants and residues in foodstuffs even if no commercial standards are available.
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.