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Eingeladener Vortrag
- nein (46)
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.
Raman and laser-induced breakdown spectroscopy is integrated into a single system for molecular and elemental microanalyses. Both analyses are performed on the same ~ 0.002 mm² sample spot allowing the assessment of sample heterogeneity on a micrometric scale through mapping and scanning. The core of the spectrometer system is a novel high resolution dual arm Echelle spectrograph utilized for both techniques. In contrast to scanning Raman spectroscopy systems, the Echelle-Raman spectrograph provides a high resolution spectrum in a broad spectral range of 200-6000 cm- 1 without moving the dispersive element. The system displays comparable or better sensitivity and spectral resolution in comparison to a state-of-the-art scanning Raman microscope and allows short analysis times for both Raman and laser induced breakdown spectroscopy. The laser-induced breakdown spectroscopy performance of the system is characterized by ppm detection limits, high spectral resolving power (15,000), and broad spectral range (290-945 nm). The capability of the system is demonstrated with the mapping of heterogeneous mineral samples and layer by layer analysis of pigments revealing the advantages of combining the techniques in a single unified set-up.
Polyethylene (PE) frits were used to quantify sulphur in copper and its alloys by isotope dilution combined with LA-ICP-MS as an alternative approach to conventional sample preparation: the copper samples were spiked, the spiked samples were dissolved, the resulting solutions were absorbed in the PE frits and finally the PE frits were analysed by LA-ICP-MS. A prerequisite for such a support material is a low sulphur blank and thus PE was selected for this purpose. The absorption efficiency of the PE frits was studied for varying sulphur amounts ranging from 2 mg S to 80 mg S showing that more than 99.5% of the loaded sulphur was absorbed by the frit. The so prepared PE frits were measured by LA-ICP-MS and yielded a good linearity (R2 ¼ 0.999) for the sulphur ion intensities corresponding to sulphur amounts up to 40 mg S; the associated sensitivity is approximately 3.4 x 10⁴ cps μg⁻¹ for ³²S. For the validation of the developed procedure the reference materials BAM-M376a, BAM-228 and BAM-227 were applied such that 2 μg S, 5 μg S and 11 μg S were absorbed in the PE frits, respectively. These samples were pre-quantified for the adsorbed sulphur amount by external calibration LA-ICP-MS yielding sulphur amounts of 0.9 μg, 5.1 μg and 8.5 μg (quantified for ³²S only), respectively. Relative Standard deviations of the isotope ratios were below 5% in average (n ¼ 3 lines) in all cases (except for the pure spike solution). These samples were then analysed by LA-ICP-IDMS and the measurement results were validated by comparing them with the results obtained by conventional ICP-IDMS. The obtained relative expanded measurement uncertainties ranged between 10% and 26%. Pearson's coefficient was used to express the correlation between both techniques; the obtained value was 0.999 demonstrating a strong correlation. Contrary to most published LA-ICP-IDMS procedures, the developed procedure enables SI-traceability for the measurement results. The metrological traceability to the SI for the sulphur mass fractions in copper was established by an unbroken chain of comparisons, each accompanied by an uncertainty budget. Thus, the measurement results are considered reliable, acceptable and comparable within the stated measurement uncertainty. The metrological traceability chain from the kg down to mass fraction in the samples obtained by LA-ICP-IDMS is presented as well.
Triacetone triperoxide (TATP) is a primary explosive, which was used in various terrorist attacks in the past. For the development of biosensors, immunochemical µ-TAS, electronic noses, immunological test kits, or test strips, the availability of antibodies of high quality is crucial. Recently, we presented the successful immunization of mice, based on the design, synthesis, and conjugation of a novel TATP derivative. Here, the long-term immunization of rabbits is shown, which resulted in antibodies of extreme selectivity and more than 1,000 times better affinity in relation to the antibodies from mice. Detection limits below 10 ng L-1 (water) were achieved. The working range covers more than four decades, calculated from a precision profile. The cross-reactivity tests revealed an extraordinary selectivity of the antibodies—not a single compound could be identified as a relevant cross-reactant. The presented immunoreagent might be a major step for the development of highly sensitive and selective TATP detectors particularly for security applications.
An efficient solid phase extraction (SPE) method using bis-(2-ethylhexyl)-phosphate (HDEHP) coated reverse phase C18 support has been developed for the pre-concentration of Gadolinium (Gd) and Gd contrast agents widely used in magnetic resonance imaging (MRI). Enrichment of Gd in the ionic form has been compared with strong cation exchange material Chromabond SA (SCX), weak ion exchange material Chelex-100 and also with lanthanide specific HDEHP modified reverse phase C18. The determination of Gd and its complexes after enrichment were performed using inductively coupled plasma mass spectrometry (ICP-MS) and on the basis of 158Gd. Among the three SPE materials, HDEHP coated reverse phase C18 SPE has been found to be most efficient, yielding a hundredfold Gd enrichment with > 95% recovery for linear and cyclic contrast agents like Gd-DTPA (Magnevist), Gd-DOTA (Dotarem), Gd-BOPTA (Multihance), and Gd-BT-DO3A (Gadovist). The developed SPE method has been successfully applied to the surface water and waste water samples originated from different places in Berlin, Germany. The results were in good agreement with the results obtained with direct measurement with ICP-MS. The developed pre-concentration method can be efficiently used for the determination of trace levels of gadolinium in the environment even with less sensitive analytical techniques.
Calibration-Free Laser-Induced Breakdown Spectroscopy (CF-LIBS) has been proposed several years ago as an approach for quantitative analysis of Laser-Induced Breakdown Spectroscopy spectra. Recently developed refinement of the spectral processing method is described in the present work. Accurate quantitative results have been demonstrated for several metallic alloys. However, the degree of accuracy that can be achieved with Calibration-Free Laser-Induced Breakdown Spectroscopy analysis of generic samples still needs to be thoroughly investigated. The authors have undertaken a systematic study of errors and biasing factors affecting the calculation in the Calibration-Free Laser-Induced Breakdown Spectroscopy spectra processing. These factors may be classified in three main groups: 1) experimental aberrations (intensity fluctuations and inaccuracy in the correction for spectral efficiency of a detection system), 2) inaccuracy in theoretical parameters used for calculations (Stark broadening coefficients and partition functions) and 3) plasma non-ideality (departure from thermal equilibrium, spatial and temporal inhomogeneities, optical thickness, etc.). In this study, the effects of experimental aberrations and accuracy of spectral data were investigated, assuming that the analytical plasma is ideal. Departure of the plasma conditions from ideality will be the object of future work. The current study was based on numerical simulation. Two kinds of metallic alloys, iron-based and aluminum-based, were studied. The relative weight of the error contributions was found to depend on the sample composition. For the here-investigated samples, the experimental aberrations contribute to the overall uncertainty on the quantitative results more than theoretical parameters. The described simulation method can be applied to the Calibration-Free Laser-Induced Breakdown Spectroscopy analysis of any other kind of sample.
Particle-based assays are becoming versatile analytical tools due to their cost-effectiveness, speed, straightforward and diverse functionalization chemistries, especially when polystyrene particles are used. The introduction of functional groups (–COOH, –NH2, etc.) to the surface of such polystyrene particles promotes their application in bioanalytics. However, the traditional method to determine the amount of surface carboxylate groups is conductivity titration, which is usually time- and resources-consuming and discontinuous. Here, we synthesized polystyrene microparticles with different contents of carboxylate groups, and then investigated a simpler and potentially continuous approach to determine the amount of surface carboxylate groups by Zeta potential measurements. The results were compared to the traditional titration method and to actual coupling efficiencies of the functionalized particles with a model oligonucleotide probe as determined by flow cytometry. All quantification methods revealed good agreement.
The accurate knowledge of the properties of polycapillary X-ray semi-lenses has a significant influence on the quantitative results in a widespread field of applications involving microfocus X-ray beams. A routine procedure for the characterisation of a polycapillary X-ray semi-lens with a scanning electron microscope (SEM) having attached an energy dispersive spectrometer (EDS) is presented in this paper. A key issue of the procedure consists of fitting the semi-lens in front of the EDS for spectra acquisition. Relevant semi-lens parameters such as focal distance, full width at half maximum (FWHM) of the acceptance area, and transmission are determined in parallelising mode of the semi-lens. Special attention has been paid to the calculation of the transmission.
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.