4 Material und Umwelt
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X-ray fluorescence analysis, due to its non-destructive nature and ist suitability to work with historic objects in situ, quickly became one of the most important methods for the evaluation of iron-gall ink. The main advantage of this qualitative and semi-quantitative method is that it makes it easy to differentiate between inks, based on the assumption that the differences result from the manufacture of the ink.
This work explores the question whether the ink ‘fingerprint’ results strictly from the elemental composition of the basic ink ingredients even if it is stored in vessels made of metals or metal alloys. In addition, we tested and compared the performance of three different XRF spectrometers.
We prepared various lab-grade inks according to historical ink recipes and measured the metal content of the ink deposited on sized cotton Linters paper with three types of XRF spectrometers: a simple hand-held device with an interaction spot of 4 mm and two devices equipped with poly-capillary Xray optics for line scanning and imaging. Since the exact elemental mass composition of the non-aged ink samples was known, we were able to evaluate the accuracy of the research procedure. Lab-grade inks were then aged in the metal jars imitating inkwells. The aging of the inks in the metal containers resulted in the significant change of the primary inks fingerprint as opposed to that of the control inks stored in glass containers. This effect was independently confirmed by the measurements conducted with every instrument we used. We will present a brief comparison of the results 43 achieved when using different spectrometers and a possible hypothesis explaining the processes that occurred.
This work presents the non-destructive spectroscopic characterisation of original Dead Sea Scrolls (DSS)parchment fragments from Ronald Reed collection. The fragments are of paramount importance becausethey have never been subjected to any treatment of preservation and restoration, this allows to investi-gate the manufacturing method of real original Jewish parchments. The manufacture of “sacred” Jewishparchments, in fact, is traditionally supposed to use a superficial tannin treatment. To study the DSS frag-ments, it was necessary both to analyse mock-up samples, especially manufactured in order to reproduceancient Oriental Jewish ritual parchments, and to compare the results with those obtained in the analysisof modern and ancient Western Jewish ritual parchments, in order to test the effectiveness of the selectedspectroscopic techniques. Traditionally, the main difference between Oriental and Western traditionalparchment preparation consisted in the dehairing method: enzymatic for Oriental and lime-based forWestern. Moreover, a finishing treatment with tannin was supposed to be applied on ritual Jewish parch-ments. The need of reference samples derives from the knowledge that each parchment preparation,treatment and degradation can induce structural modifications that affect the spectral features. FourierTransform Infrared Spectroscopy by Attenuated Total Reflection (ATR-FTIR), FT-Raman and m-Ramanwere used in this study. The experimental results allowed us to recognise, with different sensitivity, thepresence of tannin by using m-Raman and IR spectroscopies and to prove that not all the archaeologicalsamples were manufactured in the same way with vegetal extracts. Many salts (tschermigite, dolomite,calcite, gypsum and iron carbonate) were found on the surface of DSS fragments. They can derive fromthe degradation processes and storage environment before the discovery or from the manufacture. More-over, the different sensitivities and instrumental characteristics of the used techniques permitted us toestablish an analytical protocol, useful for further studies of similar materials.
The present study shows the potential of high-resolution imaging and nano-Fourier-transform infrared (nano-FTIR) spectroscopy for corrosion science. The protective oxidation layers of different chlorine-gas treated silicon
carbides (SiCs) were characterized with these techniques. A nitrified SiC showed the highest resistant strength against chlorine corrosion at 1000 °C compared to the other SiCs. Nano-FTIR spectroscopy with a lateral resolution below 40 nm detected differences in the crystallinity of the bulk-SiC and in the transitional region to the protective layer. Furthermore, high-resolution imaging provides deep insight in the interfacial layer between bulk-SiC and the protective oxidation layer on sub-micrometer scale.
Chemical-free pest control by dielectric
heating with radio waves and microwaves:
Thermal effects
(2018)
Thermal pest control with hot air is widely accepted as an alternative to chemical methods. However, it requires relatively long treatment times owing to the low thermal conductivity of wood. Direct dielectric heating that applies radio waves or microwaves has the advantage of more homogeneous heating. However, Sound experimental data on this technique are currently rare. Therefore, the thermal treatment of wood-destroying insects with radio waves and microwaves was studied with two model pests, Anobium punctatum and Hylotrupes bajulus, and with Tenebrio molitor as a reference. The secure elimination of pests was achieved, and the corresponding treatment time was in the range of a few minutes. Temperature profiles were more homogeneous when applying radio waves.
A pot experiment was carried out with maize to determine the phosphorus (P) plant-availability of different secondary P-fertilizers derived from wastewater. We analyzed the respective soils by P K-edge X-ray absorption near-edge structure (XANES) spectroscopy to determine the P chemical forms that were present and determine the transformation processes. Macro- and micro-XANES spectroscopy were used to determine the chemical state of the overall soil P and identify P compounds in P-rich spots. Mainly organic P and/or P adsorbed on organic matter or other substrates were detected in unfertilized and fertilized soils. In addition, there were indications for the formation of ammonium phosphates in some fertilized soils. However, this effect was not seen in the maize yield of all P-fertilizers. The observed reactions between phosphate from secondary P-fertilizers and cofertilized nitrogen compounds should be further investigated. Formation of highly plant-available compounds such as ammonium phosphates could make secondary P-fertilizers more competitive to commercial phosphate rock-based fertilizers with positive effects on resources conservation.
Today glass is broadly used in modern architecture. For applications indoor it is possible to produce decor glass by using enamel colors and glass painting techniques without any problems. However, this is more limited for applications outdoor. Humidity and environmental pollution attack the surface of the coating and damage it strongly. There are only few colors on the market which are resistant towards acids and bases until now. Additionally, most of those colors are opaque. In order to extend the color palette, chemically resistant colored glasses are being developed which are transparent, relatively low melting and intensively toned even in thin coat thickness. To achieve such ambitious aim, many parameters have to match which act in complex manner. Metal oxides were used to color the glasses. A lead-free glass composition was developed to avoid an exposition of heavy metals to the environment. The glasses were characterized, in particular in terms of their thermal properties, their crystallization and corrosion behavior as well as their chemical and environmental durability. Different practical applications will be shown.
Fluorometric sensing is a versatile approach for trace analysis outside of the laboratory, requiring suitable sensor materials and their integration into sensing devices. The versatility of fluorophores as probes, especially in terms of the possibility to tailor their optical as well as their recognition properties by synthetic modifications in a wide range, renders them as superior active component for the preparation of optical sensing devices. Recent works at BAM in this field include, for example, the detection of nerve gas agents, illustrating impressively the aforementioned benefits of fluorophores in optical sensing applications.
In the interdisciplinary project presented here, we target hazardous gases such as ammonia, benzene, and hydrogen sulfide, next to others, which pose a major threat to human health and environmental safety and for which the availability of a sensitive and reliable detection method is highly desirable. The dyes presented follow a “turn-on” fluorescence schematic, which allows for the selective and sensitive detection of the respective gaseous analyte. The immobilization of the probe in polymeric matrices is then the next step toward the fabrication of a prototype device for molecular sensing. Further steps in the project include the assembly of instruments for test-atmosphere generation, the referencing of the sensor system, development and implementation of an optical setup, and the testing of the prototype device under laboratory conditions and in the field.
In this presentation, we give an overview over the recent developments on this topic in our groups. Highlights are hydrogen sulfide sensitive, BODIPY based transition metal complexes, which allow for a sensitive as well as selective detection of the toxic gas. In addition, we present a novel class of highly substituted BODIPY derivatives – pocket-BODIPYs – which are of a synthetically high versatility and can readily be modified to create pockets in the periphery of the molecule of defined geometries. This is illustrated on the successful encapsulation of benzene by a pocket-BODIPY derivative, confirmed by X-ray crystallographic analysis as well as by further spectroscopic and analytical methods.
The challenge of the project ASHES is focused on the recycling of nutrients from residues of thermochemical processing of by-products of sugar cane industry (bagasse/straw) in Brazil to increase the energy efficiency of thermal conversion and to enable the recycling of process ashes as fertilisers. Dry lignocellulosic biomass (straw, bagasse) are combusted, gasified and subsequently combined with post-thermochemical treatment in the AshDec process to increase the plant availability of phosphorus. Different fertilizer formulations are granulated/pelletized and tested regarding their storage/handling characteristics.
There is a need for an assessment of the emission properties of volatile organic compounds (VOCs) from consumer products. A method comparison was carried out to evaluate adapted and cost-effective procedures for such items. Smaller and automated emission chambers depicted similar kinetics compared to a 203 L standard chamber. Toy samples made of PVC (Polyvinyl chloride) emitted more VOCs compared to other tested polymeric products. The emissions from 2 selected samples were studied to allow an evaluation of the resulting room concentration and external exposure of a child. Obtained concentrations were not of concern.
The manuscript Codex germanicus 1 (Cod. germ. 1) of the Staats- und Universitätsbibliothek Hamburg is a fifteenth-century German-language manuscript. It comprises two codicological units and has an especially complex developmental history. To trace this developmental history, neglected until now in the research literature, the manuscript was investigated, for the first time not solely with classical codicological and palaeographical methods, but also with the aid of X-ray fluorescence spectroscopy, in order to determine the composition of the writing materials. These methods made it possible, first, to support and check palaeographic findings and, second, to gain information about the stratigraphy of the manuscript where palaeographic methods find their limits – in regard to short entries, rubrications, and non-alphabetical signs.