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Temperature Dependency of Morphological Structure of Thermoplastic Polyurethane using WAXS and SAXS
(2016)
Polyurethanes achieved an exceptional position among the most important organic polymers due to their highly specific technological application areas. Polyurethanes represent a polyaddition product of isocyanate and diols. In terms of their enormous industrial importance, the chemistry of isocyanates has been extensively studied.
3D-Printing is an efficient method in the field of additive manufacturing. In order to optimize the properties of manufactured parts it is essential to adapt the curing behavior of the resin systems with respect to the requirements. Thus, effects of resin composition, e.g. due to different additives such as thickener and curing agents, on the curing behavior have to be known. As the resin transfers from a liquid to a solid glass the time dependent ion viscosity was measured using DEA with flat IDEX sensors. This allows for a sensitive measurement of resin changes as the ion viscosity changes two to four decades. The investigated resin systems are based on the monomers styrene and HEMA. To account for the effects of copolymerization in the calculation of the reaction kinetics it was assumed that the reaction can be considered as a homo-polymerization having a reaction order n?1. Then the measured ion viscosity curves are fitted with the solution of the reactions kinetics - the time dependent degree of conversion (DC-function) - for times exceeding the initiation phase representing the primary curing. The measured ion viscosity curves can nicely be fitted with the DC-function and the determined fit parameters distinguish distinctly between the investigated resin compositions.
The analysis of Δ9-tetrahydrocannabinol (THC) and its metabolites 11-hydroxy-Δ9-tetrahydrocannabinol (11-OH-THC), and 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THC-COOH) from blood serum is a routine task in forensic toxicology laboratories. For examination of consumption habits, the concentration of the phase I metabolite THC-COOH is used. Recommendations for interpretation of analysis values in medical-psychological assessments (regranting of driver’s licenses, Germany) include threshold values for the free, unconjugated THC-COOH. Using a fully automated two-step liquid-liquid extraction, THC, 11-OH-THC, and free, unconjugated THC-COOH were extracted from blood serum, silylated with N-methyl-N-(trimethylsilyl) trifluoroacetamide (MSTFA), and analyzed by GC/MS. The automation was carried out by an x-y-z sample robot equipped with modules for shaking, centrifugation, and solvent evaporation. This method was based on a previously developed manual sample preparation method. Validation guidelines of the Society of Toxicological and Forensic Chemistry (GTFCh) were fulfilled for both methods, at which the focus of this article is the automated one. Limits of detection and quantification for THC were 0.3 and 0.6 μg/L, for 11-OH-THC were 0.1 and 0.8 μg/L, and for THC-COOH were 0.3 and 1.1 μg/L, when extracting only 0.5 mL of blood serum. Therefore, the required limit of quantification for THC of 1 μg/L in driving under the influence of cannabis cases in Germany (and other countries) can be reached and the method can be employed in that context. Real and external control samples were analyzed, and a round robin test was passed successfully. To date, the method is employed in the Institute of Legal Medicine in Giessen, Germany, in daily routine. Automation helps in avoiding errors during sample preparation and reduces the workload of the laboratory personnel. Due to its flexibility, the analysis system can be employed for other liquid-liquid extractions as well. To the best of our knowledge, this is the first publication on a comprehensively automated classical liquid-liquid extraction workflow in the field of forensic toxicological analysis.
We examined the cytotoxic effects of chaetocin on clear cell renal cell carcinoma (ccRCC) cells and the possibility to combine the effects of chaetocin with the effects of cytokine-induced killer cells (CIK) assayed by MTT assay and FACS analysis. Chaetocin is a thiodioxopiperazine produced by fungi belonging to the chaetomiaceae family. In 2007, it was first reported that chaetocin shows potent and selective ex vivo anti-cancer activity by inducing reactive oxygen species. CIK cells are generated from CD3+/CD56- T lymphocytes with double negative CD4-/CD8- phenotype that are isolated from human blood. The addition of distinct interleukins and antibodies results in the generation of CIK cells that are able to specifically target and destroy renal carcinoma cells. The results of this research state that the anti-ccRCC activity of chaetocin is weak and does not show a high grade of selectivity on clear cell renal cell carcinoma cells. Although the CIK cells show a high grade of selective anti-ccRCC activity, this effect could not be improved by the addition of chaetocin. So chaetocin seems to be no suitable agent for specific targeting ccRCC cells or for the combination therapy with CIK cells in renal cancer.
One of the most common problems in Regenerative Medicine is the regeneration of damaged bone with the aim of repairing or replacing lost or damaged bone tissue by stimulating the natural regenerative process. Particularly in the fields of orthopedic, plastic, reconstructive, maxillofacial and craniofacial surgery there is need for successful methods to restore bone. From a regenerative point of view two different bone replacement problems can be distinguished: large bone defects and small bone defects. Currently, no perfect system exists for the treatment of large bone defects.
Bone regeneration and replacement is a major focus in regenerative medicine since degenerative diseases and tumor surgery as well as accidents or dangerous recreational behavior is leading to an increasing need for bone reconstruction strategies. Especially for critical size bone defects, tissue engineering with mesenchymal stem cells is extensively studied because these cells are functioning as precursors for osteoblast in vivo. Nevertheless to reproduce the complex interaction of various factors in vitro is not an easy approach and further investigations have to be done. The status quo is summarized. A variety of growth and transcription factors are known to be involved in osteogenesis with bone morphogenetic proteins (BMPs) and the transcription factor Runx2 being the most extensively studied ones. But also PPAR γ and Osterix are generally regarded as the master regulators of osteoblast differentiation. Recently the large family of purinergic receptors has proven to be essential molecules in osteogenesis as well. In addition, scaffolding is needed to create a three-dimensional tissue. Recent developments in scaffold design are summarized, including natural and synthetic materials with or without the use of bioactive molecules constructed to mimic the natural environment. The status quo of scaffold fabrication methods such as 3D nanoprinting and their influence on cell-scaffold interactions is discussed. In this review we summarize the most interesting results and our related work focusing on two joined approaches: 1) the complex interaction of the most promising factors improving or accelerating osteogenic differentiation and ii) the development of scaffold materials with osteoconductive and osteoinductive properties.
Polyether and polyether/ester based TPU (thermoplastic polyurethanes) were investigated with wide-angle XRD (X-ray diffraction) and SAXS (small angle X-ray scattering). Furthermore, SAXS measurements were performed in the temperature range of 30 °C to 130 °C. Polyether based polymers exhibit only one broad diffraction signal in a region of 2 θ 15° to 25°. In case of polyurethanes with ether/ester modification, the broad diffraction signal arises with small sharp diffraction signals. SAXS measurements of polymers reveal the size and shape of the crystalline zones of the polymer. Between 30 °C and 130 °C the size of the crystalline zone changes significantly. The size decreases in most of investigated TPU. In the case of Desmopan 9365D an increase of the particle size was observed.
Recessive mutations in the MPV17 gene cause mitochondrial DNA depletion syndrome, a fatal infantile genetic liver disease in humans. Loss of function in mice leads to glomerulosclerosis and sensineural deafness accompanied with mitochondrial DNA depletion. Mutations in the yeast homolog Sym1, and in the zebra fish homolog tra cause interesting, but not obviously related phenotypes, although the human gene can complement the yeast Sym1 mutation. The MPV17 protein is a hydrophobic membrane protein of 176 amino acids and unknown function. Initially localised in murine peroxisomes, it was later reported to be a mitochondrial inner membrane protein in humans and in yeast. To resolve this contradiction we tested two new mouse monoclonal antibodies directed against the human MPV17 protein in Western blots and immunohistochemistry on human U2OS cells. One of these monoclonal antibodies showed specific reactivity to a protein of 20 kD absent in MPV17 negative mouse cells. Immunofluorescence studies revealed colocalisation with peroxisomal, endosomal and lysosomal markers, but not with mitochondria. This data reveal a novel connection between a possible peroxisomal/endosomal/lysosomal function and mitochondrial DNA depletion.
We investigated graphene structures grafted with fullerenes. The size of the graphene sheets ranges from 6400 to 640,000 atoms. The fullerenes (C60 and C240) are placed on top of the graphene sheets, using different impact velocities we could distinguish three types of impact. Furthermore, we investigated the changes of the vibrational properties. The modified graphene planes show additional features in the vibronic density of states.
Low-frequency vibrational excitations in zeolite ZSM-5 and its partially crystalline derivatives
(2004)
Molecular dynamics investigation of vibrational properties of zeolite ZSM-5-based amorphous material
(2003)
Matrix metalloproteinases (MMPs) are matrix-degrading enzymes that are over-expressed in joints of rheumatoid arthritis (RA) patients. However, the contribution of specific MMPs for the development of arthritic joints is unknown. This study is aimed at studying the role of matrix metalloproteinase-9 (MMP-9) in mice, using the K/BxN serum-transfer model of RA. Arthritis was induced in Balb/c mice by injecting K/BxN serum. Development of arthritis was followed in these mice by measuring ankle thickness and clinical index score. MMP-9 expression in the joints of mice killed at various time points during the disease progression was determined by gelatin zymography using ankle lysates. We found that MMP-9 expression increased with the severity of arthritis. Importantly MMP-9 deficient mice injected with K/BxN serum showed a milder form of arthritis in comparison to the control C57BL/6 mice injected with K/BxN serum. We therefore conclude that MMP-9 promotes arthritis in mice.
In der vorliegenden Arbeit wird ein neuartiges Verfahren zur Echtzeitüberwachung von Laserbohrprozessen vorgestellt. Die Untersuchungen werden an unterschiedlichen Materialien unter Einsatz eines passiv-gütegeschalteten Nd:YAG Lasers durchgeführt. Prozessbegleitend findet eine Aufzeichnung der akustischen Emissionen mit anschließender Analyse durch schnelle Fourier-Transformation statt. Hierdurch lassen sich der Durchbruch beim Bohren durch ein Material sowie der Materialübergang mehrschichtiger Systeme detektieren. Die akustischen Messungen werden durchAuswertung der Pulsfolge des Lasers mittels einer Fotodiode gestützt. Hierbei zeigt sich eine gute Übereinstimmung der im akustischen Spektrum dominanten Frequenz mit der jeweils im Laserburstauftretenden Pulsfrequenz. Das vorgestellte Verfahren ermöglicht eine Echtzeitüberwachung beim Laserbohren mittels kostengünstiger und einfacher Hardware. Zudem zeichnet es sich im Gegensatz zu bestehenden Verfahren durch eine hohe Robustheit gegen äußere Störeinflüsse aus, da eine frequenzbasierte Auswertung stattfindet.
Unkonventionelle Spreng- und Brandvorrichtungen sind Bedrohungen in den weltweiten Konfliktherden und werden bei terroristischen Aktivitäten verwendet. Der Schutz von Menschen und Material erfordert daher effektive Gegenmaßnahmen. Dazu gehört auch die Anforderung an Sicherheitskräfte oder militärisches Personal, unbekannte Substanzfunde mit geringem zeitlichem und logistischem Aufwand vor Ort als gefährdend oder unkritisch einzustufen. Um Explosivstoffe von nicht-explosiven Materialien zu unterscheiden, kann die bei Explosivstoffen initiierbare, stark exotherme Reaktion genutzt werden. Diese resultiert in Strahlungsemissionen sowie in lokaler Druck- und Temperaturerhöhung. Die Messung dieser Reaktionseffekte und die Anforderung an eine mobile, einfach zu bedienende und robuste Analytik werden durch ein System ermöglicht, das Proben im einstelligen mg-Bereich durch schnelles Erhitzen auf mikrostrukturierten Heizern zum chemischen Umsatz anregt. Die emittierte Strahlung wird mit Photodioden im Bereich des sichtbaren und nah-infraroten Lichts aufgenommen, ein Sensor registriert die Druckerhöhung in einer geschlossenen Versuchskammer. In einem zweiten Aufbau werden die gasförmigen Reaktionsprodukte über ein Sensorarray von vier kommerziellen Gassensoren geleitet und die Signalantworten der Halbleitergassensoren mittels Hauptkomponentenanalyse ausgewertet. Die Ergebnisse zeigen, dass die schnelle thermische Aktivierung für die untersuchten primären Explosivstoffe, Treibladungspulver, sowie Trinitrotoluol (TNT) reproduzierbar erfolgt. Nicht-Explosivstoffe werden dabei im untersuchten Umfang sicher als unkritisch erkannt. Die Auswertung der Gassensorsignale liefert eine Unterscheidung von Nitrat- und Peroxid-basierten Sprengstoffen sowie von nicht-explosiven Substanzen.
Durch Dotierung eines nematischen Flüssigkristalles mit einer chiralen Substanz wird eine helikal strukturierte Phase induziert, die in der Lage ist, einfallendes Licht wellenlängenselektiv zu reflektieren. Bei der Reaktion des Dotiermittels mit einem gasförmigen Analyten verändern sich die Ganghöhe dieser Struktur und damit die reflektierte Wellenlänge. Liegt diese im Bereich des sichtbaren Lichts, ist eine Farbänderung mit dem menschlichen Auge zu beobachten. Es ist dabei sinnvoll den Flüssigkristall z.B. in einem Polymer einzukapseln, um ihn vor mechanischen Einflüssen und Umwelteinflüssen zu schützen. Eine Möglichkeit zur Einkapselung ist das koaxiale Elektrospinnen. Vorteile sind unter anderem die Realisierung einer großen Oberfläche und einer sehr geringen Wanddicke der schützenden Schale, die die Diffusion von Gasen durch die Wand hindurch ermöglicht. Um die Funktionsfähigkeit eines solchen Sensors zu testen, wurde ein CO2-sensitiver Flüssigkristall verwendet. Dieser wurde in eine Schale aus Polyvinylpyrrolidon (PVP) versponnen und die Reaktion mit CO2 spektroskopisch analysiert.
The analytical pyrolysis technique hyphenated to gas chromatography–mass spectrometry (GC–MS) has extended the range of possible tools for the characterization of synthetic polymers and copolymers. Pyrolysis involves thermal fragmentation of the analytical sample at temperatures of 500–1400 °C. In the presence of an inert gas, reproducible decomposition products characteristic for the original polymer or copolymer sample are formed. The pyrolysis products are chromatographically separated using a fused-silica capillary column and are subsequently identified by interpretation of the obtained mass spectra or by using mass spectra libraries. The analytical technique eliminates the need for pretreatment by performing analyses directly on the solid or liquid polymer sample. In this article, application examples of analytical pyrolysis hyphenated to GC–MS for the identification of different polymeric materials in the plastic and automotive industry, dentistry, and occupational safety are demonstrated. For the first time, results of identification of commercial light-curing dental filling material and a car wrapping foil by pyrolysis–GC–MS are presented.
The criteria for assessing the quality of rubber materials are the polymer or copolymer composition and the additives. These additives include plasticizers, extender oils, carbon black, inorganic fillers, antioxidants, heat and light stabilizers, processing aids, cross-linking agents, accelerators, retarders, adhesives, pigments, smoke and flame retardants, and others. Determination of additives in polymers or copolymers generally requires the extraction of these substances from the matrix as a first step, which can be challenging, and the subsequent analysis of the extracted additives by gas chromatography (GC), GC–mass spectrometry (MS), high performance liquid chromatography (HPLC), HPLC–MS, capillary electrophoresis, thin-layer chromatography, and other analytical techniques. In the present work, nitrile rubber materials were studied using direct analytical flash pyrolysis hyphenated to GC and electrospray ionization MS in both scan and selected ion monitoring modes to demonstrate that this technique is a good tool to identify the organic additives in nitrile rubber.
Asymmetric threats require powerful surveillance technology which helps to preserve the security. Security checks which focus on Improvised Explosive Devices (IED’s) or the identification of persons carrying hazardous substances are the major task of our research within the HAMLeT+ (Hazardous Material Localization and Person Tracking) project. Further on, there is a pressing need for assisting the security personnel, either civil or military, by extending the detection capabilities and to deliver efficient and reliable, real time decision support for their task to percept threats. Military camp protection with heterogeneous net-worked sensors and comprehensive sensor data fusion could be such an element. The technology developments concentrate on the integration of different sensor types (video, tracking sensors, CBRNE sensors) in order to get a better and comprehensive understanding in a defined entry area. Data fusion is used to combine kinematic data of persons (where, when) with additional attribute information of them (what) in order to identify that single person carrying the attributes and to classify the threat. The project was initiated as a Supporting Activity funded by the EU within the PASR 2006 scheme. With regards to the specific task for military camp protection it was extended and redesigned. In HAMLeT+ several chemical sensors for hydrocarbons like fuels, alcohols or solvents were used. Such chemicals are available in bigger amounts on the free market. Using them e.g. as fire accelerants they can cause a huge damage. Therefore their detection or the detection of persons carrying such substances or having contaminations on their clothes is of great interest. Sensitive devices for the detection of these analytes are e.g. metal oxide sensors [1]. Our presentation illustrates experimental data, which were gathered with the experimental system HAMLeT+ during the NATO “Defense Against Terrorism (DAT)” campaign „COMMON SHIELDS” in August and September 2008.