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We report the selective ring opening copolymerisation (ROCOP) of
oxetane and phthalic thioanhydride by a heterobimetallic Cr(III)K
catalyst precisely yielding semi-crystalline alternating poly(esteralt-
thioesters) which show improved degradability due to the
thioester links in the polymer backbone.
The site of Schöningen (Germany), dated to ca. 300,000 years ago, yielded the earliest large-scale record of humanly-made wooden tools. These include wooden spears and shorter double-pointed sticks, discovered in association with herbivores that were hunted and butchered along a lakeshore. Wooden tools have not been systematically analysed to the same standard as other Palaeolithic technologies, such as lithic or bone tools. Our multianalytical study includes micro-CT scanning, 3-dimensional microscopy, and Fourier transform infrared spectroscopy, supporting a systematic technological and taphonomic analysis, thus setting a new standard for wooden tool analysis. In illustrating the biography of one of Schöningen’s double-pointed sticks, we demonstrate new human behaviours for this time period, including sophisticated woodworking techniques. The hominins selected a spruce branch which they then debarked and shaped into an aerodynamic and ergonomic tool. They likely seasoned the wood to avoid cracking and warping. After a long period of use, it was probably lost while hunting, and was then rapidly buried in mud. Taphonomic alterations include damage from trampling, fungal attack, root damage and compression. Through our detailed analysis we show that Middle Pleistocene humans had a rich awareness of raw material properties, and possessed sophisticated woodworking skills. Alongside new detailed morphometrics of the object, an ethnographic review supports a primary function as a throwing stick for hunting, indicating potential hunting strategies and social contexts including for communal hunts involving children. The Schöningen throwing sticks may have been used to strategically disadvantage larger ungulates, potentially from distances of up to 30 metres. They also demonstrate that the hominins were technologically capable of capturing smaller fast prey and avian fauna, a behaviour evidenced at contemporaneous Middle Pleistocene archaeological sites.
In a laboratory test, transparent high‐density polyethylene (HDPE) jerrycans have been exposed to both UV radiation and 55 wt‐% nitric acid solution at (41 ± 2)°C, for up to 20 days. For comparison, UV radiant exposure (21 days) and nitric acid exposure (up to 6 weeks) were performed separately, at nearly equal temperatures. The damages are compared with FTIR spectroscopy in ATR and HT‐gel permeation chromatography(GPC) on a molecular level and with hydraulic internal pressure testing as a component test. For the used jerrycans, relevant oxidation can only be found after the combined exposure. This is caused by the decomposition of nitric acid into nitrous gases by UV radiation, which is also observed at lower concentrations (28 wt‐%). After 6 days of laboratory exposure, this is rated as critical, which corresponds to about 1/10 year in Central Europe, according to the UV radiant exposure. The gradual increase in oxidative damage shows the reproducibility of the test.
In the present study, a simple approach was used to investigate the effect of UV-exposure on two high density Polyethylene materials (PE-HD), commonly used for storage tanks, on fuel sorption behavior and colonization by microorganisms. The aim was to investigate whether the sorption behavior of the fuels (diesel/biodiesel) and the colonization by microorganisms, frequently occurring in the fuel, is affected and may lead to undesirable or safety-relevant material changes. We showed that the UV-irradiation leads to significant changes of the sorption behavior due to chemi-crystallization and crosslinking. The fuel Sorption is affected by the UV-induced formation of polar carbonyl and hydroxyl groups predominantly occurring at the surface. With respect to microbial colonization behavior for Bacillus subtilis and Pseudomonas aeruginosa, isolated from a contaminated diesel sample, differences of the initial adhesion could be shown depending on the initial type of polyethylene as well as on the degree of UV-induced degradation.
The impact fracture behavior of two common high-density polyethylene grades for container applications were intensively studied by the instrumented Charpy impact test after well-defined exposure to UV-irradiation. Individual stages of the impact event, such as crack initiation and crack propagation energy as well as maximum impact load, were investigated from the recorded load–deflection curves. UV-induced material property changes were further investigated by infrared spectroscopy, differential scanning calorimetry, and dynamic-mechanical analysis as well as density measurements. Based on the results of the Charpy impact test, three indicators were identified to describe the extend of photooxidation on high-density polyethylene: (a) a reduced Charpy impact strength—at least to half of its initial value for a distinctly brittle impact fracture, (b) a marked decrease in the crack propagation contribution to the impact strength, and (c) an increase of the brittle features of the fracture surface.
Scientific publications addressing the durability of the flame retardance of cables during their long-term application are rare and our understanding lacks. Three commercial flame retardants, aluminum hydroxide, aluminum diethyl phosphinate (AlPi-Et), and intumescent flame retardant based on ammonium polyphosphate, applied in ethylene-vinyl acetate copolymer (EVA) model cables, are investigated. Different artificial aging scenarios were applied: accelerated weathering (UV-irradiation/temperature/rain phases), humidity exposure (elevated temperature/humidity), and salt spray exposure. The deterioration of cables’ surface and flame retardancy were monitored through imaging, color measurements, attenuated total reflectance Fourier transform infrared spectroscopy, and cone calorimeter investigations. Significant degradation of the materials’ surface occurred. The flame retardant EVA cables are most sensitive to humidity exposure; the cable with AlPi-Et is the most sensitive to the artificial aging scenarios. Nevertheless, substantial flame retardance persisted after being subjected for 2000 h, which indicates that the equivalent influence of natural exposure is limited for several years, but less so for long-term use.
Additively manufactured test specimens made of polyamide 12 (PA 12) by Laser Sintering as well as of acrylonitrile butadiene styrene (ABS) by Fused Layer Modelling, were characterised with active thermography directly after manufacturing and after artificial weathering. For this, two different excitation methods (flash and pulse heating) were used and compared, regarding their suitability for the detection of constructed and imprinted defects inside the test specimens. To increase the quality of the thermograms, data processing methods like thermal signal reconstruction (TSR) and Fourier Transformation after TSR were applied. To further investigate the long-term stability of the additively manufactured test specimens towards environmental stress, like UV radiation, heat, humidity, water contact and frost with active thermography, an artificial weathering test over 2000 hours (~3 months) was applied to the specimens. The monitoring of the changes in the optical properties of the weathered plastics was supplemented by spectral reflectance and UV/VIS spectroscopy.
Polyether and -ester urethanes (PU) were exposed to artificial weathering at 40 °C and artificial UV radiation in a weathering chamber. In 3 parallel exposures, humidity was varied between dry, humid, and wet conditions. Material alteration was investigated by various analytical techniques like size exclusion chromatography
(SEC), liquid chromatography-infrared spectroscopy (LC-FTIR), thermal-desorption gas chromatography-mass spectrometry (TD-GC-MS), fluorescence mapping and dynamic mechanical analysis (DMA). Our results show that depending on the weathering conditions, different degradation effects can be observed. By means of SEC an initial strong decrease of the molar masses and a broadening of the mass distributions was found. After a material dependent time span this was followed by a plateau where molar mass changes were less significant. A minor moisture-dependent degradation effect was only found for polyester PU. Fluorescence measurements on two materials revealed an increase in the luminescence intensity upon weathering process reaching a saturation level after about 500 h. The changes in the optical properties observed after different exposure conditions and times were very similar. The TD-GC-MS data showed the fate of the stabilizers and antioxidant in the course of weathering. LC-FTIR measurements revealed a change in peak intensities and the ratio of urethane and carbonyl bands.
Exposure response function for a quantitative prediction of weathering caused aging of polyethylene
(2019)
The exposure response function of the carbonyl formation over the bulk has been determined for a high-density polyethylene of a thickness of 200 μm, which was used as a weathering reference material according to ISO TR 19032. To this end, spectral sensitivity was studied by local measurement of the effect of spectrally dispersed irradiation. Both the exposure device and the methodology of determination are described.
The temperature dependency of photooxidation was determined by UV exposure at various temperatures between 23 and 80 °C. Deviations from linearity and thus reciprocity below 40 °C are discussed and assumed to be related to diffusion limitations. An Arrhenius approach –based on data of linear carbonyl formation – has been incorporated into the exposure response function. Using this exposure response function, aging in terms of the distribution of a quantitative property change over a plastic component can be predicted for a specific outdoor location with real chronologic weather data as input for the exposure. Thus, artificial and natural weathering can be linked and compared. The established exposure response function has been validated by outdoor exposure results from the literature. If an estimated diffusion limitation is taken into consideration, calculations and published data are in good agreement.
The effects of weathering exposure on unfilled and filled thermoplastic polyurethanes (TPU) materials are described as performed under different humidity conditions. For this purpose, a weathering device was used with UV-A 340 nm lamps at a constant temperature of 40 °C. The effects of environmental (UV and humidity condition) degradation on the frictional properties of TPU materials are presented along with surface analyses to characterize the chemistry of the degradative process. Photooxidative degradation of unfilled polymer leads to deterioration of physical and mechanical properties, which affects its tribological behavior significantly. Due to crosslinking, the stiffness of the material increases, reducing drastically the friction coefficient of unfilled TPUs. The frictional behavior of glass fiber reinforced TPU is less affected by radiation.