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Organisationseinheit der BAM
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Eingeladener Vortrag
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Adaption of the Acid Dew and Fog (ADF) Test for Service Life Predicitons of Aircraft Coatings
(2003)
While artificial weathering is a long-established tool to investigate long-term behaviour of polymers at outdoor conditions, the use of chemiluminescence as a highly sensitive and broadly applicable sensor for the effected change is a recent addition. This combination of artificial weathering with chemiluminescence could already be successfully applied to differentiate and evaluate long-term stability of various real use polymeric building materials relatively to each other and promises to be a useful tool for a variety of other polymeric materials as well.
Adaption of the acid dew and fog (ADF) test for service life predicitons of aircraft coatings
(2003)
Degradation effects of automotive coatings after weathering as detected by thermoluminescence
(2004)
Adaption of the Acid Dew and Fog (ADF) Test for Service Life Predictions of Aircraft Coatings
(2003)
Photo-oxidative ageing of polymers under defined exposure (UV, humidity) was investigated from two points of view: a) the ageing process Starts from the topmost surface and penetrates slowly towards bulk and b) radicals play an important role among ageing. Therefore, X-ray photoelectron (XPS) and electron spin resonance (ESR) spectroscopy were applied to show both, the progressive incorporation of oxygen during in-situ UV irradiation (XPS) and the formation of radicals (ESR) in the polymer. The intensity of ESR Signals served as measure for radical concentration. The Validation of this correlation was checked for polyethylenes (PE) equipped with different concentrations of Hostavin N30 UV stabilizer.
The outdoor weathering of polymers is mainly due to UV radiation, water, Pollution, humidity, temperature etc. To understand the effects of weathering, simulated tests need to be undertaken in lab scale. Such tests must be quite efficient and similar to the effects of natural weathering. This paper mainly focuses on the effects of UV radiation along with humidity on LDPE.
To determine a polymer’s spectral response of photo degradation, two main methods have been established. The so-called “filter technique” uses polychromatic radiation, which is filtered by a set of various sharp cut-on filters. This procedure provides separated reading points of an activation spectrum of the investigated material. With the "spectrographic technique” a specimen is irradiated with pectrally dispersed radiation, locally quasi monochromatically, and the local property changes.are related to the radiant exposure at the respective wavelengths. A third method, the irradiation of specimens with quasi monochromatic radiation behind interference filters, is rarely used.
These methods have advantages and disadvantages and therefore, there are limits for conclusions from these spectral data. Concerning the quasi monochromatic Irradiation of specimens the development of new UV radiation sources looks promising.
With the rapid development of inexpensive UV Light-emitting diodes (LEDs), new : sources of nearly monochromatic radiation in the UV ränge are available, even down to about 250 nm. To determine the spectral response, the use of such UV-LEDs in TO-18 ) and TO-39 metal cases combines the advantages of low cost and energy efficiency, stable spectral irradiance, temperature.and humidity control, larger specimen areas, and an easy and stable analysis.
Combinations of different UV LEDs are also discussed as replacement for xenon arc ' radiation sources, see patent application EP01528388A1.
Artificial weathering of LDPE under dry conditions (<10% of relative humidity) by UV radiation was monitored
by dielectric spectroscopy. For an apolar polymer like LDPE, dielectric study yields information
about the change in structure and dynamics of the system. The fluctuations of the polar groups which
are generated as a result of photooxidation such as carbonyl groups can be monitored as characteristic
relaxation processes like the αc or β mode. The dielectric loss characterized by typical dielectric parameters
like the activation energy and dielectric strength are strongly dependent upon changes induced
by photooxidation in the amorphous and crystalline domains. This paper discusses in detail how the foil
reached its mechanical disintegration. It was found that initial stages of weathering induce chain scission
and/or crosslinking in the amorphous domains of the polymer and the motional processes in the crystalline
regions are not affected. After this induction period, an increase in the degree of crystallization was
observed by employing differential calorimetry. The increasing crystallinity is considered as one of the
reasons for embrittlement which finally leads to the complete loss of the structural integrity.
Chemiluminescence (CL) is a sensitive method of investigating the thermo-oxidative stability of polymers in the early stages of degradation. Therefore, CL measurements were applied to different automotive coatings to evaluate their degradation behavior during artificial weathering. In this work, CL measurements were carried out for different automotive coatings to follow their degradation behavior during artificial weathering. The CL emission depends on sample-specific parameters like stabilizer, matrix, or hardener; experimental parameters like the oxygen partial pressure; and exposure parameters like the duration of weathering. The potential of CL could be demonstrated by classifying materials into categories of good, medium, and low degradation performance at a much earlier stage of weathering exposure than in combination with the usual visual detection of weathering effects.
Accelerated weathering test for plastics and coatings that are exposed to acidic precipitation
(2009)
Due to the occurrence of acidic precipitation, and due to the fact that polymers and stabilizers may be sensititve to acids, it is important to have a laboratory test that combines weathering exposure with acidic exposure. The loss of stabilization caused by an acid damage of stabilizing system gets evident only over the weathering progress. For solid samples, for wich mostly the surface properties are relevant, the "Acid Dew and Fog Test" (ADF test) was established. For woven or tufted materials, the "Acid Rain Test" (AR test) was developed. The proposed weathering tests aim at plastics as well as at coatings.
The thermo-oxidative stability of commercially available polymer optical fibers (POFs) and their components (cores and claddings) was investigated. All the bare POFs (core and cladding only) studied here were based on poly(methyl methacrylate) (PMMA) core. The fibers were exposed to 100 °C/low humidity for about 4200 h. Chemiluminescence (CL) technique was applied to investigate the thermo-oxidative stability and for measuring the transmission loss during exposure a prototype device called multiplexer was used. POFs exhibited variation in thermo-oxidative stability although they possessed identical core material PMMA. This was due to difference in the chemical compositions of claddings. Claddings were more susceptible to the thermo-oxidative degradation compared to cores. The thermo-oxidative degradation of both the cladding and the core was found in POFs as a result of climatic exposure. POFs showed an early drop-off followed by a slow decline of transmission. The early drop-off of transmission was attributed to physical changes like thermal expansion and the slow decline of transmission to chemical changes like oxidative degradation of POFs. A good linear relationship between optical transmission stability and thermo-oxidative stability of POFs was established from these studies.
Combined impact of ultraviolet and chemical fluids on high-density polyethylene packaging material
(2012)
To investigate the ageing behaviour of filled plastic containers outdoors, square cuts of the wall of two high-density polyethylene (HDPE) types were exposed to ultraviolet (UV) radiation at their front side and to specific liquid chemicals (de-ionized water, surfactant or White Spirit) at their back. The UV radiant exposure at the front side was 80 MJ/m².
To compare the actions of the different exposures, separate dark backside fluid exposures were performed, in parallel. Besides, UV weathering was carried out until a UV radiant exposure of 325 MJ/m², being roughly comparable to outdoor exposure of one year in Northern Australia.
An unpigmented HDPE included in the investigation gave no sufficient protection for the White Spirit. In addition, it showed clear degradation after several of these exposures. In combination with the White Spirit, an increase of carbonyl bonds was measured, presumably assignable to degradation products of the White Spirit.
For a pigmented HDPE material, with the implemented combined exposures, no relevant damage was observed, within applied the exposure period.
Scrap tyres are widely reused in the form of granules as infill materials or component of sub-base layers in construction of sporting grounds such as synthetic turf areas and athletic track surfaces. The recycled rubber may contain organic and inorganic pollutants due to the presence of vulcanisation catalysts, stabilisers and other additives which can be released into soil and groundwater in the case of outdoor sports facilities. In order to evaluate the amount of potentially mobile pollutants, leaching tests can be employed. This study aimed particularly at the investigation of the feasibility of column tests using complete synthetic surface flooring or turf system assemblies. The release of zinc and polycyclic aromatic hydrocarbons (PAH) leached from components of sports surfaces containing recycled rubber granules was considered. Additionally, batch tests on coated and uncoated styrene butadiene rubber (SBR) granules aged by artificial weathering were performed to indicate its possible influence on the leaching behaviour of zinc and PAH. The chosen approach of column tests simulating typical complete synthetic sports surface installations has been proven to be feasible and robust. The time-dependent leaching behaviour and interactions between single components can be evaluated by column tests. Zinc was the most relevant contaminant in the eluates and its leachability was enhanced after accelerated ageing by artificial weathering. Leachable PAH were found in relatively low but well detectable amounts which increase by ageing as well.
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.
Waste disposal of carbon nanotube (CNT) containing products is expected to be the most important pathway for release of CNTs into the environment. In the present work, the use of radiolabelled CNTs (14C-CNT) for polycarbonate polymer nanocomposites with 1 wt% 14C-CNT content allowed for the first time to quantify and differentiate the CNT release according to the type of impact along the materials' ageing history. After an initial exposure of the nanocomposite by solar-like irradiation, further environmental impacts were applied to composite material. They aimed at mimicking disposal site conditions that may induce further ageing effects and CNT release. This study included shaking in water, rapid temperature changes, soaking in humic acid solution as well as waste water effluent, and, finally, gentle mechanical abrasion. All ageing impacts were applied sequentially, both on pristine (control) and on solar-irradiated nanocomposites. All experiments were accompanied by absolute quantification of radioactive release as well as chemical and morphological analyses of the nanocomposite surfaces using infra-red (IR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The morphological analysis showed that spectral irradiation can uncover CNT networks on the outer nanocomposite surface layers by polymer degradation. After having subjected the solar-irradiated nanocomposite to all studied disposal site effect, the total radioactive release was quantified to amount to 64 mg CNT/m2, whereas only 0.8 mg CNT/m2 were found for the un-irradiated control sample. Solar degradation of polymers was thus found to significantly increase the propensity of the studied polymer nanocomposites to release CNTs during ageing effects at the product's end-of-life typical for disposal sites.
After several months of operation, many photovoltaic (PV) modules develop a discolouration defect called snail trails which appear as irregular dark traces across the cells. These traces are caused by silver nanoparticles accumulating within the encapsulation foil directly above the grid finger. In this work we systematically investigate combinations of encapsulation and back-sheet foils with respect to their susceptibility for snail trails. We can show that certain additive compositions within the encapsulation and back sheet foils are critical for the formation of the discolouring silver nanoparticles. We suggest a reaction model explaining the formation of snail trails from a chemical point of view. This fundamental understanding allows the rapid testing of foils for their snail trail sensitivity as well as the special design of resistant foils.
Jerrycans made from three different types of high-density polyethylene (HDPE) were exposed outdoors, for one Berlin summer season. They were filled with a 55 percent nitric acid solution (HN03), pure water, or air, and half of them were protected from sunlight by an UV absorbing canvas. Thus, the separate effects of UV radiation and nitric acid could be compared to the combined impact. Combined impact was mainly affected by decomposition of nitric acid, resulting in presence of reactive nitrogen oxides, increased oxygen partial pressure, and UV radiation energy, simultaneously in vapour phase.
To investigate the degradation effects after the outdoor exposure, jerrycans were exposed to a so called hydraulic internal pressure test, similar to an approval test for dangerous goods packaging. After combined impact of UV radiation and nitric acid, internal pressure tests showed very fast failures, whereas after separate impacts no remarkable deteriorations were observed, compared to unaged jerrycans.
Temperature is an important parameter in weathering tests. In many (photo-)chemical degradation processes a Variation of the specimen temperature by A t = + 1 °C can cause a Variation of AP(property change) by ± 8%.
Since the early eighties it is well known that some types of black panel thermometers can show temperatures that are far below the maximum surface temperature of a black specimen. Although, there were precise requirements for the black coating of the BPT, a replacement by a white coating - depending on the design of the BPT - did not really change the temperature shown by the thermometer. There was no correlation between the BPT and the specimen surface temperature.
In Europe and later at ISO the so-called black- and white-standard thermometers BST/WST were introduced. Now, there are BST and WST (ISO) and there are thermally uninsulated and insulated BPT and WPT (ASTM), partly for artificial or for outdoor exposure. And there are other adventurous procedures to determine surface temperatures.
The different types of thermometers and different procedures will be discussed and it will be shown that there is no procedure which establishes a correlation between outdoor surface temperatures and surface temperatures in artificial exposure tests.
The aim of the joint project ViPQuali (Virtual Product Qualification) was to describe a components ageing behaviour in a given environment, by numerical simulation.
Having chosen polypropylene (PP) as the material, which does not show sensitivity to moisture, the relevant weathering parameters of the doseresponse functions could be limited to spectral irradiance and temperature.
In artificial irradiation tests, for PP plates of varied stabiliser content, spectral sensitivity as well as temperature dependence of irradiation-caused crack formation was quantified. For that purpose, samples were exposed both to artificial weathering tests at various constant temperatures and to spectrally resolved irradiation. The temperature dependence could be modelled by an Arrhenius fit. For fitting the spectral sensitivity, a plateau function was chosen. Subsequently, the stabiliser content was parameterised and extrapolated.
The formed dose–response functions were incorporated into a Computational Fluid Dynamics (CFD) software program, simulating the environment of a sample within a Phoenix-exposed IP/DP (Instrument Panel/Door Panel box) box, based on sun position and weather conditions, including radiation interactions. Observed local effects as well as the general ageing advance of PP hats are compared with respect to simulation and experiment.
Resulting from this project, for this most simple example of PP of varied stabiliser content, the time to failure can be estimated for each weathering exposure environment with known time-resolved irradiance and temperature conditions.