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Zeitstandverhalten und strukturelle Veränderungen von vielfach wiederverarbeiteten Polyethylenen
(1985)
Wiederverarbeitung von Produktionsabfällen, möglichst in demselben Produktionsbetrieb oder Produktionszweig, in dem sie entstanden sind. Im Unterschied zu Recycling liegen hier vor Beginn der Wiederverarbeitung sortenreine, nicht verunreinigte und nicht durch Praxisbeanspruchung geschädigte Abfälle vor, sogenannte Reststoffe.
Two polyethylene types with ultra high (UHMWPE) and high molecular weight (HMWPE), which are used as neutron radiation shielding materials in storage casks for radioactive waste, were subjected to gamma irradiation doses up to 600 kGy and subsequent thermal ageing at 125 °C for up to one year. One material was a medical grade UHMWPE and the other a HMWPE containing an antioxidant. Degradation effects in the materials were characterized using colorimetry, UV-Vis spectroscopy, MIR and FTIR measurements, DSC and, in the case of HMWPE, insoluble content determination. Both materials exhibited a yellowing upon irradiation. The discoloration of UHMWPE disappeared again after thermal ageing, which is why it was attributed to annealable color centers in the form of free radicals entrapped in the crystalline regions of the polymer that recombine during thermal ageing. Furthermore, oxidation species were observed with MIR and FTIR spectroscopy. For HMWPE, the yellowing occurred during both irradiation and thermal ageing and was correlated to antioxidant decomposition. Additionally, black spots were observed after thermal ageing of HMWPE that were attributed to reaction products of antioxidant derivatives and catalyst residues. While only little evidence of oxidation species was found in the light material parts, oxidation is expected to concentrate in the black spots as the catalyst residue promotes hydroperoxide decomposition and thus radical formation that initiate polymer oxidation
Plastic storage tanks for heating oil have been on the market since the early 1970s in Germany, mainly made from polyethylene grades. Tank manufacturers and experts examining the tanks recommend the replacement of the tanks to ensure the safety after a period of 30 years. The tank manufacturer is legally obliged to specify the service life of the tanks.
Polyethylene is subject to ageing by alteration of the properties during its life cycle. A distinction is made between internal and external ageing processes. The internal ageing, such as the breakdown of internal stresses, post-crystallization, phase sepa-ration of multicomponent systems and plasticizer migration is attributed to thermodynamically instable conditions of the plastic material. The external ageing in form of stress cracking, fatigue cracking, thermooxidative degradation or swelling is based on physical or chemical effects of the environment of the polyethylene grade. The degree of ageing and the nature of the degradation process mainly depend on the chemical degradation of the polyethylene, the wall thickness of the tank and the environmental conditions. There are no results available on the long-term behaviour of the polyethylene grades used as materials for heating oil storage tanks, especially after a service life of more than 25 years.
The aim of this investigation was the determination of the factual degree of damage in comparison to the uncontaminated polyethylene grades. Data on the melt flow rate (MFR) and density of the used polyethylene grades are available because the BAM was the competent authority for the approval of the plastic heating oil storage tanks until the end of the 1980s.
The technical service of specialist companies for fuel tank disposal supplied tank sections from the bottom, the shell and the roof of 8 segregated heating oil storage tanks. Some of the tanks had been in service for more than 30 years. Two polyethylene grades mainly were used as materials for these tanks over this time. The determination of the MFR according to EN ISO 1133 and the FTIR spectroscopy followed standard test methods.
The highest average percentage increase in the MFR was determined as 31- 43 % for the bottom section of the tanks, for both the inner shell and the outer shell. The lowest increase in MFR was measured for the top of the tank, with 6 - 12 % for the inner shell and 0 - 8 % for the outer shell. The tank shell sections had an average percentage increase in MFR of 10 - 33 % for the inner shell and of 14 - 40 % for the outer shell.
The oxidative damage of the polyethylene grades was highest in the bottom area due to the permanent contact with the heating oil and degradation products.
The microtome cuttings were analyzed with image-guided infrared microscopy in the transmission mode and confirmed the results obtained with the MFR measurements.
In summary it can be concluded that the oxidative damage of the polyethylene grades after long-term contact with heating oil is relative low.
In this paper, we demonstrate the effects of radiation exposures of polymeric materials with UV-A 340 nm lamps (ISO 4892-3, Type 1A) at -10 °C in comparison to an irradiation at +50 °C using a Global UV Test 200 fluorescent lamp device from Weiss Umwelttechnik GmbH, which incorporates an active cooling appliance. While the effects at -10 °C actually are lower than at + 50°C their extent was clearly beyond expectations.
High and ultra-high molecular weight polyethylenes were gamma-irradiated with doses up to 600 kGy. The changes in the material properties were analysed using DSC, DMA, IR spectroscopy, as well as measurements of density and insoluble content. The irradiation led to an increase of the degree of crystallinity because of chain scissions during irradiation, leading to shorter and thus more mobile chains. Both the plateau value of the shear modulus G′ and the insoluble content increased with Irradiation dose, indicating the formation of additional crosslinks. Furthermore, IR spectroscopy revealed irradiation induced oxidation and the formation of double bonds, indicating that some of the hydrogen atoms responsible for the neutron shielding capability have been released.
Tanks for heating oil made of polyethylene grades have been on the market since the early 1970s in Germany. Tank manufacturers recommend the replacement of the tanks after a period of 30 years due to guarantee safety. Polyethylene grades are subject to ageing by alteration of the properties during their life cycle. The degree of ageing and the nature of the degradation process mainly depend on the chemical degradation of the polyethylene, the wall thickness of the tank and the environmental conditions. There are no results available on the long-term behavior of the polyethylene grades, especially after a service life of more than 30 years. The aim of this investigation was the determination of the factual degree of damage in comparison to the uncontaminated polyethylene grades. Material data of the used polyethylene grades are available because the BAM was the competent authority for the tests and expert reports for the approval of these tanks until the middle of the 1990s.
The determination of the Melt Flow Rate (MFR) and the Fourier Transmission IR Spectroscopy (FTIR) of tank sections from the bottom, the shell and the roof of 10 segregated heating oil storage tanks produced of polyethylene grades A and B were used as tests methods.
The MFR measurements of the tank sections showed differences in the values depending on the weight which was used (5 kg or 21.6 kg). A reduction of the MFR values was measured for most of the sections of tanks made of polyethylene grade B after a service life of the tanks of more than 30 years. This grade is mainly subject to the internal ageing by cross-linkages, increased degree of branched molecules and loss of the plasticizer, and to a lesser extent by oxidative degradation. The FTIR analysis, especially of tank sections of the bottom and the shell showed that the intensity of the CH2 asymmetric and symmetric stretching vibrations in the range: 2800 - 2900 cm-1 and the CH2 bending deformation vibration at 1400 cm-1 increased due chain scissions. The intensity of the carbonyl stretching vibration C=O at 1740 cm-1 is low. The carbonyl index characterizes the degree of oxidation.
Unpigmented HDPE jerrycans filled with nitric acid (55%) and water respectively had been exposed to outdoor conditions for one Berlin summer season. As both liquids underwent equal temperature progression, exposure effects of UV radiation and nitric acid as well as of their combination can be separated and compared. On the basis of various property changes after these exposures, synergistic action is evaluated and compared to a damaged Intermediate Bulk Container (IBC) from a transport accident.
It is found that carbonyl formation goes along with lightness increase in color measurement due to microcracking and with a worsening in mechanical behavior, all of them showing synergistic effects of UV and nitric acid exposure. In contrast, embedding nitrogen compounds goes along with yellowing of the material but cannot be correlated to oxidation.
The reason for intensified damaging is the decomposition of the 55-percent nitric acid and formation of nitrogen oxides even at ambient temperatures, caused by UV radiation. Thus, damaging effects become similar to those caused by fuming nitric acid exposure at temperatures above 60 °C, with the result of strong oxidative degradation of the polyethylene.
In contrast, exclusive exposure to the 55-percent nitric acid at 40 °C does not cause any failure.
It can therefore be assumed that also the damaged IBC had been exposed to both UV radiation and nitric acid, probably outdoors.
In this study, femtosecond laser-induced sub-micrometer structures are generated to modify polyethylene (PE) surface topographies. These surfaces were subjected to bacterial colonization studies with Escherichia coli and Staphylococcus aureus as test strains. The results reveal that the nanostructures do not influence S. aureus coverage, while the adhesion of E. coli is reduced.
Heating oil storage tanks made of polyethylene grades have been on the market in Germany since the early 1970s. To ensure safety, their replacement is recommended by tank manufacturers after a period of 30 years. Polyethylene is subject to ageing by alteration of the properties during its life cycle. The degree of degradation and the nature of the process mainly depend on the chemical alteration of the polyethylene, the wall thickness of the tank and the environmental conditions. There are no data available on the long-term behaviour of the polyethylene grades, especially after a service life of more than 30 years.
The aim of this investigation was to find a suitable test method to determine the factual degree of damage in comparison to the uncontaminated polyethylene grades. Material data of the used polyethylene grades are available because the BAM was the competent authority for the tests and expert reports for the approval of these tanks until the middle of the 1990s. Therefore, tank sections from the bottom, the shell and the roof of 22 individual storage tanks produced of polyethylene grades A and B have been examined by Melt Flow Rate (MFR) and Attenuated Total Reflectance (ATR). Their service life was in the range between 20 and 41 years.
The MFR measurements of the tank sections showed differences in the values depending on the weight which was used (5 kg or 21.6 kg). An increase of the MFR was determined for the samples of polyethylene grade A, whereas a reduction of the MFR values was measured for most samples of polyethylene grade B. This grade is mainly subject to the internal ageing by cross-linkages, increased degree of branched molecules and loss of the plasticizer.
ATR analysis exhibits an absorption band at 909 cm‒1 predominantly in samples of polyethylene grade A indicating chain scission and concomitantly formed terminal vinyl groups. This absorption band can be used for the characterization of the ageing of the polyethylene grades.
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.