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Die Bewertung der Werkstoffbeständigkeit ist von großer Bedeutung bei Änderung der Zusammensetzung der Kraftstoffe und des Heizöls, insbesondere die Frage nach der Beständigkeit der Dichtungswerkstoffe bei Zusätzen von Bioethanol und Biodiesel (Rapsölfettsäuremethylester).
Vorhergehende Untersuchungen (Messungen der Veränderungen der Masse, der Zugeigenschaften und der Härte) bezogen sich auf die Bewertung der Beständigkeit häufig verwendeter Dichtungswerkstoffe wie FKM, FVMQ, VMQ, EPDM, CR, CSM, IIR, PA, NBR und PUR in Kraftstoffen und Heizöl mit 10 % Biodiesel (nicht gealtert und bis zu 5 Jahre gealtert) unter statischen Bedingungen.
Ziel der Untersuchungen war die Bewertung der Beständigkeit von Fluorkautschuk unter verpressten Bedingungen in Analogie zu den Einsatzbedingungen in der Praxis. Die Masse und der Druckverformungsrest von Prüfkörpern aus FKM wurden vor und nach der Auslagerung über einen Zeitraum von 3, 7, 14, 28, 56 und 90 Tagen in E10 (Kraftstoff mit max. 10 % Ethanol), E85 (Kraftstoff mit 85 % Ethanol), Biodiesel (Rapsölfettsäuremethylester), Super (Kraftstoff mit max. 5 % Ethanol), Dieselkraftstoff mit max. 5 % Biodiesel, Super Plus (Kraftstoff ohne Ethanolzusatz) und Heizöl mit 10 % Biodiesel (B10) bei 40 °C gemäß ISO 815-1 bestimmt. Die Druckverformungsrestprüfung zählt neben der Messung der Härte, der Dichte und der Zugeigenschaften zu den wichtigsten Grundprüfverfahren der Elastomerindustrie. Nach Ende der Auslagerung in den Kraftstoffen und der Aufhebung der Verpressung wur-de der Druckverformungsrest der Prüfkörper in regelmäßigen Zeitabständen bis zu einer Rücktrocknung > 90 Tage bestimmt. Zum Vergleich wurden Prüfkörper aus FKM ohne Kraftstoff oder Heizöl unter Verpressung bei 40 °C ausgelagert.
Die Masseänderung der Prüfkörper aus FKM betrug nach 90 Tagen Auslagerung in E10 9 %, in Super 8 %, in E85 4% und 0,6 % in Biodiesel. Die Erhöhung der Masse und die damit verbundene Quellung der Prüfkörper in E10 und Super mit 5 – 10% Ethanolzusatz hatte einen Einfluss auf den Druckverformungsrest, der sprunghaften Veränderungen unterlag im Vergleich zu den Werten nach Auslagerung in Biodiesel, Dieselkraftstoff und Heizöl B10 bei 40 °C. Zum Vergleich, unter statischen Bedingungen verringerte sich die Zugfestigkeit der Prüfkörper aus FKM nach Auslagerung in E10 bei 40 °C um 31 % und die Reißdehnung um 18 %.
Biodiesel (FAME) from rapeseed is an environmentally friendly alternative to common fossil fuels. It is also suitable to serve as blending component to fuels like heating oil. If the fuel composition is changed, materials compatibility must be guaranteed. Adding polar biodiesel to nonpolar heating oil, changes the blend’s solvency and might cause swelling, extraction and solvation of polymers.
The objective of this research was to investigate the compatibility of polymeric materials, which are commonly used for components in middle distillate facilities, along with blends of heating oil and 20 % biodiesel (B20). For this propose, ACM, HNBR, FKM, PE, PA 6, POM, PUR and PVC were exposed to heating oil and B20 for 42 and 84 days at 40 °C. In addition, the polymers HNBR, FKM, PA, POM and PVC were also exposed at 70 °C. Furthermore, the resistance of polymers in eight-year aged B10 at 40 °C was evaluated. Ageing of biodiesel increases acidity which might propagate polymer corrosion.
The materials were evaluated as resistant, if the loss in tensile properties (tensile strength and elongation at break) and Shore hardness remained under 15 % compared to the initial unexposed material values. For investigations under compressed conditions, the compression set was determined for specimens of ACM, FKM and HNBR after exposure in heating oil B0 and B20 for 3,7,14, 28, 56 and 90 days at 40 °C according to ISO 815-1.
It was found that the resistance in B20 at 40 °C was given for all tested polymers except PUR. In the 8 years aged B10, PUR and POM were not compatible and ACM just conditionally compatible. At 70 °C, FKM and PVC were resistant in B20, whereas HNBR and PA 6 were not compatible. Swelling occurred for the elastomers ACM, HNBR and PUR.
Biodiesel (FAME) from rapeseed is an environmentally friendly alternative to common fossil fuels. It is also suitable to serve as blending component to fuels like heating oil. If the fuel composition is changed, materials compatibility must be guaranteed. Adding polar biodiesel to nonpolar heating oil, changes the blend’s solvency and might cause swelling, extraction and solvation of polymers. The objective of this research was to investigate the compatibility of polymeric materials, which are commonly used for components in middle distillate facilities, along with blends of heating oil and 20 % biodiesel (B20). For this propose, ACM, HNBR, FKM, PE, PA 6, POM, PUR and PVC were exposed to heating oil and B20 for 42 and 84 days at 40 °C. In addition, the polymers HNBR, FKM, PA, POM and PVC were also exposed at 70 °C. Furthermore, the resistance of polymers in eight-year aged B10 at 40 °C was evaluated. Ageing of biodiesel increases acidity which might propagate polymer corrosion. The materials were evaluated as resistant, if the loss in tensile properties (tensile strength and elongation at break) and Shore hardness remained under 15 % compared to the initial unexposed material values. For investigations under compressed conditions, the compression set was determined for specimens of ACM, FKM and HNBR after exposure in heating oil B0 and B20 for 3,7,14, 28, 56 and 90 days at 40 °C according to ISO 815-1. It was found that the resistance in B20 at 40 °C was given for all tested polymers except PUR. In the 8 years aged B10, PUR and POM were not compatible and ACM just conditionally compatible. At 70 °C, FKM and PVC were resistant in B20, whereas HNBR and PA 6 were not compatible. Swelling occurred for the elastomers ACM, HNBR and PUR.
The objective of this research was to determine the resistance of frequently used sealing materials such as FKM (fluorocarbon rubber), FVMQ (methyl-fluoro-silicone rubber), VMQ (methyl-vinyl-silicone rubber), EPDM (ethylene-propylene-diene rubber), CR (chloroprene rubber), CSM (chlorosulfonated polyethylene), IIR (butyl rubber), PA (polyamides), NBR (acrylonitrile-butadiene rubber) and PUR (polyester urethane rubber) in fuels and heating oil with admixtures of biogenic sources such as E10 (fuel with 10 % ethanol), E85 (fuel with 85 % ethanol), non-aged and aged biodiesel, diesel fuel with 5 % biodiesel, non-aged and aged B10 (heating oil with 10 % biodiesel) at 20 °C, 40 °C and 70 °C.
Mass, tensile strength and breaking elongation of the test specimens were determined before and after the exposure for 84 days in the fuels. The visual examination of some elastomer test specimens clearly showed the great volume increase until break or partial dissolution. Shore hardness A and D (for PA) were determined before and after exposure of the test specimens in the biofuels for 42 days.
There is not determined a threshold for the reduction in tensile properties and Shore hardness in the international standards. Therefore a threshold of 15 % was determined for the evaluation of the compatibility.
In summary, it can be therefore stated that the chemical resistance of the fluoropolymers FKM and FVMQ in fuels and biofuels is the best one.
Due to the increasing demand for utilization and improvement of energy efficient materials, especially concerning requirements in lightweight construction and design, polyolefin materials are used extensively and in an increasingly broad range of applications.
Although loaded with stresses under yield stress, preformed voids, inhomogeneities or notches can possibly lead to damage and unexpected failure induced by liquid media in polyolefin materials. For PE-HD, slow crack growth (SCG) as well as environmental stress cracking (ESC) are relevant mechanisms of damage. SCG appears without influence of a surrounding medium or in “inert” media whereas ESC occurs in “active” media, which have decisive influence on damage mechanism and time to failure. To characterize the intrinsic resistance of the material against those damage mechanisms, the Full-Notch Creep Test (FNCT) is widely used and of paramount importance particularly for the assessment of pipe and blow molding types of PE-HD.
In this study, the FNCT – usually applied as a standardized testing method (ISO 16770) using a few universal model liquid media – is extended by investigations of selected relevant PE-HD materials with a variety of properties also in real media. Mainly topical fuels, customary in the market such as diesel and biodiesel are examined. Especially the influence of temperature, and the ESC behavior of PE-HD in media that are sorbed to a significant extent, are addressed. The underlying diffusion-controlled sorption process was assessed before comparing non-saturated specimens with samples previously saturated with sorbing media.
The investigations were performed using a novel FNCT-device with 12 individual sub-stations, each equipped with individual electronic stress and temperature control and continuous online monitoring of the specimen elongation.
In addition to acquired results concerning time to failure and elongation behavior, imaging techniques, such as light microscopy (LM), laser scanning microscopy (LSM) and X-ray computed tomography (CT scan) were utilized to obtain data concerning crack propagation and media migration. Fracture surface analysis (LM, LSM) and quasi in-situ imaging (CT scan) via measurement in different load stages are considered explicitly. Correlations of elongation behavior and data derived from imaging analysis such as fracture plane roughness and height of areas of ductile deformation were obtained.
Renewable resources become more and more relevant to maintain energy demands for an increasing global population. Biosynthetic fuels like biodiesel might replace conventional petrochemical fuels, such as diesel. However, more research is needed to characterize the interaction between the different fuels and the polymeric material, especially with respect to ageing and degradation.
The poster will present several interaction and degradation phenomena of high density polyethylene (PE-HD) induced by diesel and biodiesel 1-3. Also the possible influence of microbial growth (fungi and bacteria) is considered. The chosen PE-HDs are typical thermoplastic resins for container and storage tank applications. Degradation of PE-HD will be investigated by changes of the mechanical properties – with main emphasis on the Charpy impact strength 2. Furthermore, with alternating sorption and desorption cycles in combination with oven ageing the co-oxidation 3 of PE-HD in contact with biodiesel will be addressed.
Effect of different sulphur-based crosslink networks on the nitrile rubber resistance to biodiesel
(2017)
Biodiesel possesses some comparable physical properties to petroleum diesel in addition to its improved environmental benefits. Nonetheless, both fuels differ greatly with respect to their chemical compositions.
Therefore, the compatibility of the materials, which are commonly employed in contact with diesel, must also be assured for biodiesel. This paper assessed the influence of sulphur-based curing systems on the resistance of nitrile rubber to soybean biodiesel. Formulations were prepared using highacrylonitrile-content nitrile rubber by employing a two-level experimental design. The amounts of two different accelerators and sulphur were varied to achieve different types of vulcanisation systems.
Thermal analyses, mechanical tests and microscopy analyses were conducted to evaluate the behaviour of the material after contact with biodiesel. The results showed that the choice of the accelerator played an important role on the resistance of the rubber to the biofuel, and crosslink density was not a key factor with respect to the resistance.
Für Bauteile (Komponenten) von Versorgungsanlagen für flüssige Brenn- und Kraftstoffe muss die Beständigkeit der metallenen Werkstoffe und Polymere nachgewiesen werden. Im Anwendungsfall von Heizöl mit 20 % biogenen Anteilen in Form von Rapsölfettsäuremethylester (FAME, Biodiesel) ist es für eine konservative Beurteilung des Korrosionssystems Werkstoff/Medium/Umgebung wichtig, die Alterungseffekte des Mediums einzubeziehen.
Entwicklung eines Prüfverfahrens für die Untersuchung der Beständigkeit von metallenen Werkstoffen und Polymeren in Heizöl und Heizöl-FAME-Blends, das für eine Vorauswahl der Werkstoffe und zum Nachweis der Beständigkeit im Hinblick auf die bauaufsichtlichen Zulassungsverfahren geeignet ist.
Environmental Stress Cracking (ESC) and Slow Crack Growth (SCG) of PE-HD induced by external fluids
(2020)
High-density polyethylene (PE-HD) is widely used as a packaging material. Typical applications are pipes and containers for storage and transport of dangerous goods. For these applications, the understanding of the craze-crack damage mechanisms slow crack growth (SCG) and environmental stress cracking (ESC) is of importance. Since these mechanisms are considered to be the major causes of failure, their understanding is essential for inspection and release of those materials.
A well-established test method for the assessment of these damage mechanisms is the full-notch creep test (FNCT). It is used in this study for a detailed investigation of crack propagation phenomena in PE-HD container materials under the influence of different fluids such as air, water and aqueous detergent solutions (Arkopal N 100) as well as biodiesel and diesel. Based on the results of the FNCT, a classification scheme of different fluids is proposed, which allows for an assignment of the respective damage mechanisms. Hereby, it is differentiated between (i) inert, (ii) purely surface-active and (iii) additionally sorptive, bulk-active fluids with respect to SCG. If the test fluid changes the intrinsic properties (at the surface or in the bulk), the damage mechanism is addressed to ESC behavior.
In FNCT investigations, stress, temperature and specimen geometry were varied systematically. In addition to the time to failure as common measure for the resistance of a PE-HD type against crack propagation, specimen elongation was considered in detail.
Several imaging techniques were applied for fracture surface analysis of specimens tested in FNCT to gain novel information on SCG and ESC behavior. From height profiles obtained by laser scanning microscopy (LSM) and information on surface structures from scanning electron microscopy (SEM), indicators for the differentiation of the crack propagation mechanisms could be derived. Based on the LSM data, an algorithm for the distinction between ductile shear deformation and brittle crack growth as dominating failure mechanism was developed. Imaging techniques were also used for determination of crack propagation rates, which were related to time-resolved FNCT elongation data. From the time-resolved determination of crack lengths of partly damaged FNCT specimens, an increasing length of craze zone with a progressively propagating crack was revealed for the first time. This relation of crack and craze zones was specified by fracture mechanical considerations.
The FNCT is widely used to characterize the slow crack growth (SCG) behavior of polyolefinic materials in “inert” media as well as effects of environmental stress cracking (ESC) in which the medium has decisive influence on damage mechanism and time to failure. The test is of greatest importance for pipe and blow molding types of PE-HD - especially for transport and packaging of dangerous goods but also for most other high-performance applications.
Usually the FNCT is applied as a standardized testing method (ISO 16770) using a few universal liquid media, such as solutions of Arkopal N 100.
In our study, selected relevant PE-HD materials are investigated also in real media – practical formulations as well as representative pure chemicals – and influences of temperature and geometry of specimen and notch are explicitly addressed. Furthermore, the investigations comprise also the ESC behavior of PE-HD in media that are sorbed to a significant extent – one example are fuels, such as diesel and biodiesel – based on comparison with samples previously saturated with those media. Thus, also the underlying diffusion controlled sorption process has to be assessed before.
The investigations were performed using a FNCT-device with 12 individual sub-stations, each equipped with individual electronic stress and temperature control and continuous online monitoring of the specimen elongation.