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Eingeladener Vortrag
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Compatibility of high density polyethylene grades with bioethanol-gasoline blends and biodiesel
(2012)
Compatibility of high density polyethylene grades with bioehanol-gasoline blends and biodiesel
(2012)
Biofuels represent an important renewable fuel alternative to petroleum-derived transport fuels. Materials compatibility is a major concern whenever the fuel composition is changed. The aim of this work is to study the interaction of the elastomers: FKM, EPDM, CR, CSM, NBR, IIR, VMQ and FVMQ and biofuels such as biodiesel (FAME), E85 (fuel with 85% ethanol) and B10 (heating oil with 10% biodiesel). Exposure tests were performed with test specimens at 40°C (104°F) and 70°C (158°F) for 84 days to document the changes in mass, volume and tensile properties according to ISO 1817. The exposure tests in E85 showed that the weight gain caused by swelling was in the range up to 12%. The lowest decrease in the tensile properties was determined for FKM, VMQ and IIR. The weight gain of the elastomers in biodiesel varied between 10% (FKM) and 126% (CSM) and the loss of tensile strength between 16% (FKM) and 100% (CSM) at 70°C (158°F). FKM and FVMQ absorbed much less B10 and swelled less. NBR, EPDM, CR, CSM, IIR and VMQ were not resistant to B10 at all as the decrease in the tensile properties was significantly over 50%. Among all of the elastomers FKM showed high compatibility with these biofuels up to 70°C (158°F).
The objective of this research was to determine the resistance of frequently used sealing materials such as EPDM, FKM, FVMQ, CR, CSM, IIR, NBR, PA, PUR and VMQ in aged biodiesel and heating oil B10 with 10 % biodiesel.
The mass, tensile strength, breaking elongation and Shore hardnesses of the test specimens were determined before and after exposure in non-aged, one-year, two-year, three-year and four-year aged biodiesel and B10 at 20 °C, 40 °C and 70 °C.
A threshold for the reduction in tensile properties and Shore hardness is not set in the international standards. Therefore, a threshold of 15 % was set for the evaluation of the compatibility. The decrease in tensile properties and Shore hardness increased with the age and the temperature of the biodiesel and the heating oil.
The age of the biodiesel was not relevant for the sealing materials CR, CSM, EPDM, IIR and NBR, which were generally not resistant to biodiesel and B10. FKM and PA showed high compatibility in non-aged and aged biodiesel. FVMQ and PA could be evaluated as resistant in non-aged and aged B10 at 20°C and 40°C, whereas FKM was resistant up to 70°C despite of the age of B10.
The objective of this research was to determine the resistance of frequently used sealing materials such as EPDM, FKM, FVMQ, CR, CSM, IIR, NBR, PA, PUR and VMQ in aged biodiesel and heating oil B10 with 10 % biodiesel.
The mass, tensile strength, breaking elongation and Shore hardnesses of the test specimens were determined before and after exposure in non-aged, one-year, two-year, three-year and four-year aged biodiesel and B10 at 20 °C, 40 °C and 70 °C.
A threshold for the reduction in tensile properties and Shore hardness is not set in the international standards. Therefore, a threshold of 15 % was set for the evaluation of the compatibility. The decrease in tensile properties and Shore hardness increased with the age and the temperature of the biodiesel and the heating oil.
The age of the biodiesel was not relevant for the sealing materials CR, CSM, EPDM, IIR and NBR, which were generally not resistant to biodiesel and B10. FKM and PA showed high compatibility in non-aged and aged biodiesel. FVMQ and PA could be evaluated as resistant in non-aged and aged B10 at 20°C and 40°C, whereas FKM was resistant up to 70°C despite of the age of B10.
The notched impact strength at -30 °C is one of the selected properties, together with the corresponding test method and tolerances, for a comparison of polyethylene grades of one design type in the procedural rule on suitability proof for alternative plastic resins used for packagings and intermediate bulk containers (IBCs) for the transport of dangerous goods.
The marginal drop heights determined with the drop test at -18 °C after pre-storage of the test samples with 55 % nitric acid at 40 °C only partly related to the notched impact strength at -30 °C. The Charpy method is only suitable for classifying the grade in relation to toughness behavior and using this classification for comparison with other grades. Notched impact strength can provide a qualitative indication if the test samples fail under shock forces.
Conditioning the design types with 55 % nitric acid for 21 days at 40 °C causes an increase in the marginal drop heights of the design types in drop tests at -18 °C when compared with design types without pre-storage. Post-crosslinking of the grades increases stiffness because of the acidic influence.
Resistance to stress cracking by wetting solution is one of the selected properties together with the corresponding test method FNCT and tolerances for a comparison of polyethylene grades of one design type in the procedural rule on suitability proof for alternative plastic resins used for packagings and intermediate bulk Containers (IBCs) for the transport of dangerous goods.
The environmental stress crack resistance determined by Full Notch Creep Test (FNCT) represents the impacts from the stacking tests at 40 °C performed with Standard liquid wetting solution (without pre-storage) and with normal butyl acetate saturated wetting solution (pre-storage with normal butyl acetate). Environmental stress crack resistance determined with FNCT for the polyethylene grades was related to the times to failure of different jerrican samples made of these grades in stacking tests with 5 % wetting solution and a n-butyl acetate saturated wetting solution (pre-storage with n-butyl acetate) at 40 °C. The FNCT is suitable for comparison of polyethylene grades in relation to environmental stress crack resistance independent of their use as drum, IBC or jerrican material. The stiffness of polyethylene grades should be taken into account to the comparison as jerricans are not only chemically but also mechanically stressed.
Technically high-quality hollow articles made of polyethylene have proved many times their value as dangerous goods packagings. Design type tests according to the international regulations for the transport of dangerous goods - drop test, stacking test, hydraulic pressure test and leakproofness test must be performed for every design type and manufacturer. The properties melt flow rate (MFR), relative density (D), low temperature notched Impact strength (N.I.S.) at -30 °C, environmental stress crack resistance (FNCT) and resistance to oxidative degradation Ox by nitric acid (determined by the increase of MFR) have been selected together with the corresponding test methods and tolerances for a comparison of polyethylene grades of one design type in the procedural rule on suitability proof for alternative plastic resins used for dangerous goods packagings and intermediate bulk containers (IBCs) – EN 15507. We wanted to proof the practical relevance of this standard by comparing the relationship between the results of the FNCT and the times to failure of design types in stacking tests with wetting solution and normal butyl acetate saturated wetting solution.
Resistance to stress cracking by wetting solution is one of the selected properties together with the corresponding test method FNCT and tolerances for a comparison of polyethylene grades of one design type in the procedural rule on suitability proof for alternative plastic resins used for packagings and intermediate bulk containers (IBCs) for the transport of dangerous goods.
The environmental stress crack resistance determined by Full Notch Creep Test (FNCT) represents the impacts from the stacking tests at 40 °C performed with standard liquid wetting solution (without pre-storage) and with normal butyl acetate saturated wetting solution (pre-storage with normal butyl acetate).
Environmental stress crack resistance determined with FNCT for the polyethylene grades was related to the times to failure of different jerrican samples made of these grades in stacking tests with 5% wetting solution and a n-butyl acetate saturated wetting solution (pre-storage with n-butyl acetate) at 40 °C. The FNCT is suitable for comparison of polyethylene grades in relation to environmental stress crack resistance independent of their use as drum, IBC or jerrican material. The stiffness of polyethylene grades should be taken into account to the comparison as jerricans are not only chemically but also mechanically stressed.
More than 400 Mt of dangerous materials are transported in Germany every year, of which 150 Mt are by road. Tank containers, tank vehicles and rail tank cars are used for the carriage of dangerous goods in large quantities. Data on the operating life of tanks are only available, in practice, to a minor degree. They are only partly published, mainly after accidents.
The BAM-List - Requirements for Tanks for the Carriage of Dangerous Goods, which has compatibility evaluations of metallic and polymeric materials, has been the basis for substance-related prototype approvals for tank containers and portable tanks designed for the carriage of dangerous goods by the BAM since publication of the first edition in 1989. These data are also used for the approval of rail tank cars and road tank cars and are used as a source of knowledge not only in Germany but also worldwide.
Tank leakages caused by tanks or rail tank cars being made of tank and sealing materials which are not resistant to the fill goods are avoided by using the material resistance data of the BAM.
Corrosion damage is among the main causes of damage. Uniform and non-uniform area corrosion without mechanical stress in aqueous substances is one of the most frequent types of corrosion during the transport of chemicals in tanks. Much damage by pitting corrosion occurs during the transport of substances containing chlorides or substances which separate chloride ions in the presence of moisture.
Operational stresses are caused by the effects of both the road and the dangerous goods being transported. Mechanical damage often results from long-term overstressing and occurs after longer operating times.
Operational failures cause damage which may appear during the service of tank containers, road tank cars or rail tank cars. The damage results from the inattention of employees when opening and closing the valves. Traffic accidents also cause damage to tanks and frames.
Many cases of damage are due to weld area cracks resulting from four basic errors in construction, material, manufacturing and operation. Manufacturing errors can be undetected and the starting point of cracks which only grow under service conditions.
Manufacturing errors result from variations in measurement and design, fittings, state of surface (hardness, abrasiveness) and mechanical surface damage (scratches, cracks). Incorrectly welded joints and errors during mechanical deformation are typical mistakes when installing the component parts. Variations in the wall thickness or combinations of different materials lead to manufacturing errors too. A lot of tanks are not used for the transport of dangerous goods before the end of their service life as they do not fulfil the revised technical safety requirements in the Dangerous Goods Regulations.
Predictions in the BAM-List based on literature data and corrosion test results are reflected in the service (operating) life. Rail tank cars made of carbon steel, for example, which are mainly used for the transport of petroleum products, can achieve a service life of 40 – 50 y.
Rail tank cars produced of austenitic CrNi- or CrNiMo-steel can reach an operating life of at least 30 y, whereby the corrosiveness of the transport substances plays an important role.
The notched impact strength at -30 °C is one of the selected properties, together with the corresponding test method and tolerances, for a comparison of polyethylene grades of one design type in the procedural rule on suitability proof for alternative plastic resins used for packagings and intermediate bulk containers (IBCs) for the transport of dangerous goods.
The marginal drop heights determined with the drop test at -18 °C after pre-storage of the test samples with 55 % nitric acid at 40 °C only partly related to the notched impact strength at -30 °C. The Charpy method is only suitable for classifying the grade in relation to toughness behavior and using this classification for comparison with other grades. Notched impact strength can provide a qualitative indication if the test samples fail under shock forces.
Conditioning the design types with 55 % nitric acid for 21 days at 40 °C causes an increase in the marginal drop heights of the design types in drop tests at -18 °C when compared with design types without pre-storage. Post-crosslinking of the grades increases stiffness because of the acidic influence.
The material parameters melt flow rate MFR, density D, notched impact strength N.I.S. at -30 °C, stress crack resistance FNCT and resistance to oxidative degradation Ox (determined by the increase of MFR) have been selected for a comparison of polyethylene grades for one design type in the “European Standard EN 15507 - Transport packaging for dangerous goods - Comparative material testing of polyethylene grades”. The parameters have a systematic relationship with design type tests. The notched impact strength at -30 °C and the resistance to oxidative degradation of polyethylene grades determined with test specimens of compression moulded sheets are directly comparable with drop tests at -18 °C of design types produced of these grades after pre-storage with 55 % nitric acid for 21 days at 40 °C. The impact of the pre-storage time of jerricans with 55 % nitric acid at 40 °C and 23 °C on the marginal drop heights in drop tests at -18 °C, on the MFR and on the tensile properties tensile strength, breaking elongation and the elastic modulus were investigated. Packaging design types (jerricans) made of three polyethylene grades from different producers were pre-stored with 55 % nitric acid for 21,42 and 84 days at 40 °C as well as for six months at 23 °C. The MFR and tensile properties of test specimens taken from the design type side walls as well as the marginal drop heights of the jerricans in drop tests at -18 °C were determined.
The values of the notched impact strength at -30 °C of polyethylene grades are not comparable with the marginal drop heights determined in drop tests at -18 °C. The oxidative damaging impact of nitric acid has a greater effect on the grade with lower resistance to oxidative degradation by reducing more significantly the marginal drop heights with increasing pre-storage time.
Pre-damage with 55 % nitric acid for 21 days at 40 °C, as recommended in ISO 16101 and EN 15507 caused an increase in the marginal drop heights of most design types in drop tests when compared with design types without pre-damage. The test results demonstrated clearly that pre-storage of the jerricans for six months at 23 °C caused a higher increase in the MFR and lower marginal drop heights of the jerricans in drop tests at -18 °C compared with pre-storage of the jerricans for 21 days at40 °C.
The mechanical properties change as a result of diffusion of nitric acid into the polyethylene grades and the reaction of the nitric acid with the polymers. The percentage decrease and increase in the tensile strength, breaking elongation and elasticity modulus of test specimens taken from the design type side walls after different pre-storage times were only partly comparable with the marginal drop heights in drop tests at -18 °C.
The material parameters melt flow rate (MFR), density (D), notched impact strength (NIS) at –30°C, stress crack resistance [determined with the Full Notch Creep Test (FNCT)] and resistance to oxidative degradation (Ox) have been selected for a comparison of polyethylene grades in the European standard EN 15507. These parameters have a relationship with design type tests of packagings for the transport of dangerous goods.
This paper presents the results of additional investigations to determine the impact of the pre-storage time of jerricans with 55% nitric acid at 40°C and 23°C on the marginal drop heights in drop tests at –18°C, on the MFR and on the tensile properties. Jerricans made of different polyethylene grades were pre-stored with 55% nitric acid for 21, 42 and 84 days at 40°C and for six months at 23°C.
The tests showed that the NIS values at –30°C of polyethylene grades were not comparable with marginal drop heights determined in drop tests at –18°C.
Pre-damage with 55% nitric acid for 21 days at 40°C led to an increase in the marginal drop heights of the jerricans. Altering the test regulations by increasing pre-storage time with 55% nitric acid to 42 days would be an alternative.
The test results demonstrated clearly that pre-storage of the jerricans for six months at 23°C caused a higher increase in the MFR and lower marginal drop heights for the jerricans when compared with pre-stored jerricans for 21 days at 40°C.
The chemical industry has expressed great interest in using polyethylene terephthalate (PET) as material for packagings for the transport of dangerous goods. Due to the high strength and stiffness of PET, the wall thickness and weight of packagings can be reduced. This is a relevant cost factor. PET is a semi-crystalline thermoplast which is produced by polycondensation of terephthalic acid and ethylene glycol.
According to the European dangerous goods regulations RID and ADR, samples of PET design types of packagings for dangerous goods must be pre-stored with the original filling good for six months at 23°C, before the design type tests can be carried out. For packagings made of polyethylene (PE) tests to prove the stress cracking resistance by using laboratory methods are possible to reduce time and costs. Therefore, standard liquids, simulating the different types of damaging effects on PE are defined in RID and ADR. However, there is no information and research available about the damaging mechanisms on PET in comparison to PE, especially regarding to stress cracking resistance and test methods.
The aim of this work is to compare the stress cracking resistance of PE and PET with the Full Notch Creep Test (FNCT), which was developed by chemical industry and is described in the standards EN ISO 16101 and EN 15507. It was investigated whether testing specimens made of PE and PET with a full coplanar notch around the middle of the specimens show weakening after the impact of a tensile force in a wetting solution (Lutensol® FSA 10) at 50°C in a test device on the basis of the FNCT.
The test results confirmed the suitability of the method for eight PE grades. Unfortunately, this method couldn’t be used for PET because the specimens broke during notching. In addition the molding of the sheets and the following temper process for twelve hours are very time-consuming, and the specimens broke during notching due to the high brittleness of PET.
Another possibility to provide evidence of stress cracking resistance of PE packagings is laid down in BAM’s Dangerous Goods Rule BAM-GGR 015. This test was carried out with PE and PET bottles to compare both materials. Therefore 1l test bottles were filled with a 5% wetting solution and mounted with a clamping tool for 28 days at 40°C. Tensile test specimens were cut out afterwards from the middle of the bottles in the deformed areas. Tensile strength and breaking elongation of PE specimens were determined in comparison to the PET specimens. The tensile properties of the PET specimens couldn’t be determined due to the strength and the stiffness of the material.
In conclusion the only way to provide information about the stress cracking resistance of PET was to perform stacking tests. 1l bottles made of PE and PET were filled with a 5% wetting solution and stored with a stacking load for 28 days at 40°C according to EN ISO 16495. Design types of PE and PET both passed the stacking tests.
Comparison of the corrosion resistance to dangerous goods of austenitic CrNiMo and duplex steels
(2014)
The “BAM-List - Requirements for Tanks for the Transport of Dangerous Goods” is the basis in Germany for substance-related prototype approvals for tank Containers in Germany. Compatibility evaluations of selected metallic materials and polymeric materials under the influence of approximately 7200 dangerous goods have been published in the BAM-List since 1989. The austenitic CrNi- and CrNiMo-steels - UNS S30403, UNS S31600, UNSS31603 and UNS S31635 - are the materials mostly used worldwide for transport tanks. The duplex Steel UNS S31803 has been put on the BAMList due to the great interest of tank producers and transport Companies. Using UNS S31803 instead of 316L, the weight of the tanks can be reduced, and the list of transportable goods can be extended. The objective of these investigations was to compare the corrosion resistance of duplex Steel UNS S31803 and austenitic Steel UNS S31603. Therefore, test specimens of both steels were exposed to selected corrosive substances, such as formic acid, acetic acid, phosphoric acid, sulfuric acid, nitrating acid, monochloroacetic acid and trichloroacetone at 55 °C (30 °C, 70 °C). The test results have shown that the duplex Steel UNSS31803 is a good alternative to austenitic CrNiMo-steel UNS S31603 for tanks carrying corrosive dangerous goods.
Comparison of the Corrosion Resistance to Dangerous Goods of Austenitic CrNiMo and Duplex Steels
(2014)
For the characterization and the comparison of polyethylene grades used for the manufacture of packaging and intermediate bulk container, the following parameters are required: melt flow rate (MFR), density (D), low-temperature notched impact strength, full notch creep test (FNCT) and increase of MFR by molecular degradation (resistance to oxidative degradation). The relationship between these material parameters determined on the basis of specimens prepared from compression-moulded sheets of polyethylene grades and the test behaviour of packaging has been investigated in several tests. The environmental stress crack resistance determined by FNCT represents the impacts from the stacking tests performed with standard liquid wetting solution (without pre-storage) and with normal butyl-acetate-saturated wetting solution (pre-storage with normal butyl acetate). Resistance to molecular degradation by the determination of MFR increase is related to the impacts in drop tests and stacking tests performed after pre-storage for 21 days with standard liquid 55% nitric acid at 40°C. The low-temperature impact strength is directly comparable with the impacts in drop tests at -18°C performed without pre-storage and after pre-storage with 55% nitric acid. A partly good relationship was found between the test results and the material parameters. Conditioning the design types with 55% nitric acid for 21 days causes an increase in the marginal drop heights of the design types in drop tests at -18°C when compared with design types without pre-storage. Post-cross-linking of the grades increases stiffness because of the acidic influence.
Materials compatibility is a major concern whenever the fuel composition is changed in a fuel system. Therefore 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), N8R (acrylonitrile-butadiene rubber) and PUR (polyester urethane rubber) were exposed to E1 0, diese I fuel with 5% biodiesel, non-aged and 2 year aged 810 (heating oil with 10% biodiesel), and for comparison to pure diese! fuel, standard heating oil and Super plus without bioethanol at 20 °C, 40 oc and 70 oc for 84 days. Mass, tensile strength and breaking elongation of the test specimens were determined before and after the exposure. 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 to 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.
The sealing materials FKM, EPDM, N8R, FMVQ, CSM and PA were evaluated on the basis of this threshold as resistant in E1 0 at 20 oc and 40 °C. FKM, FVMQ and PA were resistant at 40 oc , and none of the materials were resistant at 70 °C. FKM and FVMQ absorbed much less 810 and swelled less. CR, CSM, EPDM, IIR, N8R and VMQ were not resistant to 810 at all at 20 oc, 40 oc and 70 oc as the decrease in the tensile properties was significantly over 50%. FVMQ and PA could be evaluated as resistant in non-aged and two year aged 810 at 20 oc and 40 oc, whereas FKM was resistant up to 70 °C. FKM, PA and PUR were evaluated as resistant in standard heating oil and pure diese! fuel at temperatures up to 40°C, only FKM was resistant up to 70°C. FVMQ, FKM, N8R, VMQ, CR and IIR can be evaluated as resistant in premium grade fuel Super plus without ethanol at 20 oc. FKM, FVMQ, VMQ and IIR were still resistant at 40 °C. FKM and FVMQ were evaluated as resistant with restrictions at 70 °C.
ln summary, it can be therefore stated that the chemical resistance of the fluoropolymers FKM and FVMQ in fuels and biofuels is the best one.
The objective of this research was to determine the resistance of frequently used sealing materials such as FKM, FVMQ, VMQ, EPDM, CR, CSM, IIR, PA, NBR and PUR in fuels and heating oil with and without admixtures of biogenic sources such as E10, diesel fuel with 5 % biodiesel, non-aged and 2 year aged B10 (heating oil with 10 % biodiesel), pure diesel, standard heating oil and premium grade fuel Super plus 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.
Zusammenfassend wird aufgrund der Ergebnisse der durchgeführten Untersuchungen die Aussage getroffen, dass die Fluorpolymere FKM und FVMQ die beständigsten Dichtungswerkstoffe in Biokraftstoffen und Heizöl B10 im Temperaturbereich bis 70 °C sind. In E10 und E85 kann keiner der Dichtungswerkstoffe bei 70 °C als beständig bewertet werden. Diese Erkenntnisse können vielen Wirtschaftszweigen ein Innovationspotential bieten und ihre Wettbewerbsfähigkeit steigern.
In der Bundesrepublik Deutschland werden über 400 Mio.t Gefahrgüter jährlich in Tankfahrzeugen, Aufsetztanks, Batteriefahrzeugen, Eisenbahnkesselwagen und Tankcontainern befördert, davon etwa 150 Millionen Tonnen im Straßengüterverkehr. Zu den Hauptschadensursachen zählt die Korrosion, wobei die gleichmäßige und ungleichmäßige Flächenkorrosion die Korrosionsart ist, die beim Chemikalientransport in Tanks am häufigsten auftritt. Viele Schäden durch Lochkorrosion entstehen beim Transport von chloridhaltigen Medien bei Anwesenheit von Feuchtigkeit.
Die BAM-Liste - Anforderungen an Tanks für die Beförderung gefährlicher Güter - ist Grundlage für die stoffbezogenen Baumusterzulassungen für Tankcontainer und ortsbewegliche Tanks zur Beförderung gefährlicher Güter durch die BAM seit der Herausgabe der 1. Auflage 1989. In die BAM-Liste wurden vorrangig solche gefährlichen Güter aufgenommen, die potenziell in Tanks befördert werden können. Die Beständigkeitsbewertungen gebräuchlicher metallischer Tankwerkstoffe und polymerer Dichtungs-, Beschichtungs- und Auskleidungswerkstoffe werden auch bei der Zulassung von Kesselwagen und Tankfahrzeugen als Erkenntnisquelle verwendet. Diese Daten sind aber unter sorgfältiger Überprüfung der Übertragbarkeit auch für andere praktische Anwendungen und unter Berücksichtigung der jeweiligen Praxisbedingungen auch als Ratgeber für Verpackungen, IBC, Lagerbehälter, Rohrleitungen usw. aus metallischen Werkstoffen anwendbar.
In den internationalen Gefahrgutverordnungen ADR, RID und IMDG-Code wird nach einer vorgegebenen Prüffrist eine innere Besichtigung der Tanks gefordert. Bei Tankcontainern beträgt diese Prüffrist im ADR/RID, Kap. 6.8 , fünf Jahre (bei der Beförderung von ortsbeweglichen Tanks nach ADR/RID, Kap. 6.7, und nach dem IMDG-Code 2½ Jahre) und bei Tankfahrzeugen sechs Jahre. Im RID wird für Eisenbahnkesselwagen eine Prüffrist von acht Jahren für die Innenbesichtigung vorgeschrieben. Für die Dauer der Prüfintervalle muss die Werkstoffbeständigkeit der Tankwerkstoffe gewährleistet sein.
Die BAM-Liste - Anforderungen an Tanks für die Beförderung gefährlicher Güter – mit den Beständigkeitsbewertungen metallischer und polymerer Werkstoffe ist Grundlage für die stoffbezogenen Baumusterzulassungen für Tankcontainer und ortsbewegliche Tanks zur Beförderung gefährlicher Güter durch die BAM seit der Herausgabe der 1. Auflage 1989. Diese Beständigkeitsbewertungen werden nicht nur bundesweit, sondern weltweit als Erkenntnisquelle genutzt. Für die Zulassung von Kesselwagen und Tankfahrzeugen werden diese Daten auch herangezogen. Die Werkstoffbeständigkeitsdaten und der damit verbundene Informationsservice der BAM haben mit Sicherheit dazu beigetragen, Leckagen von Tanks aufgrund des Einsatzes von Tanks/Kesselwagen aus einem gegenüber dem Füllgut unbeständigem Tankwerkstoff oder Dichtungswerkstoff zu vermeiden.
In der DIN 6601 - Beständigkeit der Werkstoffe von Behältern/Tanks aus Stahl gegenüber Flüssigkeiten (Positiv-Flüssigkeitsliste) ist die Beständigkeit unlegierter Stähle, austenitischer CrNi- und CrNiMo-Stähle gegenüber den reinen Ottokraftstoffen bewertet. Mit der verstärkten Verwendung bioethanol- und biodieselhaltiger Kraftstoffe und Heizöl stellt sich auch die Frage nach der Beständigkeit der handelsüblichen Tank- und Behälterwerkstoffe sowie der Dichtungswerkstoffe unter dem Einfluss dieser Medien.
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-Biodiesel-Blends, das für eine Vorauswahl der Werkstoffe und zum Nachweis der Beständigkeit im Hinblick auf die bauaufsichtlichen Zulassungsverfahren geeignet ist. Ein Schwerpunkt wird bei den metallenen Werkstoffen auf der Erprobung von Messmethoden liegen, mit denen sich in kurzer Versuchszeit ein Korrosionsangriff detektieren lässt.
Beständigkeitsbewertungen von Werkstoffen für den Transport von Gefahrgütern durch die BAM-Liste.
(2005)
Beständigkeitsbewertungen von Werkstoffen für den Transport von Gefahrgütern durch die BAM-Liste
(2005)
BAM, IKS Dresden und ThyssenKrupp VDM haben ein umfangreiches Versuchsprogramm mit geschweißten Werkstoffprüfblechen durchgeführt, um neue Erkenntnisse über das Korrosionsverhalten der Superaustenite und der Nickelbasislegierung zu gewinnen und um diese Bewertungen im Abschnitt 5 der BAM-Liste zu berücksichtigen. Das Versuchsprogramm umfasste Korrosionsbeständigkeitsbewertungen der drei höherlegierten Werkstoffe in Stoffen aus 12 Gruppen von korrosiven Gefahrgütern, wie z. B. anorganische Halogenide, organische Säurehalogenide, Halogencarbonsäuren, Chlorsilane, Chlorate, Perchlorate, Chlorite, Hypochlorite, Hydrogensulfate und Nitriersäuren.
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 %.
Die ökonomische Bewertung der immissionsbedingten Materialschäden der Sachgütergruppen Freileitungsmaste, Brücken der Bundesautobahnen, Eisenbahnbrücken und -fahrleitungsmaste, fernmeldetechnische Einrichtungen der Deutschen Bundespost, Industrieanlagen, Wohngebäude und Denkmäler basiert auf sogenannten „Stock-at-risk“-Informationen, Dosis-Wirkungs-Funktionen der der Atmosphäre ausgesetzten Werkstoffe und auf in der Praxis vorliegenden Erfahrungswerten über Zeitintervalle der Erneuerung der Korrosionsschutzsysteme und Bauteile. In jenen Fällen, in denen der immissionsbedingte Anteil am Gesamtschaden noch nicht eindeutig nachgewiesen werden konnte, werden die Forschungslücken aufgezeigt bzw. Modellrechnungen durchgeführt.
Rohrleitungssysteme sind aufgrund ihrer Funktion und Ausdehnung für den Betrieb, die Verfügbarkeit und die Sicherheit von Industrieanlagen von besonderer Bedeutung. Die bisher in definierten Intervallen durchgeführten, wiederkehrenden Prüfungen zur Sicherstellung leckagefreier Rohrleitungen sind kostenintensiv und mit einem erhöhten Aufwand verbunden.
Mit dem interdisziplinären Forschungsprojekt AGIFAMOR (Ageing Infrastructures – Akustisches Monitoring von Rohrleitungen) arbeitet die BAM an der Entwicklung und Erprobung einer örtlich und zeitlich kontinuierlichen Zustandsüberwachung von Rohrleitungen basierend auf einem faseroptischen akustischen Messsystem, welches einen vergleichsweise geringen Installationsaufwand der Sensoren erfordert. Mit diesem Verfahren sollen vor allem betriebsbedingte Schädigungen infolge von Korrosion sowie daraus entstehende Pittings oder Risse erkannt und damit Leckagen verhindert werden.
Im Rahmen einer Machbarkeitsstudie zum Teilaspekt „Detektion von Risswachstum“ wurde ein 2,5 m langes, definiert vorgekerbtes Stahlrohr mit der faseroptischen Sensorik (FOS) ausgestattet und quasistatisch unter 4-Punkt-Biegung belastet. Mit fortschreitender Belastung wächst, ausgehend vom vorhandenen Außenumfangskerb, ein Riss im Stahlrohr bis zum Erreichen der Leckage – in der Praxis ein gefährliches Schadensszenario.
Parallel zur FOS erfolgten Messungen mit Schallemissionssensoren, Beschleunigungssensoren und Potentialsonden, deren Ergebnisse die Interpretation der FOS-Messergebnisse unterstützen sollen.
Zum Vergleich der Polyethylenformstoffe für eine Bauart von Gefahrgutverpackungen und IBC wurden die Materialkennwerte: Schmelze-Massefließrate MFR, Dichte D, Kerbschlag-zähigkeit acN bei -30 °C, Spannungsrissbeständigkeit (bestimmt mit dem Full Notch Creep Test) und Beständigkeit gegen oxidativen Abbau Ox (bestimmt durch den prozentualen Anstieg des MFR in Salpetersäure) in der DIN EN 15507 – Verpackung – Verpackungen zur Beförderung gefährlicher Güter – Vergleichende Werkstoffprüfung von Polyethylensorten ausgewählt.
Das Ziel der Untersuchungen war die Auswahl eines Kennwertes für die Bestimmung des mechanischen Leistungsniveaus von Polyethylenformstoffen, da unter Druck Verpackungen beulen oder knicken. Zur Auswahl standen drei Prüfverfahren:
a) Bestimmung der Biegesteifigkeit S nach DIN 53 350 (Prinzip von Ohlsen).
b) Bestimmung der Biegefestigkeit σfM und Biegedehnung ɛfM nach DIN EN ISO 178
c) Bestimmung der Druckkraft Fmax und Verformung dL bei Fmax nach DIN EN ISO 604.
Die Prüfmethode zur Bestimmung der Biegesteifigkeit nach DIN 53 350 eignet sich zum Vergleich des mechanischen Leistungsniveaus der Formstoffe. Zur Verbesserung der Reproduzierbarkeit der Ergebnisse sollte der Skalierungsbereich der Prüfapparatur erweitert wer-den, um genauere Messergebnisse zu erzielen.
Der Dreipunktbiegeversuch nach DIN EN ISO 178 eignet sich bei verformungsfähigen Kunststoffen, wie dem Polyethylen, zur Bestimmung der Biegefestigkeit σfM. Dieser Ver-such besitzt den Nachteil, dass am Ort des maximalen Biegemoments in der Randschicht, wo auch die maximale Biegespannung erzeugt wird, zusätzlich der Biegestempel angreift.
Die Messergebnisse haben gezeigt, dass die Druckprüfung nach DIN EN ISO 604 sich sehr gut zur Bewertung des mechanischen Verhaltens der Polyethylenformstoffe unter Druckbelastung (Stapeldruckprüfung der Verpackungen) eignet.
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.
Schäden an Rohrleitungen können zu hohen Umweltbelastungen und wirtschaftlichen Schäden führen. Um die dauerhafte Verfügbarkeit der Infrastruktur zu gewährleisten, wird im Rahmen des Projekts AGIFAMOR an der Bundesanstalt für Materialforschung und -prüfung (BAM) erprobt, inwiefern das Verfahren der verteilten akustischen faseroptischen Sensorik (Distributed acoustic sensing – DAS) zur kontinuierlichen Überwachung von Rohrleitungen eingesetzt werden kann. Neben der DAS werden erprobte Verfahren der zerstörungsfreien Prüfung wie Schallemissionsanalyse (SEA) und Beschleunigungssensoren eingesetzt. An dieser Stelle soll detailliert auf die Hauptschadensursachen an Rohrleitungen, den Versuchsstand zur mechanischen Belastung von Rohren sowie die Möglichkeiten zu Untersuchungen im Realmaßstab eingegangen werden.
In der Prozessindustrie werden häufig gefährliche Stoffe eingesetzt, so dass auch kleinste Leckagen der medienführenden Anlagenteile zu Gefährdungen der Arbeitnehmer sowie zur Belastung der Umwelt führen können. Für die Gewährleistung einer dauerhaften Verfügbarkeit der Infrastruktur ist die frühzeitige Erkennung und Ortung von potentiell gefährlichen Veränderungen an den Wandungen von Rohrleitungen und Behältern (in Form von Rissen, Pittings und Ablagerungen) erforderlich. Am Beispiel von Rohrleitungen, sollen im Rahmen des Projekts AGIFAMOR an der Bundesanstalt für Materialforschung und -prüfung (BAM), im Sinne einer Machbarkeitsstudie die Verfahren der verteilten akustischen und faseroptischen Sensorik zur kontinuierlichen Überwachung und Detektion potentiell gefährlicher Veränderungen in Industrieanlagen erprobt und qualifiziert werden. Dabei sollen die Applikation der optischen Sensorfasern hinsichtlich der Signalübertragung auf den Sensor optimiert und die Erkennung der für dieses Anwendungsgebiet relevanten Schallsignaturen entwickelt werden. Mithilfe eines solchen Messsystems können mit geringem Aufwand ausgedehnte Strukturen, auch unter erschwerten Bedingungen (z.B. hohe Temperatur, Einfluss von Chemikalien) kontinuierlich überwacht werden.
Pipelines and industrial piping systems are particularly relevant regarding technical safety, availability and maintenance. Large flow rates of hazardous substances imply that even smallest leakages can lead to high environmental impacts. Therefore, and to ensure the availability of infrastructure, an early detection and localization of potentially hazardous degradations to the walls (e.g. cracks, pittings, sedimentation, etc.) of the containments is necessary. However, in many cases it is not feasible to equip pipelines with a large number of point sensors at reasonable expense.
The principle of distributed fibre optic sensing relies on one single optical fibre, which simultaneously acts as a spatially continuous sensor as well as the signal transducer. Therefore, extensive structures can be provided with this type of sensor with comparatively low efforts.
As a consequence, monitoring oil and gas pipelines using distributed fibre optic sensors is on the upswing. Besides the established methods to measure temperature and strain, distributed acoustic sensing (DAS) has lately received considerable attention as a means to detect and localize third party threats to pipelines (approach of vehicles, digging, mechanical manipulation).
The so far not utilized potential of DAS as a means for continuous condition monitoring of pipes by detecting and localizing acoustic signals that point to certain damage scenarios, is currently under investigation in an interdisciplinary research project at BAM (AGIFAMOR, Ageing Infrastructures – Fibre Optic Monitoring of Pipes).
In order to qualify distributed acoustic fibre optic sensors for this application area, we especially focus on detecting and identifying the relevant acoustic emissions of interesting degradations as well as on the optimal way of application of the optical fibres to the specimen to achieve an optimal signal transmission of acoustic signals.