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- 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide; DOPO (1)
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Eingeladener Vortrag
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Anlaß und Aufgabe der Untersuchungen — Versuchsausführung: Holzauswahl; Tränkung, Verwiegen; Lagerung der getränkten Maste; Probenentnahme; Bestimmung der Fluorid-Eindringtiefen; Bestimmung des Schutzsalz-Gehaltes und seiner Verteilung; Statistische Auswertungsverfahren — Aufnahme an Schutzsalz-Lösung — Fluorid-Eindringtiefe : Fichte; Kiefer — Mengen-Verteilung von Fluor und Chrom: Fichte; Kiefer — Folgerungen aus den Ergebnissen: Einfluß von Holzart und Holzeigenschaften; Bemerkungen zum Tränkerfolg; Gesichtspunkte für eine Gütekontrolle — Zusammenfassung — Schrifttum.
Federal Institute for Materials Research and Testing (BAM) is the responsible authority for the
assessment of mechanical and thermal safety as well as quality issues within the licensing procedure
for transport casks for radioactive materials. The assessment includes a brittle fracture analysis of all
relevant cask components.
For cask bodies where a steel bottom is welded to a steel shell, specimens for testing of sufficient
fracture resistance can normally not be extracted directly from the welding seam area of the cask.
Therefore, a methodology has to be developed to ensure compliance with the safety analysis
considerations and the approved design specification. This paper describes such a methodology
including brittle fracture analysis and de-termination of required material properties as well as aspects
of quality assurance during manufacturing.
We present a new high resolution X-ray imager based on a pnCCD detector and a polycapillary optics. The properties of the pnCCD like high quantum efficiency, high energy resolution and radiation hardness are maintained, while color corrected polycapillary lenses are used to direct the fluorescence photons from every spot on a sample to a corresponding pixel on the detector. The camera is sensitive to photons from 3 to 40 keV with still 30% quantum efficiency at 20 keV. The pnCCD is operated in split frame mode allowing a high frame rate of 400 Hz with an energy resolution of 152 eV for Mn Kα (5.9 keV) at 450 kcps. In single-photon counting mode (SPC), the time, energy and position of every fluorescence photon is recorded for every frame. A dedicated software enables the visualization of the elements distribution in real time without the need of post-processing the data. A description of the key components including detector, X-ray optics and camera is given. First experiments show the capability of the camera to perform fast full-field X-Ray Fluorescence (FF-XRF) for element analysis. The imaging performance with a magnifying optics (3×) has also been successfully tested.
Aufgabe der Untersuchung — Versuchsausführung — Ergebnisse von Eindringtiefen-Messungen: Radiale und axiale Tiefenverteilung des Fluorids; Von Fluorid durchsetzte Holzmassen; Über die Streuung der Eindringtiefe des Nachschutz-Fluorids — Ergebnisse quantitativer Fluor-Analysen: Mengenmäßige Fluorid-Verteilung nach ljähriger Versuchsdauer; Mengenmäßige Fluorid-Verteilung nach gjähriger Versuchsdauer; Erklärung von Besonderheiten der mengenmäßigen Fluorid-Verteilung; Veränderungen zwischen 1- und gjähriger Versuchsdauer und ihre Ursachen; Reichweite einer sicheren Wirksamkeit des Nachschutz-Fluorids nach 5 Jahren; Gesamtmengen an Nachschutz-Fluorid in den Masten — Zusammenfassung — Schrifttum.
The molecular dynamics of addition-type poly(tricyclononenes) with Si-substituted bulky side groups has been investigated by a combination of neutron time-of-flight and neutron backscattering spectroscopy methods on a time scale from 0.1 ps to ca. 3 ns. The investigated poly(tricyclononenes) PTCNSi1 and PTCNSi2g both bear a high microporosity which makes them promising candidates for active separation layers for gas separation membranes. At least for larger gas molecules it is assumed that the pathways for diffusion require an enlargement of pre-existing micropores in terms of an activated zone. A low temperature relaxation process was found for both polymers by the performed neutron scattering experiments. This process was assigned to the methyl group rotation. It was analysed in terms of a jump diffusion in a three-fold potential. The analysis of the dependence of the elastic incoherent structure factor on the scattering vector yields the number of methyl groups which might be immobilized. For PTCNSi1 (3 methyl groups in the monomeric unit) it was found that all methyl groups take part in the methyl group rotation whereas for PTCNSi2g (6 methyl groups in monomeric unit) a considerable number of methyl groups are blocked in their rotation. This immobilization of methyl groups is due to the sterically demanding arrangement of the methyl groups in PTCNSi2g. This conclusion is further supported by the result that the activation energy for the methyl group rotation is three times higher for PTCNSi2g than that of PTCNSi1.
Ein Impuls-Wirbelstromprüfsystem mit rechnergestützter Erfassung und Auswertung der Meßsignale
(1982)
In accordance with IAEA SSR-6 para 306 a management system shall be established and implemented to ensure compliance with the relevant provisions of the IAEA regulations. BAM has issued an update of the guideline: the BAM-GGR 011. The new revision describes necessary quality assurance measures for design, manufacture, testing, documentation, use, maintenance and inspection of packagings for package designs requiring competent authority approval for the transport of radioactive material.
The measures can be categorised as system-related and design-related. They are independently approved and monitored by the German competent authority BAM and its authorised expert (BAM/T). The qualification of the organisation applying for the design approval certificate is reviewed in the context of the design approval procedure. The quality assurance measures for manufacture consist of three main steps. Pre-assessment of manufacturing documents such as quality plans, specifications etc., Manufacturing inspections according the pre-assessed documents and inspection before commissioning including documentation review. Periodic inspections during operation as well as relevant specifications for use and maintenance ensure that the properties specified in the approval certificate are preserved over the package life time. Special provisions for the return on
experience regarding operational feedback for design, manufacture, use, maintenance and inspection are given. Special focus shall be given here to the rearranged and meanwhile established system of manufacturing inspections. This includes more transparent roles for a) the Producers authorised inspection 11282 representative, b) the independent inspection expert (S), acting on behalf of the manufacturer with acceptance of BAM, and c) BAM or its authorised expert (BAM/T). Additional attention shall be drawn to the management of deviations during manufacturing and provisions for maintenance and periodic inspections.
The concreting of prefabricated concrete structures can lead to insufficient bonding or even to remaining cavities. Honeycombs (aggregate clusters without cement) represent potential weakening of the structure and need to be detected non-destructively. In our study we tested the capability of ground penetrating radar (GPR)techniques for this purpose. We applied GPR in reflection mode and zero-offset profiling (ZOP) Transmission mode on a precast concrete twin wall with built-in honeycombs. GPR measurements were performed as twochannel measurement with ground coupled antennas with centre frequencies of 1.5 GHz and 2.6 GHz mounted to an automated scanner system.
Our findings show that ZOP transmission measurements are a more efficient method to detect voids in reinforced concrete structures compared to reflection mode measurements. This holds for both the effort needed for the measurement and the evaluation as well as the validity of the data. Honeycombs (basically representing voids) are usually characterized by strongly reduced amplitudes and earlier arrivals of the transmitted wave.
Compact pnCCD-based X-ray camera with high spatial and energy resolution: a color X-ray camera
(2011)
For many applications there is a requirement for nondestructive analytical investigation of the elemental distribution in a sample. With the improvement of X-ray optics and spectroscopic X-ray imagers, full field X-ray fluorescence (FF-XRF) methods are feasible. A new device for high-resolution X-ray imaging, an energy and spatial resolving X-ray camera, is presented. The basic idea behind this so-called 'color X-ray camera' (CXC) is to combine an energy dispersive array detector for X-rays, in this case a pnCCD, with polycapillary optics. Imaging is achieved using multiframe recording of the energy and the point of impact of single photons. The camera was tested using a laboratory 30 µm microfocus X-ray tube and synchrotron radiation from BESSY II at the BAMline facility. These experiments demonstrate the suitability of the camera for X-ray fluorescence analytics. The camera simultaneously records 69696 spectra with an energy resolution of 152 eV for manganese Kα with a spatial resolution of 50 µm over an imaging area of 12.7 × 12.7 mm². It is sensitive to photons in the energy region between 3 and 40 keV, limited by a 50 µm beryllium window, and the sensitive thickness of 450 µm of the chip. Online preview of the sample is possible as the software updates the sums of the counts for certain energy channel ranges during the measurement and displays 2-D false-color maps as well as spectra of selected regions. The complete data cube of 264 × 264 spectra is saved for further qualitative and quantitative processing.
A series of new flame retardants (FR) based on dibenzo[d,f][1,3,2]dioxaphosphepine 6-oxide (BPPO) incorporating acrylates and benzoquinone were developed previously. In this study, we examine the fire behavior of the new flame retardants in polyisocyanurate (PIR) foams. The foam characteristics, thermal decomposition, and fire behavior are investigated. The fire properties of the foams containing BPPO-based derivatives were found to depend on the chemical structure of the substituents. We also compare our results to state-of-the-art non-halogenated FR such as triphenylphosphate and chemically similar phosphinate, i.e. 9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide (DOPO), based derivatives to discuss the role of the phosphorus oxidation state.
Flexible polyurethane foams (FPUF) are easy to ignite and exhibit rapid flame spread. In this paper, the fire phenomena of two standard foam formulations containing tris (1,3-dichloro-2-propyl) phosphate (FR-2) and a halogen-freepoly (ethyl ethylene phosphate) (PNX), respectively, as flame retardants are compared. A multimethodological approach is proposed which combines standard fire tests as well as new investigatory approaches. The thermophysical properties of the foams were determined by thermogravimetric analysis (TG), reaction to small flames was studied by means of the limiting oxygen index (LOI) and UL 94 HBF test, and the burning behavior was investigated with the cone calorimeter. Further, temperature development in burning cone calorimeter samples was monitored using thermocouples, and rheological measurements were performed on pyrolyzed material, delivering insight
into the dripping behavior of the foams. This paper gives comprehensive insight into the fire phenomena of flame-retarded FPUFs that are driven by the two-step decomposition behavior of the foams. LOI and UL 94 HBF tests showed a reduced flammability and reduced tendency to drip for the flame-retarded foams. TG and cone calorimeter measurements revealed that the two-step decomposition behavior causes two stages during combustion, namely structural collapse and pool fire. The flame-retardant mode of action was identified to take place primarily during the foam collapse and be based mainly on flame inhibition. However, some condensed-phase action was been measured, leading to significantly increased melt viscosity and improved dripping behavior for foams containing PNX.
This work investigates the fire phenomena of rigid polyurethane foams (RPUFs) in detail. To elucidate structure-property relationships, systematically varied sets of materials were prepared covering polyurethane, polyisocyanurate-polyurethane and flame retarded polyurethane foams. Advanced cone calorimeter investigations provide insight into the fire behavior under forced flaming conditions. Thermocouples inside specimens give information about the temperature gradient during combustion. Furthermore, fire phenomena were characterized using cross sections of quenched samples and the scanning electron microscope. By using a Multi methodological approach and systematically varied sets of foam materials, new insights into the burning of RPUFs were won. For the flame retarded foams, the dominant flame retardant mode of action changed with density. PIR foams exhibited a cellular structure in the residue leading to the superior fire performance compared to polyurethane foams. The understanding of fire phenomena contributes to future development of tailored flame retardant strategies for RPUFs.
The impact of phosphorus-containing flame retardants (FR) on rigid polyisocyanurate (PIR) foams is studied by systematic variation of the chemical structure of the FR, including non-NCO-reactive and NCO-reactive dibenzo[d,f][1,3,2]dioxaphosphepine 6-oxide (BPPO)- and 9,10 dihydro-9-oxa-10 phosphaphenanthrene-10-oxide (DOPO)-containing compounds, among them a number of compounds not reported so far. These PIR foams are compared with PIR foams without FR and with standard FRs with respect to foam properties, thermal decomposition, and fire behavior. Although BPPO and DOPO differ by just one oxygen atom, the impact on the FR properties is very significant: when the FR is a filler or a dangling (dead) end in the PIR polymer network, DOPO is more effective than BPPO. When the FR is a subunit of a diol and it is fully incorporated in the PIR network, BPPO delivers superior results.
Rigid polyurethane foams (RPUFs) typically exhibit low thermal inertia, resulting in short ignition times and rapid flame spread. In this study, the fire phenomena of RPUFs were investigated using a multi-methodological approach to gain detailed insight into the fire behaviour of pentaneand water-blown polyurethane (PUR) as well as pentane-blown polyisocyanurate Polyurethane (PIR) foams with densities ranging from 30 to 100 kg/m3. Thermophysical properties were studied using thermogravimetry (TG); flammability and fire behaviour were investigated by means of the limiting oxygen index (LOI) and a cone calorimeter. Temperature development in burning cone calorimeter specimens was monitored with thermocouples inside the foam samples and visual investigation of quenched specimens’ cross sections gave insight into the morphological changes during burning. A comprehensive investigation is presented, illuminating the processes taking place during foam combustion. Cone calorimeter tests revealed that in-depth absorption of radiation is a significant factor in estimating the time to ignition. Cross sections examined with an electron scanning microscope (SEM) revealed a pyrolysis front with an intact foam structure underneath, and temperature measurement inside burning specimens indicated that, as foam density increased, their burning behaviour shifted towards that of solid materials. The superior fire performance of PIR foams was found to be based on the cellular structure, which is retained in the residue to some extent.
Flexible polyurethane foams with densities of 40 ± 2 kg m−3 were prepared by combining different ecofriendly fillers such as layered double hydroxides (LDH) and kraft lignin (a byproduct of the pulp and paper industry) with a phosphorous polyol (E560) in order to study their effect on the mechanical performance and fire behavior of the foams. Two series of foams were prepared, some containing lignin or LDH separately, and some with a combination of both: one of the series was prepared without E560 (0E foam series) and the other with 5 parts per hundred of E560 polyol (5E series). The use of fillers resulted in increased viscosity of the reactive mixture, requiring higher blowing agent content in order to hold the density of the foams constant. It was observed that urea phase segregation was favored in the series of 0E foams due to their lower viscosity than the 5E series. This had consequent effects on the resilience, compression force deflection and compression set of these foams. In terms of fire behavior it was observed that while the limiting oxygen index decreased, cone calorimeter results showed that the combination of lignin, LDH and E560 decreased the heat release of the foams. In addition, the combination of fillers and E560 contributed to increase the viscosity of the pyrolysis products, preventing the dripping of the molten polymer, which is a key factor in flame propagation towards adjacent objects in fire scenarios.
This work investigates the fire phenomena of rigid polyurethane foams (RPUF) in detail. To elucidate structure-property relationships systematically varied sets of foams were prepared. RPUF were synthesized with different densities using water and pentane as blowing agent. What is more, a flame retarded RPUF and rigid polyisocyanurate-polyurethane foams were examined. The comprehensive understanding of the processes taking place during combustion is the foundation of customized development of successful flame retardant approaches.
Advanced cone calorimeter investigations provide insight into the fire behavior under forced flaming conditions. Thermocouples in the inside of specimens give information about the temperature gradient and temperature of the pyrolysis zone during combustion. Furthermore, fire phenomena were characterized using SEM, LOI and thermal analysis. By using a multi-methodological approach and systematically varied sets of foam materials, new insights into the burning of RPUF were won. The detailed knowledge of fire phenomena is essential for future development of tailored flame retardant strategies for RPUF.
Polyurethane (PU) bilden eine der vielseitigsten Klassen der Polymerwerkstoffe. Kein anderer Kunststoff wird sowohl als Thermoplast, als Elastomer wie auch als Duroplast verarbeitet und eingesetzt. Entsprechend vielfältig sind auch die Anforderungen an den Flammschutz. Je nach Material und Anwendung müssen spezifische Brandnormen erfüllt werden. Der vorliegende Aufsatz gibt einen Überblick über die verfügbaren Ansätze, um durch geeignete Auswahl der Rohstoffe und der Flammschutzmittel diese verschiedensten Anforderungen an das Brandverhalten zu erfüllen.
Polyurethanes (PU) represent one of the most versatile classes of plastics. They are processed and used as thermoplastic, elastomer, and thermoset. The requirements regarding flammability are correspondingly versatile. Depending on the material and the field of application, specific fire tests have to be fulfilled. This paper describes the different concepts used to fulfil these requirements by choosing the right raw materials and flame retardants.
Rigid polyurethane foams (RPUF) are widely used in industry and daily life because of their outstanding mechanical and thermal insulating properties. While their convenient mechanical characteristics predestine these materials for shock absorption, their low thermal conductivity is responsible for their excellent thermal insulation properties. A principal characteristic affecting not only the use properties, but also the burning behaviour, is the density of RPUF.
In case of fire, cellular polymers like RPUF behave differently from bulk materials. The reason for their comparatively high ignitability is the high rate of temperature rise on the surface when exposed to heat, which is due to their cellular structure and characterised as low thermal inertia. The heat build-up on the surface results in a short time to ignition. Therefore foams are able to develop fire and large amounts of smoke within a short period of time. Even though their fire load is quite low because of their low density, their heat release rate is high. These burning properties are not only a consequence of the chemical consistence of such materials, but also a result of their morphology.
The aim of the work is to investigate the fire phenomena of RPUF. Characterised by simultaneous physical and chemical processes which interact, depend, and compete with each other, the combustion of RPUF is a highly complex occurrence. Therefore it is necessary to study all aspects in detail. The fire phenomena that were examined are gasification, liquefaction, charring and structural integrity as well as collapse. The melting of cellular polymers and dripping of pyrolysis products, together with the ability to form pool fires, are the main hazards in fires involving foams. Structural collapse via melting or decomposition, or the retention of the foam’s morphology through charring, are the main characteristics of their burning behaviour. Cellular structure is a further important factor influencing the materials’ response to fire, and deserves examination in greater depth. Since the cells in closed-cell foam are filled with the blowing agent used to produce the material, and this blowing agent can be inert (carbon dioxide) or highly flammable (pentane), this component also affects the burning properties and will be investigated. Examination of the influence of the macroscopic morphology, namely the cell size and thickness of cell walls, will contribute to the study.
In order to provide comprehensive insight into the processes taking place during combustion, and to elucidate structure-property relationships, a set of foams with systematically varied properties was prepared. RPUF was obtained using water and pentane as a blowing agent. Besides RPUF, a flame-retarded RPUF and rigid polyisocyanurate-polyurethane foam were examined, since these foams are known for their higher stability from a thermodanymic point of view. As a flame retardant active in the gas phase, triethylphosphate was used.
Using a multi-methodological approach, the complex interaction of fire phenomena was studied in detail. Cone calorimeter measurements provide insight into fire behaviour under forced-flaming conditions. They were carried out in an horizontal and a vertical orientation to account for the effects of melt flow and dripping. Sample-holders were equipped with glass windows to monitor the materials’ response to forced-flaming conditions with a video camera. Thermocouples were inserted into the specimens, giving information about the temperature gradient in the inside of the sample and the temperature of the pyrolysis zone during combustion. Changes in the morphology and thickness of the pyrolysis zone were examined using a hot-stage microscope, as well as SEM images of cross-sections of quenched foam specimens. The determination of the Oxygen Index and the use of thermogravimetry measurements rounded out the investigation.
This work investigates the fire phenomena of rigid polyurethane foams (RPUF) in detail. Rigid polyurethane foams (RPUF) are widely used in industry and daily life because of their outstanding mechanical and thermal insulating properties. In case of fire, cellular polymers like RPUF behave differently from bulk materials, the reason for this is their low thermal inertia. The aim of this study is to investigate the fire phenomena of RPUF in detail. Characterized by simultaneous physical and chemical processes which interact, depend, and compete with each other, the combustion of RPUF is a highly complex occurrence. Therefore it is necessary to study all aspects in detail. The fire phenomena that were examined are gasification, liquefaction, charring and structural integrity as well as collapse. The comprehensive understanding of the processes taking place during combustion is the foundation of customized development of successful flame retardant approaches. Advanced cone calorimeter investigations provide insight into the fire behavior under forced flaming conditions. Thermocouples in the inside of specimens give information about the temperature gradient and temperature of the pyrolysis zone during combustion. Changes in the morphology and thickness of the pyrolysis zone were examined using a hot-stage microscope, as well as SEM images of cross-sections of quenched foam specimens. Furthermore, fire phenomena were characterized using LOI and thermal analysis. By using a multimethodological approach and systematically varied sets of Polyurethane and Polyisocyanurate foams, new insights into the burning of RPUF were won. The detailed knowledge of fire phenomena is essential for future development of tailored flame retardant strategies for RPUF.
Rigid polyurethane foams (RPUFs) exhibit short times to ignition as well as rapid flame spread and are therefore considered to be hazardous materials. This paper focuses on the fire phenomena of RPUFs, which were investigated through a multimethodological approach. Water-blown polyurethane (PUR) foams without flame retardants (FRs) as well as waterblown PUR foams containing triethyl phosphate as a gas phase-active FR were examined. The aim of this study is to clarify the influence of the FR on the fire phenomena during combustion of the foams. Additionally, materials’ densitieswere varied to range from 30 to 100 kg/m3. Thermophysical properties were studied bymeans of thermogravimetry; fire behavior and flammability were investigated via cone calorimeter and limiting Oxygen index, respectively. During the cone calorimeter test, the temperature development inside the burning specimens was monitored with thermocouples, and cross sections of quenched specimens were examined visually, giving insight into the morphological changes during combustion.
The present paper delivers a comprehensive study, illuminating phenomena occurring during foam combustion and the influence of a FR active in the gas phase. The superior fire performance of flameretarded PUR foams was found to be based on flame inhibition, and on increased char yield leading to a more effective protective layer. It was proven that in-depth absorption of radiation is a significant factor for estimation of time to ignition. Cross sections investigated with the electron scanning microscope exhibited a pyrolysis front with an intact foam structure underneath. The measurement of temperature development inside burning specimens implied a shift of burning behavior towards that of non-cellular materials with rising foam density.