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In vielen Bereichen der Industrie und im verarbeitenden Gewerbe werden eine Vielzahl brennbarer Stäube gezielt oder ungewollt produziert, verarbeitet, transportiert oder anderweitig verwendet. Je nach Material- und Staubeigenschaften weisen diese eine teilweise sehr hohe Reaktivität auf. Es gilt weiterhin als allgemein bekannt, dass die Partikelgröße einen entscheidenden Einfluss auf das Brand- und Explosionsverhalten von Stäuben ausübt. Mit Abnahme der Partikelgröße nehmen die gefährlichen Auswirkungen im Falle einer Explosion und die Zündempfindlichkeit der Stäube zu. Aufgrund der veränderten Eigenschaften im Nanometerbereich hat die Produktion solcher Stäube mit sehr geringen Primärpartikelgrößen in den letzten Jahren zugenommen. Diese Entwicklung wird sich in den folgenden Jahren fortsetzen. Über das Brand- und Explosionsverhalten solcher Stäube war bis vor wenigen Jahren jedoch kaum bis wenig bekannt.
In vielen Bereichen der Industrie und im verarbeitenden Gewerbe werden eine Vielzahl brennbarer Stäube gezielt oder ungewollt produziert, verarbeitet, transportiert oder anderweitig verwendet. Je nach Material- und Staubeigenschaften weisen diese eine teilweise sehr hohe Reaktivität auf. Es gilt weiterhin als allgemein bekannt, dass die Partikelgröße einen entscheidenden Einfluss auf das Brand- und Explosionsverhalten von Stäuben ausübt. Mit Abnahme der Partikelgröße nehmen die gefährlichen Auswirkungen im Falle einer Explosion und die Zündempfindlichkeit der Stäube zu. Aufgrund der veränderten Eigenschaften im Nanometerbereich hat die Produktion solcher Stäube mit sehr geringen Primärpartikelgrößen in den letzten Jahren zugenommen. Diese Entwicklung wird sich in den folgenden Jahren fortsetzen. Über das Brand- und Explosionsverhalten solcher Stäube war bis vor wenigen Jahren jedoch kaum bis wenig bekannt.
Aufgrund von Erfahrungen mit Stäuben mit Partikelgrößen im Mikrometerbereich ist bekannt, dass Stoffe mit abnehmender Partikelgröße kritischer einzustufen sind, da z.B. maximaler Explosionsdruck (pmax), maximaler zeitlicher Druckanstieg (dp/dtmax) und Zündempfindlichkeit durch die Zunahme der reaktiven Oberfläche des Staubes zunehmen. Eine Übersicht des Verlaufes der Explosionsauswirkungen metallischer Stäube vom Mikrometerbereich bis in den Nanometerbereich konnte bislang nur vereinzelt durch wenige Ergebnisse gegeben werden.
Dieser Beitrag präsentiert einen detaillierten Überblick über das Explosionsverhalten von Metallstäuben vom Mikrometer- bis in den Nanometerbereich. Hierfür wurden verschiedene Metallstäube untersucht und deren Explosionsauswirkungen in Abhängigkeit der mittleren Primärteilchengröße entweder durch BET-Messungen, Partikelgrößenverteilung oder REM-Mikroskopie bestimmt. Um den Verlauf des Explosionsverhaltens für diese Metalle darzustellen, wurde einerseits eine umfangreiche Literaturrecherche durchgeführt. Darüber hinaus wurden die im Rahmen deutscher und französischer Forschungsprogramme durchgeführten experimentellen Untersuchungen genutzt, um insbesondere die Datenlage für nanoskalig hergestellte Stäube zu verbessern. Auch bei Metallstäuben im Allgemeinen führt eine Verringerung der Teilchengröße zu einem kritischeren Verhalten der Stäube. Es scheint jedoch, dass diese Aussage nur bis zu einem kritischen Durchmesser gilt, unterhalb dessen die Auswirkungen einer Explosion (pmax, dp/dtmax) für alle betrachteten Stäube wieder abnehmen. Diese kritische Größe kann durch theoretische Überlegungen zur Art der thermischen Übertragung in der Flamme erklärt werden. Der Einfluss der Schlüsselparameter wird in diesem Beitrag ebenfalls diskutiert, um die Mechanismen besser zu verstehen und das Verständnis letztendlich auch auf andere pulverförmige Materialien auszudehnen.
Protection from explosion events requires the determination of key safety parameters like lower explosion limit. maximum Explosion over-pressure. and maximum rate of pressure rise. These Parameters are routinely obtained through standard tests performed typically either in a 20 L -sphere or a 1 m3-container. But several aspects are worth a closer investigation. Firstly, the test apparatus must be able to disperse a fairly uniform dust cloud. However. previous investigations showed that actually the current dispersion System can be improved. Secondly, the influence of humidity on the explosivity is not considered in current standards. lt is just stated that the relative humidity should be checked and noted down.
though some provisions exist in American standards. Thirdly. the ignition delay time is sometimes modified to study the impact of the dust cloud turbulence on flame propagation but is often misunderstood.
Maybe these aspects have not been thoroughly considered for micron powders. However. in the case of nanopowders. the importance of these influencing factors was shown in order to duly evaluate explosion parameters. Experimental evidences confirm these aspects and alternative solutions will be presented.
Die Produktion von Materialien mit Abmessungen im Nanometerbereich hat in den letzten Jahren immer weiter zugenommen. Um die Sicherheit beim Umgang mit diesen Produkten zu gewährleisten, muss das Gefahrenpotenzial solcher innovativen Materialien bekannt sein. Während bereits in mehreren Studien die Auswirkungen von Explosionen (wie z.B. maximaler Explosionsdruck und maximaler zeitlicher Druckanstieg) von Stäuben mit Primärpartikeln im Nanometerbereich untersucht wurden, ist darüber hinaus bislang wenig über die Zündtemperaturen und die Flammenausbreitungsgeschwindigkeiten solcher Pulver bekannt.
Problematisch bei der Untersuchung der Flammengeschwindigkeiten von Staubexplosionen allgemein ist, dass die Stäube vor dem Entzünden dispergiert werden müssen. Auf diese Weise wird eine gute Verteilung der Partikel im entsprechenden Prüfvolumen sichergestellt. Dies führt jedoch dazu, dass zum Zündzeitpunkt in den Standardprüfapparaturen hohe Turbulenzbedingungen vorherrschen. Aus wissenschaftlicher Sicht wäre es jedoch wünschenswert, die laminare Flammenausbreitungsgeschwindigkeit bestimmen zu können.
Im Beitrag werden Ergebnisse von Versuchen mit verschiedenen metallischen Materialien und Partikelgrößenverteilungen vorgestellt.
Ziel dieser Versuche war es, die Turbulenzbedingungen zum Zündzeitpunkt durch einen speziellen Versuchsaufbau möglichst zu minimieren.
Die Flammenausbreitung wurde experimentell in einem vertikalen Rohr untersucht, das an einer Seite offen ist. Das Rohr wird auf einen metallischen Boden gestellt, der gleichzeitig die Staubprobe vorhält und die Luftzufuhr in das Rohr ermöglicht. Eine poröse Platte befindet sich innerhalb des metallischen Bodens, um die Turbulenzen im Luftstrom zu reduzieren. Die Zündquelle wird durch einen Hochspannungsfunken von zwei Elektroden bereitgestellt, die sich auf einem Drittel der Rohrlänge befinden. Die Staubkonzentration wird optisch (durch Lichtdämpfung) mit zwei Konzentrationssonden gemessen, die jeweils unter den Elektroden (unten) und über ihnen (oben) angeordnet sind. Die Flammenausbreitung wurde mit einer Hochgeschwindigkeitskamera aufgezeichnet.
Zur besseren Einordnung der Versuchsergebnisse wurden die untersuchten Proben eingehend charakterisiert und die Zündtemperaturen und unteren Explosionsgrenzen der untersuchten Staubproben bestimmt.
This work presents an overview about the explosion behaviour of metallic powders from micron to nanosize.
Aluminium, magnesium, titanium, iron and zinc were considered and their explosion safety parameters were analysed as a function of their mean primary particle size either determined by BET measurements, particle size distribution. To depict the course of explosion behaviour for these metals, extensive literature review has been performed and additional experimental tests were also performed. Generally, decreasing the particle size in a metallic powder leads to a higher explosion severity. It appears that this statement is true till a critical Diameter below which the explosion severity (pmax, dp/dtmax) decreases for all the considered powders. This critical size can be explained by theoretical considerations on the nature of thermal transfer in the flame, namely by analysing the Cassel model. Finally, semi-empirical models were also developed for aluminium to highlight the specific micrometre and nanometre behaviour and the influence of turbulence, particle burning time, Diameter and concentration. The influence of these key parameters needs to be further assessed in a future work in order to better understand the mechanisms involved and to extend the scope to other powdered materials.
In diesem Verbundvorhaben werden standardisierte Messverfahren für hybride Gemische erarbeitet, die der Bestimmung sicherheitstechnischer Kenngrößen des Explosionsschutzes dienen. Unter einem hybriden Gemisch wird dabei ein mehrphasiges System aus Brenngas oder brennbarem Dampf, sowie Luft und brennbarem Staub verstanden. Die Veröffentlichung der Ergebnisse erfolgt in einem Abschlussbericht und als DIN-Spezifikation (DIN SPEC). Diese DIN SPEC versetzt Prüfinstitute und Industrie in die Lage, Explosionsgefahren beim Betrieb technischer Anlagen mit hybriden Gemischen einzuschätzen und damit Prozesse sowohl sicherer als auch effizienter zu steuern. Dieses Projekt wird im Rahmen des WIPANOProgramms (Wissens- und Technologietransfer durch Patente und Normen) vom BMWi gefördert.
Quasi-static dispersion of dusts for the determination of lower explosion limits of hybrid mixtures
(2020)
Knowledge of explosion limiting concentration of explosible materials is necessary for the design of explosion protection measures. Currently employed methods of testing MEC of a dust cloud or LEL of a hybrid mixture are based on arbitrary assumptions and possess technical limitations that often lead to values of MEC/LEL, which are unrealistically low or poorly reproducible.
This contribution presents an improved method for experimental determination of MEC of a combustible dust cloud or LEL of a flammable gas or hybrid mixture. The new set-up operates under laminar conditions and allows a uniform suspension of dust particles in an open top acrylic glass tube. Dust concentration is measured with the help of infrared sensors installed a few centimeters above and below the ignition source.
In order to evaluate the dependence of MEC on flow front velocity, MEC of lycopodium was determined at four flow velocities. The results show that the flow field intensity does not significantly influence the MEC of lycopodium for the flow ranges tested in this work. Moreover, LEL of hybrid mixtures of lycopodium and methane was also tested at flow velocities of 4.7 cm/s, 5.8 cm/s, 7 cm/s and 11 cm/s and compared with the values obtained from other sources. The results suggest that the requirement of high energy pyrotechnical igniter may be relinquished, provided that a truly homogeneous suspension of dust particles could be achieved.
Moreover, the effect of relative amount of dust and gas, on the course of ignition and flame propagation in hybrid mixtures at their LEL, was studied by the help of high speed videos. For hybrid mixtures of carbonaceous dusts (like lycopodium) at their LEL, ignition occurs in the gas phase, however, flame propagation is only possible through a two-way interaction of dust and gas during the course of combustion.
The maximum explosion overpressure and the maximum rate of pressure rise, which characterize thedust explosion severity, are commonly measured in apparatuses and under specific conditions defined byinternational standards. However, those standards conditions, designed for micropowders, may not befully adapted to nanoparticles. Investigations were conducted on different nanopowders (nanocellulose,carbon black, aluminum) to illustrate their specific behaviors and highlight the potential inadequacyof the standards. The influence of the sample preparation was explored. Various testing procedureswere compared, focusing on the dust cloud turbulence and homogeneity. Dust dispersion experimentsevidenced the importance of the characterization of the dust cloud after dispersion, due to the frag-mentation of agglomerates, using metrics relevant with nanoparticles reactivity (e.g. surface diameterinstead of volume diameter). Moreover, the overdriving phenomenon (when the experimental resultsbecome dependent of the ignition energy), already identified for micropowders, can be exacerbated fornanoparticles due to their low minimum ignition energy and to the high energy used under standardconditions. It was evidenced that for highly sensitive nanopowders, pre-ignition phenomenon can occur.Finally, during severe explosions and due to a too long opening delay of the ‘fast acting valve’, the flamecan go back to the dust container.
Entwicklungen zu Bestimmungsverfahren für sicherheitstechnische Kenngrössen hybrider Gemische
(2020)
Zur Bestimmung sicherheitstechnischer Kenngrößen (STK) von hybriden Gemischen (Gemisch aus mindestens zwei brennbaren Phasen, wie z.B. Staub/Gas- oder Gas/Dampf-Gemisch) existieren bislang keine einheitlichen, genormten Prüfmethoden. Die Normen und Regelwerke zur Bestimmung der STK von einphasigen brennbaren Systemen (Staub, Gas, Dampf) unterscheiden sich teilweise erheblich. Beispielsweise sind in den jeweiligen Normen für Stäube, Gase und Dämpfe unterschiedliche Zündquellen und Zündenergien definiert. Des Weiteren unterscheiden sich die in den Normen definierten Prüfabläufe bei der Gemischherstellung. Bei der Entwicklung einer einheitlichen Norm für hybride Gemische muss der Einfluss dieser beiden Parameter ermittelt werden, um die Vergleichbarkeit mit den STK der einzelnen Komponenten Gas, Staub und Dampf gewährleisten zu können und bisherige Erkenntnisse zu hybriden Gemischen interpretieren und bewerten zu können.
For the determination of safety characteristics of gases, vapors and dusts different types of ignition sources are used in international standards and guidelines. Table 1 compares technical relevant ignition sources with their main features. The paper presents test results of a comparative calorimetric and visual study between four different types of ignition sources. The ignition procedures were analyzed visually with a high-speed camera and electric recordings. In addition to that, the influence of the electrode-orientation, -distance as well as ignition energy on the reproducibility of the exploding wire igniter was tested.
The exploding wire is already in use for standardized determination of safety characteristics of gases, first tests on the suitability of the exploding wire igniter for dust testing have been carried out by Scheid et al. Using the exploding wire, the ignition energy can be varied from 2 to 10 000 J (2 x 5 000 J) and thus it could be used for gases, vapors, dusts and hybrid mixtures. Moreover it can be used at high initial pressures and it is the only ignition source with an easily measurable ignition energy release. Furthermore, it does not introduce another chemical reaction into the system.
Finally, a proposal for a standard ignition source for explosion tests on hybrid mixtures is derived from the test results.
The explosion characteristics of anthracite coal dust with/without small amount of CH4 (1.14 vol %) were investigated by using a 20 L spherical explosion apparatus with an emphasis on the roles of oxygen mole fraction and inert gas. Two methods based on overpressure and combustion duration time were used to determine the minimum explosion concentration (MEC) or the lower explosion limit (LEL) of the pure anthracite coal dust and the hybrid coal-methane mixtures, respectively. The experiment results showed that increasing oxygen mole fraction increases the explosion risk of coal dust: with increasing oxygen mole fraction, the explosion pressure (Pex) and the rate of explosion pressure rise ((dp/dt)ex)) increase, while MEC decreases. The explosion risk of anthracite dust was found to be lower after replacing N2 with CO2, suggesting that CO2 has a better inhibition effect on explosion mainly due to its higher specific heat. However, the addition of 1.14% CH4 moderates the inhibition effect of CO2 and the promotion effect of O2 on anthracite dust explosion for some extent, increasing explosion severity and reducing the MEC of anthracite dust. For hybrid anthracite/CH4 mixture explosions, Barknecht’s curve was found to be more accurate and conservative than Chatelier’s line, but neither are sufficient from the safety considerations. The experimental results provide a certain help for the explosion prevention and suppression in carbonaceous dust industries.
The production of materials with dimensions in the nanometre range has continued to increase in recent years. In order to ensure safety when handling these products, the hazard potential of such innovative materials must be known. While several studies have already investigated the effects of explosions (such as maximum explosion pressure and maximum pressure rise) of powders with primary particles in the nanometre range, little is known about the ignition temperatures and flame velocities. Therefore, the minimum ignition temperature (MIT) of metallic nano powders (aluminium, iron, copper and zinc) was determined experimentally in a so called Godbert-Greenwald (GG) oven. Furthermore, the flame velocities were determined in a vertical tube. In order to better classify the test results, the tested samples were characterised in detail and the lower explosion limits of the tested dust samples were determined. Values for the burning velocity of aluminium nano powders are higher compared to values of micrometre powd
ers (from literature). While MIT of nanometre aluminium powders is within the range of micrometre samples, MIT of zinc and copper nano powders is lower than values reported in literature for respective micrometre samples.
The production of materials with dimensions in the nanometre range has continued to increase in recent years. In order to ensure safety when handling these products, the hazard potential of such innovative materials must be known. While several studies have already investigated the effects of explosions (such as maximum explosion pressure and maximum pressure rise) of powders with primary particles in the nanometre range, little is known about the ignition temperatures and flame velocities. Therefore, the minimum ignition temperature (MIT) of metallic nano powders (aluminium, iron, copper and zinc) was determined experimentally in a so called Godbert-Greenwald (GG) oven. Furthermore, the flame velocities were determined in a vertical tube. In order to better classify the test results, the tested samples were characterised in detail and the lower explosion limits of the tested dust samples were determined. Values for the burning velocity of aluminium nano powders are higher compared to values of micrometre powders (from literature). While MIT of nanometre aluminium powders is within the range of micrometre samples, MIT of zinc and copper nano powders is lower than values reported in literature for respective micrometre samples.
Influence of pre-ignition pressure rise on safety characteristics of dusts and hybrid mixtures
(2021)
For the determination of the safety characteristics of dusts it is necessary to disperse the dust in the oxidating atmosphere (usually air). In the standard procedures for dusts this is realized by a partially evacuated explosion vessel (20L-sphere) in which the dust gets injected from a dust chamber pressurized with air. Shortly after that injection (60 ms) the dust cloud gets ignited under turbulent conditions, that are otherwise seen as almost ambient with 20 ◦C and about 1 bar (abs). While there has been a lot of research about the influence of the ignition delay time and the level of turbulence in the recent years little attention was paid to the pre–ignition pressure rise and the allowed variations in the standards. In the following work we showed that the allowed ranges for the pressures in the different dust standards influence the safety characteristics of dust alone severely.
Even though hybrid mixtures are an emerging risk problem in an interconnected industry there is no standard for the determination of their safety characteristics. In this work it is shown that especially for the preparation of hybrid mixtures of flammable dust and gas the pressures after injection of the dust and the mixing procedure have a large influence on the composition of the tested mixtures and therefore on the safety characteristics.
Considering both effects, wrong concentration of gas and wrong initial pressure, the discrepancy of safety characteristics from different facilities will be too big to applicable. The methods to overcome these weaknesses are also presented.
For the determination of safety characteristics of gases, vapors and dusts different types of ignition sources are used in international standards and guidelines. The paper presents test results of a comparative calorimetric and visual study between four different types of ignition sources. The ignition procedures were analyzed visually with a high-speed camera and electric recordings. In addition to that, the influence of the electrode-orientation, -distance as well as ignition energy on the reproducibility of the exploding wire igniter was tested.
The exploding wire is already in use for standardized determination of safety characteristics of gases, first tests on the suitability of the exploding wire igniter for dust testing have been carried out but are not standardized yet. Using the exploding wire, the ignition energy can be varied from 2 J to 10 000 J (2 x 5000 J) and thus it could be used for gases, vapors, dusts and hybrid mixtures. Moreover it can be used at high initial pressures and it is the only ignition source with an easily measurable ignition energy release. Furthermore, it does not introduce another chemical reaction into the system.
Finally, a proposal for a standard ignition source for explosion tests on hybrid mixtures is derived from the test results.
The publicly available document encapsulates the first version of the Catalogue of Services of the future EC4Safenano Centre (CoS 2019).
The CoS 2019 is structured in 12 Service Categories and 27 Service Topics, for each of the 12 categories considered. This architecture configures a 12 x 27 matrix that allows ordering the potential EC4Safenano offer in 324 types of services/groups of services.
Each type of service/group of services is described, in a simple and friendly way, by means of a specific service sheet: the EC4Safenano - Service Data Sheet (EC4-SDS). These EC4-SDSs allow structuring and summarizing the information of each service, providing the customer with a concise view of characteristics of the service and also the contact details with the service provider.
The CoS 2019 deploys a map of services consisting of a set of 100 EC4-SDSs, covering 7 of the 12 Service Categories and 17 of the 27 Service Topics.
The harmonization of services is visualized as a future necessary step in EC4Safenano, in order to strengthen the offer and provide added value to customers with a growing offer of harmonized services in future versions of the CoS.
The information contained in this document is structured in 3 main sections, as follows:
• Catalogue structure. This section describes in short the main characteristics of the CoS 2019.
• Catalogue content. This section represents the core part of the document and encapsulates the set of 100 SDSs displaying the offer proposed by the CoS 2019.
• Online Catalogue. This section describes the resources implemented by EC4Safenano to facilitate the on-line consultation of the CoS 2019 by customers and other interested parties.
There are several standardized ignition sources in use for the determination of explosion characteristics of gases, vapors and dusts. In the standards the ignition source is stated, but they vary in stating other characteristics like burning duration, energy or burning volume. Since heat is not visible under normal circumstances a Schlieren-Technique was used to make the full heating volume and not just the flames visible.
While an earlier paper of the authors focused on the ignition energy and burning duration of four standardized ignition sources, this paper focuses on the initial igniting volume, the ratio between initial igniting volume and the test-vessel size and other phenomena that were observed with the Schlieren-Technique-.
The article summarizes a short review of the literature focused on safety in the field of alternative energy sources. With an increasing orientation towards sustainable and renewable energy sources, new technologies will come to the fore. These facts must be demonstrated in occupational health and safety. Several studies focused on alternative energy sources are mentioned and show the trends for the future. Especially in the area of hydrogen and battery technologies, systems should pay attention to acquisitions as a normal part of our lives.
Safety research is essential for the acceptance of cleaner, efficient, and sustainable future.
There is no applicable existing standard for the determination of safety characteristics for hybrid mixtures. While developing a new standard in a joint research project in Germany first results from parameter studies led to a standard procedure that can be adopted by laboratories that are already testing dusts in the so called 20L-sphere with as little additional effort as necessary. In fact, one of the main objectives of this research project was to keep modifications and adjustments from the generally accepted dust testing procedures as easy and minimal as possible so as to limit potential deviations from one laboratory to another.
In this first round robin test on hybrid mixtures ever, with methane as gas component and a specific corn starch as dust sample, the practicality of the whole procedure, the scattering of the results and the deviation between the testing apparatuses is investigated. This paper summarizes the experimental procedure adopted and objectives of the first round-robin phase involving three of the four original German companies, plus volunteering laboratories from Australia, Belgium, Czech Republic, France, Poland and P.R. China. The results will have an impact on the new standard and may lead to robust data for later simulation purposes.