TY - RPRT A1 - Frost, K. A1 - Lüth, Peter A1 - Schmidt, Martin A1 - Simon, K. A1 - Uhlig, St. T1 - Evaluation of the interlaboratory test 2015-2016 on the method DIN EN 15188:2007 "Determination of the spontaneous ignition behaviour of dust accumulations" N2 - For the classification, safe handling and use of the chemicals, special standardized testing procedures have been developed and are used worldwide. Safety experts must be able to fully rely on the precise execution of the respective laboratory tests and assessments. In this context, interlaboratory tests are a crucial element of a laboratory's quality system. Participation in interlaboratory tests is explicitly recommended by the standard ISO/IEC 17025. The present document reports the results of the interlaboratory test 2015-2016, which was performed on the test method DIN EN 15188:2007 “Determination of the spontaneous ignition behaviour of dust accumulations”. It was organized by BAM in the frame of the co-operation project CEQAT-DGHS Centre for Quality Assurance for Testing of Dangerous Goods and Hazardous Substances. The test method DIN EN 15188:2007 is applied to characterize the self-ignition behaviour of combustible dusts. The experimental basis for describing the self-ignition behaviour of a given dust is the determination of the self-ignition temperatures (TSI) of differently-sized volumes of the dust sample by isoperibolic hot storage experiments (storage at constant oven temperatures) in commercially available ovens. The results measured this way reflect the dependence of the self-ignition temperatures on the volume of a dust accumulation. The interlaboratory test 2015-2016 on the method DIN EN 15188:2007 is the latest in a systematic stepwise built up series of method validation interlaboratory tests and internal laboratory investigations. The aim of this interlaboratory test was to determine measurement uncertainties of the modified method DIN EN 15188 for different substances, covering a sufficiently wide range of self-ignition behaviours in the scope of the DIN EN 15188 of the four basket test to extrapolate to storage volumes up to 1000 m³ and the single basket test for a basket volume of 1000 cm³. The precision of the four basket test and the single basket of the modified method DIN EN 15188 can be assessed as acceptable for the four sample materials investigated in the current interlaboratory test 2015-2016. It was possible to derive a functional equation for the measurement uncertainty U depending on the storage volume V. The measurement uncertainty cannot be ignored and must be considered, if TSI results should be used in practice. KW - Gefahrgut KW - Gefahrstoff KW - Ringversuch KW - Prüfmethode KW - Validierung KW - Qualitätssicherung KW - Messunsicherheit KW - Dangerous goods KW - Hazardous substances KW - Round robin test KW - Interlaboratory comparison KW - Test method KW - Validation KW - Measurement uncertainty PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-387343 SN - 978-3-9818270-0-2 SP - 1 EP - 106 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38734 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Antoni, S. A1 - Clemens, J. A1 - Kunath, K. A1 - Rabe, J. A1 - Simon, K. A1 - Uhlig, S. A1 - Wehrstedt, Klaus-Dieter T1 - Evaluation of the 3rd round robin on solid oxidizer test (UN O.1) with calcium peroxide, sodium nitrate, sodium perborate monohydrate N2 - The classification of solid oxidizers according to the regulations on the transport of dangerous goods (based on the UN Recommendations/Model Regulations and accepted by all international organisations for the transport of dangerous goods as ADR, IMO, IATA) and in future also according to the GHS (Globally Harmonized System of Classification and Labelling of Chemicals) is performed on the basis of the results of the UN test O.1 (UN test O.1 ―Test for oxidizing solids‖ described in chapter 34.4.1 in the Recommendations on the Transport of Dangerous Goods – Manual of Tests and Criteria, see [1]). This test was introduced into the UN Manual of Tests and Criteria in 1995 as a replacement for a similar test from 1986. Even if the UN O.1 test as described in the current 5th revised edition of UN Manual of Tests and Criteria gives some improvements compared to the old test, which had had many deficiencies, there are still some problems left with this test in terms of e.g. repeatability or reproducibility of test results, how to handle compacted or multilayer formulations like tablets, toxicity and partly significantly varying particle size distribution within defined fractions of 150 μm to 300 μm of the reference oxidizer potassium bromate (KBrO3). For this reason the IGUS EOS working group installed an ad-hoc working group in 2002 assigned with the task to propose solutions for the existing problems. The appropriateness of such proposed solutions has to be proved by the method of interlaboratory (round robin) tests before they are presented for the adoption to the UN Committee of Experts on the TDG and on the GHS with a proposal of a completely revised test procedure. KW - Round robin KW - Solid oxidizer test KW - United Nations KW - IGUS KW - EOS KW - Calcium peroxide KW - Sodium nitrate KW - Sodium perborate monohydrate PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-232246 SN - 978-3-9813853-7-3 IS - Final Report, 2009 - 2011 SP - 1 EP - 192 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-23224 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Antoni, S. A1 - Kunath, K. A1 - Lüth, Peter A1 - Simon, K. A1 - Uhlig, S. T1 - Evaluation of the interlaboratory test on the method UN O.2 / EC A.21 'Test for oxidizing liquids' 2009 - 2010 N2 - For the classification of chemicals, special standardized test procedures have been developed and are used world-wide. Safe handling and use of these chemicals depend on the correct classification which therefore must be based on the precise and correct execution of the tests and their evaluation. In this context interlaboratory tests (round robin tests, interlaboratory comparisons / intercomparisons) are a crucial element of a laboratory's quality system. Participation in interlaboratory tests is explicitly recommended by the standard ISO/IEC 17025. The present document reports on the results of the interlaboratory test 2009/2010 on the test methods UN O.2 “Test for oxidizing liquids” [1] / EC A.21 “Oxidizing Properties (Liquids)” [2] which was organized by the Center for Quality Assurance for Testing of Dangerous Goods and Hazardous Substances. The test methods UN O.2 and EC A.21 are applied to characterize the oxidizing properties of liquid chemical substances or mixtures. To differentiate between chemicals with hazardous / dangerous oxidizing properties and chemicals which are not classified as hazardous / dangerous, the substance’s oxidizing properties are compared to those of a standard reference substance. Since the methods (UN O.2 / EC A.21) were developed and came into force in the early nineties a systematic review concerning the practical application of the test method has not been carried out. KW - Oxidiser KW - Oxidierend KW - Gefahrgut KW - Dangerous goods KW - UN O.2 KW - Prüfmethode KW - Test method PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-250904 SN - 978-3-9814634-0-8 SP - 1 EP - 95 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin ET - Final report AN - OPUS4-25090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Antoni, S. A1 - Kunath, K. A1 - Lüth, Peter A1 - Schlage, R. A1 - Simon, K. A1 - Uhlig, S. A1 - Wildner, W. A1 - Zimmermann, C. T1 - Evaluation of the interlaboratory test on the method UN test O.1 'Test for oxidizing solids' with sodium perborate monohydrate 2005 / 06 N2 - The classification of solid oxidizers according to the GHS (Globally Harmonized System of Classifica-tion and Labelling of Chemicals) and according to regulations on the transport of dangerous goods (based on the UN Recommendations/Model Regulations and implemented in all carrier domains as transport by road, railway, sea, air) is performed on the basis of the results of the UN test O.1 (―Test for oxidizing solids‖ described in chapter 34.4.1 in the Recommendations on the Transport of Danger-ous Goods, Manual of Tests and Criteria, Fifth revised edition, United Nations, New York and Geneva, 2009). This test was introduced into the UN Test Manual in 1995 as a replacement for a similar test from 1986. Even though the O.1 test is much better than the previous one there are still many prob-lems with this test. For this reason the IGUS-EOS working group (international group of experts on the explosion risks of unstable substances – working group: energetic and oxidizing substances) installed an ad-hoc working group in 2002 assigned with the task of proposing solutions for the existing prob-lems. The adequacy of such proposals has to be proven preferably by interlaboratory comparison (interlaboratory test) before they are presented to the UN Sub Committee for adoption into the UN Test Manual. The present report is the evaluation of an interlaboratory test which was designed by the Ad-hoc working group in order to find out whether the current method of comparing combustion times of test mixtures with those of reference mixtures is suitable in principle and whether some approaches for improvement of the method can be identified. KW - Oxidiser KW - Oxidierend KW - Gefahrgut KW - Dangerous goods KW - UN O.1 KW - Prüfmethode KW - Test method PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-250919 UR - http://www.bam.de/de/service/publikationen/publikationen_medien/un_test_for_oxidizing_solids_final_report_on_interlab_test.pdf SN - 978-3-9814281-2-4 SP - 1 EP - 65 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin ET - Final report AN - OPUS4-25091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Schmidt, Alexandra A1 - Bresch, Harald A1 - Kämpf, K. A1 - Bachmann, V. A1 - Peters, T. A1 - Kuhlbusch, T. T1 - Development of a specific OECD Test Guideline on Particle Size and Particle Size Distribution of Nanomaterials N2 - In this research project, a new OECD Test Guideline (TG) for the determination of “Particle Size and Particle Size Distributions of Nanomaterials” was developed as the existing OECD TG 110 is considered to be outdated in terms of applicable size range (not covering sizes <200 nm) and methods. By its scope with an applicable size range from 1 to 1000 nm the new Test Guideline (TG PSD) covers the whole nanoscale. The TG PSD is applicable for particulate and fibrous nanomaterials. The prescribed, pairwise measurement of fibre diameter and length in the TG PSD allows for the first time to differen-tiate fibres with regard to their size-dependent hazard properties. Measurement instructions for each included method were validated within two separated interlaboratory comparisons, as a distinction between near spherical particles and fibres when applying the methods has to be made. Besides information on content and structure of the TG PSD, this final report outlines essential steps, considerations and organisational aspects during the development of the TG. Insights into the selec-tion, preparation and prevalidation of test materials used in the interlaboratory comparison are given. Finally, main results of the interlaboratory comparisons and their impacts on the TG PSD are pre-sented. N2 - Im Rahmen des Forschungsprojekts wurde eine neue OECD-Prüfrichtlinie (TG) für die Bestimmung von Partikelgrößen und Partikelgrößenverteilungen von Nanomaterialien entwickelt, da die existie-rende OECD TG 110 zur Bestimmung von Partikelgrößen in Bezug auf den anwendbaren Größenbe-reich und die gegebenen Methoden veraltet ist bzw. den Nanometerbereich < 200 nm nicht abdeckt. Mit ihrem Anwendungsbereich von 1 bis 1000 nm deckt die neue Prüfrichtlinie (TG PSD) die gesamte Nanoskala ab. Die TG PSD ist für partikel- und faserförmige Nanomaterialien anwendbar. Durch die, in der TG PSD vorgeschriebene, paarweise Messung von Faserdurchmesser und -länge ermöglicht diese TG zum ersten Mal Fasern hinsichtlich ihrer größenabhängigen Gefahrstoffeigenschaften zu unter-scheiden. Die Messanweisungen aller enthaltenen Methoden wurden im Rahmen von zwei getrennten Ringversuchen validiert, da bei der Anwendung der Methoden eine Unterscheidung zwischen Parti-keln und Fasern gemacht werden muss. Neben Angaben zum Inhalt und Struktur der TG PSD, befasst sich der vorliegende Abschlussbericht mit den wesentlichen Schritten, Überlegungen und organisatorischen Aspekten bei der Entwicklung der Prüfrichtlinie. Darüber hinaus werden Einblicke in die Auswahl, Vorbereitung und Prävalidierung der im Ringversuch verwendeten Testmaterialien gegeben. Schließlich werden die wichtigsten Ergeb-nisse aus den Ringversuchen und ihre Auswirkungen auf die TG PSD vorgestellt. KW - Nano KW - OECD KW - Particle size distribution KW - Testguideline KW - Nanoparticle PY - 2021 VL - 2021 SP - 1 EP - 47 PB - German Environment Agency CY - Dessau AN - OPUS4-54021 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Piquemal, François A1 - Hoffmann, Johannes A1 - Gautier, Brice A1 - Hertwig, Andreas A1 - Frabricius, Norbert T1 - Publishable Summary for 20IND12 Elena Electrical nanoscale metrology in industry N2 - Consumer electronics, innovative quantum technologies, and Internet of Things applications all rely on semiconductors, where reliable characterisation of electrical properties at the nanoscale is essential for European innovation and competitiveness. The measurement of these properties allows the evaluation of critical parameters used to define the performance of electronic materials and components. Currently, Conductive Atomic Force Microscopes and Scanning Microwave Microscopes enable nanoscale electrical characterisation, but they are costly, complicated and, in many cases where they are used, unreliable as measurements are not traceable. The aim of the project was to make such measurements traceable for the first time, with stated uncertainties, and affordable by developing and testing cost effective instrumentation and the first “out of lab” reference standards from DC to GHz and by elaborating robust calibration methods and good practice guides using simplified uncertainty budgets. All the objectives were achieved. The project has successfully improved the user-friendly uncertainty quantification for the electrical measurements at the nanoscale in the industrial environment. The design of calibration standards has been improved and new standards for DC resistance / current as well as HF impedance have been introduced and quantified. Good practice guides for the calibration and uncertainty quantification have been written and will be available to the users’ community. New ways of determining the properties of standard samples like ellipsometry have been evaluated. The interaction with stakeholders and industry collaborators was very important for the consortium and several case studies were carried out with industry-relevant samples. All data, procedures, and example uncertainty data from the project are included into the standardisation process and two IEC standards projects have been started during this project. These standards will be used as one important dissemination ways for the results of the project. KW - Electrical Properties KW - Nanometrology KW - Scanning Probe Microscopy KW - Optical Surface Analysis PY - 2024 SP - 1 EP - 9 AN - OPUS4-61812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Hahn, Oliver A1 - Nehring, G. A1 - Freisitzer, R. A1 - Rabin, Ira T1 - A study on early european inks from St. Paul in lavanttal N2 - Typology of Inks Archives and museums around the world contain a vast number of manuscripts that were written in different inks: carbon inks, plant inks, iron-gall inks and mixed inks. Yet most archaeometric studies of manuscripts focus on the palette of pigments found in illuminated manuscripts whereas identification of the inks is still largely based on cultural-historical studies and visual inspections. One of the reasons of this disproportion in the studies can be explained by the properties of Raman spectroscopy, the technique of choice for identification of pigments. In contrast, this technique is only partially viable when dealing with organic colourants. Brown and Clark discuss these difficulties and the uncertainties of identification of iron-gall inks by Raman spectroscopy in their pioneering work on early medieval Anglo-Saxon manuscripts (K. Brown and R. Clark 2004). To facilitate instrumental analysis of inks, we have developed a protocol that starts with the identification of the inks type (Rabin et al. 2012) which doesn’t require complicated instrumentation and can be carried out by paleographers and codicologists. Three typological ink classes The black writing materials used in manuscript production in Antiquity und Middle Ages can be sorted in three typologically different ink classes: soot, plant and iron-gall. Soot ink is a fine dispersion of carbon pigments in a water soluble binding agent; plant-based ink consists of a solution of the tannins extracted from gallnuts or tree bark; iron-gall ink, is produced by mixing a soluble compound of iron (II) with gallic or tannic acid extracted from gallnuts or tree bark. Therefore, iron-gall ink presents a boundary case between solution and dispersion ink, in which a water-soluble preliminary stage oxidizes and evolves into a black, insoluble precipitate similar to the carbon pigments when the writing is exposed to air (Krekel 1999). The additional category of mixed inks, i.e. inks produced by addition of various metals to the soot inks or intentional mixing of iron-gall and soot - based inks started attracting scholarly attention only recently because their significance was established only a short while ago (Brun et al. 2016, Colini 2018, Nehring et al. 2021). We suggest that plant and mixed inks build a bridge from the carbon ink of Antiquity to the properly formulated iron-gall ink that became a standard black ink from the late Middle Ages to the 19th century when it gave way to modern inks. KW - Early european inks KW - Typology of Inks KW - Raman spectroscopy KW - Illuminated manuscripts KW - Archaeometric studies KW - Dispersion of carbon pigments PY - 2021 VL - 2021 SP - 56 EP - 75 PB - Gazette du livre médiéval CY - Paris AN - OPUS4-53844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Kannengießer, Thomas T1 - List of questions relating to the revision of ISO 3690 regarding the acceptance of the carrier gas hot extraction method N2 - Is it reasonable to restrict ISO 3690 any longer to the determination of the weld metal hydrogen content of ferritic steel? In what respect is the determination of the content of the diffusible and of the total hydrogen content, respectively, (still) merely a research task (supermartensite, duplex materials, austenite, magnesium, aluminium), or is there actually a demand in industry and is there already a first cause for monitoring in view of damage prevention, respectively? Is there a need, arising from the development of materials and filler materials and from their intended applications, for more extensive standards dealing with hydrogen analyses for these materials? Which parts of ISO 3690 could also be applied to any other metallic material/filler material, if necessary, and where would a complete alteration be required, respectively? KW - ISO 3690 KW - List of questions KW - Carrier gas KW - Extraction method PY - 2004 SP - 1 EP - 11 PB - IIW CY - USA AN - OPUS4-39260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Meggyes, Tamás A1 - Debreczeni, Ákos A1 - Reddy, Krishna R. A1 - Karri, Madhusudhana R. A1 - Riddler, Gordon P. A1 - Roehl, Karl Ernst A1 - Czurda, Kurt A1 - Sarsby, Robert W. A1 - Simon, Franz-Georg A1 - Biermann, Vera T1 - Sustainable environmental protection N2 - Permeable reactive barriers (PRBs) offer an alternative as opposed to more cost-intensive active methods for groundwater remediation, e.g. pump-and-treat. Long-term performance of PRBs, however, is crucial for the technology’s success. The paper summarises the results of long-term column experiments with elemental iron (Fe0) and hydroxyapatite (HAP) as reactive materials for the removal of uranium from groundwater. Good removal results have been achieved using elemental iron with possible reaction paths being reductive precipitation and adsorption on to corrosion products of Fe0. T3 - BAM Forschungsberichtreihe - 280 PY - 2007 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-1710 SN - 978-3-9811655-2-4 SN - 0938-5533 VL - 280 SP - 1 EP - 54 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Klingelhöffer, Hellmuth A1 - Ledworuski, Siegmar A1 - Brookes, Stephan-Peter A1 - May, Thomas T1 - Computer controlled tensile testing according to EN 10002-1 Results of a comparison test programm to validate a proposal for an amendment of the standard N2 - Tensile testing according to EN 10002-1 is one of the basic mechanical tests to characterise the mechanical properties of metallic materials. This testing procedure has been regularly under development for many decades in order to modify and amend it and to bring it up to an up to date standard. Today tensile testing for quality control in metals manufacturing industry is routinely performed automatically with computer controlled testing machines. Due to economical needs of industry proposals were made by a European Standard Committee to amend the standard EN 10002-1. A European research project with the acronym TENSTAND was started to validate the proposed modifications of the tensile testing standard. The work package 4 of the project was to validate the machine control characteristics. A comparison test program was started with ten partners, 4 test piece geometries and 3 test parameters for 6 materials, partly with upper and lower yield strength and partly with 0.2 % proof strength to compare experimental results according to the proposal to modify the standard EN 10002-1. Initially testing in the strain control mode was introduced as well as switching of the control mode to crosshead control 1 and switching of the testing speed at appropriate points during the test. The comparison test was evaluated statistically and scientifically. The following conclusions were derived from the comparison test and summarised as recommendations to the standard committees. The scatter of the material properties were not significantly reduced by introducing the amended testing procedure. Few of the reasons for the continuously observed scattercan be identified as follows: The material properties are observed to be widely dependent on the testing speed. As a consequence the range for the allowed testing speed must be reduced. The closed loop control was not optimised sufficiently in some tests, the use of complicated testing machine software led to misinterpretation of software commands, individual testing equipment and implementation of the tensile testing procedure led also to scatter of the material properties which lay in a range of few percent. This is blurred by the inhomogeneity of the material. T3 - BAM Forschungsberichtreihe - 268 PY - 2005 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-1835 SN - 978-3-86509-318-3 SN - 0938-5533 VL - 268 SP - 1 EP - 44 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-183 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -