TY - RPRT A1 - Koch, Matthias A1 - Liebich, Almuth A1 - Win, Tin A1 - Nehls, Irene T1 - Certified Reference Materials for the determination of mineral oil hydrocarbons in water, soil and waste N2 - The international research project HYCREF, funded by the European Commission in the 5 th Framework programme, aimed to develop methods to prepare homogenous and stable water-, soiland waste reference materials contaminated with mineral oil hydrocarbons and to test certify the mineral oil content by gas chromatographic methods. As mineral oil products are important sources for environmental contaminations a high need exists for certified reference materials for their determination using the new gas chromatographic methods (soil: ISO/FDIS 16703, waste: ENpr 14039, water: ISO 9377-2). The experimental conditions and results for preparation and characterisation of a total of nine reference materials (3 water-, 3 soil- and 3 waste materials) are described and discussed. Target values for the reference materials were defined at the beginning of the project in order to have clear quality criteria, which could be compared with the achieved results at the end of the project. These target specifications were related to the maximum uncertainty from test certification exercises (< 5 % for soil/waste and < 10 % for water), the maximum inhomogeneity between bottles (< 3 %) and minimum requirements for stability (> 5 years for soil/waste and > 2 years for water). The feasibility studies showed that solid materials (soil, waste) could be prepared sufficiently homogenous and stable. The test certified values of the 6 solid materials comprise a wide range of mineral oil content from about 200-9000 mg/kg with expanded uncertainties between 5.7-13.1 % using a coverage factor k (k = 2). The development of new water reference materials –the so-called “spiking pills” for an offshore- and a land-based discharge water represents one of the most innovative aspects of the project. The spiking pill technology facilitates the application and storage and improves the material stability compared with aqueous materials. Additional to the preparation and test certification of the reference materials investigations on the analytical method for the determination of mineral oil hydrocarbons were performed. The results obtained in relation to the optimisation of analytical method (extraction procedure, sample pretreatment, clean-up and measurement) were provided to the respective working group of ISO/TC 190, ISO/TC 147 and CEN/TC 292 and were incorporated into the ongoing standardisation procedures. The new version of ISO/FDIS 16703 (July 2004) includes the improvements based on HYCREF results, for example the increase of the solvent/sample ratio, the removal of acetone from the organic extracts and the use of column technique instead of batch technique for clean-up. T3 - BAM Forschungsberichtreihe - 272 PY - 2005 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-1795 SN - 978-3-86509-363-9 SN - 0938-5533 VL - 272 SP - 1 EP - 92 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-179 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 U6 - http://nbn-resolving.de/urn/resolver.pl?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 - TY - RPRT A1 - Beck, Uwe A1 - Fritz, Thomas A1 - Gamer, Nadja A1 - Wirth, Thomas T1 - VAMAS - Versailles Project on Advanced Materials and Standards N2 - Glühentladung optischer Ausstrahlungsspektroskopie (GDOES) wurde ursprünglich für die elementare Analyse von Größenmaterialien entwickelt. Mehrere Gruppen führten diese Methode zur Analyse von Anstrichen, Laienstapeln und dünnen Filmen durch. In den frühen Neunzigern wurde eine ISO-TC 201-Arbeitsgruppe gegründet, um Normen für alle Formen der Glühentladungsspektroskopie (GDS) zu entwickeln und die Fähigkeiten der Oberflächenchemikalien-Analyse zu beurteilen, insbesondere für die Tiefe von gestuften Systemen. Die Quantifizierung von Tiefenprofilen, d.h. die Umwandlung von Intensitäts-Zeit- Profilen in Konzentrierungs-Tiefen-Profile ist für dc-mode entwickelt worden. 1997 wurde ein VAMAS TWA 2 Vorschlag für ein Referenzanstrich für GD-OES Tiefe gemacht. Entsprechend dem VAMAS Beurteilungsverfahren wurde dieser Vorschlag 1998 mit einigen geringfügigen Änderungen genehmigt. T3 - BAM Forschungsberichtreihe - 242 PY - 2001 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-2083 SN - 978-3-89701-713-X SN - 0938-5533 VL - 242 SP - 1 EP - 64 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Konersmann, Rainer A1 - Kühl, Christiane A1 - Ludwig, Jörg T1 - On the risks of transporting liquid and gaseous fuels in pipelines N2 - Because they are laid underground and because their job is to connect widely distant places, pipelines have some particular technical safety features. Chemical industry installations have fixed and instantly recognisable sites. Pipeline routes must be adapted to the constraints of infrastructure and topography, and environmental protection must be taken into account, as well as the possibility that the pipe system may be damaged by external influences. Even minor leakages can have considerable effects on watercourses and the soil, and in many cases, people are also injured. Numerous incidents abroad have proved this. In the recent past, even Germany has not been spared from sudden damage to pipelines. However, not much notice was taken of these incidents, as the resulting damage was minor and there were no fatalities. With hindsight, when seeking the causes of the damage, it is often the case that the rupture of a pipeline is associated with certain recurring features. The scene of the damage is often located near traffic infrastructure. Pipelines must of necessity cross roads and railways or are laid in parallel to such lines of communication. As a result of vibrations caused by traffic, this proximity can lead to ruptures. Road or rail accidents can lead to stresses which pipelines are unable to withstand. But a pipeline failure can have many other causes which cannot be predicted with any certainty and which even show regional particularities. In the interests of safe transport and land planning, it would therefore be worthwhile to be able to evaluate at least the possible consequences in terms of damage that might result from a pipeline rupture. There are hardly any publications on pipeline accidents, at least in German speaking countries; most of what is available is in the form of reports by the fire services. However, these are not sufficient to provide an overview of the situation. For this reason, the Federal Institute for Materials Research and Testing has evaluated many international reports of investigations and publications and summarised what they have to say about the risks inherent in pipeline failures, particularly the damage that results. This report is the outcome of this work. T3 - BAM Forschungsberichtreihe - 289 PY - 2009 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-1624 SN - 978-3-9813346-3-0 SN - 0938-5533 VL - 289 SP - 1 EP - 65 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-162 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 U6 - http://nbn-resolving.de/urn/resolver.pl?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 U6 - http://nbn-resolving.de/urn/resolver.pl?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 - 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 U6 - http://nbn-resolving.de/urn/resolver.pl?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 - Kuchenbecker, Petra A1 - Lindemann, Franziska T1 - Final report proficiency test LS BAM-5.5-2021: Measurement of the particle size distribution of ceramic powders by laser diffraction in accordance with ISO 13320 N2 - This is the final report on the proficiency test (PT) „Measurement of the particle size distribution of ceramic powders by laser diffraction”. The PT was organized by the Federal Institute for Materials Research and Testing (BAM), division 5.5 “Advanced technical ceramics”. The measurements took place from 12/2021 to 03/2022. The aim of the interlaboratory comparison was the proficiency assessment of the participating laboratories. Management and realization of PT were performed in accordance with DIN EN ISO/IEC 17043:2010. The basis of the harmonized measuring procedure and the instructions for the interlaboratory comparison was the standard ISO 13320:2020. The statistical analysis was performed in accordance with DIN ISO 13528:2020 by use of the software PROLab Plus (QuoData GmbH, Dresden, Germany). A group of 44 laboratories from 17 countries participated in the PT. Laser diffraction analyzers produced by 7 different manufacturers were used. The three test materials were commercial products. Overall, the measured characteristic values of the particle distributions (d10, d50 and d90) were in the size range between 0.5 and 25 μm. The final report contains all individual results in an anonymous way. KW - Proficiency test KW - Particle size KW - Laser light scattering PY - 2022 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-548640 SP - 1 EP - 33 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-54864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Hodoroaba, Vasile-Dan A1 - Fontanges, R. A1 - Delvallée, A. A1 - Deumer, J. A1 - Salzmann, C. A1 - Crouzier, L. A1 - Gollwitzer, C. A1 - Klein, T. A1 - Koops, R. A1 - Sebaihi, N. A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Artous, S. A1 - Taché, O. A1 - Feltin, N. T1 - Report on full algorithm sequences for nanoparticle detection and size measurement as developed on both a physical basis and by machine learning N2 - he main objective of the nPSize project is to improve the measurement capabilities for nanoparticle size based on both measurement methods traceable to SI units and new reference materials. Two basic approaches have been used in order to develop measurement procedures resulting in traceable results of the nanoparticle size distribution: physical modelling for the methods used in the project (TSEM, SEM, AFM and SAXS) and machine learning. Physical modelling: In this part, the physical models associated with different shape measurements for the techniques TSEM, SEM, AFM and SAXS have been collected and further developed with the aim to simulate the resulting signal as measured by the individual methods. Uncertainties and traceability associated with each model were investigated and evaluated. In the following, the progress on these physical models is reported for each individual method. Machine Learning modelling: The aim of this part is to use machine learning to enable automatic measurement of nanoparticle shape from expert a-priori information only. No physical model will be used as a-priori information in this task. The accuracy and traceability of the size results obtained by each technique will be analyzed and compared with the physical modelling. A machine learning database will then be used to create automatic detection algorithms. KW - Nanoparticles KW - Particle size distribution KW - SEM KW - TSEM KW - TEM KW - SAXS KW - AFM PY - 2022 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-546531 SP - 1 EP - 20 PB - Zenodo CY - Geneva AN - OPUS4-54653 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 -