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The main objective was to assess homogeneity of two bimodal gold materials, namely nPsize1 and nPSize2, containing approximately 1:1 and 10:1 particle number-based ratio of ~30nm and ~60nm particles. Particle number-based concentration within the two size fractions was determined with spICP-MS using the particle frequency method of calibration.
A state-of-the-art (SOTA) review on characterisation of spent nuclear fuel (SNF) properties in terms of source term and inventory assessment (neutron, gamma-ray emission, decay heat, radionuclide inventory, elemental content) and in terms of out-of-core fuel performance (cladding performance and fuel integrity in view of the safety criteria for SNF interim storage, transport and canister packaging) using several numerical and experimental approaches and methodologies is presented. This SOTA report is a result of the spent fuel characterisation (SFC) work package as part of the European Joint Programme on Radioactive Waste Management (EURAD), which offers an overview of the status of knowledge in the field of SNF characterisation and assessment during the pre-disposal phase. The document aims to focus on the current safety-significant gaps and related challenges, providing a direct link to the goals of the mandated actors of EURAD. The report is expected to be used by all EURAD colleagues in their national programmes as a key resource for knowledge management programmes and to contribute to demonstrating and documenting the state-of-the-art.
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Africa. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2023. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
This study is part of a global project that covers various other countries (see www.qi-fokus.de).
For the safety of prestressed concrete structures, a test of prestressing steel products for hydrogen-induced stress corrosion cracking is mandatory. The current standardized test methods according to DIN EN ISO 15630-3 have proven deficiencies concerning the reproducibility of the results and thus make it difficult to assess the susceptibility clearly. The WIPANO research project funded by BMWK aimed to improve the test method regarding reproducibility and reliability of results. The project created constant and reproducible test conditions by modifying material, electrolyte, and process parameters. This allowed a clear differentiation between good and bad products. As part of the project, a round robin test was initiated to confirm the applicability and reproducibility of the new test method. The new test method was evaluated for its applicability to the prestressing steel product wire. A draft standard with a proposed conformity criterion for these products was submitted to the responsible ISO committee for approval. According to the current feedback from the committee, the draft standard will be included in the informative annex of the testing standard, which could pave the way for mirroring at European and national standardization levels.
The ground vibrations, which are generated by trains on different slab tracks, have been calculated by finite-element boundary-element models. The slab track is modelled in detail by the finite element method.
The infinite soil is modelled by the boundary element method as a homogeneous half-space. The track-soil system is coupled with a simple rigid mass model of the vehicle so that the vehicle-track interaction is completely included. Transfer functions are calculated in frequency domain without and with vehicle-track interaction, the compliance of the track and the mobilities of the soil at different distances from the track.
Finally, the ratios between the ground vibration amplitudes with and without mitigation measure are calculated to quantify the effectiveness of the mitigation measure.
Tracks with under sleeper pads have been investigated in a parameter study. The main parameter that influences the reduction of ground vibration is the stiffness of the under sleeper pad. The softest sleeper pad yields the best reduction of the ground vibration.
The influence of other parameters has been examined. The stiffness of the rail pads, the stiffness of the slab material, the stiffness of the sleeper material, and the distance of the sleepers. All these parameters show no or only a minor influence on the mitigation effect.
As the standard isolated track, a track with an under sleeper pad of a stiffness of kS = 5 107 N/m has been chosen, which can also be expressed as a stiffness per area of kS ’’ = 3.7 107 N/m3 = 0.037 N/mm3.
The resonance frequency for this pad stiffness is observed between 32 and 40 Hz. The reduction of the ground vibration is about vi,I /vi,U = 0.1 at 100 Hz.
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in North Macedonia. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
This study is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Croatia. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
This study is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in the United Kingdom. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
This study is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in New Zealand. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
This study is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in West Africa. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
This study is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Mexico. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
This study is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Peru. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
This study is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Singapore. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
This study is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Colombia. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
The study on Colombian CABs is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Spain. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
The study on Spanish CABs is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Brazil. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
The study on Brazilian CABs is part of a global project that covers various other countries (see www.qi-fokus.de).
One aim of the EMPIR nPSize project 17NRM04 was to develop and validate three classes of candidate reference (test) materials (RTMs), with i) well-defined non-spherical shape, ii) relatively high polydispersity index, and iii) accurate particle concentrations.
To fulfil the requirements of the project, 11 different types of materials were prepared. Following the initial assessment of the materials suitability, nPSize5_PT_UNITO, nPSize6_AC_UNITO and nPSize7_GN_CEA materials were found unsuitable for the project, due to various reasons. PT material was deemed unsuitable due to its predominantly agglomerated nature. AC material contained relatively high amount of impurities (other particle forms). GN material was found too heterogeneous in both the length and width for the purpose of the project. The remaining 8 candidate RTMs were assessed for their homogeneity and stability and used for successful delivery of the associated activities within the nPSize project.
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in the Netherlands. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
The study on Dutch CABs is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Latvia. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
The study on Latvian CABs is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Ireland. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
The study on Irish CABs is part of a global project that covers various other countries (see www.qi-fokus.de).
This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Italy. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends.
The study on Italian CABs is part of a global project that covers various other countries (see www.qi-fokus.de).
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.
In 2019 the Bundesanstalt für Materialforschung und –prüfung (BAM) conducted a benchmarking to compare the operations of European accreditation bodies and to identify best practices, with the aim of improving key processes in accreditation. Ten European accreditation bodies attended the comparison, four of which had already taken part in the pilot phase of the benchmarking project, which was conducted in 2017 by the German accreditation body Deutsche Akkreditierungsstelle GmbH (DAkkS) and BAM.
The study, designed to examine and compare the operation of accreditation bodies in Europe, used a management tool called Process Maturity Benchmarking Tool, which was especially elaborated and validated for this purpose in the pilot phase, in order to determine the values of indicators, thus enabling a comparison of the accreditation bodies despite different operational processes and organizational forms. The management tool is based on the analysis of selected processes with high relevance for the operation of accreditation bodies. The processes are derived from a process map designed for accreditation bodies in a universally applicable way. The indicators used to characterize the processes come from two sources: The first source relates to data already available from internal databases, reports, financial audits, and others. The second source is derived from the self-evaluation of process maturity performed by the accreditation bodies. The criteria for evaluating process maturities were designed by applying the criteria of the EFQM excellence model 2013 of the European Foundation for Quality Management (EFQM) to the processes identified in the process map.
The results of the analysis were presented to and discussed with representatives of the ten accreditation bodies at a Results-Workshop that took place at BAM on 21/22 January 2020.
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.
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.
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.
Gas adsorption is based on physical properties between gases and solid materials, enriching the surface with packed gas molecules with a higher density than in the bulk phase. For using this mechanism as a gas storage strategy, highly porous materials are necessary since large surfaces in small volumes can provide the storage system with a higher density than the gas phase. In the case of hydrogen gas, the interaction forces with solid surfaces are generally low at room temperature but can increase considerably at low operating temperatures. As a counterpart, the storage pressure is considerably lower than that necessary by traditional gas compression.
Amongst ultra-porous adsorbent materials for hydrogen cryoadsorption, metal-organic frameworks (MOFs) are a group of remarkable solids made from metallic nodes linked by organic molecules exhibiting a wide variety of composition, geometry, porous properties, and chemical functionality. The scientific community focused in the last years on enhancing both the specific area of materials and the interaction energy to extend the storage properties of cryoadsorption to ambient-temperature and use it as hydrogen storage mechanisms in vehicles. However, the found difficulty in achieving ultra-porous structures with high-enough interaction energies decreased this research interest in the last years.
However, for a stationary application like hydrogen refueling stations, where space and weight are not such limits as in vehicles, cryoadsorption can still be considered a feasible candidate for hydrogen storage. Cryoadsorption is the only fast and fully reversible approach to store hydrogen at similar density values as compressed gas. Cryogenic operation is a technological challenge, but first, liquid nitrogen is cheap, and second, it is less energy-demanding than hydrogen liquefaction, which is indeed considered as feasible for transportation and storage. Cryoadsorption involves lower pressure
than compressed gas, increasing safety in the storage facilities, but additional research on the construction materials properties is necessary to better understand their behavior in contact with hydrogen at cryogenic temperatures. However, the knowledge of all these mechanisms is important to identify the improvement opportunities based on, probably, the interphase between different solutions.
To achieve the set project goals, this internal research report describes the work packages realised within the framework of the project.
This study was designed to examine and compare the operation of accreditation bodies in Europe. A management tool, the Process Maturity Benchmarking Tool (PMBT), was elaborated and validated by applying it to various accreditation bodies. By applying the tool, the values of indicators were determined, thus enabling a comparison of the accreditation bodies despite different operational processes and organizational forms.
The management tool PMBT is based on the analysis of selected processes with high relevance for the operation of accreditation bodies. The processes are derived from a process map designed for accreditation bodies in a universally applicable way. The indicators used to characterize the processes come from two sources: The first source relates to data already available from internal databases, reports, financial audits etc. The second source is derived from a self-evaluation of process maturity performed by the accreditation bodies. The criteria for evaluating process maturity were designed by applying the criteria of the EFQM excellence model 2013 of the European Foundation for Quality Management (EFQM) to the processes identified in the process map.
The project Comparison of the Operation of Accreditation Bodies in Europe comprised three stages. In the first stage, the processes of accreditation bodies were systematically analyzed. A process map was developed and processes of special relevance for the performance of accreditation bodies were identified and underpinned by indicators as described above. In the second stage, the processes of the German accreditation body DAkkS were assigned to the tool. This stage was used to check and modify the indicators when necessary. In the third stage, the transferability of the model was analyzed by extension to seven other accreditation bodies operating in Europe. The third stage of the project ended with a workshop attended by the eight accreditation bodies, which was used to present and discuss the results of the comparison and to identify best practices.
Nuclear Power Plants have been in operation for ca. 50 years. Based on this experience, non-destructive testing tasks specific to thick and highly reinforced nuclear containment structures have materialized. The performance based Service life extension of existing NPPs also needs a measurement based decision to support continuing the service of the concrete part of the installations.
By nature, concrete is a very durable material and any natural Deterioration processes may take a long time to become critical to the structure. The experience of more than 50 years of service limits the testing tasks to a few ones which are not yet solved.
Research in NDT of concrete structures is performed by many research institutions all over the world with different technical and systematic approaches. Results are mainly obtained on laboratory specimens, sometimes additional field studies are reported. This research takes place independently without coordination and as a result, the outcomes mostly lack full comparability.
Software for data analysis has become indispensable and very powerful. This part of testing needs more attention when it comes to evaluate test results. Validation of NDE solutions is becoming a critical part in concrete structure testing.
Validation is by definition the proof that a customer´s requirements in the test are being met by the testing solution. This includes equipment, personnel qualification and data analysis. In the following tables, the research recommendation Validation is used in the sense, that proof of the performance of existing solutions needs to be adressed. In general, a validation methodology for NDE solutions for concrete testing in itself needs to be researched and established.
Comparability of research also needs an accepted and easily accessible reference. From experience, it is almost impossible to manufacture exact copies of test specimens at different locations. Round Robin tests are therefore needed to evaluate the performance of a test.
Data evaluation is generally done using dedicated software, sometimes Hardware dependant and not interchangeable between systems. Software is ever more increasingly becoming more powerful and sophisticated. An in-depth evaluation needs to address the comparability and validation of Software used for data analysis and evaluation. The vision of a unified software pool for NDE investigations would undoubtedly support research tremendously.
Quantitative NDE is mostly recommended to assess the condition of a structure. However, qualitative data can be very useful, especially for processes which change the material properties or deteriorate the structure (e.g. corrosion of reinforcement). The need for reliable baseline data is a key factor for such monitoring tasks.
Thermodynamics of LNG
(2020)
Densities of eight gravimetrically prepared ternary and quaternary gas mixtures consisting of methane, ethane, propane, and partially nitrogen were investigated along the four isotherms of –250, –230, –210, and –190 °F at pressures of 350, 500, 650, and 1000 psig using a cryogenic single-sinker densimeter. The experimental densities were compared to densities calculated by various models, namely the EOS-LNG fundamental Helmholtz equation of state, the COSTALD correlation, the Lee-Kessler-Plöcker equation of state, and the Peng-Robinson equation of state. The best performance was shown by the EOS-LNG equation of state which is capable of predicting the liquid densities within the specified uncertainty of the model of 0.05 %. The other models, however, showed significant differences that disqualify for calculation within the p,T-region investigated of the gas mixtures.
An inter-laboratory comparison on the surface charge, expressed as zeta potential ζ, of nanoscaled SiO2 has been performed using #14 BAM Silica (see D.5.41/5.42) nanoparticles. The comparability of results delivered by participants has been tested.
The Task 5.4 of NanoValid is designed to test, compare and validate current methods to measure and characterize physicochemical properties of selected engineered nanoparticles. The measurand is Surface charge expressed as zeta-Potential. The measurements are to be accompanied by estimates of the uncertainties at a confidence level of 95%, deduced from the standard uncertainties. Therefore an uncertainty budget comprising statistical (Type A) and systematic (Type B) errors has to be established and delivered for the measurand. The protocol comprises two Annexes addressing the establishment of uncertainty budgets following GUM. The final goal of the comparison is to identify those methods of measurement which have potential as reference methods in pc characterization of nanoparticles for the determination of a given measurand.
This Report describes an inter-laboratory comparison aiming on the establishment of the used method (BET) as a reference method. Another purpose was the certification of the porous reference material #15 BAM Titania as CRM BAM-P110 (cf. D 5.41/42). The certified values determined by nitrogen ad-sorption at 77.3 K according to the international standards ISO 15901-2 and ISO 9277 are summarized in the Table below.
An inter-laboratory comparison on the particle size, expressed as mean diameter d, of nanoscaled SiO2 (#14 BAM Silica (see NanoValid DoW, D.5.41/5.42)) has been performed. The majority of participants used Dynamic Light Scattering (DLS). A few used Electron Microscopy as method. Following methods had been applied by only one partner, respectively: Small Angle X-ray Scattering, Analytical Ultracentrifugation, Atomic Force Microscopy and Atomizer with electric mobility spectrometer.
This report describes a standard operation procedure for dispersion of nanomaterials in liquids prior to toxicological or ecotoxicological testing. Main factors, who determine the state of agglomeration and aggregation of ENMs after dispersion are specific energy input, particle concentration and fluid composition. The method was validated in two round robin tests, where two typical nanomaterials (a nanopowder and a nanodispersion) were investigated. One main result arising out of the data comparison was that only those participants, who were able to follow the instructions in the SOPs completely, received similar results regarding particle size and zeta potential. The SOP is easy to adapt for other types of nanomaterials. The results provide the standardization process and were presented at DIN working group.
A novel approach for rating fatigue-initiating inclusions in highly demanding steel (INCAFAT)
(2018)
INCAFAT project aimed to improve existing fatigue damage models by establishing the most suitable combination of measurement techniques to characterise harmful inclusion populations in highly demanding steels. The different inclusion assessments carried out confirm that, chemical composition, secondary metallurgy and manufacturing route affect content, nature, size and shape of inclusions. According to the FEM model, inclusions produce an alteration of the stress field in their surrounding region, which can promote a fatigue failure. Experimental work on fatigue testing has demonstrated that depending on the stressed direction fatigue failures in highly demanding steels could be produced by different types of inclusions. Fractography analyses confirmed that meso-inclusions harmful in fatigue cannot be rated by standard methods, nor 10 MHz ultrasonic testing (macro) or micro-cleanness assessments. The necessity of rating these meso-inclusions has led to critical evaluation of Extreme Value Analysis according to ASTM E2283-08 and the development of high frequency immersion ultrasonic testing. EVA methodology based on inclusion width can be applied reliably when principal stress is parallel to the rolling direction. On the contrary, if inclusions are testing in the elongated directions its fails. On the other hand, the guidelines and recommendations for high frequency ultrasonic testing have been compiled in a new European standard draft. This method based on focal beam probes and high-resolution devices is able to provide information on meso-inclusion distribution.
Digital holographic cytometry (DHC) is a state-of-the-art quantitative Phase imaging (QPI) method that permits time-lapse imaging of cells without induced cellular toxicity. DHC platforms equipped with semi-automated image segmentation and analysis software packages for assessing cell behavior are commercially available. In this study we investigate the possible uptake of nanoprobes in macrophages in vitro over time.
Isotope amount ratios (hereafter referred to as simply isotope ratios) are proving useful in an ever increasing array of applications that range from studies unravelling transport processes, to pinpointing the provenance of specific samples as well as trace element quantification by using isotope dilution mass spectrometry (IDMS). These expanding applications encompass fields as diverse as archaeology, food chemistry, forensic science, geochemistry, medicine and metrology. However, to be effective tools, the isotope ratio data must be reliable and traceable to enable the comparability of measurement.
The importance of traceability and comparability in isotope ratio analysis has already been recognized by the Inorganic Analysis Working Group (IAWG) within the CCQM. Three pilot studies have focused on the quality of isotope ratio determinations (P48 “U isotope ratios in urine”, P75 “stable isotopes in Methionine”, P105 “87Sr/86Sr in wine”). Moreover, isotope ratio measurements are fundamental to IDMS amount of substance determinations. For example, when Pb quantification using IDMS is undertaken, this requires the measurements of Pb isotope ratios. While the requirements for isotope ratio accuracy and precision in the case of of IDMS are generally quite modest, “absolute” Pb isotope ratio measurements for geochemical age dating and source rock characterization as well as forensic provenance and fingerprinting studies require Pb isotope ratio measurements of the highest quality. To support present and future CMCs on isotope ratio determinations, a Key Comparison was urgently needed. Therefore, it was decided at the IAWG meeting in Paris in April 2011 that a Key Comparison on the determination of Pb isotope ratios in a pure Pb solution and in a bronze sample should be organized and accompanied by a pilot study.
Measuring Pb isotope amount ratios in a pure Pb solution, while seemingly straight forward, rigorously tests the ability of analyst to correct for any instrumental effects (such as mass discrimination and blank correction) on the measured ratios. Pb, present in trace amounts in a metal matrix sample (e.g. Pb in bronze), provides a real world test of the whole chemical and instrumental procedure, from chemical separation and sample purification to analysis and subsequent correction of appropriate instrumental effects on the separated samples.
A suitable bronze material with a Pb mass fraction between 10 and 100 mg·kg-1 was available at BAM. A high purity solution of Pb with a mass fraction of approximately 100 mg·kg-1 was also available. By comparing the Pb isotope ratio results obtained for the bronze sample with the Pb isotope ratio results from the Pb solution, potential biases arising from the processing of the bronze sample could be effectively identified and separated from the instrumental effects arising from the measurement and data processing protocol.
Flow-back and produced waters from shale gas and shale oil fields contain high ammonium, which can be formed by methanogenic degradation of methylamines into methane and ammonium. Methylamines are added to fracturing fluid to prevent clay swelling or can originate from metabolism of the osmolyte triglycinebetaine (GB).
We analyzed field samples from a shale gas reservoir in the Duvernay Formation and from a shale oil reservoir in the Bakken formation in Canada to determine the origin of high ammonium. Fresh waters used to make fracturing fluid, early flow-back waters, and late flow back waters from the shale gas reservoir had increasing salinity of 0.01, 0.58, and 2.66 Meq of NaCl, respectively. Microbial community analyses reflected this fresh water to saline transition with halophilic taxa including Halomonas, Halanaerobium, and Methanohalophilus being increasingly present. Early and late flow-back waters had high ammonium concentrations of 32 and 15 mM, respectively.
Such high concentrations had also been found in the Bakken produced waters.
Enrichment cultures of Bakken produced waters in medium containing mono, di-, or trimethylamine, or triglycinebetaine (GB) converted these substrates into ammonium (up to 20 mM) and methane. The methylotrophic methanogen Methanohalophilus, which uses methylamines for its energy metabolism and uses GB as an osmolyte, was a dominant community member in these enrichments. Halanaerobium was also a dominant community member that metabolizes GB into trimethylamine, which is then metabolized further by Methanohalophilus. However, the micromolar concentrations of GB measured in shale reservoirs make them an unlikely source for the 1,000-fold higher ammonium concentrations in flow-back waters. This ammonium either originates directly from the reservoir or is formed from methylamines, which originate from the reservoir, or are added during the hydraulic fracturing process. These methylamines are then converted into ammonium and methane by halophilic methylotrophic methanogens, such as Methanohalophilus, present in flow-back waters.
This study was designed to examine and compare the operation of accreditation bodies in Europe. A management tool, the Process Maturity Benchmarking Tool (PMBT), was elaborated and validated by applying it to various accreditation bodies. By applying the tool, the values of indicators were determined, thus enabling a comparison of the accreditation bodies despite different operational processes and organizational forms.
The management tool PMBT is based on the analysis of selected processes with high relevance for the operation of accreditation bodies. The processes are derived from a process map designed for accreditation bodies in a universally applicable way. The indicators used to characterize the processes come from two sources: The first source relates to data already available from internal databases, reports, financial audits etc. The second source is derived from a self-evaluation of process maturity performed by the accreditation bodies. The criteria for evaluating process maturity were designed by applying the criteria of the EFQM excellence model 2013 of the European Foundation for Quality Management (EFQM) to the processes identified in the process map.
The project Comparison of the Operation of Accreditation Bodies in Europe comprised three stages. In the first stage, the processes of accreditation bodies were systematically analyzed. A process map was developed and processes of special relevance for the performance of accreditation bodies were identified and underpinned by indicators as described above. In the second stage, the processes of the German accreditation body DAkkS were assigned to the tool. This stage was used to check and modify the indicators when necessary. In the third stage, the transferability of the model was analyzed by extension to seven other accreditation bodies operating in Europe. The third stage of the project ended with a workshop attended by the eight accreditation bodies, which was used to present and discuss the results of the comparison and to identify best practices.
Validation report on NMR
(2017)
The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug and play integration, even though they may appear to be more complex at first sight. Smart sensors enable concepts like self-diagnostics, self-calibration, and self-configuration/ parameterization whenever our current automation landscape allows it.
Here we summarize the currently discussed general requirements for process sensors 4.0 and introduce a smart online NMR sensor module as example, which was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (www.consensspire.eu).
The cement proficiency testing (PT) scheme was set up by the German Metrology Institute (PTB) and the Federal Institute for Materials Research and Testing (BAM) in 2012. The PT scheme was a spin-off from a European Commission and African, Caribbean and Pacific-Group of States funded project entitled SPIN – Spearhead Network for Innovative, Clean and Safe Cement and Concrete Technologies (www.spin.bam.de). The SPIN project aimed at crosslinking experts in industry and policy making bodies, with the prospect of establishing a sustainable cement and concrete construction capacity in Africa.
After a successful first pan-African proficiency testing scheme in 2012/2013, it was decided to establish the scheme permanently and independent of the SPIN project.
The main focus of setting up a testing scheme was to enable all cement testing laboratories in Africa to evaluate their competence and efficiency in cement testing and further enhance their capacity to obtain better quality products according to their environment. The acronym developed for the PT scheme is PACE-PTS (Pan-African Cement Proficiency Testing Scheme). The framework for the PT scheme was set up jointly among the organisers and the first participants. The first PT scheme was initiated in Dar Es Salaam in 2012 followed by a final workshop in Berlin in 2013. The second PT scheme began in 2014. A final workshop was organised in Dar es Salaam in 2015. The third and current scheme was started in 2016 and the final workshop is held in Yaoundé.
In October 2011 the European Commission (EC) published a "Recommendation on the definition of na-nomaterial" (2011/696/EU), to promote consistency in the interpretation of the term "nanomaterial" for legislative and policy purposes in the EU. The EC NM Definition includes a commitment to its review in the light of experience and of scientific and technological developments. This review is ongoing in 2017 and as a contribution to the review the Joint Research Centre of the European Commission (JRC) has already developed a series of three scientific-technical reports with the title: “Towards a review of the EC Recommendation for a definition of the term nanomaterial” which provides to the EC policy services sci-ence-based options on how the definition could be revised or supported with additional guidance.
The overarching nature and wide scope of the EC NM Definition, as it does not exclude a priori any particulate material regardless the state, form and size, creates many analytical challenges in its imple-mentation for all stakeholders, including enterprises and regulators.
The NanoDefine project has as core objective to support the implementation of the EC NM Definition. In an earlier report1 key aspects of the EC NM Definition were addressed, with the goal to improve the implementability of the EC NM Definition. Based on further developments and results obtained in NanoDefine project that first report was updated and is presented here. The key aspects are discussed based on the results of four years of research performed within the framework of the project. As a result this report assesses how well the requirements of the EC NM Definition can be fulfilled with currently available analytical possibilities. It presents recommendations and options on a revision of the EC NM Definition to improve the implementability of the definition based on currently available analytical possi-bilities, according to the state of the art in 2017. Of the technical issues considered in this report, the following seem to deserve the most attention in terms of clarification of the definition and/or provision of additional implementation guidance: 'external dimension', ‘number based particle size distribution‘, ‘polydispersity‘ and ‘upper size limit‘, the term ‘particle’, the ‘means to prove that a material is not a nanomaterial‘ and ‘the role of the volume specific sur-face area (VSSA)‘, and "particulate materials'.
Recommendations on a Revision of the EC Definition of Nanomaterial Based on Analytical Possibilities
(2015)
In October 2011 the European Commission (EC) published a "Recommendation on the definition of nanomaterial" (2011/696/EU), to promote consistency in the interpretation of the term "nanomaterial" for legislative and policy purposes in the EU. The EC NM Definition includes a commitment to its review in the light of experience and of scientific and technological developments. This review is ongoing in 2015 and as a contribution to the review the Joint Research Centre of the European Commission (JRC) has already developed a series of three scientific-technical reports with the title: “Towards a review of the EC Recommendation for a definition of the term nanomaterial” which provides to the EC policy services science-based options on how the definition could be revised or supported with additional guidance.
The overarching nature and wide scope of the EC NM Definition, as it does not exclude a priori any particulate material regardless the state, form and size, creates many analytical challenges in its imple-mentation for all stakeholders, including enterprises and regulators.
The NanoDefine project has as core objective to support the implementation of the EC NM Definition. In this report key aspects of the EC NM Definition are addressed, with the goal to improve the implement-ability of the EC NM Definition. These aspects are presented and discussed based on the results of two years of research performed within the framework of the project. As a result this report assesses how well the requirements of the EC NM Definition can be fulfilled with currently available analytical possi-bilities. It presents recommendations and options on a revision of the EC NM Definition to improve the implementability of the definition based on currently available analytical possibilities, according to the state of the art of mid-2015.
Of the technical issues considered in this report, the following seem to deserve the most attention in terms of clarification of the definition and/or provision of additional implementation guidance:
The term ‘external dimension’.
A clear definition of 'External dimension' should be included in the text of the EC NM definition and more precise guidance on what is considered as an external dimension and how to properly character-ise it should be provided.
The ‘number based particle size distribution‘.
The EC NM Definition uses a threshold related to the number based size distribution of particles. Yet most of the easily available techniques provide a mass-, volume- or scattered light intensity-based size distribution which needs to be converted into a number based distribution to be used for regulatory pur-poses. A specific guidance on the conditions under which these methods can be used to identify a na-nomaterial by employing appropriate quantity or metrics conversion should be provided.
The ‘polydispersity‘ and ‘upper size limit‘
Polydispersity is a challenge for the measurement of particle size distribution for the EC NM definition, specifically for materials with high polydispersity index and broad size distribution especially when the volume or mass of the fraction containing particles below 100 nm is very small. Therefore a dedicated guidance should be provided that allows applying an upper size limit in measurements and particle statistics.
The test methods UN Test L.2 / EN ISO 9038:2013 DIN EN 15188:2007 are applied to characterize the sustained combustibility of liquids i.e. the behaviour of a material under specified test conditions, whereby its vapour can be ignited by an ignition source and sufficient flammable vapour is produced to continue burning for at least 15 s after the source of ignition has been removed.
The aims of this interlaboratory test (IT) are the verification and/or the improvement (if necessary) of the verification data (reference material) in Annex B of EN ISO 9038:2013, the assessment of influencing (disturbing) factors (laboratory specific factors, which possibly may have an influence on the test result) and the assessment of the performance of the participating laboratories.
It could be demonstrated that the reference materials n-Dodecane, n-Decane and n-Undecane as mentioned in the standard are suitable and the verification shall continue to be valid.
Sustained combustibility tests are influenced by several factors like the presence of a draught shield, the experience of the laboratory assistant, verification of the apparatus, calibration of the metering device.
Based on the interlaboratory test, the gained experience and the actual results, well-founded measures / actions can be recommended to improve execution of the method.
The IT was organized by PTB, BAM and QuoData GmbH in the framework of the co-operation project CEQAT-DGHS Centre for Quality Assurance for Testing of Dangerous Goods and Hazardous Substances.
The VSSA approach has the important advantage over classifying, imaging and counting techniques that it does not involve dispersion protocols. Further, the BET technique as the basis for VSSA determination it is in widespread use, generates low costs and is specified for many commercial materials. Finally, the same equipment allows for a deeper analysis by full isotherm evaluation.
The present deliverable assesses all NanoDefine powders, supplemented by further real-world materials (in total 26 powders), and quantitatively compares the relationship between the median size (by Electron Microscopy – considered as benchmark for the EC nanomaterial definition) vs. the size derived from VSSA. The VSSA method mitigates the challenges of EM to assess the thickness of platelets, but worked as well on fibbers and particles of irregular shapes. A screening strategy is proposed. If applied to the further data from real-world materials as validation set, this screening does achieve a correct classification, leaving only borderline materials for tier 2 assessment.
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?
Lead (Pb) isotope amount ratios are commonly used in applications ranging from archaeology and forensic sciences to terrestrial and extra-terrestrial geochemistry. Despite their utility and frequency of use, only three certified isotope amount ratio reference materials are currently available for Pb: NIST SRMs 981, 982 and 983. Because SRM 981 has a natural Pb isotopic composition, it is mainly used for correcting instrumental mass discrimination or fractionation. This means that, at present, there are no other certified isotope reference materials with natural Pb isotopic composition that could be used for validating or verifying an analytical procedure involving the measurement of Pb isotope amount ratios.
To fill this gap, two new reference materials, both certified for their Pb isotopic composition, have been produced together with a complete uncertainty assessment. These new reference materials offer SI traceability and an independent means of validating or verifying analytical procedures used to produce Pb isotope amount ratio measurements.
ERM-EB400 is a bronze material containing a nominal Pb mass fraction of 45 mg/kg. ERM-AE142 is a high purity solution of Pb with a nominal mass fraction of 100 mg/kg. Both materials have been specifically produced to assist analysts in verifying or validating their analytical procedures. Note that while one of these reference materials requires the chemical separation of Pb from its matrix (ERM-EB400), the other does not (ERM-AE142). Details on the certification of these isotope reference materials are provided in this report.
We report on calibration standards of nanoparticles meeting the definition of a nanomaterial given by the European Commission (EU 2011) which are relevant for the characterisation methods applied in the NanoDefine project. We found that the Impact of nanoparticles is outstanding in the scientific literature. A number of 270.000 paper titles on nanoparticles are listed in the Web of Science data base. But surprisingly, the availability of suitable certified standard reference materials is scarce. Only a few sources were found. For example, BAM provides the database Nanoscaled Reference Materials at http://www.nano-refmat.bam.de/en/ in cooperation with the ISO/TC 229 Nanotechnologies. In addition, two publications from 2013 on nanoscale reference materials are available. Candidates of nano-(certified) reference materials from other ongoing or just finished FP6 and FP7 nano-metrology projects have been extracted from the Compendium of Projects in the European NanoSafety Cluster (Compendium NSC, 2013). Recommendations for selection of representative test materials and calibration standards for NanoDefine internal tasks, respectively, are also given.
The EU FP7 NanoDefine project was launched in November 2013 and will run until October 2017. The Project is dedicated to support the implementation of the EU Recommendation on the Definition of Nanomaterial
by the provision of the required analytical tools and respective guidance. Main goal is to develop a novel
tiered approach consisting of (i) rapid and cost-efficient screening methods and (ii) confirmatory measurement
methods. The "NanoDefiner" eTool will guide potential end-users, such as concerned industries and regulatory bodies as well as enforcement and contract laboratories, to reliably classify if a material is nano or not. To achieve this objective, a comprehensive inter-laboratory evaluation of the performance of current
characterisation techniques, instruments and software is performed. Instruments, software and methods are
further developed. Their capacity to reliably measure the size of particulates in the size range 1-100 nm and
above (according to the EU definition) is validated. Technical reports on project results are published to
reach out to relevant stakeholders, such as policy makers, regulators, industries and the wider scientific community, to present and discuss our goals and results, to ensure a continuous exchange of views,
needs and experiences obtained from different fields of expertise and application, and to finally integrate the resulting feedback into our ongoing work on the size-related classification of nanomaterials.
The content of the paper is the assessment of the performance of (conventional) measurement techniques (MTs)with respect to the classification of disperse materials according to the EC recommendation for a definition of nanomaterial. This performance essentially refers to the accurate assessment of the number weighted median of (the constituent) particles. All data and conclusions are based on the analytical study conducted as real-world performance testing.
It comprised different types of MTs (imaging, counting, fractionating, spectroscopic and integral) as well as different types of materials. Beside reference materials with well-defined size distribution the study also included several commercial powders (variation of particle composition, morphology, coating, size range and polydispersity). In order to ensure comparability of measurement results, the participants were guided to use uniform protocols in sample preparation, conducting measurements, data analysis and in reporting results. Corresponding documents have been made public, in order to support the reviewing process of the paper, respectively to ensure the reproducibility of data by other users under the same conditions.
The scientific paper relies on a comprehensive set of revised measurement data reported in uniform templates, completely describes the experimental procedures and discusses the MTs’ performance for selected materials in detail. Even more, the study is summarised and evaluated, which leads to recommendations for the use of MTs within a tiered approach of NM characterisation. In addition, the paper critically examines the factors that may affect the outcome of such a comparison among different MTs.
This report is the result of a comprehensive study on the available CMs which come potentially in question for the reliable analysis of the number based size distribution of a nanomaterial according to the EC recommendation for a definition of nanomaterial. Based on the performance criteria already established in NanoDefine the potential CMs are evaluated according to studies available in the literature as well as following the expertise of the NanoDefine consortium partners. The specific advantages and disadvantages of each method with respect to its applicability to the scope of NanoDefine are particularly highlighted. An CM evaluation table is produced so that the mostly suited CMs with respect to the EC definition can be grouped and recommended to the corresponding NanoDefine work packages for further specific development (improvement and adaption), or for direct validation and standardisation, respectively. The actual evaluation report including the recommended CMs will be revised and, if necessary, eventually updated at the mid time of the project. The update will be jointly discussed in the NanoDefine consortium on the basis of the results of testing the methods on the NanoDefine real world materials.
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.
IND15 JRP SurfChem: Traceable quantitative surface chemical analysis for industrial applications
(2016)
The SurfChem project has made a significant contribution to traceable quantitative surface chemical analysis for industrial applications by delivering new certified reference materials and test samples for specific technical applications. Regular performance tests of instruments, metrological methodology for the detection of (bio)organic surface species, ambient and non-destructive surface chemical analysis for in-line process control and new in situ characterisation techniques of catalytically active surfaces have been achieved.
It is important to protect critical buildings (shopping centres, government buildings and embassies), infrastructure and utilities, train and underground stations against being damaged, destroyed or disrupted by deliberate acts of terrorism, criminal activity and malicious behaviour. Normal regulations and building guidelines do not generally take into account these threats. The introduction of appropriate regulations or guidelines, where deemed necessary, should enhance the resilience of buildings and infrastructure against explosion incidents. In order to protect the built infrastructure, methods are required to quantify the resistance of structural components against explosive loading and to assess the hazards resulting from the failure of an element. The applicable state-of-the-art techniques may include either experimental or numerical methods, or a combination of both. Therefore, the thematic group (TG) on the resistance of structures to explosion effects was formed in order to bring the required expertise together, make it commonly available and to find and define harmonised methods and solutions which can be provided to the decision-makers responsible for critical infrastructure protection. This report discusses the differences between the existing standards for testing blast-resistant glazing and windows and it presents basic recommendations for the future development of the suite of European standards in this area.
It is important to protect critical buildings (shopping centres, government buildings and embassies), infrastructure and utilities, train and underground stations from being damaged, destroyed or disrupted by deliberate acts of terrorism, criminal activity and malicious behaviour. Normal regulations and building guidelines do not generally take into account these threats. The introduction of appropriate regulations or guidelines, where deemed necessary, should enhance the resilience of buildings and infrastructures against explosion incidents. In order to protect the built infrastructure, testing methods are required which can answer the question whether certain building elements can withstand certain loading conditions created by an explosive event. The applicable state-of-the-art techniques may include either experimental or numerical methods, or a combination of both. Therefore, the thematic group (TG) on the resistance of structures to explosion effects was formed in order to bring the required expertise together, to make it commonly available and to find and define harmonised methods and solutions which can be provided to the decision-makers responsible for critical infrastructure protection. The TG described in a fist report JPC87202 the physical phenomena which have to be understood in order to ensure a proper testing of the elements and a correct interpretation of the results. In a second step, the differences between the existing standards for testing blast-resistant glazing and windows have been derived, and a basis for fundamental recommendations for the future development of the suite of European standards has been addressed JRC94930. Based on the prior findings, this report now formulates the proper enhancements of the existing standards in terms of actual recommendations for the improvement of the test standards.
The determination of the blast protection level of laminated glass windows and facades is of crucial importance, and it is normally done by using experimental investigations. In recent years numerical methods have become much more powerful also with respect to this kind of application. This report attempts to give a first idea of a possible standardisation concerning such numerical simulations. Attention is drawn to the representation of the blast loading and of the behaviour of the material of the mentioned products, to the geometrical meshing, as well as to the modelling of the connections of the glass components to the main structure. The need to validate the numerical models against reliable experimental data, some of which are indicated, is underlined.
It is important to protect critical buildings (shopping centres, government buildings and embassies), infrastructure and utilities, train and underground stations against being damaged, destroyed or disrupted by deliberate acts of terrorism, criminal activity and malicious behaviour. Normal regulations and building guidelines do not generally take into account these threats. The introduction of appropriate regulations or guidelines, where deemed necessary, should, enhance the resilience of buildings and infrastructure against explosion incidents. In order to protect the built infrastructure, methods are required to quantify the resistance of structural components against explosive loading and to assess the hazards resulting from the failure of an element. The applicable state-of-the-art techniques may include either experimental or numerical methods, or a combination of both. Therefore, the thematic group (TG) on the resistance of structures to explosion effects was formed in order to bring the required expertise together, make it commonly available and to find and define harmonised methods and solutions which can be provided to the decision-makers responsible for critical infrastructure protection. The current report summarizes existing best practices for the numerical finite element modelling of blast loading, including the important topics of domain discretisation, implicit/explicit formulation, Lagrangian/Eulerian solvers, the mathematical description of the material behaviour etc. Furthermore recommendations for the modelling of laminated glass elements are formulated and knowledge gaps in this application area are pointed out. Hence the report builds the basis for an actual evaluation of the different numerical methods, their suitability to certain problems, and their capability to support/complement the experimental testing of glass components. It thus provides helpful information to design architects and engineers, and more generally to critical infrastructure stakeholders, responsible for the structural integrity and security of the infrastructure in case of an explosion.
Isotope dilution mass spectrometry often is applied for the quantification of platinum group elements in environmental and geological samples. In most cases, however, certified spike solutions offering complete uncertainty statements and SI-traceability are missing. This report describes the production and certification of two isotope reference materials, ERM-AE140 and ERM-AE141, serving as calibrated spike solutions for IDMS based quantification of Pd and Pt, respectively. Both materials were produced by dissolving highly enriched isotopes 106Pd and 194Pt and determining the mass fraction of 106Pd and 194Pt in the final solution by reverse IDMS. Two independent back-spikes were produced for each material from high purity Pd and Pt. Characterization measurements were carried out by MC-ICPMS. For ERM-AE140 the certified mass fractions are w(106Pd) = 20.24(5) mg/kg and w(Pd) = 20.54(5) mg/kg. For ERM-AE141 the certified mass fractions are w(194Pt) = 18.18(11) mg/kg and w(Pt) = 19.90(12) mg/kg. These values are traceable to the International System of Units (SI) in the shortest possible way.
Isotope reference materials are essential to enable reliable and comparable isotope data. Besides the correction of mass fractionation or mass discrimination, isotope reference materials are indispensible for validation and quality control of analytical procedures. This report describes the production and certification of two isotope reference materials, ERM-AE123 and ERM-AE124, for boron isotope analysis. The isotopic composition of ERM-AE123 is the unaltered natural-like isotopic composition of the base material. The isotopic composition of ERM-AE124 has been adjusted by mixing two boron stock solutions enriched in 10B and 11B respectively under full gravimetric control. All stock solutions have been prepared fully under gravimetrical control. The corresponding boron isotopic composition has been analysed by TIMS. For both reference materials the isotopic composition obtained on the basis of the gravimetric data agrees very well with the isotopic composition obtained by TIMS. The certified isotope abundances for 10B are 0.19832 (21) for ERM-AE123 and 0.96006 (6) for ERM-AE124. Together with the formerly certified ERM-AE101, -AE102a, -AE103, -AE104a, -AE120, -AE121 and AE122, a unique set of nine certified reference materials (CRM) for boron isotope analysis is now available from BAM covering a range for the 10B isotope amount fraction from 0.2 to 0.96 and for the δ11B value from -20 ‰ to +40 ‰.
Certification report for the reference materials ERM-AE102a, -AE104a, -AE120, -AE121 and -AE122
(2010)
Isotope reference materials are essential to enable reliable and comparable isotope data. Besides the correction of mass fractionation or mass discrimination isotope reference materials are indispensible for validation and quality control of analytical procedures. This article describes the production and certification of a set of five isotope reference materials ERM-AE102a, 104a, AE120, 121 and 122, for boron isotope analysis. The isotopic composition of all materials has been adjusted by mixing boron mother solutions enriched in 10B or 11B with a boron mother solution having natural-like isotopic composition under full gravimetric control. All mother solutions have been analysed for their boron mass fraction as well as their boron isotopic composition by TIMS using IDMS as calibration technique. For all five reference materials the isotopic composition obtained on the basis of the gravimetric data agrees very well with the isotopic composition obtained from different TIMS techniques. Performed stability and homogeneity studies show no significant influence on the isotopic composition as well as on the related uncertainties.
The certified isotope abundances for 10B are 0.29995 (27) for ERM-AE102a and 0.31488 (28) for ERM-AE104a. The certified δ11B values are -20.2 (6) ‰ for ERM-AE120, 19.9(6) ‰ for ERM-AE121 and 39.7 (6) ‰ for ERM-AE122.
Together with the formerly certified ERM-AE101 and -AE103 a unique set of seven certified reference materials (CRM) for boron isotope analysis is now available from BAM.
Three petrol reference materials were certified for their total sulfur content in support of Directive 2003/17/EC of the European Parliament and of the European Council, which stipulates that petrol with a maximum S content of 10 mg/kg must be available in all member states by 2009. Commercially available petrol was obtained and filled into borosilicate ampoules without further treatment. Homogeneity of the materials was tested and no heterogeneity was detected for two of the materials, whereas minor heterogeneity was observed for the third material. Stability of the materials was tested for 8-12 months at 60 °C and no degradation was observed. Characterisation was based on isotope-dilution mass spectrometry (IDMS) applied as primary method of measurement by three European metrology institutes and certified values were assigned using all results. The certified uncertainties include contributions of (potential) heterogeneity, potential degradation as well as characterisation. The final assigned values are:
ERM-EF211: 48.8 ± 1.7 mg/kg
ERM-EF212: 20.2 ± 1.1 mg/kg
ERM-EF213: 9.1 ± 0.8 mg/kg
The materials are available from IRMM (ERM-EF211), LGC (ERM-EF212) and BAM (ERMEF213)
HIIRM final report
(2002)
Accurate analytical results have become more and more an absolute essential tool for further progresses in technology and science. Precision however, often used in this context as a quality criterion for analytical methods, is not a replacement for accuracy in any way. Therefore, analytical procedures are necessary, which will generate reliable and accurate results and can be used for evaluation of other analytical procedures and certification of reference materials (RM). Especially the certification of reference materials for the amount content of trace elements requires highly accurate results with a small combined uncertainty. The best example for an analytical procedure having this capability is undoubtedly Isotope Dilution Mass Spectrometry, for inorganic as well as for organic applications. Applied on Thermal Ionization Mass Spectrometry (TIMS) isotope dilution provides results of highest quality and proven high accuracy especially in the field of RM certifications for more than 30 years.
The major drawback of this approach often is the necessity for a complex chemical separation step. A major advantage of Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is the potential to cope with a simplified or an on-line-carried-out sample preparation. A key requirement of isotope dilution analysis however is the accurate and precise determination of isotope ratios, because of its limiting factor for the accuracy and the total uncertainty of the result. Very precise isotope ratios can be determined in combination with a detection system that is capable of simultaneous detection of different isotopes, a so-called multi-collector system.
The objective of the presented project is to evaluate the advantages of such a multi-collector ICP-MS for the application of IDMS in the field of trace elemental analysis in reference materials. The focus is on the development of simple and fast procedures for isotope ratio measurements in general and IDMS analysis in particular. Furthermore, it is an objective to develop and evaluate on-line spiking procedures.
One of the first conclusions, which had a severe impact on the HIIRM project, arose during the early days of the project. Currently most certification experiments are accomplished by certification campaign based on a variety of participants’ results. The sample preparation, sending, analyzing and data evaluation however require lot of resources and the process may take a long time. An alternative way is given by using fewer participants with methods of higher metrological quality. For elemental amount contents such a method undoubtedly is isotope dilution analysis and multi-collector ICP-MS offers the necessary precision and matrix robustness and ruggedness as said above. Therefore, a multiple collector ICP-MS was manufactured as part of the project instead of the originally planned high-resolution instrument. Due to the novelty of the multicollector ICP-MS instrument, a lot of additional fundamental research became necessary. Especially interferences needed further attention. Fortunately, the IsoProbe is additionally equipped with a high-resolution option and with a brand new collison cell. The high-resolution option however can only be used to identify interferences but cannot be used to quantify them. On the other hand, the use of the collision cell proved to be a vital tool to overcome interferences. This is especially true because high resolution would have reduced the available sensitivity by a factor of ~100. Applying the collision cell technology the high sensitivity was maintained whilst most interferences were eliminated. However finding the right parameters of operation for the collision cell became a huge part of the method development process. A variety of gases like argon, helium, hydrogen, deuterium, nitrogen, krypton and xenon were tested for their suitability. Especially the tests accomplished for iron determinations revealed that carefully selected parameters have an incredible influence on the quality of the final results. Nonetheless collision cell technology will undoubtedly be widely used for newer ICP-MS instrumentation and contribute to eliminate wrong analytical values caused by interferences.
The enhanced sensitivity of the instrument revealed also problems not detectable by other means. The control of contaminations seems to be one of the major analytical challenges in the future. Sector field based ICP-MS will give the user an opportunity to trace sources of contamination back to their origin and eliminate them. Even lower limits of detection will be the result as well as an enhanced reliability for analysts dealing with higher amount contents. The analyst will also benefit in controlling blank levels when the method of isotopically spiked procedure blanks is used as demonstrated in this project.
Another main part of the project was the validation of the developed procedures. The first validation step was successfully accomplished by applying these procedures on the standard solutions provided by NRG. The main part of this validation however consisted of the evaluation of the fundamental parameters of the isotope dilution process and related measurements. This approach turned out to be superior compaired to the first step as a highly reliable uncertainty calculation can be easily performed. The best reputation and acceptance of the methods can however only be accomplished by participating in certification campaigns or in interlaboratory comparisons on highest metrological level. The results of the participations in general were brilliant. Not only the results but also the obtained realistic uncertainties were of superior quality. Direct comparisons at BAM with the results obtained by a multicollector TIMS applying the same calculation schemes showed the benefits of using multicollector ICP-MS. The main benefits of ICP-MS were identified, of which the first one is the enhanced precision of the isotope ratio measurement. For a variety of elements the values obtained by multicollector ICP-MS are even more precise than the ones obtainable by multicollector TIMS. The second important advantage identified was the simplified sample preparation. The laborious and time consuming analyte-matrix-separation step as necessary for TIMS measurements can either be omitted or at least be drastically reduced. Therefore, the advantages regarding time and enhanced sample throughput will result in further spread of ICP-MS in general and multicollector ICP-MS in particular.
The third major part in terms of the method development process was mainly focused on developing an online isotope dilution system. The volumetric instead of the gravimetric IDMS approach proved difficult, if the high demands necessary for RM definition measurements are to be fulfilled. The major obstacle in this case is the missing stability and precision in terms of mass flow. Consequently, the initial development failed as the system made up of two piezoelectric droplet injectors was unable to reach the required stability as well as precision. The thereupon-created system consisting of two HPLC pumps proved to be far more valuable regarding automation and particularly the quantification of transient signals. Nevertheless, such a system will probably be rarely used in certification campaigns, as the gain of time is too small compared to the loss of reliability. However, this system proved most valuable in terms of species-specific elemental analysis as preliminary investigations showed. In this context this system will be suitable for certification measurements, as the major uncertainty contributions derive from sampling, sample treatment and species distribution and as moreover all availabel methods demonstrate far beyond.
During the whole project, one of the main concerns regarding the multicollector ICP-MS instrument were software issues caused by the early development state of the original control programs. A lot of effort was necessary to accomplish the necessary data manipulations externally. The development of a new software suite by Micromass for the HIIRM project has solved this issue almost completely. With the new software suite and the validated parameters of measurement a step forward for institutes dealing with reference material certifications was achieved.
Future certifications campaigns for minor elemental contents in different matrices should be performed by a small number of participants from highly qualified institutes. These institutes should apply very reliable methods of measurement like the ones developed in the HIIRM project. Many resources may be saved that way while the outcome of the certifications may easily be improved. ICP-MC-MS has the potential to be an important method in this context. Stable isotope dilution analysis in combination with a multi-detector ICP-MS, equipped with a hexapole collision cell for the suppression of important spectral interferences and for enhanced sensitivity, proved to be an advanced method of elemental analysis with a high potential for matrix independent measurements. Since ICP mass spectrometers of this type have only recently been introduced, no systematic evaluation of the capabilities of this specific application of the ICP-IDMS method has yet been made.
This Report describes the certification of the reference material antimony implanted in Si/SiO2 intended to be used for calibration of surface and near surface analytical methods. It describes the preparation, homogeneity measurements and the analytical work performed for the certification of both Areal density of antimony Atoms (retained dose) and the isotope amount Ratio as well as giving considerations on the stability of the material.
This report supports the implementation of European regulations on biocidal products for the product types 7, 9 and 10. Emission of active substances from material preservatives into environmental compartments can occur due precipitation. Risk characterisations have to be based on estimations of environmental concentrations of target substances leached from material preservatives. Harmonised test procedures are required to predict environmental impact due to leaching. Seventeen treated articles, mainly paints, but also a textile, sealing tapes and sealing masses were investigated by intermittent contact to water to prove suitability of the proposed laboratory test procedure. Parameters that affect leaching of active substances were examined.
Further development of a semi-analytical model to describe laboratory leaching data revealed that the model can be improved if changes of the leachability of substances during the test are supposed and integrated. Six paints and a textile were exposed to weathering to compare results from laboratory and field experiments. Similarities between leaching processes in both test approaches were observed. Generally, emissions of active substances are considerably higher in laboratory tests than from vertically installed test specimens exposed to weathering. Competing processes that cause losses of active substances can occur in both tests, but to a higher degree in field experiments. In addition, the influence of meteorological parameters on leaching processes was investigated. Factors besides the amount of driving rain were identified that effect leaching processes by complex interaction. Relations between laboratory and field data were analysed, and the applicability of the semi-analytical model was tested for field data. Guidance documents for leaching tests under laboratory and field conditions were drafted and discussed with experts on EU Level workshop 3./4. July 2014, BAM, Berlin), and are included in this Report.
This guideline is intended to be used as an aid to laboratories when they are managing the
use of software and computers with respect to the requirements of ISO/IEC 17025. The
working group consisted of representatives from accreditation bodies and conformity assessment
operators, specifically laboratory organisations, but also included certification
bodies, inspection bodies and metrology institutes.
The objective of the FATWELDHSS project was to study post-weld treatment techniques and their effect on the fatigue life of MAG welded attachments in High Strength Steel (HSS). Fatigue cracks in steel structures often occur at welded joints, where stress concentrations due to the joint geometry and tensile residual stresses are relatively high. Fatigue life improvement techniques, which rely on improving the stress field and/or the surface geometry around the welded joints, are generally known to be beneficial. Therefore, within the framework of this project, the following were examined: diode laser weld toe re-melting; High Frequency Mechanical Impact (HFMI) treatment; Low Transformation Temperature (LTT) filler wires Laser diode re-melting was used to improve the surface profile at the weld toe and thus reduce stress concentrations. HFMI treatment involving high frequency hammering of the weld toe is another technique that can produce a smooth weld toe profile but, more significantly, which also can introduce compressive residual stresses. Lastly, two new LTT filler wires were developed within the project as these can decrease or even remove tensile residual stresses resulting from weld zone shrinkage. An extensive fatigue testing programme was set up to establish the levels of improvement in the fatigue lives of the welded attachments achieved by application of the selected improvement techniques. Furthermore, two industrial demonstrators were selected that could show the project achievements in terms of facilitating the introduction of high strength steels by overcoming the limitations posed by the fatigue properties of the welded joints. In addition, modelling tools were developed to predict the residual stresses at the welded joint. Finally, practical guidelines were developed for enhancing the fatigue strength of HSS welded structures
While in 2012 a commercially available acrylic sealant was used as sample material, in 2014 a lacquer doped with specific substances was sent to the participants for the VOC and odour measurement. The resulting measurement values for the perceived intensity were evaluated in consideration of various boundary conditions to identify parameters that could possibly influence the measurement procedure significantly. For the comparison of both interlaboratory comparisons qualified data sets were taken as a basis. Potential for improvement identified in 2012 was mainly confirmed by the interlaboratory test 2014 as well. Besides the accurate conduction as essential part of the measurement it became obvious again that the boundary conditions of the DIN ISO 16000-28 are not defined tight enough. Moreover the thesis that measurements based on the utilisation of comparison scales with only one funnel generate results especially imprecise could not be verified. Both interlaboratory comparisons resulted in relative standard deviations of reproducibility that lay between 20 and 40 % and such are quite comparable with those of well-established interlaboratory VOC comparisons.
This report gives technological information about processes for the recovery of phosphorus from sewage sludge ash including mass- and energy balance, process conditions and product quality.
The information in this report aim at giving an overview on different concepts for the recovery of phosphorus from sewage sludge ash and are intended to allow a general qualitative comparison between the different technical approaches. This report also describes the technological backgrounds of the processes that were furthermore investigated by life cycle assessment (LCA) and life cycle cost (LCC) analysis. However, most process data stated in this report are site specific data. The LCA/LCC study includes the definition of a common base line for all processes, detailed process modeling and plausibility assessments. Results of the LCA/LCC-studies are reported in deliverables D9.2 und D10.1.
This work was sponsored by the Federal Highway Administration in cooperation with the American Association of State Highway and Transportation Officials. It was conducted in the second Strategic Highway Research Program (SHRP 2), which is administered by the Transportation Research Board of the National Academies. The project was managed by Monica Starnes, Senior Program Officer for SHRP 2 Renewal.
The research reported herein was performed by the Center for Advanced Infrastructure and Transportation (CAIT) at Rutgers University (RU); the Center for Transportation Infrastructure Systems (CTIS) at The University of Texas at El Paso (UTEP); the Federal Institute for Materials Research and Testing (BAM), Germany; and Radar Systems International, Inc. (RSI). Rutgers University was the coordinator and contractor for this project. Dr. Nenad Gucunski, professor and chair of Civil and Environmental Engineering and director of CAIT’s Infrastructure Condition Monitoring Program at RU, was the principal investigator. The other authors of this report are Dr. Soheil Nazarian, professor of Civil Engineering and director of CTIS at UTEP; Dr. Deren Yuan, research associate at CTIS at UTEP; Dr. Herbert Wiggenhauser, head of Non-Destructive Testing (NDT) in Civil Engineering at BAM; Dr. Alexander Taffe, leader of Combination and Automation of NDT of Buildings at BAM; Dr. Parisa Shokouhi, Alexander von Humboldt Research Fellow, hosted by BAM; and Doria Kutrubes, president of RSI. Arezoo Imani and Touraj Tayebi, graduate research assistants at RU, helped conduct the validation testing, data analysis, and web manual content preparation. Hoda Azari, a graduate research assistant, and Dr. Manuel Celaya, a research engineer at UTEP, assisted in the validation study as well. Hooman Parvardeh, research assistant at RU, helped build the reference database and develop the framework for the web manual, while Erica Erlanger, a research staff member at RU, edited the manuscript. Their contributions are gratefully acknowledged.
The research team also gratefully acknowledges contributions of the participants from industry and academia in the validation testing. The participants include NDT Corporation; Germann Instruments; Olson Engineering; Dr. Ralf Arndt, National Research Council associate at FHWA Turner–Fairbank Highway Research Center; Ingegneria Dei Sistemi S.p.A. (IDS), Italy; 3D-RADAR, Norway; Dr. John Popovics, University of Illinois at Urbana-Champaign; Dr. Jinying Zhu, The University of Texas at Austin; Rutgers University—Center for Advanced Infrastructure and Transportation; and The University of Texas at El Paso—Center for Transportation Infrastructure Systems. The contributions of these participants were critical for the evaluation and grading of the performance of NDT technologies.
It is important to protect critical buildings (shopping centres, government buildings and embassies), infrastructure and utilities, train and underground stations against being damaged, destroyed or disrupted by deliberate acts of terrorism, criminal activity and malicious behaviour. Normal regulations and building guidelines do not generally take into account these threats. The introduction of regulations or guidelines should support the resilience of the buildings and infrastructure against explosive incidents. In order to protect the infrastructure, methods are required to quantify the resistance of structural elements against explosive loading and to assess the hazards resulting from failure of an element. The applicable state-of-the-art techniques may be either experimental or numerical methods, or a combination of both. Therefore, the thematic group (TG) on the resistance of structures to explosion effects was formed in order to bring the required expertise together, make it commonly available and to find and define harmonised methods and solutions which can be provided to the decision-makers responsible for critical infrastructure protection. This first report of the TG gives a comprehensive summary of the existing methods which can be used to analyse and test the resistance of glazing and windows under blast-loading conditions. Within this context, the experimental methods of testing using high explosives and testing using blast simulators called shock tubes is presented and explained. In addition, the potential of numerical simulations is highlighted in terms of their applicability to the different glass materials. A short, comprehensive theoretical background is given for each method. Based on this, each method is described with its requirements, realisation and the related measurement techniques. Furthermore, an interpretation of the measurements is highlighted. For the numerical simulations, the basic discretisation and calculations schemes are presented in combination with the available constitutive material descriptions for the different significant materials. Finally the chances for verification and validation of the numerical results are presented. Hence the report builds the basis for an actual evaluation of the different test methods and their applicability to certain problems, and provides helpful information for critical infrastructure stakeholders, owners and operators considering the structural resistance of the infrastructure to the effects of explosion in a comprehensive document.
This report describes the progress in understanding and describing the detectability of the ultrasonic inspection technique developed by SKB for the inspection of copper tubes used for the final disposal of the Swedish spent nuclear fuel. In former research activities dedicated to the different parts of the canister, the probability of detection (POD) evaluation technique, as developed for thin aircraft components, was further developed for the application on complex hick-walled components. The result of this development was the introduction of a “multi-parameter” POD framework. In contrast to taking only the defect size into consideration (as for aircraft components) additional influencing factors, relevant for thick components, such as depth position, orientation and part geometry, were included. Furthermore, the variation of ultrasonic attenuation due to various material properties was included.
The variety of risks present during the application of mechanised non-destructive testing (NDT) methods for the final disposal of spent nuclear fuel has not been investigated. Therefore, a need exists to identify these risks and find ways to prevent them. The Failure Modes and Effects Analysis (FMEA), a widely used risk assessment technique, was used to achieve this goal.
One of the aims of considering human factors in the reliability of non-destructive testing (NDT) – for the purposes of the disposal of spent nuclear fuel – is to identify factors that can lead to errors in the completion of the NDT task and to determine how to prevent these errors. The current study is the first to examine mechanised NDT from the human factors perspective. A number of risks were identified and further analysed. Among a number of influencing factors, the NDT inspection procedure was identified as a potential error source and, therefore, was examined in this study. NDT inspection procedures and instructions are, without question, some of the most important tools in the everyday life of an NDT inspector. Experience and research have shown that NDT procedures and instructions, despite being written according to requirements and by certified personnel, are not always used as foreseen and may need to be optimised. The suggested approach for developing and optimising NDT procedures and instructions consists of applying human factors principles by adopting a user-centred approach. The user-centred approach refers to involving users in the process of instruction development by learning from their errors during the data evaluation task and connecting those errors to the shortcomings in the instructions.
The first study assessed the quality of the selected NDT instruction by observing four experienced inspectors during the evaluation of data that were collected with the ultrasonic testing (UT) method while the participants followed the instruction. Through the use of an eye-tracking methodology, the participants’ eye movements across the screen were observed and further analysed. This analysis, together with discussions with the individual users, led to the identification of a number of errors and error sources. Such error identification, combined with theoretical considerations, led to the creation of a new version of the instruction. This new instruction was evaluated using the same method in a follow-up study, resulting in the creation of a third (and final) NDT instruction. Throughout this iterative process, version 4.0 of the instruction was replaced first by version 5.5 and then by version 6.0. As a result of these studies, changes were introduced to the instruction content (e.g. adding missing content) and to the instruction format (e.g. changing the layout, highlighting, presenting the information differently, altering the writing style). The participants reported higher satisfaction with the instruction after the changes were implemented. The main changes included using consistency in writing, highlighting information (e.g. number values, reporting levels, exceptions, reminders), improving navigation throughout the instruction (e.g. through the use of titles and subtitles), and presenting information more uniformly (e.g. all tasks being listed stepwise following the “one action per step” rule).
Considering the benefits of including the user in the development of the NDT instructions and procedures, the main lesson that was learned in this study is that the review process must be carried out through action rather than by solely reading the instructions. This study exposed a number of problems of which the writer and the reviewer were unaware.
After the new instruction was developed, two empirical studies with 20 participants were conducted to evaluate the instruction information by investigating 1) whether the instruction content was understood by the users (the understanding study) and 2) whether the new format supported a more efficient (i.e. less effortful), effective (i.e. more accurate and complete), and satisfying use of the instruction (the usability study). The aim of these studies was to increase the understanding of the factors that contribute to a high-quality NDT instruction.
In the understanding study, the participants were asked to read the NDT instruction and then to answer a number of questions. Based on their answers, specific problems that were related to their understanding of the written content were identified. The results showed that the understanding of the information can be affected by the information order, information organisation, logics and clarity in the writing, and cognitive demands. The study also emphasised the relevance of placing information in a logical order.
The report 'Probability of Defect Detection of Posiva's electron beam weld' describes POD curves of four NDT methods radiographic testing, ultrasonic testing, eddy current testing and visual testing. POD-curves are based on the artificial defects in reference blocks. The results are devoted to the demonstration of suitability of the methods for EB weld testing. Report describes methodology and procedure applied by BAM.
Report creates a link from the assessment of the reliability and inspection performance to the risk assessment process of the canister final disposal project. Report ensures the confirmation of the basic quality of the NDT methods and their capability to describe the quality of the EB-weld.
The probability of detection curves are determined based on the MIL-1823 standard and it's reliability guidelines. The MIL-1823 standard was developed for the determination of integrity of gas turbine engines for the US military.
In the POD-process there are determined as a key parameter for the defect detectability the a90/95 magnitudes, i.e. the size measure a of the defect, for which the lower 95 % confidence band crosses the 90 % POD level. By this way can be confirmed that defects with a size of a90/95 will be detected with 90 % probability. In case the experiment will be repeated 5 % might fall outside this confidence limit.
The use of hydrogen sensors can be categorized into three types
of application:
- Safety monitoring
- Leak detection
- Process control
When applied in one of these areas hydrogen sensors fulfill the
following tasks:
- Indicate a hazardous condition
- Provide warnings or alarms for out-of-limits conditions
- Monitor and control System Operation
- Provide performance data
For the classification, safe handling and use of chemicals, special standardised test methods 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 (round robin tests, interlaboratory comparisons / intercomparisons) are a crucial element of both the further development and improvement of the methods and of a laboratory's quality system. Participation in interlaboratory tests is explicitly recommended by the standard ISO/IEC 17025. This document reports on the results of the interlaboratory test 2012-2013 on the test method EN 14522:2005 “Determination of the auto ignition temperature of gases and vapours“ / IEC 60079-201, part 7 ”Method of test for auto-ignition temperature”. The auto ignition temperature is an important safety characteristic for explosion protection and prevention. It is the basis for classifying substances and explosion protected equipment into temperature classes. Because safety characteristic data are not a pure substance constant but a figure which denotes a special property of the substance, the determination methods are standardised. Currently EN 14522 and IEC 60079-20-1, part 7 are under revision with the aim to combine both to a standard accepted worldwide. An important part of the standard is the laboratory’s verification of their apparatus and procedure. To base this forthcoming standard on reliable and up-to-date verification data an interlaboratory test appears as the method of choice. The verification data given in the recent issues of the standards are based on comparison measurements which date back to a long time ago and did not include automated apparatuses.
The requirement for a metrological infrastructure to ensure the interchangability of 'nonconventional’ energy gases within existing European infrastructure1 was the driving force behind the work undertaken in the three-year EMRP Characterisation of energy gases project EMRP ENG01 (June 2010 - May 2013).
As part of work package one of the project, Standards and methods were used to perform composition and impurity measurements on samples of real energy gases collected from around Europe. The aim of this study was to compare the results obtained from different labs, and thereby provide an evaluation of the labs’ capabilities and provide insight into the feasibility of different analytical methodologies for use with future measurements.
For the classification and safe handling and use of the chemicals, special standardized testing proce-dures have been developed and are used world-wide. Safety experts must be able to fully rely on the precise execution of the respective laboratory tests and assessments. 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 2010/2011 on the test method DIN EN 15188:2007 “Determination of the spontaneous ignition behaviour of dust accumulations” [1] which was organized by the Center for Quality Assurance for Testing of Dangerous Goods and Haz-ardous Substances.
The test method DIN EN 15188:2007 is applied to characterize the self-ignition behaviour of combus-tible dusts. The experimental basis for describing the self-ignition behaviour of a given dust is the de-termination 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 availa-ble ovens. The results thus measured reflect the dependence of self-ignition temperatures upon dust volume [1].
Several internal investigations and interlaboratory comparisons in the past have shown significant differences between the lab-specific results of hot storage tests.
Figure 2-1 shows the Pseudo-Arrhenius plot of hot storage tests of eight different laboratories (Round Robin Test 2002, BAM). The dust under this investigation was Lycopodium powder (spores). The par-ticipants of this interlaboratory test used different laboratory ovens (size, ventilation) as well as differ-ent sample baskets (shape, mesh size, single- and double-walled).
Figure 2-1 shows clearly that this test failed to produce reasonable reproducibility of the TSI between the different laboratories. As possible reasons for the deviations have been identified lab-specific dif-ferences, e.g.:
- oven ventilation (enforced, natural convection),
- oven size,
- sample baskets,
- radiation effects,
- measuring precision (temperature difference between tests with ignition and no ignition),
- minimum sample size.
To reduce the differences between the labs it was necessary to ameliorate the testing method and to improve the execution of the method by the lab. From there, the installation of an inner chamber into the laboratory oven was suggested as experimental set-up in EN 15188:2007 to provide more repro-ducible test conditions. The aappropriateness of this set-up has not been verified yet.
The current interlaboratory test 2010-2011 focuses on the use of a special mesh wire screen and spe-cial volumes of the sample baskets (cubes) to normalise/harmonise the test conditions in the different labs. In preparation for the interlaboratory test a joint program between Syngenta and BAM has been initiated in 2009. As a result of these investigations a modified set-up ( chapter 3) has been identi-fied to be probably more appropriate than the suggested set-up in DIN EN-15188:2007.
Due to the time-consuming test procedure and to optimize the workflow for the laboratories this in-terlaboratory test should be performed stepwise as a multi-level test ( chapter 5.4) on one typical test sample.
NM 105, Ti02 (P25) could not be ignited as dust layer and dispersed in air as dust/air-mixture as well. This dust is not dust explosible and the burning behaviour corresponds to Burning Class 1 (no Ignition). The results have shown that the tested sample is thus not combustible at all, because it is already oxidized completely.
Anwendungen von Bioziden in Materialien für Außenanwendungen sind mögliche Quellen für Biozide in Umweltkompartimenten infolge von witterungsbedingten Auswaschprozessen. Im Bericht werden Leachingprozesse und -parameter als auch Methoden zu deren Untersuchung unter Labor- und Freilandversuchsbedingungen beschrieben. Vorteile und Grenzen der verschiedenen Herangehensweisen zur Untersuchung von Leachingprozessen werden diskutiert. Standardisierte Auswaschtests sowie in der Fachliteratur publizierte Auswaschexperimente werden zusammenfassend dargestellt. Es wird beschrieben, wie Leachingdaten gemäß Technischem Leitfaden zur Biozidprodukten-Richtlinie 98/8/EG für eine Risikobewertung genutzt werden. Ein alternativer Ansatz zur mathematischen Modellierung von Leachingtest-Daten wurde erprobt und wird im Bericht erläutert. Potentiell lassen sich mit dem vorgeschlagenen Ansatz bestimmte gegenwärtig auftretende Schwierigkeiten bei der Risikobewertung umgehen.
Applications of biocides in outdoor materials are potential sources of biocides in environmental compartments due to leaching processes under weathering conditions. Leaching processes and parameters as well as methods to investigate leaching processes under laboratory and semi-field conditons are described in the report. Benefits and limitations of different test approaches are discussed. Standardised leaching tests as well as leaching experiments reported in scientific literature are listed. The application of leaching data for risk assessments according to the Technical Guidance Documents for the Biocidal Products Directive (98/8/EC) is described. An alternative approach for mathematical modelling of leaching data was tested and is Explained in the report. Certain difficulties that currently appear during risk assessments may be circumvented by the proposed approach.
Within the framework of the research project promoted by the Saxon Ministry of State for Environment and Agriculture (SMUL) (Reference: 13-8802.3521140), on April 27, 1999 a test was conducted on the BAM test premises in Horstwalde, administrative district Teltow-Fläming, in the Federal State of Brandenburg, during the course of which a 45 m³ railway tank car filled approximately 22% with liquefied petroleum gas was subjected to a fire test in which the railway tank car failed 17 minutes after commencement of the test (15 minutes after the fire had formed) (BAM Test Report No. III.2/9907 dated 30.06.1999).
Due to the uniqueness of such a test, which to the knowledge of the authors had never before been performed in this manner in Germany or in Europe as a whole, the Saxon State Ministry agreed to provide in addition to the railway tank car a Castor of the type THTR/AVR (without this having been part of the original project), which was also to be subjected to a fire. This report only deals with the test results of the Castor container where they are relevant to the overall project.
A detailed evaluation of the effects on the Castor container will be carried out by the BAM (Specialist Group III.3 "Safety of tanks for transport and storage").
SMT4-CT98-2238 - A certified reference material for the scratch test - REMAST - Synthesis report
(2002)
Emissions from building products can considerably impair the quality of indoor air. The AgBB scheme is employed to evaluate the emissions of volatile organic compounds (VOC) from building products. The hygienic evaluation according to the AgBB scheme requires product-specific measuring procedures.
These are available for a range of products. They have been validated in co-operation with several research and testing institutes and have been included in the criteria for awarding the Blue Angel ecolabel.
The evaluation is, however, stricter and generally has lower limits. VOC emissions and odours can cause health problems so testing using sensors is an important element in the evaluation of building products and has – for reasons of precaution – been set down in the AgBB scheme. The main goal of the project was to derive a method of evaluation using sensors and limits for awarding the Blue Angel and for the AgBB scheme. Based on the research conducted (see Chapter 5 Results and Discussion), perceived intensity and hedonics were suggested as a suitable Evaluation method. The derivation of limits for the evaluation using sensors on the 28th day was effected in the present study through the additional questioning of the test subjects on the reasonability of a sample.
For the Blue Angel, there could be different limits of perceived intensity and hedonics for each group of products. A preliminary suggestion for possible limits – for all product groups – is a perceived intensity of 7 pi (5 pi + 2 pi as confidence coefficient, Chapter 5.1.5) and -1 (0+/-0.8, rounded to -1) for the hedonic value.
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 2007 on the method UN Test N.5 “Test method for substances which in contact with water emit flammable gases” [1] / EC A.12 “Flammability (contact with water)” [2] which was organized by the Center for Quality Assurance for Testing of Dangerous Goods and Hazardous Substances.
In dependence on the chemical structure and/or the physical form and state (e.g. particle size) substances or mixtures may be able to react with water (even water damp / air humidity) under normal ambient temperature conditions. Sometimes this reaction can be violent and/or with significant generation of heat. Especially if gases are evolved this reaction may become dangerous. In addition, it is important to know whether a substance emits flammable gases due to contact with water because
special precautions are necessary especially with regard to explosion protection. The methods UN Test N.5 and EC A.12 are applied to characterize chemical substances or mixtures which in contact with water emit flammable gases. To differentiate between chemicals with these properties and chemicals which are not classified as hazardous / dangerous, the substance’s gas evolution rate is determined and compared to the classification criteria(s) in the last step of the test
method. In the methods UN Test N.5 / EC A.12 no special laboratory apparatus / measuring technique to determine gas evolving flow is required. However, practical experience shows that the testing procedure for substances and mixtures which in contact with water emit flammable gases is sensitive to a number of influencing factors. Since the methods (UN N.5 / EC A.12) 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.
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.
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.