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Supplementary comparison study - measurement capabilities for the quantification of ethanol in water
(2022)
The accurate quantification of ethanol in water is essential for forensic applications such as blood and breath alcohol testing and for commercial applications such as the assessment of alcoholic beverages.
The intercomparison EURAMET.QM-S14 is part of a capacity building project named ALCOREF “Certified forensic alcohol reference materials”
that is running within the European Metrology Programme for Innovation and Research (EMPIR). The intercomparison should allow project partners and other interested National Metrology Institutes (NMIs) and Designated Institutes (DIs) to benchmark their analytical methods for the quantification of ethanol in water. The study plan was agreed by the European Association of National Metrology Institutes (EURAMET) Subcommittee Bio- and Organic Analysis (SCBOA) and the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) in February and April 2019, respectively. The intercomparison was coordinated by BAM. Two concentration levels relevant for the calibration and verification of evidential breath alcohol analysers were distributed to study participants. Fifteen institutes from 15 countries registered for the intercomparison and returned results. Participants mostly applied gas chromatography with flame ionisation detection (GC-FID) or mass spectroscopy (GC-MS), one participant used titrimetry and one participant employed a test bench for breath analyser calibration (“bubble train”). Participants did either in-house purity assessment of their commercial ethanol calibrants by Karl-Fischer titration, chromatographic methods, quantitative nuclear magnetic resonance spectroscopy (qNMR) and/or density measurements; or they used ethanol/water Certified Reference Materials (CRMs) from NMIs/DIs for calibration.
CCQM OAWG agreed to use a consensus value from participants results that utilizes the reported uncertainties as Key Comparison Reference Value (KCRV). The Gaussian Random effects model with Hierarchical Bayesian solution (HB-REM) is a reasonable approach in this case. The KCRVs and Degrees of Equivalence (DoEs) were calculated with the NIST consensus builder version 1.2 Hierarchical Bayes procedure.
Successful participation in the interlaboratory comparison has demonstrated the capabilities in determining the mass fraction of ethanol in aqueous matrices in the range 0.1 mg/g to 8 mg/g. Fourteen out of 15 participants have successfully quantified both samples, one participant successfully quantified only the lower-level (0.6 mg/g) sample.
Objectives: Using a murine model of multiple sclerosis, we previously showed that repeated administration of gadopentetate dimeglumine led to retention of gadolinium (Gd) within cerebellar structures and that this process was enhanced with inflammation. This study aimed to compare the kinetics and retention profiles of Gd in inflamed and healthy brains after application of the macrocyclic Gd-based contrast agent (GBCA) gadobutrol or the linear GBCA gadopentetate. Moreover, potential Gd-induced neurotoxicity was investigated in living hippocampal slices ex vivo.
Materials and Methods: Mice at peak of experimental autoimmune encephalomyelitis (EAE; n = 29) and healthy control mice (HC; n = 24) were exposed to a cumulative dose of 20 mmol/kg bodyweight of either gadopentetate dimeglumine or gadobutrol (8 injections of 2.5 mmol/kg over 10 days). Magnetic resonance imaging (7 T) was performed at baseline as well as at day 1, 10, and 40 post final injection (pfi) of GBCAs. Mice were sacrificed after magnetic resonance imaging and brain and blood Gd content was assessed by laser ablation-inductively coupled plasma (ICP)-mass spectrometry (MS) and ICP-MS, respectively. In addition, using chronic organotypic hippocampal slice cultures, Gd-induced neurotoxicity was addressed in living brain tissue ex vivo, both under control or inflammatory (tumor necrosis factor α [TNF-α] at 50 ng/μL) conditions.
Results: Neuroinflammation promoted a significant decrease in T1 relaxation times after multiple injections of both GBCAs as shown by quantitative T1 mapping of EAE brains compared with HC. This corresponded to higher Gd retention within the EAE brains at 1, 10, and 40 days pfi as determined by laser ablation-ICP-MS. In inflamed cerebellum, in particular in the deep cerebellar nuclei (CN), elevated Gd retention was observed until day 40 after last gadopentetate application (CN: EAE vs HC, 55.06 ± 0.16 μM vs 30.44 ± 4.43 μM). In contrast, gadobutrol application led to a rather diffuse Gd content in the inflamed brains, which strongly diminished until day 40 (CN: EAE vs HC, 0.38 ± 0.08 μM vs 0.17 ± 0.03 μM). The analysis of cytotoxic effects of both GBCAs using living brain tissue revealed an elevated cell death rate after incubation with gadopentetate but not gadobutrol at 50 mM. The cytotoxic effect due to gadopentetate increased in the presence of the inflammatory mediator TNF-α (with vs without TNF-α, 3.15% ± 1.18% vs 2.17% ± 1.14%; P = 0.0345).
Conclusions: In the EAE model, neuroinflammation promoted increased Gd retention in the brain for both GBCAs. Whereas in the inflamed brains, efficient clearance of macrocyclic gadobutrol during the investigated time period was observed, the Gd retention after application of linear gadopentetate persisted over the entire observational period. Gadopentetate but not gadubutrol appeared to be neurotoxic in an ex vivo paradigm of neuronal inflammation.
The paper presents a comparison between two different numerical modelling approaches aimed to simulate the in-plain behaviour of rammed earth walls, namely under axial, diagonal and cyclic shearcompression loading. In the first part of the study the mechanical characterisation of wallets tested under uniaxial compression and diagonal compression and walls tested under in-plane cyclic shear-compression loading is presented. The results were used to implement and validate the finite element simulations.
The numerical modelling of the rammed earth samples tested is then discussed in the second part. A non-linear constitutive law based on the total strain rotating crack model (TSRCM) was employed as implemented in the DIANA® software. The aim of the numerical analyses presented here is to simulate the behaviour of rammed earth under different inplane loading conditions. For the wallets, tests under static loading both macro- and micro-modelling
approaches were considered for the simulation of the experimental tests. For the walls subjected to cyclic loading only the micro-modelling approach was applied for the simulation of the experimental tests.
The respective FEM model was calibrated with the experimental results. The rammed earth layers were represented by continuum elements, the contact surfaces between layers by interface elements. This approach allowed assessing the influence of the apparent weakness of the interfaces between layers on the shear behaviour of rammed earth.
The goal of the numerical simulation of the cyclic tests was to establish the adequacy of common analytical methods (e. g. used for masonry) applied to the analysis of rammed earth. Rammed earth exhibits brittle characteristics similar to masonry materials and is used in geometrical typologies, such as walls, common in masonry construction.
Der Beitrag präsentiert einen Vergleich zwischen verschiedenen numerischen Modellierungsansätzen die dazu dienen sollen, das flächige Verhalten von Stampflehmwänden, genauer unter axialer, diagonaler und zyklischer Scherkraftbelastung zu simulieren.
Im ersten Teil der Studie werden die mechanischen Eigenschaften der Wandscheiben, die unter einachsiger und diagonaler Druckbelastung getestet wurde und der Wände, die in flächigen, zyklischen Scherkraftbelastung getestet wurden, dargestellt. Die Ergebnisse werden verwendet, um die Finite Elemente Simulation anzuwenden und zu bewerten. Die numerische Modellierung der getesteten Stampflehmproben
wird dann im zweiten Teil diskutiert. Ein nichtlineares Materialgesetz basierend auf dem Gesamtdehnungsrissmodell (total strain rotating crack model – TSRCM) wurde, wie durch die Software DIANA® verwendet, angesetzt. Ziel dieser hier präsentierten numerischen Analyse ist es, das Verhalten von Stampflehm unter verschiedenen Lasteinflüssen
zu simulieren. Für die Wandscheiben wurden Versuche unter linearer Last, sowohl in Makro- als auch Mikromodellansätze für die Simulation der experimentellen Versuche gewählt. Für die Wände, welche zyklischer Belastung ausgesetzt waren, wurden nur die Mikromodellansätze für die Simulation der experimentellen Versuche gewählt. Das betreffende FEM Modell wurde mit den experimentellen Ergebnissen kalibriert. Die Stampflehmlagen wurden mit durchgehenden Elementen, die Kontaktflächen zwischen den Lagen mit Oberflächenelementen repräsentiert.
Dieser Ansatz erlaubte die Bewertung des Einflusses der auftretenden Schwächung in den Oberflächen zwischen den Lagen auf das Scherverhalten des Stampflehms. Ziel der numerischen Simulation von zyklischen Versuchen war es, die Eignung allgemeiner Analysemethoden (z. B. für Mauerwerk) für die Analyse von Stampflehm einzuführen und anzuwenden. Stampflehm zeigt brüchige Eigenschaften vergleichbar zu Mauerwerksbaustoffen und wird in geometrischen Formen, wie Wänden, genutzt, die im Mauerwerk üblich sind.
The paper presents the results of a series of combined mechanical and in-situ morphological investigations on highstrength strain-hardening cement-based Composites (SHCC). Tension and compression experiments were performed in a CT scanner employing a dedicated mechanical testing rig. The in-situ microtomographic scans enabled correlating the measured specimen response with relevant microstructural features and fracture processes. The microstructural segmentation of SHCC was performed in the framework of Deep Learning and it targeted an accurate segmentation of pores, fibers and aggregates. Besides their accurate volumetric representation, these phases were quantified in terms of content, size and orientation. The fracture processes were monitored at different loading stages and Digital Volume Correlation (DVC) was employed to spatially map the strains and cracks in the specimens loaded in compression. The DVC analysis highlighted the effect of loading conditions, specimen geometry and material heterogeneity at the mesolevel on the strain distribution and fracture localization.
The aim of this paper is to implement a numerical model to reproduce the nonlinear behavior of cob walls under shear loading.
Axial compression, pull-off, and diagonal compression tests were carried out to derive the mechanical parameters. In addition, the stressstrain relationships, the nonlinear behavior, and the failure modes were defined. The experimental results were then used to calibrate a finiteelement model. The material behavior was simulated through a macromodeling approach adopting the total strain rotating crack model.
A sensitivity analysis was conducted to assess the effects of varying the parameters with higher uncertainty on the structural behavior.
The numerical model achieved good correspondence with the experimental results in terms of simulation of the shear stress–shear strain relationship and of damage pattern.
The paper presents a comparison between different numerical modelling approaches aiming to simulate the in-plain behaviour of three types of earthen materials, namely adobe masonry, rammed earth and cob. For this purpose, uniaxial and diagonal compression tests were carried out, which allowed determining important mechanical parameters, such as compressive strength, Young’s modulus, Poisson’s ratio, shear strength and shear modulus. Furthermore, the tests allowed assessing the level of non-linear behaviour of the respective stress–strain relationships as well as the failure modes. The experimental results were then used for the calibration of numerical models (based on the finite element method) for simulating the non-linear behaviour of the earth materials under in-plane shear loading. Both macro- and micro-modelling approaches were considered for this purpose. The procedures adopted for model calibration established the reliability of various modelling strategies for the different loading conditions. The simplified Approach based on macromodelling shows a satisfactory accuracy and low computational costs. The results reproducing the uniaxial compression are in good correspondence with the post-elastic behaviour observed in the experimental campaign. The micro-modelling approach adopted to reproduce the shear behaviour, even with higher computational cost, represents a suitable tool to predict the adobe masonry and rammed earth collapse mechanisms.
The paper presents an experimental program aiming at assessing the mechanical performance of rammed earth walls, namely under compression and shear loading. Axial compression and diagonal compression tests were carried out for this purpose, which allowed determining important mechanical parameters, such as compressive strength, Young's modulus, Poisson's ratio, shear strength and shear modulus. Furthermore, it allowed assessing the level of non-linear behaviour of the respective stress–strain relationships as well as the failure modes. The experimental results were then used in the calibration of numerical models (finite element method) for simulating the non-linear behaviour of rammed earth under shear loading. Both macro- and micro modelling approaches were considered for this purpose. The total strain rotating crack model was used to simulate the behaviour of the rammed earth material, while the Mohr–Coulomb failure criterion was used to simulate the behaviour of interfaces between layers. In general, the numerical models achieved good agreement with the experimental results, but uncertainties related to the definition of the input parameters required to perform a sensitivity analysis. The compressive strength, the Poisson's ratio, the tensile strength and the tensile fracture energy revealed to be the most important parameters in the analyses.
The aim of this work is to evaluate the feasibility of the direct radiography on weld
inspection in oil pipelines and gas pipeline during the manufacturing process. To that, 6 specimens
with 6 different thickness and varied height of reinforced weld with 5 different kinds of defects
were made. All samples were radiographied using Class I films and flat panel. For all specimens the
inspection length was 8''. Thus, with the flat panel the detector-to-object distance varied so that it
may adequate to several diameters of the tubes.
The detector-to-object distance was calculated based on the physical size of the detector
taking into consideration a safe distance between the tube curvature and the flat panel extremities,
keeping the lowest possible magnification factor so that it could be obtained the length of the
inspection. Images with 6 integration time for each experimental arrangement were obtained.
The images obtained with the Flat Panel/YXLON system were analyzed according to their
quality by using the Contrast parameters (essential wire) (DNV 2007/ IS0 12096 with
reinforcement and ISO 10893-7 basis material), Basic Spatial Resolution BSR (ISO 10893-7)
and normalized signal-to-noise ratio - SNRN (ISO 10893-7) and by detectability using as reference
the conventional radiography.
The results showed that for all thickness, the exposure time used to meet the image quality
requirements were below with direct radiography. However the BSR were not reached for thickness
of 4.85, 6.40 and 9.67 mm, therefore the compensation principle established by ISO 10893-7 was
considered, that is, one more contrast wire for a less wire pair.
The digital technique proved to be more sensitive to real defects found on welds than the
conventional technique. Then it can be conclude that the digital radiography utilizing the flat panel
can be applicable to the oil and gas segment with advantages over conventional technique as to
quality aspects, productivity, environment, safety and health.
The intensive use of earth as a building material since ancient times resulted in an important and significant earthen built heritage currently existing worldwide spread. The rammed earth technique has a significant presence in this heritage, where it served to build from simple dwell-ings to fortresses. However, the high vulnerability of rammed earth constructions to decay agents and to seismic events puts in risk their further existence and the lives of millions of peo-ple. With respect to the seismic behaviour of rammed earth walls, the understanding and mod-elling of their shear behaviour are topics underdeveloped in the bibliography. Nevertheless, these topics are of extreme importance in the preservation and strengthening of rammed earth constructions. Therefore, this paper presents a numerical work aiming at modelling the non-linear behaviour of unstabilised rammed earth under shear loading, resorting to the finite ele-ments method (FEM). The models were used to simulate the behaviour of a set of rammed earth wallets tested under diagonal compression. Both macro- and micro-modelling approach-es were considered, where the objective of this last approach was to evaluate the influence of apparent weakness of the interfaces between layers on the shear behaviour. The total strain ro-tating crack model (TSCRM) was used to simulate the behaviour of the rammed earth material, while the Mohr-Coulomb failure criterion was used to simulate the behaviour of interfaces be-tween layers. Furthermore, uncertainties related to the definition of the input parameters re-quired performing a sensitivity analysis. The numerical models achieved good agreement with the experimental results and the compressive strength, the Poisson’s ratio, the tensile strength and the tensile fracture energy revealed to be the most important parameters in the analyses.