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- Friction stir welding (3)
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- Albumin (1)
- Axial force (1)
- BSA (1)
- Bisphenol-A (1)
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Organisationseinheit der BAM
KEY COMPARISON
Under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a key comparison, CCQM K55.c, was coordinated by the Bureau International des Poids et Mesures (BIPM) in 2012. Twenty National Measurement Institutes or Designated Institutes and the BIPM participated. Participants were required to assign the mass fraction of valine present as the main component in the comparison sample for CCQM-K55.c. The comparison samples were prepared from analytical grade L-valine purchased from a commercial supplier and used as provided without further treatment or purification.
Valine was selected to be representative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of low structural complexity [molecular weight range 100300] and high polarity (pKOW > –2).
The KCRV for the valine content of the material was 992.0 mg/g with a combined standard uncertainty of 0.3 mg/g. The key comparison reference value (KCRV) was assigned by combination of KCRVs assigned from participant results for each orthogonal impurity class. The relative expanded uncertainties reported by laboratories having results consistent with the KCRV ranged from 1 mg/g to 6 mg/g when using mass balance based approaches alone, 2 mg/g to 7 mg/g using quantitative 1H NMR (qNMR) based approaches and from 1 mg/g to 2.5 mg/g when a result obtained by a mass balance method was combined with a separate qNMR result.
The material provided several analytical challenges. In addition to the need to identify and quantify various related amino acid impurities including leucine, isoleucine, alanine and a-amino butyrate, care was required to select appropriate conditions for performing Karl Fischer titration assay for water content to avoid bias due to in situ formation of water by self-condensation under the assay conditions. It also proved to be a challenging compound for purity assignment by qNMR techniques.
There was overall excellent agreement between participants in the identification and the quantification of the total and individual related structure impurities, water content, residual solvent and total non-volatile content of the sample. Appropriate technical justifications were developed to rationalise observed discrepancies in the limited cases where methodology differences led to inconsistent results.
The comparison demonstrated that to perform a qNMR purity assignment the selection of appropriate parameters and an understanding of their potential influence on the assigned value is critical for reliable implementation of the method, particularly when one or more of the peaks to be quantified consist of complex multiplet signals.
The allergenic potential of airborne proteins may be enhanced via post-translational modification induced by air pollutants like ozone (O3) and nitrogen dioxide (NO2). The molecular mechanisms and kinetics of the chemical modifications that enhance the allergenicity of proteins, however, are still not fully understood. Here, protein tyrosine nitration and oligomerization upon simultaneous exposure of O3 and NO2 were studied in coated-wall flow-tube and bulk solution experiments under varying atmospherically relevant conditions (5–200 ppb O3, 5–200 ppb NO2, 45–96% RH), using bovine serum albumin as a model protein. Generally, more tyrosine residues were found to react via the nitration pathway than via the oligomerization pathway. Depending on reaction conditions, oligomer mass fractions and nitration degrees were in the ranges of 2.5–25% and 0.5–7%, respectively. The experimental results were well reproduced by the kinetic multilayer model of aerosol surface and bulk chemistry (KM-SUB). The extent of nitration and oligomerization strongly depends on relative humidity (RH) due to moisture-induced phase transition of proteins, highlighting the importance of cloud processing conditions for accelerated protein chemistry. Dimeric and nitrated species were major products in the liquid phase, while protein oligomerization was observed to a greater extent for the solid and semi-solid phase states of proteins. Our results show that the rate of both processes was sensitive towards ambient ozone concentration but rather insensitive towards different NO2 levels. An increase of tropospheric ozone concentrations in the Anthropocene may thus promote pro-allergic protein modifications and contribute to the observed increase of allergies over the past decades.
The CCQM-K148.a comparison was coordinated by the BIPM on behalf of the CCQM Organic Analysis Working Group for NMIs and DIs which provide measurement services in organic analysis under the CIPM MRA. It was undertaken as a "Track A" comparison within the OAWG strategic plan. CCQM-K148.a demonstrates capabilities for assigning the mass fraction content of a solid organic compound having moderate molecular complexity, where the compound has a molar mass in the range (75 - 500) g/mol and is non-polar (pKow < −2), when present as the primary organic component in a neat organic solid and where the mass fraction content of the primary component in the material is in excess of 950 mg/g.
Participants were required to report the mass fraction of Bisphenol A present in one supplied unit of the comparison material. Participants using a mass balance method for the assignment were also required to report their assignments of the impurity components present in the material. Methods used by the seventeen participating NMIs or DIs were predominantly based on either stand-alone mass balance (summation of impurities) or qNMR approaches, or the combination of data obtained using both methods. The results obtained using thermal methods based on freezing-point depression methods were also reported by a limited number of participants. There was excellent agreement between assignments obtained using all three approaches to assign the BPA content.
The assignment of the values for the mass fraction content of BPA consistent with the KCRV was achieved by most of the comparison participants with an associated relative standard uncertainty in the assigned value in the range (0.1 - 0.5)%.
Simultaneous measurement of tool torque, traverse force and axial force in friction stir welding
(2013)
Simultaneous measurement of the tool torque, traverse force and axial force during friction stir welding process is of great significance to the understanding of the underlying process mechanism and the optimizing of the process parameters. Different from the traditional measurement methods using load cell or rotating component dynamometer, an indirect but economical methodology is used in this study for the simultaneous measurement of the traverse force, axial force and tool torque by monitoring the output torques of the servo motors and main spindle three-phase AC induction motor inside the FSW machine. The values of the traverse force, axial force and tool torque are determined under different welding conditions, and the influencing factors are examined. The measured results in friction stir welding of AA2024-T4 aluminum alloys at different combinations of tool rotation speed and welding speed lay foundation for process optimization.
The accurate prediction of the thermal energy generation and distribution in friction stir welding process is of great significance for the optimization of the process parameters and the understanding of the underlying mechanisms. In this study, a new method of integrative calculation and measurement is proposed to obtain the more reasonable values of the frictional coefficient and the slip rate, which are both used to characterize the heat generation rate at the tool-workpiece contact interfaces. A three-dimensional model is established to fully couple the energy generation, heat transfer and material flow in friction stir welding of aluminum alloys. The energy produced by both interfacial friction and plastic deformation are taken into consideration. The analysis accuracy of the thermal energy generation and distribution is improved, and the distribution features of thermal energy density in the vicinity of the tool are elucidated. The predicted peak temperature values at some locations are in agreement with the experimentally measured ones.
Understanding the influence of tool/pin shapes on the thermal and material flow behaviors in friction stir welding is of great significance for the optimal design of tool/pin based on a scientific principle. In this study, a numerical method based on computational fluid dynamics is employed to quantitatively analyze the thermo-physical phenomena in friction stir welding with two tools of different pin shapes (axisymmetrical conical tool and asymmetrical triflat tool). Through combining a steady state model with a transient state model, both the computation efficiency and accuracy are ensured. The boundary conditions of heat transfer and material flow are determined with considering a partial sticking/sliding contact condition at the toolworkpiece interface. The total heat generation, heat density and temperature distribution during the welding process with triflat tool are elucidated and compared with that of conical tool, and the material flow patterns and deformation regions of various pin orientations are illustrated in detail. It is found that the deformation zone caused by triflat tool is larger than that by conical tool, which is validated by the weld macrographs. The computed thermal cycles and peak temperature values at some locations are in good agreement with the experimentally measured ones.
Magnesium (Mg) alloys have attracted much attention due to their merits of meeting requirements of lightweight, energy-efficient and environmental friendly engineering. In this study, a modified refill friction stir spot welding (refill-FSSW) method is proposed to weid AMSO Mg alloy, in which pin and sleeve rotate at different states. Effects of process parameters on the microstructure, material flow, and mechanical properties of welds were studied. Results showed that, the modified refill-FSSW technology could enhance the intennixing of material by changing the flow state. Lap shear strength of welds could be significantly improved with changed failure modes. The modified refill FSSW technology is a competitive welding method for Mg alloy.