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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.
Thermoelectric generator (TEG) has been proved as a promising technology for directly converting heat into electricity based on Seebeck effect. On the contrary, this electricity can trigger a solid-state cooling based on conventional Peltier effect. However, these two effects induce a coupling between heat and electric flux, especially for the quantitative relationship still remaining a mystery. Here, we show experimental evidence and theoretical calculation for the coupling by monitoring transient response of fluid temperature and output power. The experimental maximum heat flow in open circuit is 1162 W at cold fluid flow rate = 0.3 m3/h and fluid temperature difference ΔTf = 70 °C, enhanced by 13% owing to heat compensation from intrinsic coupling in closed-loop circuit. Meanwhile, the measured maximum output power of TEG is 18.2 W, and subsequently decreases to 15.4 W due to the objective existence of coupling. This double-edged sword in coupling vigorously inspires the potential applications in heat-dissipation situation such as spacecraft, electronic components, photovoltaic, refrigerator and etc. Present findings open a novel avenue for manipulating heat-electricity conversion in practical engineering.
The topographic effect of steel counterface, finished by mechanical grinding with Ra ranging from 0.01 to 0.95 µm, on the structure and functionality of the tribofilm of a hybrid nanocomposite, i.e. epoxy matrix filled with monodisperse silica nanoparticles, carbon fibers and graphite, was systematically investigated. The nanostructure of the tribofilm was comprehensively characterized by using combined focused ion beam and transmission electron microscope analyses. It was identified that oxidation of the steel surface, release, compaction and tribosintering of silica nanoparticles and deposition of an epoxy-like degradation product as well as fragmentation of carbon fibers are main mechanisms determining the structure and functionality of the tribofilm. The size of roughness grooves determines the type and size class of wear particles to be trapped at the surface. An optimum groove size leading to a maximum of surface coverage with a nanostructured tribofilm formed mainly from released silica nanoparticles was identified.
Exploring the influence of counterpart materials on tribological behaviors of epoxy composites
(2016)
The dependence of the friction and wear of epoxy (EP) composites materials on counterpart materials, such as standard bearing steel, medium carbon steel and chrome-plating (Cr), was investigated. The conventional composite filled with short carbon fiber (SCF) and graphite shows the highest tribological performance when rubbing against Cr, whereas, the hybrid nanocomposite (EP filled with SCF, graphite and silica nanoparticles) exhibits the lowest friction and wear when sliding against the standard bearing steel. The role of nanoparticles in the tribological performance is distinctly different when sliding against with various counterpart materials. It is demonstrated that counterpart materials exert an important influence on material transfer, tribo-oxidation and mechanical mixing of wear products, resulting in the different formation mechanisms of transfer film.
The composition and nanostructure of a beneficial tribofilm formed during sliding of a hybrid nanocomposite against steel were characterized comprehensively. A similar nanostructure was produced by high energy ball milling of the three identified tribofilm constituents: silica, hematite and graphite. By supplying powders to a pin-on-disc test it has been shown that neither silica, nor hematite, nor a mixture of both provide the low coefficient of friction (COF) observed for the hybrid composite. Only if graphite was blended with the oxides, the low COF was obtained. Thus, a film of finely dispersed stable inorganic wear products containing 15 vol% graphite provides low friction and wear in the considered case.
We applied a combination of Raman spectroscopy (RS) and cross-sectional transmission electron microscopy (X-TEM) to identify silicone oil residues and tribofilms at steel disc surfaces after tribological testing. Neither chemical cleaning nor mechanical removal of a 50 µm thick surface layer produced a surface without any silicone residue. Nevertheless, long-term tribological properties are not affected due to silicone degradation which has been proved by Raman spectroscopy. Excellent anti-wear and anti-friction properties of a nanocomposite at severe stressing conditions correlated with the formation of a silica-based tribofilm containing amorphous and graphite-like carbon nanoparticles. Since reliable carbon quantification by analytical TEM is difficult, RS is a useful complementary method for carbon identification at wear scars.
The effect of steel counterface topography on the formation mechanisms of nanostructured tribofilms of polyetheretherketone (PEEK) hybrid nanocomposites was studied. Three types of surface finishes with mean roughness Ra ranging from nano- to micro-scale were investigated. Tribo-sintering of nanopartides, oxidation of counterface steel and compaction of wear debris are identified to be competing factors dominating the formation and function of the tribofilms. Counterface topography played an important role on the competing factors, and thereby influenced significantly the final structure, the load-carrying capability and the lubrication performance of the tribofilms. It was disclosed that a thin tribofilm, which mainly consists of silica nanoparticles and which forms on the counterface with a submicron roughness, benefits best the tribological performance of the composites
The comparison required the assignment of the mass fraction of folic acid present as the main component in the comparison sample. Performance in the comparison is representative of a laboratory's measurement capability for the purity assignment of organic compounds of medium structural complexity [molecular weight range 300–500] and high polarity (pKOW < −2).
Methods used by the eighteen participating NMIs or DIs were based on a mass balance (summation of impurities) or qNMR approach, or the combination of data obtained using both methods. The qNMR results tended to give slightly lower values for the content of folic acid, albeit with larger associated uncertainties, compared with the results obtained by mass balance procedures. Possible reasons for this divergence are discussed in the report, without reaching a definitive conclusion as to their origin.
The comparison demonstrates that for a structurally complex polar organic compound containing a high water content and presenting a number of additional analytical challenges, the assignment of the mass fraction content property value of the main component can reasonably be achieved with an associated relative standard uncertainty in the assigned value of 0.5%
The method of movable cellular automata (MCA) was applied to simulate the stress-strain behavior of a nano composite consisting of an epoxy matrix and 6 vol. % silica nano particles. The size of the elements used for modelling was fixed at 10 nm, corresponding approximately to the diameter of the filler particles. Since not only the stress-strain response of the two constituents but also debonding of neighboring particles and granular flow was taken into account, plastic deformation as well as crack initiation and propagation could be simulated with the model. Modelling results were compared with tensile test results of both, pure epoxy as well as the epoxy-6 vol. % SiO2 composite. Since assuming bulk properties of the two constituents did not yield satisfactory results, slight modifications of the nanoparticle response functions and nanostructures were tested numerically. Finally, it was observed that only the assumption of slightly increased strength properties of the epoxy yielded good correlation between experimental and modelling results. This was attributed to an increased cross linking of the epoxy caused by the presence of silica nano particles.