Well-established Analytical Methods Research Articles

A Sensitivity Matrix-Based Temperature-Augmented Probabilistic Load Flow Study

This paper proposes a hybrid method for probabilistic load flow (PLF) study to analyze the influence of uncertain photovoltaic generations and load demands on transmission system performance. Besides, the paper focuses on accurate approximation of multimodal distributions of result variables in a temperature-augmented PLF model without using any series expansion methods. The effect of uncertain ambient temperature on result variables is discussed. Multiple correlation cases between the input bus powers are considered. The performance of the proposed method is investigated on modified New England 39-bus power system. The results are compared with four well-established analytical methods and Monte Carlo simulation. The effect of multiple input correlations on probability distributions of result variables is analyzed.

A powerful tool for assessing distribution and fate of potentially toxic metals (PTMs) in soils: integration of laser ablation spectrometry (LA-ICP-MS) on thin sections with soil micromorphology and geochemistry.

The dynamic behavior and inherent spatial heterogeneity, at different hierarchic levels, of the soil system often make the spatial distribution of potentially toxic metals (PTMs) quite complex and difficult to assess correctly. This work demonstrates that the application of laser ablation spectrometry (LA-ICP-MS) to soil thin sections constitutes an ancillary powerful tool to well-established analytical methods for tracing the behavior and fate of potential soil contaminants at the microsite level. It allowed to discriminate the contribution of PTMs in distinct soil sub-components, such as parent rock fragments, neoformed, clay-enriched or humified matrix, and specific pedogenetic features of illuvial origin (unstained or iron-stained clay coatings) even at very low contents. PTMs were analyzed in three soil profiles located in the Muravera area (Sardinia, Italy), where several, now abandoned mines were exploited. Recurrent trends of increase of many PTMs from rock to pedogenic matrix and to illuvial clay coatings, traced by LA-ICP-MS compositional data, revealed a pedogenetic control on metal fractionation and distribution, based on adsorption properties of clay minerals, iron oxyhydroxides or organic matter, and downprofile illuviation processes. The main PTMs patterns coupled with SEM-EDS analyses suggest that heavy metal-bearing mineral grains were sourced from the mine plants, in addition to the natural sedimentary input. The interplay between soil-forming processes and geomorphic dynamics significantly contributed to the PTMs spatial distribution detected in the different pedogenetic horizons and soil features.

X-ray photoelectron spectroscopy for identification of morphological defects and disorders in graphene devices

The progress in the development of graphene devices is promising, and they are now considered as an option for the current Si-based electronics. However, the structural defects in graphene may strongly influence the local electronic and mechanical characteristics. Although there are well-established analytical characterization methods to analyze the chemical and physical parameters of this material, they remain incapable of fully understanding of the morphological disorders. In this study, x-ray photoelectron spectroscopy (XPS) with an external voltage bias across the sample is used for the characterization of morphological defects in large area of a few layers graphene in a chemically specific fashion. For the XPS measurements, an external +6 V bias applied between the two electrodes and areal analysis for three different elements, C1s, O1s, and Au4f, were performed. By monitoring the variations of the binding energy, the authors extract the voltage variations in the graphene layer which reveal information about the structural defects, cracks, impurities, and oxidation levels in graphene layer which are created purposely or not. Raman spectroscopy was also utilized to confirm some of the findings. This methodology the authors offer is simple but provides promising chemically specific electrical and morphological information.

Thermorheological Behavior of Various Short- and Long-Chain Branched Polyethylenes and Their Correlations with the Molecular Structure

This paper deals with the characterization of a broad range of linear polyethylenes (PE) by means of thermorheology. It is demonstrated, in which way the thermorheological behavior can be related to the comonomer type and content of copolymers. In the first part of this paper, well-established analytical and theological methods are applied to distinguish linear and branched samples. The resolution limit of these methods is demonstrated by the investigation of a blend from a linear-low density PE (LLDPE) and a branched low density PE (LDPE). Special attention is paid to nuclear-magnetic resonance (NMR) spectroscopy in order to reliably determine the comonomer type and content of the samples chosen. The main focus of this paper lies on thermorheological investigations and correlations with the molecular structure. The comparatively high sensitivity of such investigations is highlighted: even small amounts of long-chain branches (LCB) are revealed. The activation energy (E-u) of linear samples increases with growing comonomer length and content, respectively. As such, thermorheology is demonstrated to be an interesting theological tool to get an insight into branching structures. Moreover, the experimental effort is relatively small as solely usual dynamic-mechanical experiments at different temperatures are required.

Disposable Graphite Foil Based Electrodes and Their Application in Pharmaceutical Analysis

AbstractThis paper explores a new source of graphite for working electrodes, which presents advantages such as low electrical resistance, good flexibility, favorable mechanical performance, versatility to design electrodes in almost any size and very low cost. The new electrodes were investigated in batch electrochemical cells as associated with flow injection analysis systems. Cyclic voltammetry, stripping voltammetry, and amperometry associated with flow injection analysis techniques were applied for the determination of ascorbic acid, zinc and paracetamol in pharmaceutical formulations, respectively. Well‐established analytical methods were applied for comparison purposes. The results herein demonstrate the potential of graphite foils as working electrodes in different electroanalytical methods, offering the possibility of producing disposable sensors for routine applications.

Multilingual phrase-based concordance generation in real-time

We present software that generates phrase-based concordances in real-time based on Internet searching. When a user enters a string of words for which he wants to find concordances, the system sends this string as a query to a search engine and obtains search results for the string. The concordances are extracted by performing statistical analysis on search results and then fed back to the user. Unlike existing tools, this concordance consultation tool is language-independent, so concordances can be obtained even in a language for which there are no well-established analytical methods. Our evaluation has revealed that concordances can be obtained more effectively than by only using a search engine directly.

Glacial isostatic adjustment and relative sea-level changes: the role of lithospheric and upper mantle heterogeneities in a 3-D spherical Earth

SUMMARY The response of the Earth to the melting of the Late Pleistocene ice sheets is commonly studied by spherically layered models, based on well-established analytical methods. In parallel, a few models have been recently proposed to circumvent the limitations imposed by spherical symmetry, and to reproduce the actual structure of the lithosphere and of the upper mantle. Their main outcome is that laterally varying rheological structures may significantly affect various geophysical quantities related to glacial isostatic adjustment (GIA), and particularly post-glacial relative sea-level (RSL) variations and 3-D crustal velocities in formerly ice-covered regions. In this paper, we contribute to the ongoing debate about the role of lithospheric and mantle heterogeneities by new 3-D spherical Newtonian finite elements models and we directly compare their outcomes with publicly available global RSL data. This differs from previous investigations, in that have mainly focused on extensive sensitivity analyses or have considered a limited number of RSL observations from formerly glaciated regions and their periphery. In our study the lithospheric thickness mimics the global structure of the cratons based on geological evidence, and the upper mantle includes a low-viscosity zone beneath the oceanic lithosphere. We use two distinct global surface loads, based upon the ICE1 and ICE3G deglaciation chronologies, respectively. Our main finding is that using all of the available RSL observations in the last 6000 years it is not possible to discern between homogeneous and heterogeneous GIA models. This result, which holds for both ICE1 and ICE3G, suggests that the cumulative effects of laterally varying structures on the synthetic RSL curves cancel out globally, yielding signals that do not significantly differ from those based on the 1-D models. We have also considered specific subsets of the global RSL database, sharing similar geographical settings and distances from the main centres of deglaciation. When we consider the data from the margins of the Baltic region, a laterally varying lithospheric thickness improves significantly the agreement with the observations. This is not observed in other relevant situations, including the Hudson bay region. In the regions where the disagreement between predictions and observations is particularly evident, further investigations are needed to improve the geometry of the heterogeneous structures and of the surface ice-sheets distribution.

Characterization of Ballpoint Pen Inks by Thermal Desorption and Gas Chromatography-Mass Spectrometry

The characterization of ink on paper is of importance for dating and comparing questioned ink entries in forensic document examination. Inks are commonly characterized by their colorant profile that is identified by well-established analytical methods. Numerous ink formulations show identical colorant profiles, though. In order to differentiate inks that are not distinguishable by colorant analysis, a method for the characterization of colorless ink ingredients, namely binders, solvents and additives is necessary. In this paper, we propose a technique for the analysis of colorless compounds in ballpoint inks using direct thermal desorption of the ink on paper followed by chemical analysis of the desorbed volatile compounds by gas chromatography-mass spectrometry. As compared to liquid extraction and subsequent analysis of the extracts, the technique avoids possible contamination risks. Sensitivity is very high due to the enrichment of volatile components by thermal desorption. Even from old samples, the chromatograms obtained by the method enable the determination of binder polymers, solvents and additives. Pure binders as used by ink manufacturers were analyzed for unambiguous assignment of analytical results to specific polymers. To prove the practical applicability, we analyzed 121 ballpoint pens, not all having the same colorant profile, and grouped the pens into resin and solvent categories.

Quantitative determination of loadings and oxidation products of polystyrene-bound phosphines using 31p MAS NMR.

The use of (31)P magic angle spinning (MAS) NMR for the quantitative determination of resin loadings and the building up of oxidation products was investigated. Loadings of polystyrene-bound phosphines were evaluated via addition of triphenyl phosphate as reference compound. Results for a series of phosphines are consistent with those obtained from well-established analytical methods. The compounds were also investigated with (13)C MAS NMR, and the individual oxidation stabilities were monitored under oxygen atmosphere.

Load Tests on Prestressed Precast Concrete and Timber Piles

This paper presents the results of six pile-load tests performed on timber and prestressed concrete piles. Five axial compressive pile-load tests and one lateral-load test are presented. Comparisons are made between the results of these tests and predictions made using available geotechnical computer software. These comparisons provide an insight into using the Brinch-Hansen method of pile-load test evaluation along with wave equation and other computer analyses to evaluate pile capacities from load test data. This paper demonstrates how wave equation analyses can be used to anticipate and mitigate excess driving stresses during the installation of prestressed concrete piles. This paper also demonstrates that the use of well-established analytical methods can adequately predict the vertical and lateral behavior of timber and prestressed concrete piles. However, the bending rigidity of concrete piles under lateral loading should be carefully selected to obtain a good prediction to the measured data.

Quantitative Determination of Resin Loading in Solid-Phase Organic Synthesis Using 13C MAS NMR

The use of quantitative carbon nuclear magnetic resonance spectroscopy ((13)C NMR) for the determination of resin loadings has been investigated. Magic angle spinning (MAS) NMR spectra have been obtained for solvent-swollen resins on a conventional 7 mm CP/MAS probe using the two pulse phase modulation (TPPM) proton decoupling sequence. Loadings of resin-bound organic compounds were evaluated via addition of tetrakis(trimethylsilyl)silane as reference or using the carbon resonances of the polymeric resin material as an internal standard. Results for several functionalized Wang and trityl resins are consistent with those obtained using well-established analytical methods. The (13)C NMR method has interesting applications in the field of solid-phase organic synthesis (SPOS), since no functional group acting as a support for the attachment of a quantifiable chromophore must be available in the material of interest.