Rapid Preparation of Environmental Samples by Accelerated Solvent Extraction (ASE)

Abstract

Accelerated solvent extraction (ASE) is suitable for the extraction of PAHs from solid samples, as a sample preparation technique for subsequent analytical techniques. Due to the elevated temperatures and pressures used for ASE considerable time and solvent savings are achieved. The time required is less than 15 min. per sample, and solvent usage is reduced significantly (15 mL per 10 g sample) compared to conventional solvent extraction techniques like Soxhlet extraction. Equivalency of the extraction results are shown by the cornparision of ASE to conventional extraction techniques. ASE has already been accepted by the U.S. EPA, and meets the requirement of SW-846 method 3545.     

Chemical synthesis of a dual branched malto-decaose: a potential substrate for alpha-amylases

A convergent block strategy for general use in efficient synthesis of complex alpha-(1-->4)- and alpha-(1-->6)-malto-oligosaccharides is demonstrated with the first chemical synthesis of a malto-oligosaccharide, the decasaccharide 6,6'-bis(alpha-maltosyl)-maltohexaose, with two branch points. Using this chemically defined branched oligosaccharide as a substrate, the cleavage pattern of seven different alpha-amylases were investigated. Alpha-amylases from human saliva, porcine pancreas, barley alpha-amylase 2 and recombinant barley alpha-amylase 1 all hydrolysed the decasaccharide selectively. This resulted in a branched hexasaccharide and a branched tetrasaccharide. Alpha-amylases from Asperagillus oryzae, Bacillus licheniformis and Bacillus sp. cleaved the decasaccharide at two distinct sites, either producing two branched pentasaccharides, or a branched hexasaccharide and a branched tetrasaccharide. In addition, the enzymes were tested on the single-branched octasaccharide 6-alpha-maltosyl-maltohexaose, which was prepared from 6,6'-bis(alpha-maltosyl)-maltohexaose by treatment with malt limit dextrinase. A similar cleavage pattern to that found for the corresponding linear malto-oligosaccharide substrate was observed.     

Deactivation of V2O5-WO3-TiO2 SCR catalyst at a biomass-fired combined heat and power plant

The deactivation of a commercial type V₂O₅-WO₃-TiO₂ monolith catalyst under biomass combustion was studied at a full-scale grate-fired power plant burning straw/wood using a slip stream pilot scale reactor. The aerosols in the flue gas consisted of a mixture of potassium chloride and sulphate. Three catalyst elements were exposed at 350 °C, and one element was exposed at 250 °C for comparison. The catalyst activity was measured in the reactor at the exposure temperature by addition of NH₃ and extra NO. The activity, in terms of a first-order rate constant, dropped by 52% after about 1140 h indicating a very fast deactivation compared to coal firing. It was also found that the reactor temperature was not of importance for the deactivation rate. SEM-EDX analysis showed that particle deposition and pore blocking contributed to the deactivation by decreasing the diffusion rate of NO and NH₃ into the catalyst. However, potassium also penetrated into the catalyst wall and the resulting average K/V ratio in the catalyst structure was high enough (about 0.3–0.5) for a significant chemical deactivation. Chemisorption studies carried out in situ showed that the amount of chemisorbed NH₃ on the catalyst decreased as a function of exposure time, which reveals that Brøndsted acid sites had reacted with potassium compounds and thereby rendered inactive. When washed by 0.5 M H₂SO₄ the regenerated catalyst regains a higher activity than that of the fresh catalyst at temperatures higher than 300 °C, but even though reactivation is possible, the deactivation rate appears too high for practical use of the SCR process in straw combustion.     

Predicting and rationalizing the effect of surface charge distribution and orientation on nano-wire based FET bio-sensors

A single charge screening model of surface charge sensors in liquids (De Vico et al., Nanoscale, 2011, 3, 706-717) is extended to multiple charges to model the effect of the charge distributions of analyte proteins on FET sensor response. With this model we show that counter-intuitive signal changes (e.g. a positive signal change due to a net positive protein binding to a p-type conductor) can occur for certain combinations of charge distributions and Debye lengths. The new method is applied to interpret published experimental data on Streptavidin (Ishikawa et al., ACS Nano, 2009, 3, 3969-3976) and Nucleocapsid protein (Ishikawa et al., ACS Nano, 2009, 3, 1219-1224).     

Secondary electron amplification using single-crystal CVD diamond film

The current amplification characteristics of an unbiased 8.3-μm-thick single-crystal CVD diamond film are examined using secondary-electron-emission measurements. In particular, the intensity and energy distribution of transmitted and reflected secondary electrons are measured and used to examine the transport and emission properties that govern the current amplification process. Overall, the measurements confirm the excellent transport and emission properties of single-crystal CVD diamond, as compared to polycrystalline CVD diamond films studied previously. Specifically, the transmitted and reflected energy distributions measured from the single-crystal diamond are nearly identical, with a sharp, narrow (FWHM = 0.35 eV) emission peak dominating the spectra. However, the transmitted distributions are more fully thermalized as a result of the longer transport distances. In fact, transmitted electrons are detected even after traveling more than 8 μm through the film, which demonstrates the potential for excellent transport efficiency. Maximum transmission gains of 3–4 are obtained, which is encouraging under such field-free conditions. However, the results of the study indicate that the transmission process is being limited by diffusive transport in the unbiased diamond film.     

Crosslinking of polybenzimidazole membranes by divinylsulfone post‐treatment for high‐temperature proton exchange membrane fuel cell applications

Phosphoric acid‐doped polybenzimidazole (PBI) has been suggested as a promising electrolyte for proton exchange membrane fuel cells operating at temperatures up to 200 °C. This paper describes the development of a crosslinking procedure for PBI membranes by post‐treatment with divinylsulfone. The crosslinking chemistry was studied and optimized on a low‐molecular‐weight model system and the results were used to optimize the crosslinking conditions of PBI membranes. The crosslinked membranes were characterized with respect to chemical and physiochemical properties, showing improved mechanical strength and oxidative stability compared with their linear analogues. Fuel cell tests were further conducted in order to demonstrate the feasibility of the crosslinked membranes. Copyright © 2011 Society of Chemical Industry     

Telepresence surgery

The authors' institute has established that precise surgical procedures can be carried out with Telepresence. Within this decade, Telepresence surgery may become an established component of a new, technologically enhanced mode of cost-effective health care delivery. Because of the substantial medical and financial benefit that Telepresence will bring to laparoscopic and other minimally invasive procedures, its first routine use is expected to be within the individual hospital and surgical center. Telepresence surgical procedures have been demonstrated over distances of 160 meters, and the authors are working toward demonstrating animal surgeries over a much greater distance by using microwave and fiber-optic links. Mobile Telepresence surgical equipment may prove especially effective for trauma care in combat and in civilian disasters. Because the stereographic images and the motions and forces can be readily scaled, microsurgeries of all kinds can be made easier with this technology. Arthroscopic procedures, especially difficult surgery on joints such as the wrist and shoulder, are good Telepresence candidates. In neurosurgery, excision of pituitary adenomas could benefit from the increased dexterity and tactile sensitivity of Telepresence. Eventually, neurosurgery under real-time magnetic resonance imaging could be performed by a Telepresence surgeon operating on a three dimensional reconstruction that is immediately updated to show the actual tissue changes caused by the telemanipulated instruments     

New dendrimer-peptide host-guest complexes: towards dendrimers as peptide carriers

Adamantyl urea and adamantyl thiourea modified poly(propylene imine) dendrimers act as hosts for N-terminal tert-butoxycarbonyl (Boc)-protected peptides and form chloroform-soluble complexes. Investigations with NMR spectroscopy show that the peptide is bound to the dendrimer by ionic interactions between the dendrimer outer shell tertiary amines and the C-terminal carboxylic acid of the peptide, and also through host-urea to peptide-amide hydrogen bonding. The hydrogen-bonding nature of the peptide-dendrimer interactions was further confirmed by using Fourier transform IR spectroscopy, for which the NH- and CO-stretch signals of the peptide amide moieties shift towards lower wavenumbers upon complexation with the dendrimer. Spatial analysis of the complexes with NOESY spectroscopy generally shows close proximity of the N-terminal Boc group of the peptide to the peripheral adamantyl groups on the dendrimer host. The influence of side-chain motif on interactions with the host is analyzed by using seven different N-Boc-protected tripeptides as guests for the dendrimer. Downfield shifts of up to 1.3 ppm were observed for the guest amide NH-proton signals. These shifts decreased with increasing 'bulkiness' of the amino acid side chains. Despite this, the dendrimer was capable of making multiple peptide-dendrimer complexes when presented with a library of seven peptides. The different peptides were all present in the host, which did not show specific preferences, and could be released under mild acidic conditions. These results show the general nature of the peptide-dendrimer interactions in the formation of either single- or multiple-peptide-dendrimer complexes.     

Autogenous deformation and RH-change in perspective

Autogenous deformation and change of the relative humidity (RH-change) have been described and registered for a century. However, it is only within the last decade that these phenomena have received appreciable attention. The reason for this is that autogenous deformation and autogenous RH-change are phenomena of special importance within high-strength (high-performance) concrete technology, and a significant utilisation of these concretes did not take place until the early 1980s. In the present paper an historical overview of autogenous deformation and RH-change is given. In addition, due to the present status of this research field both terminology and measuring techniques are described in detail. Finally, some expectations for future research in this field are given.     

Effect of NiO-to-Ni Transformation on Conductivity and Structure of Yttria-Stabilized ZrO2

The conductivity and structure of 8-mol%-yttria-stabilized zirconia with additions of nickel oxide has been investigated, both in the as-prepared state and after reduction of NiO in hydrogen. During reduction at 1000°C, the conductivity decreases by 40%–50% and most of the NiO dissolved in the zirconia is exsolved in the form of nickel particles. This is accompanied by the formation of tetragonal zirconia precipitates of size 10–40 nm and by an increase in the lattice parameter. On reoxidation in air at 1000°C, the change in lattice parameter is partly reversed, but the conductivity shows no further changes.