Rapid synthesis and characterization of an oxygen-deficient defect perovskite La4BaCu5O13+d phase

Oxygen-deficient defect perovskite La4BaCu5O13+d phase has been synthesized by the nitrate-citrate gel combustion method at 950 C for 2 h. Structural parameters were refined by the Rietveld refinement method using room-temperature powder XRD data. The La4BaCu5O13+d crystallizes in the tetragonal structure with space group P4/m (no. 83) and having the lattice parameters a=8.6508 c=3.8606 (1) Å and (2) Å, respectively. Oxygen content was determined by the iodometric titration. Low-temperature resistivity result reveals that La4BaCu5O13+d compound exhibit metallic behavior up to 15 K.

Effect of frequency on seismic response of reinforced soil slopes in shaking table tests

This paper studies the effect of frequency of base shaking on the dynamic response of unreinforced and reinforced soil slopes through a series of shaking table tests. Slopes were constructed using clayey sand and geogrids were used for reinforcing the slopes. Two different slope angles 45 degrees and 60 degrees were used in tests and the quantity and location of reinforcement is varied in different tests. Acceleration of shaking is kept constant as 0.3 g in all the tests to maximize the response and the frequency of shaking was 2 Hz, 5 Hz and 7 Hz in different tests. The slope is instrumented with ultrasonic displacement sensors and accelerometers at different elevations. The response of different slopes is compared in terms of the deformation of the slope and acceleration amplifications measured at different elevations. It is observed that the displacements at all elevations increased with increase in frequency for all slopes, whereas the effect of frequency on acceleration amplifications is not significant for reinforced slopes. Results showed that the acceleration and displacement response is not increasing proportionately with the increase in the frequency, suggesting that the role of frequency in the seismic response is very important. Reinforced slopes showed lesser displacements compared to unreinforced slopes at all frequency levels. (C) 2012 Elsevier Ltd. All rights reserved.

Rapid mass spectrometric determination of disulfide connectivity in peptides and proteins

Disulfide crosslinks are ubiquitous in natural peptides and proteins, providing rigidity to polypeptide scaffolds. The assignment of disulfide connectivity in multiple crosslinked systems is often difficult to achieve. Here, we show that rapid unambiguous characterisation of disulfide connectivity can be achieved through direct mass spectrometric CID fragmentation of the disulfide intact polypeptides. The method requires a direct mass spectrometric fragmentation of the native disulfide bonded polypeptides and subsequent analysis using a newly developed program, DisConnect. Technical difficulties involving direct fragmentation of proteins are surmounted by an initial proteolytic nick and subsequent determination of the structures of these proteolytic peptides through DisConnect. While the connectivity in proteolytic fragments containing one cystine is evident from the MS profile alone, those with multiple cystines are subjected to subsequent mass spectrometric fragmentation. The wide applicability of this method is illustrated using examples of peptide hormones, peptide toxins, proteins, and disulfide foldamers of a synthetic analogue of a marine peptide toxin. The method, coupled with DisConnect, provides an unambiguous, straightforward approach, especially useful for the rapid screening of the disulfide crosslink fidelity in recombinant proteins, determination of disulfide linkages in natural peptide toxins and characterization of folding intermediates encountered in oxidative folding pathways.

Employing denaturation for rapid electrochemical detection of myoglobin using TiO2 nanotubes

An alternative antibody-free strategy for the rapid electrochemical detection of cardiac myoglobin has been demonstrated here using hydrothermally synthesized TiO2 nanotubes (Ti-NT). The denaturant induced unfolding of myoglobin led to easy access of the deeply buried electroactive heme center and thus the efficient reversible electron transfer from protein to electrode surface. The sensing performance of the Ti-NT modified electrodes were compared vis a vis commercially available titania and GCEs. The tubular morphology of the Ti-NT led to facile transfer of electrons to the electrode surface, which eventually provided a linear current response (obtained from cyclic voltammetry) over a wide range of Mb concentration. The sensitivity of the Ti-NT based sensor was remarkable and was equal to 18 mu A mg(-1) ml (detection limit = 50 nM). This coupled with the rapid analysis time of a few tens of minutes (compared to a few days for ELISA) demonstrates its potential usefulness for the early detection of acute myocardial infarction (AMI).

Low temperature and rapid deposition of ZnO nanorods on Si(100) substrate with tunable optical emissions

This research article describes the large scale fabrication of ZnO nanorods of various shapes on Si(100) substrate, by using metalorganic precursor of Zn in solutions with microwave as the source of energy. This is a low temperature, environmental friendly and rapid thin film deposition process, where ZnO nanorods (1-3 mu m length) were grown only in 1-5 min of microwave irradiation. All as-synthesized nanorods are of single crystalline grown along the < 0001 > crystallographic direction. The coated nanorods were found to be highly dense having a thickness of similar to 1-3 mu m over the entire area 20 mm x 20 mm of the substrate. The ZnO thin film comprising of nanorods exhibits good adhesion with the substrate. A possible mechanism for the initial nucleation and growth of ZnO is discussed. A cross over from a strong visible light emission to an enhanced UV emission is observed, when the nature of the surfactants are varied from polymeric to ionic and nonionic. The position of the chromaticity coordinates in yellow region of the color space gives an impression of white light generation from these coatings by exciting with a blue laser.

Fastest Rapid Loading Methods of Vertical and Radial Consolidations

Fastest curve-fitting procedures are proposed for vertical and radial consolidations for rapid loading methods. In vertical consolidation, the next load increment can be applied at 50-60% consolidation (or even earlier if the compression index is known). In radial consolidation, the next load increment can be applied at just 10-15% consolidation. The effects of secondary consolidation on the coefficient of consolidation and ultimate settlement are minimized in both cases. A quick procedure is proposed in vertical consolidation that determines how far is calculated from the true , where is coefficient of consolidation. In radial consolidation no such procedure is required because at 10-15% the consolidation effects of secondary consolidation are already less in most inorganic soils. The proposed rapid loading methods can be used when the settlement or time of load increment is not known. The characteristic features of vertical, radial, three-dimensional, and secondary consolidations are given in terms of the rate of settlement. A relationship is proposed between the coefficient of the vertical consolidation, load increment ratio, and compression index. (C) 2013 American Society of Civil Engineers.

An approach for assessing the accuracy of accelerometer responses during axial impact tests

The primary objective of the present study is to show that for the most common configuration of an impactor system, the accelerometer cannot exactly reproduce the dynamic response of a specimen subjected to impact loading. An equivalent Lumped Parameter Model (LPM) of the given impactor set-up has been formulated for assessing the accuracy of an accelerometer mounted in a drop-weight impactor set-up for an axially loaded specimen. A specimen under the impact loading is represented by a non-linear spring of varying stiffness, while the accelerometer is assumed to behave in a linear manner due to its high stiffness. Specimens made of steel, aluminium and fibre-reinforced composite (FRC) are used in the present study. Assuming the force-displacement response obtained in an actual impact test to be the true behaviour of the test specimen, a suitable numerical approach has been used to solve the governing non-linear differential equations of a three degrees-of-freedom (DOF) system in a piece-wise linear manner. The numerical solution of the governing differential equations following an explicit time integration scheme yields an excellent reproduction of the mechanical behaviour of the specimen, consequently confirming the accuracy of the numerical approach. However, the spring representing the accelerometer predicts a response that qualitatively matches the assumed force-displacement response of the test specimen with a perceptibly lower magnitude of load.

The dual role of Zn-acid medium for one-step rapid synthesis of M@rGO (M = Au, Pt, Pd and Ag) hybrid nanostructures at room temperature

We report a new protocol for the synthesis of M@rGO (M = Au, Pt, Pd, Ag and rGO = reduced graphene oxide) hybrid nanostructures at room temperature in Zn-acid medium. The roles of Zn-acid are to reduce the GO by generated hydrogen and the deposition of metal nanoparticles on rGO by galvanic replacement reaction between Zn and Mn+.

Pre-clinical toxicity & immunobiological evaluation of DNA rabies vaccine & combination rabies vaccine in rhesus monkeys (Macaca mulatta)

Background & objectives: Pre-clinical toxicology evaluation of biotechnology products is a challenge to the toxicologist. The present investigation is an attempt to evaluate the safety profile of the first indigenously developed recombinant DNA anti-rabies vaccine DRV (100 mu g)] and combination rabies vaccine CRV (100 mu g DRV and 1.25 IU of cell culture-derived inactivated rabies virus vaccine)], which are intended for clinical use by intramuscular route in Rhesus monkeys. Methods: As per the regulatory requirements, the study was designed for acute (single dose - 14 days), sub-chronic (repeat dose - 28 days) and chronic (intended clinical dose - 120 days) toxicity tests using three dose levels, viz. therapeutic, average (2x therapeutic dose) and highest dose (10 x therapeutic dose) exposure in monkeys. The selection of the model i.e. monkey was based on affinity and rapid higher antibody response during the efficacy studies. An attempt was made to evaluate all parameters which included physical, physiological, clinical, haematological and histopathological profiles of all target organs, as well as Tiers I, II, III immunotoxicity parameters. Results: In acute toxicity there was no mortality in spite of exposing the monkeys to 10XDRV. In sub chronic and chronic toxicity studies there were no abnormalities in physical, physiological, neurological, clinical parameters, after administration of test compound in intended and 10 times of clinical dosage schedule of DRV and CRV under the experimental conditions. Clinical chemistry, haematology, organ weights and histopathology studies were essentially unremarkable except the presence of residual DNA in femtogram level at site of injection in animal which received 10X DRV in chronic toxicity study. No Observational Adverse Effects Level (NOAEL) of DRV is 1000 ug/dose (10 times of therapeutic dose) if administered on 0, 4, 7, 14, 28th day. Interpretation & conclusions: The information generated by this study not only draws attention to the need for national and international regulatory agencies in formulating guidelines for pre-clinical safety evaluation of biotech products but also facilitates the development of biopharmaceuticals as safe potential therapeutic agents.

An Efficient Probe for Rapid Detection of Cyanide in Water at Parts per Billion Levels and Naked-Eye Detection of Endogenous Cyanide

A new molecular probe based on an oxidized bis-indolyl skeleton has been developed for rapid and sensitive visual detection of cyanide ions in water and also for the detection of endogenously bound cyanide. The probe allows the naked-eye detection of cyanide ions in water with a visual color change from red to yellow ((max)=80nm) with the immediate addition of the probe. It shows high selectivity towards the cyanide ion without any interference from other anions. The detection of cyanide by the probe is ratiometric, thus making the detection quantitative. A Michael-type addition reaction of the probe with the cyanide ion takes place during this chemodosimetric process. In water, the detection limit was found to be at the parts per million level, which improved drastically when a neutral micellar medium was employed, and it showed a parts-per-billion-level detection, which is even 25-fold lower than the permitted limits of cyanide in water. The probe could also efficiently detect the endogenously bound cyanide in cassava (a staple food) with a clear visual color change without requiring any sample pretreatment and/or any special reaction conditions such as pH or temperature. Thus the probe could serve as a practical naked-eye probe for in-field experiments without requiring any sophisticated instruments.

Rapid determination of main constituents of packed juices by reverse phase-high performance liquid chromatography: an insight in to commercial fruit drinks

The present work reports the compositional analysis of thirteen different packed fruit juices using high performance liquid chromatography (HPLC). Vitamin C, organic acids (citric and malic) and sugars (fructose, glucose and sucrose) were separated, analyzed and quantified using different reverse phase methods. A new rapid reverse phase HPLC method was developed for routine analysis of vitamin C in fruit juices. The precision results of the methods showed that the relative standard deviations of the repeatability and reproducibility were < 0.05 and < 0.1 respectively. Correlation coefficient of the calibration models developed was found to be higher than 0.99 in each case. It has been found that the content of Vitamin C was less variable amongst different varieties involved in the study. It is also observed that in comparison to fresh juices, the packed juices contain lesser amounts of vitamin C. Citric acid was found as the major organic acids present in packed juices while maximum portion of sugars was of sucrose. Comparison of the amount of vitamin C, organic acids and sugars in same fruit juice of different commercial brands is also reported.

A rapid, efficient, and economical inverse polymerase chain reaction-based method for generating a site saturation mutant library

With the development of deep sequencing methodologies, it has become important to construct site saturation mutant (SSM) libraries in which every nucleotide/codon in a gene is individually randomized. We describe methodologies for the rapid, efficient, and economical construction of such libraries using inverse polymerase chain reaction (PCR). We show that if the degenerate codon is in the middle of the mutagenic primer, there is an inherent PCR bias due to the thermodynamic mismatch penalty, which decreases the proportion of unique mutants. Introducing a nucleotide bias in the primer can alleviate the problem. Alternatively, if the degenerate codon is placed at the 5' end, there is no PCR bias, which results in a higher proportion of unique mutants. This also facilitates detection of deletion mutants resulting from errors during primer synthesis. This method can be used to rapidly generate SSM libraries for any gene or nucleotide sequence, which can subsequently be screened and analyzed by deep sequencing. (C) 2013 Elsevier Inc. All rights reserved.

Novel spherical hierarchical structures of GdOOH and Eu:GdOOH: rapid microwave-assisted synthesis through self-assembly, thermal conversion to oxides, and optical studies

We report a novel, rapid, and low-temperature method for the synthesis of undoped and Eu-doped GdOOH spherical hierarchical structures, without using any structure-directing agents, through the microwave irradiation route. The as-prepared product consists of nearly monodisperse microspheres measuring about 1.3 mu m in diameter. Electron microscopy reveals that each microsphere is an assembly of two-dimensional nanoflakes (about 30 nm thin) which, in turn, result from the assembly of crystallites measuring about 9 nm in diameter. Thus, a three-level hierarchy can be seen in the formation of the GdOOH microspheres: from nanoparticles to 2D nanoflakes to 3D spherical structures. When doped with Eu3+ ions, the GdOOH microspheres show a strong red emission, making them promising candidates as phosphors. Finally, thermal conversion at modest temperatures leads to the formation of corresponding oxide structures with enhanced luminescence, while retaining the spherical morphology of their oxyhydroxide precursor.