Swept-frequency two-pulse phase modulation (SWf-TPPM) sequences with linear sweep profile for heteronuclear decoupling in solid-state NMR

Recently, a pulse scheme for heteronuclear spin decoupling in solid-state NMR, called swept-frequency two-pulse phase modulation (SW(f)-TPPM), was introduced which outperforms the standard TPPM and small phase incremental alteration (SPINAL) schemes. It has also been shown that the frequency-sweep profile can be varied to achieve optimal efficiency for crystalline and liquid-crystalline samples, respectively. Here we present a detailed comparison of the proton decoupling performance for SW(f)-TPPM sequences with tangential sweep profiles (SW(f) (tan)-TPPM) and linear sweep profiles (SW(f) (lin)-TPPM). Using the (13)CH(2) resonance of crystalline tyrosine as a model system, it is shown that linear profiles have a decoupling performance which is at least as good and in some instances slightly better than that obtained from tangential sweep profiles. While tangential sweep profiles require a tangent cut-off angle as an additional parameter, the lack of that parameter makes linear sweep profiles easier to implement and optimise.     

Screen‐Printed Contactless Conductivity Detector for Microchip Capillary Electrophoresis

A new method for mass fabrication of silver ink conductivity detector electrodes for poly(methylmethacrylate) (PMMA) microchip electrophoretic systems has been developed based on screen‐printing technology. Printing of silver conductivity electrodes was performed through a patterned stencil on thin PMMA sheets. Following the electrode fabrication, the PMMA sheets are cut into cover sheets, and are aligned and sealed to the channel plate thus establishing a complete microchip separation device. The effects of the electrode width and spacing on the response and resolution have been investigated and the optimized electrode performance was compared to commonly used aluminum electrodes in the determination of ammonium, methyl ammonium, and sodium. The utility of the screen‐printed contactless conductivity detector (SPCCD) electrodes is further demonstrated for the separation and detection of organic acids with excellent reproducibility (RSD values of 3.7% and 4.1% for oxalate and tartrate, respectively). The thick‐film fabrication of the electrode material demonstrates the ability to mass‐fabricate detection devices with total process of device fabrication requiring less than 4 h (including the fabrication of channel plate, cover sheet with the electrodes, and subsequent bonding). The fabrication method described here is convenient and does not compromise the detector performance, hence offers great promise for producing single use field deployable analytical microsystems.     

Covalent assembly of silver nanoparticles on hydrogen-terminated silicon surface

Synthesis of ω-alkenyl-terminated silver nanoparticles (AgNPs) and then their immobilization on a hydrogen-terminated silicon surface in two-dimensional arrangement through covalent interaction are demonstrated. The thermal-induced hydrosilylation at mild conditions facilitate nanoparticles assembly through interaction between terminal alkenyl (CH(2)=CH-) groups of AgNPs and hydrogen-terminated silicon surface. The assembly of AgNPs on a silicon surface is characterized by FESEM and XPS. Adequate coating of 10-undecene-1-thiol (UDT) on AgNPs and mild temperature hydrosilylation impede the fusion or aggregation of nanoparticles, while they immobilized on a silicon surface, which is very crucial to preserve the discrete entities of nanoparticles. This elegant and facile approach provides stable monolayer of AgNPs with very good coverage area and promises potential to fabricate electronic devices and solar cells, where nanoparticles needs to be directly attached to the silicon surface without an interfacial oxide thin film.     

Towards measurement of homonuclear dipolar couplings in 1H solid-state NMR: recoupling with a rotor-synchronized decoupling scheme

We describe a magic-angle spinning NMR experiment for (1)H-(1)H homonuclear dipole-dipole coupling estimations in organic solids. The methodology involves reintroducing dipolar interactions with rotor-synchronized homonuclear decoupling pulse sequences. Frequency-selective DANTE pulses are used to isolate a specific spin pair from a natural isotopic abundance sample. The coupling of interest, between the selected spin pair, may be extracted by a non linear least-squares fit of the experimentally observed modulation of the signal intensity to an exact analytical formula. The experiment is demonstrated on natural isotopic abundance glycine and alanine powder samples.     

An expedient route for the reduction of carboxylic acids to alcohols employing 1-propanephosphonic acid cyclic anhydride as acid activator

A simple and efficient method for the synthesis of alcohols from the corresponding carboxylic acids is described. Activation of carboxylic acid with 1-propanephosphonic acid cyclic anhydride (T3P) and subsequent reduction using NaBH₄ yield the alcohol in excellent yields with good purity. Reduction of several alkyl/aryl carboxylic acids and N^α-protected amino acids/peptide acids as well as N^β-protected amino acids was successfully carried out to obtain corresponding alcohols in good yields. All the products were fully characterized by ¹H NMR and mass spectral analyses. The procedure is mild, simple and the isolation of the products is easy.     

Convenient and simple synthesis of 2-aminothiazoles by the reaction of α-halo ketone carbonyls with ammonium thiocyanate in the presence of N-methylimidazole

Substituted 2-aminothiazole derivatives were obtained as a result of N-methylimidazole catalyzed cyclization of α-halo ketone carbonyls with ammonium thiocyanate in water-alcoholic media. The generality of the method has been demonstrated by screening a series of aromatic/heteroaromatic/aliphatic α-halo ketones, α-halo β-diketones, and α-halo β-ketoesters. The developed method is simple, mild, and general route for the preparation of diversely functionalized 2-aminothiazoles in good to moderate yields from readily available starting materials.     

Synthesis and extraction of beta-D-glucose-stabilized Au nanoparticles processed into low-defect, wide-area thin films and ordered arrays using CO2-expanded liquids

This letter presents a straightforward and economic strategy to create aqueous Au nanoparticle dispersions using small amounts of beta-D-glucose as a "green" alternative to the conventional phase-transfer catalyst approach. Furthermore, this new process provides for efficient extraction of these monodisperse Au nanoparticles into an organic phase that was successfully processed into wide-area, locally ordered nanoparticle arrays and thin films using a precisely controlled CO2-expanded liquid particle deposition technique. This CO2-based technique allows for pressure-tunable particle deposition while eliminating the detrimental surface tension and dewetting effects common to normal solvent-evaporation techniques.     

Novel bile acid-based cyclic bisimidazolium receptors for anion recognition

[structure: see text] Novel deoxycholic acid-based cyclic receptors, 3 and 4, containing two imidazolium groups and m-xylene and p-xylene as spacers have been synthesized. These receptors bind anions through hydrogen bonds utilizing two imidazolium (C-H)(+) and inwardly directed methylene hydrogens of both acetyl groups. Receptor 3 shows a moderate selectivity for fluoride ion whereas receptor 4 shows high affinity and selectivity for chloride ion in CDCl(3).     

Fuzzy based directional weighted median filter for impulse noise detection and reduction

The known median-based denoising methods tends to work well for restoring the images corrupted by random-valued impulse noise with low noise level, but it fails in denoising highly corrupted images. In this paper, a new noise reduction method based on directional weighted median based fuzzy impulse noise detection and reduction method (DWMFIDRM) has been proposed, which has been specially developed for denoising all categories of impulse noise. The contribution of this paper is threefold. The main contribution of the novel impulse noise reduction technique lies in the unification of three different methods; the impulse noise detection phase utilizing the concept of fuzzy gradient values, edge-preserving noise reduction phase based on the directional weighted median of the neighboring pixels and a final filtering step in order to deal with noisy pixels of non-zero degree. Such a unique combination has improved the efficiency of this method for high density noise removal. The experimental results of our proposed method have a significant improvement when compared to other existing filters for high density noise removal. This paper utilizes the concept of fuzzy gradient values. The noise reduction phase that preserves edge sharpness is based on the directional weighted median of neighboring pixels. Final filtering phase is performed only when there is non-zero degree of noise pixels. This phase makes our method more efficient in high noise density. Experimental results show that DWMFIDRM provides a significant improvement on other existing filters.     

Thermal and optical characterization of a novel series of supramolecular liquid crystals

Supramolecular hydrogen bonded liquid crystal (SMHBLC) homologous series is synthesized and characterized. Hydrogen bond is formed between p-n-alkyloxy benzoic acids (nOBA, where n=7 to 12) and Iodo substituted benzoic acid (I_mBA) respectively. The isolated homologs are characterized by various techniques like Polarizing Optical Microscopy (POM), Differential Scanning Calorimetry (DSC), ¹H Nuclear Magnetic Resonance Spectroscopy (NMR) and Fourier Transform Infrared Spectroscopy (FTIR). From the POM and DSC studies phase diagram has been constructed and discussed. A new smectic ordering, labeled as smectic R, has been characterized which exhibits a ribbon like texture. This phase is observed in a complex pertaining to the undecyloxy carbon number. Tilt angle in smectic R phase and in traditional smectic C of all the complexes have been experimentally deduced and the results are fitted and so obtained β value concurrences with the Mean field theory predicted value.