The influence of structural changes of the N-substituent on liquid crystalline behaviour of ester imides

Several new ester imide derivatives with different N-substituents in the imide ring were synthesized and their mesogenic properties investigated by thermal analysis, optical microscopy and X-ray diffraction. All the esters of N-4-[(4'-decyloxybiphenyl-4-yl)oxycarbonyl]phthalimideacetic acid and aliphatic alcohols exhibited monolayer SmA and SmC phases. In addition, for the ethyl and propyl esters a monotropic hexatic (F or I) phase was observed. The introduction of additional substituents at the carbon atom in the methylenemethoxycarbonyl group (in the vicinity of the nitrogen atom) substantially influenced liquid crystalline properties: the compounds with a flexible chain exhibited monotropic SmA-SmB dimorphism, but liquid crystalline properties vanished for the substituent containing the more rigid phenyl ring.     

Linear and cyclic aminomethanephosphonic acid esters derived from benzaldehyde derivatives, 3‐aminopropanol,and diethyl phosphite

A series of four diethyl {[(3‐hydroxy‐ propyl)amino](aryl)methyl}phosphonates have been prepared and characterized. In one case, the phosphonate was transformed to a seven‐membered 1,4,2‐ oxazaphosphepane heterocycle through a one‐pot intramolecular esterification. The analogous reaction with formaldehyde gave the six‐membered diethyl (1,3‐oxazinan‐3‐ylmethyl)phosphonate, which could be transformed in a posterior reaction to the corresponding aminomethanephosphonic acid. © 2006 Wiley Periodicals, Inc. Heteroatom Chem 17:75–80, 2006; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20178     

Odd–even effect in biphenyl‐based symmetrical dimers with methylene spacer – evidence of the B4 phase

A series of 4‐decyloxy‐4′‐hydroxybiphenyl esters of α,ω‐alkanedicarboxylic acids containing two mesogenic units connected by a methylene spacer was synthesized. The mesogenic properties of the compounds were investigated by polarising optical microscopy, differential scanning calorimetry and X‐ray diffraction methods. A strong influence of the spacer length and its parity on the mesomorphic properties was found. A dramatic odd–even effect was observed for the clearing temperatures and entropies. Compounds with an even number of carbon atoms in the methylene spacer formed tilted smectic phases, whereas compounds with an odd number of carbon atoms in the spacer exhibited the B4 phase, characteristic of bent‐shaped molecules.     

Quantification of Saponins in Different Plant Parts of Lysimachia L. Species by validated HPTLC—Densitometric Method

JPC – Journal of Planar Chromatography – Modern TLC - Quantitative high-performance thin-layer chromatography (HPTLC) analysis of triterpene saponins in different parts of eight...     

On chemiluminescent emission from an infiltrated chiral sculptured thin film

The theory describing the far-field emission from a dipole source embedded inside a chiral sculptured thin film (CSTF), based on a spectral Green function formalism, was further developed to allow for infiltration of the void regions of the CSTF by a fluid. In doing so, the extended Bruggeman homogenization formalism — which accommodates constituent particles that are small compared to wavelength but not vanishingly small — was used to estimate the relative permittivity parameters of the infiltrated CSTF. For a numerical example, we found that left circularly polarized (LCP) light was preferentially emitted through one face of the CSTF while right circularly polarized (RCP) light was preferentially emitted through the opposite face, at wavelengths within the Bragg regime. The centre wavelength for the preferential emission of LCP/RCP light was red shifted as the refractive index of the infiltrating fluid increased from unity, and this red shift was accentuated when the size of the constituent particles in our homogenization model was increased. Also, the bandwidth of the preferential LCP/RCP emission regime decreased as the refractive index of the infiltrating fluid increased from unity.     

Zinc oxide nanoparticles based microfluidic immunosensor applied in congenital hypothyroidism screening

In this article, we present an innovative approach for congenital hypothyroidism (CHT) screening. This pathology is the most common preventable cause of mental retardation, affecting newborns around the world. Its consequences could be avoided with an early diagnosis through the thyrotropin (TSH) level measurement. To accomplish the determination of TSH, synthesized zinc oxide (ZnO) nanobeads (NBs) covered by chitosan (CH), ZnO-CH NBs, were covalently attached to the central channel of the designed microfluidic device. These beads were employed as platform for anti-TSH monoclonal antibody immobilization to specifically recognize and capture TSH in neonatal samples without any special pretreatment. Afterwards, the amount of this trapped hormone was quantified by horseradish peroxidase (HRP)-conjugated anti-TSH antibody. HRP reacted with its enzymatic substrate in a redox process, which resulted in the appearance of a current whose magnitude was directly proportional to the level of TSH in the neonatal sample. The structure and morphology of synthesized ZnO-CH NBs were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The calculated detection limits for electrochemical detection and the enzyme-linked immunosorbent assay procedure were 0.00087 μUI mL^?1 and 0.015 μUI mL^?1, respectively, and the within- and between-assay coefficients of variation were below 6.31 % for the proposed method. According to the cut-off value for TSH neonatal screening, a reasonably good limit of detection was achieved. These above-mentioned features make the system advantageous for routine clinical analysis adaptation.     

Comparison of the Kalman filter and dedicated algorithms for processing data for solution equilibria,noise smoothing and calibration

The suitability of the Kalman filter for extracting acidity (protonation) constants from titration curves, for noise removal, and for multicomponent determinations in the presence of sample-related interferences is described. The performance of the algorithm is illustrated with simulated examples and checked by comparing the results with those obtained by dedicated methods (Savitzky-Golay and Fourier-transform procedures and the general standard-addition procedure). The ability of a combination of two Kalman filters as a fixed-interval smoother for noise removal is stressed.     

Cloud point extraction of mercury with PONPE 7.5 prior to its determination in biological samples by ETAAS

Cloud point extraction (CPE) has been used for the pre-concentration of mercury, after the formation of a complex with 2-(5-bromo-2-pyridylazo)-5-(diethylamino)-phenol (5-Br-PADAP), and later analysis by electrothermal atomic absorption spectrometry (ETAAS) using polyethyleneglycolmono-p-nonyphenylether (PONPE 7.5) as surfactant. The chemical variables affecting the separation step were optimized. Under the optimum conditions, i.e, pH 8.5, cloud point temperature 80 degrees C, 5-Br-PADAP=4x10(-5) mol L(-1), PONPE 7.5=0.2%, sample volume=1.0 mL, an enhancement factor of 22-fold was reached. The lower limit of detection (LOD) obtained under the optimal conditions was 0.01 microg L(-1). The precision for 10 replicate determinations at 2.0 microg L(-1) Hg was 4.0% relative standard deviation (R.S.D.). The calibration graph using the pre-concentration system for mercury was linear with a correlation coefficient of 0.9994 at levels near the detection limits up to at least 16 microg L(-1). The method was successfully applied to the determination of mercury in biological samples and in certified reference material (QC METAL LL3).     

The effects of cerium doping concentration on the properties and photocatalytic activity of bimetallic Mo/Ce catalyst

In this study, the characterization and photocatalytic activity of MoO₃ nanoparticles doped with various doping concentrations of cerium have been investigated. The Fourier transform infrared (FT-IR) spectra of the prepared catalysts confirmed that MoO₃ particles have been successfully doped by cerium. Field emission scanning electron microscopy (FESEM) was performed to visualize the surface morphology of the obtained catalysts. The XRD patterns suggested that the crystallinity of the sample with the lowest doping concentration of 15 mol % was higher in comparison with samples of higher doping concentrations. The volume-averaged crystal sizes of the obtained catalysts were calculated to be 25, 28, and 32 nm for 15, 35, and 60 mol % samples, respectively. The photocatalytic activity along with the reaction kinetics of Ce-doped MoO₃ nanoparticles have also been investigated through the dye degradation of methyl orange. The synthesized Ce-doped MoO₃ particles with the lowest dopant concentration of 15 mol % exhibited the highest photocatalytic activity for methyl orange dye degradation. It was observed that photo-degradation activity decreased with an increase in the doping concentration of cerium. The predicted rate constants for samples with 15, 35, and 60 mol % doping concentrations were found to be 0.0432, 0.035, and 0.029 min^–1, respectively.