Speciation of arsenic in ground water samples: A comparative study of CE-UV, HG-AAS and LC-ICP-MS

The performance of capillary electrophoresis-ultraviolet detector (CE-UV), hydride generation-atomic absorption spectrometry (HG-AAS) and liquid chromatography-inductively coupled plasma mass spectrometry (LC-ICP-MS) have been compared for the speciation of arsenic (As) in groundwater samples. Two inorganic As species, arsenite (As^III), arsenate (As^V) and one organo species dimethyl arsenic acid (DMA) were mainly considered for this study as these are known to be predominant in water. Under optimal analytical conditions, limits of detection (LD) ranging from 0.10 (As^III, AsT) to 0.19 (DMA) μg/l for HG-AAS, 100 (As^III, DMA) to 500 (As^V) μg/l for CE-UV and 0.1 (DMA, MMA) to 0.2 (As^III, As^V) μg/l for LC-ICP-MS, allowed the determination of the above three species present in these samples. Results obtained by all the three methods are well correlated (r² = 0.996*** for total As) with the precision of <5% R.S.D. except CE-UV. The effect of interfering ions (e.g. Fe²⁺, Fe³⁺, SO₄²⁻ and Cl⁻) commonly found in ground water on separation and estimation of As species were studied and corrected for. Spike recovery was tested and found to be 80-110% at 0.5 μg/l As standard except CE-UV where only 50% of the analyte was recovered. Comparison of these results shows that LC-ICP-MS is the best choice for routine analysis of As species in ground water samples.     

Synthesis,spectroscopic and crystal structure analysis of 2-(4-fluorobenzyl)-6-(4-methoxyphenyl)imidazo[2,1-b][1,3,4]thiadiazole and its morpholinomethyl derivative

The preparation of 2-(4-fluorobenzyl)-6-(4-methoxyphenyl)-5-morpholin-1-ylmethyl imidazo[2,1-b][1,3,4]thiadiazole via the intermediate 2-(4-fluorobenzyl)-6-(4-methoxyphenyl)Imidazo[2,1-b][1,3,4] thiadiazole is described. Elemental analysis, IR spectrum, ¹H NMR and X-ray crystal structure analyses were carried out to determine the compositions and molecular structures of the two compounds. The crystal packing exhibits intermolecular C–H?O, C–H?N, C–H?F and π–π stacking interactions leading to the formation of the supramolecular network.     

In vivo estimation of optical properties of rat liver using single-reflectance fiber probe during ischemia and reperfusion

Optical Review - To quantify the changes in optical properties of in vivo rat liver tissue, we applied diffuse reflectance spectroscopy (DRS) system using single-reflectance fiber probe during...     

Speciation of arsenic by ion chromatography inductively coupled plasma mass spectrometry using ammonium eluents

A method based on ion chromatography (IC) and inductively coupled plasma MS (ICP-MS) was developed for the speciation of arsenic in water and soil extracts. An anion-exchange column (G3154A/101) was used to separate As(III), As(V), dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) with excellent resolution. Various ammonium salts, including NH4H2PO4, (NH4)2HPO4, (NH4)2CO3, and NH4HCO3, were examined as eluents to reduce matrix interference from chloride and to solve clogging problems. The best arsenic speciation was obtained within 9 min with excellent resolution and without interference from high chloride concentrations using an eluent containing 7.5 mM (NH4)2HPO4 at pH 7.9. The detection limits for the target arsenic species ranged from 0.1 to 0.4 microg/L with direct injection of sample without matrix elimination. The proposed method was effectively demonstrated by determining arsenic species in contaminated waters and soils of Bangladesh.     

Synthesis,Characterization, Antimicrobial Activity Screening,and Molecular Docking Study of Pyrimidine Carbonitrile Derivatives

Russian Journal of Organic Chemistry - The present work describes the synthesis of 4-amino-6-(2-benzylidenehydrazinyl)-pyrimidine-5-carbonitrile derivatives,...     

X-ray structure of [(μ-H)Os3(CO)10(μ-1,8-η2-C9H6N)]

Decacarbonyl--hydrido--1,8-²-quinoline-triosmium crystallizes in the triclinic space group P with a = 7.8551(6), b = 9.1283(8), c = 16.7915(8) Å, = 74.788(2), = 88.086(2), = 66.392(3)°, V = 1062.22(13)° ų, T = 150 K, and Z = 2. The molecule consists of an Os₃ triangle with the hydride and the heterocyclic ligand bridging the same Os—Os edge. The heterocyclic ligand is coordinated through the C(8) carbon and nitrogen atoms in a new -1,8-²-bonding mode. The Os—Os distances lie in the close range 2.8837(4)–2.9034(4) Å with an average value of 2.892(7) Å.     

Enzyme-free impedimetric glucose sensor based on gold nanoparticles/polyaniline composite film

A non-enzymatic impedimetric glucose sensor was fabricated based on the adsorption of gold nanoparticles (GNPs) onto conductive polyaniline (PANI)-modified glassy carbon electrode (GCE). The modified electrode (GCE/PANI/GNPs) was characterized by using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and scanning electron microscopy (SEM). The determination of glucose concentration was based on the measurement of EIS with the mediation of electron transfer by ferricyanide ([Fe(CN)₆]^3?). The [Fe(CN)₆]^3? is reduced to ferrocyanide ([Fe(CN)₆]^4?), which in turn is oxidized at GCE/PANI/GNPs. An increase in the glucose concentration results in an increase in the diffusion current density of the [Fe(CN)₆]^4? oxidation, which corresponds to a decrease in the faradaic charge transfer resistance (R _ct). A wide linear concentration range from 0.3 to 10 mM with a lower detection limit of 0.1 mM for glucose was obtained. The proposed sensor shows high sensitivity, good reproducibility, and stability. In addition, the sensor exhibits no interference from common interfering substances such as ascorbic acid, acetaminophen, and uric acid.     

Mechano-optical wavelength tuning in a photonic crystal microcavity with sub-1 V drive voltage

A micro-bimorph cantilever with self-aligned nanotips is monolithically integrated with a photonic crystal based device using optical and deep UV lithography techniques. Upon electrostatic actuation, the dielectric nanotips perturb the optical field, providing electromechano-optical modulation of light. Static tuning of the optical transmission spectra by more than 600 pm is measured with a sub-1 V drive voltage, resulting in a modulation as high as 21 dB. The observed strong electromechano-optical effect may find application in power efficient devices for optical communication networks, such as wavelength routing elements.     

Preparation of Hierarchical Porous Activated Carbon from Banana Leaves for High-performance Supercapacitor: Effect of Type of Electrolytes on Performance

We demonstrate a facile efficient way to fabricate activated carbon nanosheets (ACNSs) consisting of hierarchical porous carbon materials. Simply heating banana leaves with K₂CO₃ produce ACNSs having a unique combination of macro-, meso- and micropores with a high specific surface area of ∼1459 m² g⁻¹. The effects of different electrolytes on the electrochemical supercapacitor performance and stability of the ACNSs are tested using a two-electrode system. The specific capacitance (C_sp) values are 55, 114, and 190 F g⁻¹ in aqueous 0.5 M sodium sulfate, organic 1 M tetraethylammonium tetrafluoroborate in acetonitrile, and pure ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF₆]) electrolytes, respectively. The ACNSs also shows the largest potential window of 3.0 V, the highest specific energy (59 Wh kg⁻¹) and specific power (750 W kg⁻¹) in [BMIM][PF₆]. A mini-prototype device is prepared to demonstrate the practicality of the ACNSs.