Voltammetric Determination of Isoniazid Drug in Various Matrix by Using CuOx Decorated MW‐CNT Modified Glassy Carbon Electrode

Copper oxide decorated multi‐walled carbon nanotube (MWCNT) modified glassy carbon electrode (GCE) was prepared for determination of isoniazid (INZ) in various matrices. The electrochemical behavior of INZ was tested with the aid of Cyclic Voltammetry (CV) and quantitative experiments were performed by using Linear Sweep Voltammetry (LSV). Morphological and structural characterization of the modified electrode was performed by utilizing Scanning Electron Microscopy (SEM), X‐Ray Photoelectron Spectroscopy (XPS) while electrochemical characterization was performed by using CV and Electrochemical Impedance spectroscopy (EIS). The proposed sensor exhibited well defined anodic peak at 0.30 V for INZ at pH 6.0 medium. Under the optimum conditions, a linear relation between INZ concentration and peak current was observed in the range of 2.0×10^?7 to 5.0×10^?5 M. Limit of detection was calculated as 1.0×10^?8 M and repeatability and accuracy was found as 5.60 % and 91.0 % for 5.0 10^?7 M INZ by using 3 successive measurement, respectively. Then, the analytic performance of the electrode developed was tested by analyzing commercial tablets, artificial human serum and urine samples. The results indicated that satisfactory recoveries was observed for all issue.     

Efficient synthesis of ferrocenylenones by Friedel-Crafts acylation with EtAlCl2-Me3Al

Efficient synthesis of ferrocenylenones using a Friedel-Crafts acylation reaction is described. Acryloyl, methacryloyl, crotonoyl, cinnamoyl, and β-methylcrotonoyl chlorides react with ferrocene in the presence of a Lewis acid (EtAlCl₂ or EtAlCl₂-Me₃Al) to give the corresponding ferrocenylenones (acryloyl, methacryloyl, crotonoyl, cinnamoyl, and methylcrotonoylferrocenes) in good isolated yields. Besides ferrocenylenones, chloroactylferrocene is also synthesised by this method.     

Bioengineering functional copolymers. III. Synthesis of biocompatible poly[(N‐isopropylacrylamide‐co‐maleic anhydride)‐g‐poly(ethylene oxide)]/poly(ethylene imine) macrocomplexes and their thermostabilization effect on the activity of the enzyme penicillin G acylase

Stimuli‐responsive poly[(N‐isopropylacrylamide‐co‐maleic anhydride)‐g‐poly(ethylene oxide)]/poly(ethylene imine) macrobranched macrocomplexes were synthesized by (1) the radical copolymerization of N‐isopropylacrylamide and maleic anhydride with α,α′‐azobisisobutyronitrile as an initiator in 1,4‐dioxane at 65 °C under a nitrogen atmosphere, (2) the polyesterification (grafting) of prepared poly(N‐isopropylacrylamide‐co‐maleic anhydride) containing less than 20 mol % anhydride units with α‐hydroxy‐ω‐methoxy‐poly(ethylene oxide)s having different number‐average molecular weights (M_n = 4000, 10,000, or 20,000), and (3) the incorporation of macrobranched copolymers with poly(ethylene imine) (M_n = 60,000). The composition and structure of the synthesized copolymer systems were determined by Fourier transform infrared, ¹H and ¹³C NMR spectroscopy, and chemical and elemental analyses. The important properties of the copolymer systems (e.g., the viscosity, thermal and pH sensitivities, and lower critical solution temperature behavior) changed with increases in the molecular weight, composition, and length of the macrobranched hydrophobic domains. These copolymers with reactive anhydride and carboxylic groups were used for the stabilization of penicillin G acylase (PGA). The conjugation of the enzyme with the copolymers significantly increased the thermal stability of PGA (three times at 45 °C and two times at 65 °C). © 2003 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 41: 1580–1593, 2003     

Enantioselective reduction of ketones with borane catalyzed by cyclic β- amino alcohols prepared from proline

New catalysts have been prepared from (S)- and (R)- proline and the asymmetric borane reduction of prochiral ketones using these catalysts has been studied. The secondary alcohols were obtained in 76–95% yield with 57– 96% enantiomeric excesses.     

Detection of toluene diisocyanate with a coated quartz piezoelectric crystal: Part 3. Practical coatings for a humidity-corrected detector

Dithizone and tri-n-octylphosphine oxide (TOPO) were tested as coatings for quartz piezoelectric crystals to be used in a detector for touene diisocyanate (TDI). Cobalt(II) chloride and polyethylene glycol (PEG) with molecular weights of 400 and 1540 were tested for suitability as coatings for detecting humidity variations so that correction for humidity could be obtained from a two-crystal system. Sensitivities for TDI of 12 and 75 Hz ppm^?1 were found with dithizone and TOPO, respectively, between 0 and 1 ppm TDI. Cobalt chloride-coated crystals showed a sensitivity for water of 0.053 Hz ppm^?1 at 8000 ppm water and about 40 Hz ppm^?1 for TDI at the 2 ppm level. PEG-400 and PEG-1540 provided sensitivities to water of 0.038 and 0.051 Hz ppm^?1 respectively, and the response was linear over the range 9000—13 000 ppm water. All coatings showed irreversible behaviour towards TDI.     

Selective pre-concentration of selenite from aqueous samples using mercapto-silica

Silica gel modified with 3-mercaptopropyl-trimethoxysilane was used for the selective separation and pre-concentration of selenite (Se(IV)) from aqueous solutions containing Se(IV) and selenate (Se(VI)). Over a wide range of acidity, from 2 mol l⁻¹ HCl to pH 9.00, Se(IV) was taken up by the mercaptopropyl-silica with nearly 100% efficiency; Se(VI) however was unretained. Se(IV) content was determined by hydride generation atomic absorption spectrometry (HGAAS), following batch release of the selenium from the pre-concentration medium by acidic periodate. The overall pre-concentration efficiency, including both take-up and elution, in the range of 89-106%. The method was applied to spiked seawater samples containing as low as 800 ng l⁻¹ Se in selenite form. This solid-phase extraction system offers several major advantages over conventional solvent extraction procedures. It firstly exhibits high selectivity for Se(IV) over Se(VI). Using the solid-phase media, pre-concentration of Se(IV) in dilute water samples can be carried out in the field, stabilizing the selenite-selenium in a convenient form for transport and storage. In addition, selenium stored on silica is derived solely from Se(IV) overcoming problems of selenium redox speciation changes and loss during storage.     

Chemistry and the Origin of Life

The natural genesis of life on Earth is a hypothesis of evolutionary science; it is the task of synthetic organic chemistry to test this hypothesis experimentally. The aim of an experimental aetiological chemistry is not primarily to delineate the pathways along which our (‘natural’) life on Earth could have originated, but to provide decisive experimental evidence, through the realization of model systems (‘artificial chemical life’), that life can arise as a result of the organization of organic matter.     

膜流动电位测试中Ag-AgCl电极的制备及稳定性研究

膜的动电特性研究中,往往采用流动电位方法。该方法中,Ag-Ag Cl测试电极的质量是影响测试准确性的关键要素。本文采用正交试验设计和方差分析,着重考察电解法制备Ag-Ag Cl电极过程中,电流强度(I)、氯化时间(t)、电解质溶液浓度(CHCl)、电极来源(n)、烘烤温度(T)、活化电极溶液浓度(CKCl)等因素对Ag-Ag Cl电极稳定性的影响。得到Ag-Ag Cl电极的最优制备参数为:电流密度3.0m A/cm2,氯化时间50min,盐酸浓度0.1mol·L-1,烘烤温度120℃,活化电极溶液(KCl)浓度0.001mol·L-1;最显著影响因素为电极来源,显著影响因素为氯化时间和烘烤温度。对最优条件组合下制备的AgAg Cl电极,进行了稳定性实验,结果表明:制备的电极具有较好的稳定性,24h内电极电位漂移量小于0.10mv,7天内电极电位漂移量小于0.2mv;在聚偏氟乙烯中空纤维超滤膜流动电位测试中,流动电位与流动压差具有良好的线性和可重复性,回归曲线R20.99,变化规律符合Helmholtz-Smoluehowski公式,可以较好满足膜的流动电位测试要求。