Vol. 8 & Issue 1 ; Section A : Chemical Sciences

Date : Nov.2017 to Jan.2018


Application of Full Factorial Design for Uranium Extraction from High Strength Commercial Phosphoric Acid using rganic Solvents

M. M. Ali,  Azza A. Attia,  M.H. Taha, A. M. Masoud,  and A. M. Abo-Raia,

JCBPS; Section A; November 2017 – January 2018, Vol. 8, No. 1; 001-015.

[DOI: 10.24214/jcbps.A.8.1.00115.]

  • Abstract

    Uranium extraction from high strength phosphoric acid, 45 % P2O5, has been investigated using organic solvent; D2EHPA & TOPO mixture in kerosene under various experimental conditions in order to optimize the extraction process. Three factors (D2EHPA & TOPO concentration, aqueous/ organic phase ratio, and reaction temperature) at two value levels were studied. The factorial design analysis was performed in order to identify the main and the interaction effects of the various factors. The obtained results shown that, at 95% confidence intervals, D2EHPA & TOPO concentration, aqueous/ organic phase ratio, reaction temperature and D2EHPA & TOPO concentration- aqueous/ organic phase ratiointeraction are statistically significant to uranium extraction process. The optimum conditions have been determined as, 1.0 M D2EHPA & 0.25 M TOPO mixture in kerosene, shaking time of 4 min, temperature 30 oC, and aqueous/ organic phase ratio (R aq / org) equal 4. Under these optimum conditions, the overall uranium extraction efficiency performance is 88.3 %.

Degradation and Bioremediation of The Pesticide Cypermethrin” by Pseudomonas spp and Bacillus spp

Madhu Shree. T & Priya R. Iyer,

JCBPS; Section A; November 2017 – January 2018, Vol. 8, No. 1; 016-027,

[DOI: 10.24214/jcbps.A.8.1. 01627.]

  • Abstract

    In this present study, we have used two species of bacteria namely Pseudomonas and Bacillus to degrade cypermethrin from the contaminated crop fields for the purpose of bioremediation and focussing on the reduction of pyrethroid toxicity in the surrounding environment. The above stated two microorganisms were isoloated and characterised. The various underlying factors like different pH, temperature and concentration corresponding to the growth and the degree of degradation of the pesticide cypermethrin were determined. Thin layer chromatography and spectrophotometric method were done in support of the cypermethrin degradation. The genetic transformation of the plasmids which aided in the degrading of the pesticide were carried out in a suitable vector.

Synthesis and Characterization of ZnO Nanorods for Voltammetric Detection of Dopamine, Folic Acid and Paracetamol

S.R.Kiran Kumar, G. P. Mamatha, H. B. Muralidhara, M S Raghu4, S.Archana,K. Yogesh Kumar

JCBPS; Section A; November 2017 – January - 2018, Vol. 8, No. 1; 028-039.

[DOI: 10.24214/jcbps.A.8.1.02839.]

  • Abstract

    In present global scenario the ability to detect and quantify specific biologically active molecules plays an increasingly important role in our safety and wellbeing. In this regard, the present work involves the synthesis of ZnO nanorods (ZnO) via simple hydrothermal method and the nanopowder is used for modification carbon paste electrode (MCPE) and to study voltammetric detection of Dopamine (DA), Folic acid (FA) and paracetamol (PC). The synthesized ZnO nanorods were characterized by X-ray diffraction studies (XRD), Scanning electron microscopy (SEM) and Tunneling electron microscopy (TEM). In this study the ZnOs modified carbon paste electrode was applied for the electrochemical determination of dopamine at pH 7.2 PBS solution with scan rate 50 mVs-1. The voltammograms obtained during the oxidation studies revealed that ZnO nanorods exhibits better catalytic function towards the oxidation of Dopamine, Folic acid and Paracetamol. The overlapping voltammetric response of the biomolecules at the bare electrode gets resolved into well-defined voltammetric peaks with enhanced oxidation currents. The developed ZnOs /MCPE offered high catalytic activity in sensing the dopamine, paracetamol and Folic acid in the development of biosensors

Analysis of aflatoxin B1 in Brazil nuts: method optimization and validation

Nadia Regina Rodrigues, Ana Paula Ferreira de Souza

JCBPS; Section A; November 2017 – January - 2018, Vol. 8, No. 1; 040-049.

[DOI: 10.24214/jcbps.A.8.1.04049.]

  • Abstract

    A method for the determination of aflatoxin B1 was validated according to criteria by SANTÉ 11945/2015. The samples were extracted with acetonitrile and the cleaning step was not performed. Quantification was made by liquid chromatography with fluorescence detector and pre-column derivatization with trifluoroacetic acid. No matrix effect was observed and linearity was obtained in the range of 5 - 80 μg L-1. The recoveries ranged from 73% to 85% with a coefficient of variation of less than 5%. The quantification limit was 6 μg kg-1 and the measurement uncertainty was ± 0.18 μg kg-1 for this level. This method was applied to 14 real samples purchased in the local market and contamination was found in one sample above the limit tolerated by the legislation (59 μg kg-1). It is a low cost method with good sensitivity and easy to execute.

High Performance Liquid Chromatographic Determination of Methyldopa in Bulk and Dosage forms

O. A. O. Mohammed, S.W. Shantier, I. O. Abu reid, E. A. Gadkariem

JCBPS; Section A; November 2017 – January - 2018, Vol. 8, No. 1; 050-056.

[DOI: 10.24214/jcbps.A.8.1.05056]

  • Abstract

    High performance chromatographic determination of methyldopa in bulk and tablet form was carried out on a C18 column (250 x 4.6 mm with particle size of 5 micrometer) using a mixture of phosphate buffer pH 2.8 and acetonitrile (95: 5 v/v) as the mobile phase pumped at flow rate of 1 ml/min. Constructed calibration curve was linear in the concentration range (25-250 μg/ml) with correlation coefficient of 1.0000. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.91μg/ml and 2.77μg/ml, respectively. The accuracy and the precision of the developed method were very good (RSD ˂ 2%). The validity of the proposed method was confirmed through the statistical comparison of the obtained data with those of the official USP method.

Physico-chemical Studies of Solvation Behaviour of Some Chromium (III) Complexes in Nitromethane and Dimethyl Sulfoxide at 298.15, 308.15 and 318.15 K

Priyanka Sandhu and Hardeep Anand

JCBPS; Section A; November 2017 – January - 2018, Vol. 8, No. 1; 057-067.

[DOI: 10.24214/jcbps.A.8.1.05767]

  • Abstract

    Viscosity (η) and molar conductance (Λ) of (C4H9)4NBPh4, (C4H9)4NClO4, NH4X,(C3H7)4NX and (C4H9)4NX (X= [Cr(NCS)4(NH3)2]-) have been measured in nitromethane (NM) and dimethylsulphoxide (DMSO) at 298.15, 308.15 and 318.15 K temperatures at various salt concentrations. The ultrasonic velocity data has been analysed to obtain limiting apparent molal isentropic compressibility ( Ko s , ø  ) of the electrolytes. The viscosity data has been analyzed by Jones-Dole equation to evaluate viscosity B ± coefficients. The conductance data has been analysed by the Shedlovsky method to evaluate Λo and KA. The derived limiting parameters were split into the ionic contributions of the salts using which the limiting ionic apparent molal isentropic compressibility (Ko s , ø )±, viscosity B± coefficients and solvated radii (ri) of various ions have been evaluated. Isentropic compressibility results show that all these ions possess weak interaction with different solvents involving solvophobic interactions. The A-coefficients are in reasonable good agreement with the limiting theoretical values (An) calculated using Falkenhagen-Vernon equation. Viscosity B± coefficients confirm the existence of interactions of the complex with the solvent molecules. The ion-solvent interactions are confirmed by the solvated radii (ri) values of the ions determined from the molar conductance.

Synthesis, Structural Characterization of Transition Metal Complex of an Oxydiacetic Acid

Tuğba Aycan and Hümeyra Paşaoğlu,

JCBPS; Section A; November 2017 – January - 2018, Vol. 8, No. 1; 068-076.

[DOI: 10.24214/jcbps.A.8.1.06876.]

  • Abstract

    Compound based on the [Cu (oda)(hydet-en)] (oda=dianion of oxydiacetic acid, hydet-en=[N-(2-hydroxyethyl)-ethylenediamine]) has been synthesized and characterized by various spectroscopic methods (IR, UV-Vis, EPR) and thermal analysis (TG/DTG/DTA). Copper complex with mix ligands was determinated by single crystal X-ray diffraction [oda]2- anion bridges Cu(II) ion with a bidentate coordination mode through its oxygen atoms of carboxylate groups. Single crystal X-ray data of the complex shows that the monomeric structure forms supramolecular frameworks with H-bonding. The FT-IR investigation of the complex was performed within the mid-IR region, mainly focusing on the characteristic (COO)as and (COO)s stretching vibrations of oxydiacetic acid. The powder electron paramagnetic resonance spectra of Cu(II) complex at RT was recorded. The results of EPR and UV-Vis spectra agree with the X-ray diffraction data

Influence of Nonionic Surfactants as Competitive Carriers in Bulk Liquid Membrane Transport of Metal Cations Using Macrocyclic Ligands

Mersiha Suljkanović , Edita Nurković , Jasmin Suljagić ,

JCBPS; Section A; November 2017 – January - 2018, Vol. 8, No. 1; 077-089.

[DOI: 10.24214/jcbps.A.8.1.07789.]

  • Abstract

    Surface active agents (surfactants) find wide application in different analytical procedures due to their amphiphilic properties and possibility of micellar aggregation. In previously published papers, interactions between different metal ions and surfactants were observed, mostly through different membrane transport techniques (emulsion liquid membranes, supported liquid membranes, bulk liquid membranes). However, standard explanation of those interactions, based on host-guest mechanism was expanded with the mechanism of micellar solubilization of metal ions or their complexes within the surfactant aggregates (micelles). In this paper, interactions of nonionic surfactants with metal ions and macrocyclic ligands within the nonpolar liquid organic membranes were investigated. Bulk liquid membrane systems were prepared on the basis of two aqueous phases: source phase (contained cations and counter ions), receiving phase (contained stripping agents) and nonaqueous (nonpolar organic) phase (contained ″carriers″ for cations). Nonionic surfactants were tested as possible carriers for cations, compared to macrocyclic ligands Experiments were performed using the homemade transport cell. Metal ions concentration in aqueous phases was monitored by flame atomic absorption spectrophotometry, after 3 hours of membrane transport. Macrocyclic ligands: 18-crown-6, dibenzo-18-crown-6, dicyclohexano-18-crown-6 and benzo-18-crown-6 dissolved in organic solvents (dichloromethane, 1,2-dichloroethane and chloroform) were used as carriers for cations. Nonionic surfactants: TX-100, Brij 35, Brij 58 and Brij 78 were investigated as possible competitive carriers within the membranes. Experiments were based on the transport of Pb(II) and Cd(II) ions. The effect of surfactant application results in in reduced cation transport, compared to macrocyclic ligand carriers, probably caused by additional cation-surfactant interactions within the membrane.

Nitrosylation of some aldimine / ketimine substituted group 6 metal carbonyls

Amar Srivastava, Rohit Mohan, Satyendra Nath Shukla and Sunil Kumar Gupta,

JCBPS; Section A; November 2017 – January - 2018, Vol. 8, No. 1; 090-094.

[DOI: 10.24214/jcbps.A.8.1.09094.]

  • Abstract

    Nitrosylation of cis-[(Aldimine/Ketimine)M(CO)4] ( M = Cr, Mo, W; Aldimne = N,N’-bis(4-(N,N-dimethylamino) benzylidene)-1,2-propanediamine and Ketimine = N,N’-bis(1-(2-methoxyphenyl)ethylidene)-1,2-propanediamine) with nitric oxide at room temperature under dry nitrogen gave a mixture of two unusual products (A and B). Products A were non-carbonyl [(NO)2(Ald/Ket)M(NO2)2] whereas products B were carbonyl [(NO)(Ald/Ket)M(CO)2(NO2)] derivatives. These derivatives were characterised by conductivity, magnetic and other physico-chemical and IR spectroscopic measurements