VOLUME 40, NO5, OCT-2018
12
 
Decolorization of Reactive Azo Dye Remazol Black B by Using Advanced Oxidation Processes (AOPs)

Nabeela Firdous, Irfan Ahmed Shaikh and Rukhsana Shahid

This study was carried out to ascertain the effect of photochemical and non-photochemical AOPs (O3 alone, O3/H2O2, UV alone, UV/H2O2 and Fenton’s process) on the decolorization of sulphatoethylesulphone reactive group azo dye (Remazol Black B). All experiments were performed on a laboratory scale set-up and room temperature. Initial results showed that decolorization by UV alone were not effective because dye was photolytically stable and resistant to direct UV irradiation. However, the addition of appropriate amount of H2O2 improved color removal efficacy and the dye degradation. The research results showed that color removal efficiencies by O3/H2O2, UV/H2O2 of synthetic dye solution containing 100 mg/l concentration were found efficient. Ozone assisted hydrogen peroxide (O3/H2O2) treatment yielded about 98% decolorization at pH 9 and 25 minutes ozone exposure time. At 15 minutes of UV exposure with 4.4 mM H2O2 dose, 99% color removal efficiency was achieved. It is evident from results that the addition of H2O2 in the O3 and with UV irradiation accelerated the decomposition and degradation of synthetic dye solution through an increased rate of hydroxyl radical (HO•) generation which has high oxidation potential. Fenton’s process (H2O2/Fe+2 reagent) showing remarkable results (99.9%) in terms of color removal in just 5 minutes at pH 3 while keeping optimal iron (Fe2+) dose of 0.25 mM and hydrogen peroxide (H2O2, 30% w/w ) concentration 2.2 mM in effluent. Ultraviolet (UV) assisted with H2O2 also proved promising technique after Fenton’s process. There was about 99% color removal in 15 minutes UV exposure time at pH 5 value. Findings of the study clearly revealed that synthetic dye (Remazol Black B) effluent was degraded successfully by all examined advanced oxidation processes (AOPs) except UV alone irradiation at feasible treatment time, initial pH and adequate H2O2 dose value.
Pages(828)
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Elemental Analysis in the Indigenous Medicinal Plant Moringa oleifera and their Association with Ameliorative Activity

Shahnaz Dilawar, Afzal Shah, Shahnaz, Hidayat Ullah Khan, Saima Imad and KhaulaShirin

Trace elements aid numerous biochemical processes in the human body. The main cause of many health problems in man are either deficiency or excess of minerals. Hence, screening of the definite bio-active” constituents of plant source and evaluation of elemental composition of the extensively used medicinal plants is greatly vital. An effort was made to find out the elemental constituents of diverse parts of Moringa oleifera including fruit, leaves, bark, stem and flower at trace levels from Laki Marwat, Bannu and D.I. Khan. Trace elements were quantified applying atomic absorption spectrophotometer (AAS). The amount of Selenium (Se), Zinc (Zn), Copper (Cu) and Iron (Fe) in stems, flowers, barks, leaves and fruits of Moringa oleifera from Laki Marwat is relatively greater than those of Bannu and D.I. Khan. The results reveal that the amounts of trace elements in various aerial parts of M. oleifera are highly dependent on harvesting sites.”Various aerial parts of M. oleifera were observed to have ample amounts of Zn, Se, Fe and Cu.
Pages(834)
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Adsorption-Desorption Characteristics of Zinc and Copper in Oxisol and Ultisol Amended With Sewage Sludge

Ramadan Mohamed Aishah, Jusop Shamshuddin, Che Ishak Fauziah, Abdu Arifin and Qurban Ali Panhwar

The process of adsorption-desorption of zinc and copper in highly weathered soils may affect their mobility and toxicity. In this study, we evaluated the effect of sewage sludge application on the adsorption-desorption behavior of Zn and Cu in highly weathered soils. Laboratory batch experiments were carried out to investigate the adsorption and desorption of Zn and Cu in an Oxisol and Ultisol amended with three rates of sewage sludge (T1=0% (control), T2=5% and T3 =10% sludge). The findings showed that sewage sludge application had significantly affected the processes of adsorption-desorption of the tested soils. This is shown by the systematic change of the distribution coefficients (Kd). Comparison between Kd values for both soils indicated the following selectivity of metals: Cu > Zn. It is clear that Zn adsorption was lower than that of the Cu. Generally, metals adsorption-desorption was higher in the Ultisol compared to that of the Oxisol which was due to Ultisol having higher CEC and OM content in comparison to those of the Oxisol. The adsorption isotherms of Zn and Cu of both soils were well fitted to linear Freundlich and Langmuir equations (with minimum R2 = 0.96 and maximum R2 = 0.99, respectively). The adsorption-desorption of metals was strongly correlated (p<0.05) with sewage sludge rates, CEC and OM.
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Simultaneous Determination of Piroxicam and 5-hydroxypiroxicam: HPLC/UV Method Development, Validation and Application for Pharmacokinetic Evaluation in Pakistani Population

Naila Shahbaz, Zafar Iqbal, Fazli Nasir, Fahim Ullah Khan, Amanullah Muhammad Hassan and Sumaira Irum Khan

Aim of the present study was to develop and validate a rapid, selective, sensitive and economical reverse phase high performance liquid chromatography (RP-HPLC) method for quantification of Piroxicam, 5-hydroxypiroxicam (metabolite) and internal standard (meloxicam) in human plasma and evaluation of pharmacokinetics of piroxicam in Pakistani population, using the developed RP-HPLC/UV method. Piroxicam, 5- hydroxypiroxicam and internal standard (I.S) were separated using a CNW C18 RP (250 mm × 4.6 mm, 5 µm) column as a stationary phase and mixture of acetonitrile and aqueous solution of triflouro acetic acid (0.05%) in the ratio of 62:38 was used as a mobile phase. The flow of mobile phase was adjusted at the rate of 1 mL/min under the ambient temperature and eluents were studied at 353 nm. The analysis time was 8 min. The spiked and real plasma samples were processed using acetonitrile and diethyl ether as protein precipitating agent and extraction solvent, respectively. Blood samples were collected from all volunteers at different time intervals i.e., 0.5, 1, 1.5, 2, 2.5, 3, 4, 6, 8, 24, 48, 72 and 96 hr after taking piroxicam 20 mg oral dose. Various pharmacokinetic parameters of piroxicam were determined like AUC0−96 hr (104074.2029 ± 21782.84582 ng-h/mL), clearance (2.362155 ± 0.532145 mL/min), volume of distribution (8.858337 ± 1.549941 L) and elimination half-life (55.89 ± 10.39 hr), after analyzing the human plasma samples
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Determination of Urinary Total Hydroxyproline by HPLC with UV and EC Detectors

Betül İşiner Kaya, Emrah Dural, Erdal Kendüzler and Tülin Söylemezoğlu

Hydroxyproline is found in high concentrations in connective tissue proteins. It is remarkably useful to detect it because variation in urine levels of hydroxyproline is associated with various diseases. High performance liquid chromatography methods, in which ultraviolet and electrochemical detectors were used, were developed and validated for the determination of hydroxyproline in urine. Both methods included acid hydrolysis and derivation. The most appropriate time, temperature and pH were identified to optimize derivatization processes. Limits of detection were calculated as 1.57 µg/mL, 0.9 µg/mL and limits of quantification were 4.76 µg/mL, 2.73 µg/mL for UVD and ECD methods, respectively. Precision and accuracy of the methods were obtained ≤10.9 % (RSD), ≤11.5% (RE). The recoveries were found 108±6% and 102±7% for UVD and ECD methods, respectively. A strong, positive and linear correlation was found between hydroxyproline values obtained from UVD and ECD methods (p<0.01, r=+0.98). After optimization and validation of these methods, OHP levels in urine samples which were obtained from non-smokers and smokers were analyzed and, observed OHP/creatinine levels were compared. Results of both methods showed that total urinary OHP values of smokers were significantly higher than non-smokers (p<0.05).
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Innovative Approach towards the Synthesis of Carbon Nanotubes from Natural Gas Using Iron Doped Red Mud

Muhammad Bilal, Tariq Mahmood, Javed Ali and Fozia Sultana

Red mud is a waste product of aluminum industry, produced during Bayer process. It mainly contains iron, potassium, aluminum and zinc. Currently, it is being used for the synthesis of carbon nanotubes. However, red mud, obtained from different ores, has diverse effects on the size of carbon nanotubes. Therefore, this work represents the composition of red mud produced in Pakistan. The effect of different iron concentration in red mud, on the synthesis of CNTs, was studied. Proton Induced X-rays emission was carried out to investigate the elements present in raw red mud. X-rays Diffraction crystallography of raw red mud showed that red mud had a mixture of quartz, hematite, goethite and hydro-garnet etc. Fourier Transform Infrared Spectroscopic studies gave stretching and bending vibration of OH bound to Fe, Al, and Si-O vibration. Carbon nanotubes were synthesized, using different reaction conditions i.e. temperature, un-doped and doped red mud. Methane was used as a source for carbon nanotubes. The reaction was carried out in a tube furnace over undoped and iron doped red mud separately. Scanning electron microscopy showed that CNTs with reduced sizes were observed on iron doped red mud.
Pages(876)
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Effect of Heat Treatment and La Doping on the Electrical Properties of BiFeO3

Fazal Ullah, M.S. Awan, Z. Wazir, Irfan Sabir, A. ul Haq

La doped phase-pure multiferroic BiFeO3 (BFO) was prepared by the co-precipitation method using precursor bismuth oxide and iron nitrate Nona hydrate. The pallets of pure BFO were sintered in the temperature range from 500 to 650 °C for 1h in air. The structure of as-synthesized powders and pallets were studied by Powder X-ray diffraction method. Surface morphology was characterized by the Field Emission Scanning Electron Microscope and their dielectric properties were investigated as a function of sintering temperature and La doping. The DC electrical resistivity as a function of temperature was also measured. It is concluded that optimum sintering temperature is 500 °C to obtain pure phase of BFO. The grain size of the pallets was found to increase as a function of sintering temperature for the samples whereas grain size has decreased as a function of La doping. The pallets of both pure and La doped samples exhibited high AC resistivity, dielectric constant and low dielectric loss values.
Pages(886)
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Application of Acid Dyes on Nylon Fabric and Evaluation of Fastness Properties Part III

Zeeshan Akhtar, Mohib Reza Kazmi, Syed Imran Ali, Naseem Abbas and Rasheeda Parveen

A series of novel acid dyes, based on substituted aryl amines as diazo component and aminohydroxy-naphthalene sulfonic acid as coupling component were explored for their dyeing performance over nylon fabric. The dyes were applied on fabric by exhaust dyeing procedure and the resulting dyed fabrics were characterized for washing, light, perspiration and rubbing fastness properties. The results revealed excellent fixation, binding strength and fastness properties which indicate that the newly synthesized dyes are suitable for dyeing nylon fibers.
Pages(898)
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Charge Transfer Complexes of Antihistamines with Curcumin: Spectrophotometric Determination in Pharmaceutical Formulations

Saman Naeem, Saeeda Nadir Ali, Amtul Qayoom, Haji Muhammad Urooj Haroon and Shazia Nisar

An empirical spectrophotometric method for the determination of five antihistamines is carried out. The method is based on formation of a 1:1 charge transfer complex of promethazine, diphenhydramine, desloratadine, levocetirizine and loratadine with curcumin. Association between antihistamines and curcumin was confirmed by FT-IR spectroscopy. Method showed linear calibration curves over the range 20-140, 32-128, 18-126, 22-154 and 35-107 μg mL-1 respectively with correlation coefficient greater than 0.9981. The reliability of method was conferred by satisfactory recovery values greater than 98.45%. Moreover, the spectral characteristics including oscillator’s strength, dipole moment, ionization potential, resonance energy and the thermodynamic parameters (association constant and Gibb’s free energy changes) were investigated. The implementation of proposed method can help analysis of antihistaminic drugs in pharmaceutical formulations without interference of excipients.
Pages(904)
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Synthesis, Characterization and Biological Screening of Ni(II), Co(II) and Cu(II) Complexes with Schiff Base Ligand: N,N'-Bis[1-(4-chlorophenyl)ethylidene]ethane-1,2-diamine

Muhammad Aslam, Itrat Anis, Zahra Noreen, Asad Gulzar and Muhammad Tahir Hussain

The Schiff base ligand (SBL), N,N'-Bis[1-(4-chlorophenyl)ethylidene]ethane-1,2-diamine (L), was synthesized by condensation of 4-chloroacetophenone with ethylenediamine which was then employed for the synthesis of complexes (1-3) with transition metal(II) ions. The characterization of these compounds was performed by CHN analyses, spectroscopic (1H-NMR, 13C-NMR, IR and MS) and molar conductance data. The structure of L was further confirmed by using XRD. On the basis of electronic spectra and magnetic moment data, an octahedral geometry was proposed for all synthesized complexes (1-3). The conductivity data was used for the confirmation of non-electrolytic nature of these complexes. The Schiff base ligand had a lower antibacterial activity and lethality to shrimp larvae than its complexes (1-3).
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