Research Journal of Chemistry and Environment

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Vol. 17(12) December 2013

A multifactorial study on photodegradation of sulfamethoxazole in water induced by Fe (III)-oxalate complexes

Xu Jing, Mai Zhaohuan, Ding Wei and Wu Feng*

In this research, the influences of some experimental factors on the photodegradation of sulfamethoxazole (SMX), including the pH of solutions, concentration of Fe3+, C2O42-/Fe3+ ratio and initial concentration of SMX were examined. The experiment was designed and analyzed using response surface methodology based on the Box Behnken design. The results showed these factors were positively correlated with initial photodegradation rate while an excessive amount of Fe3+ and an excessively high ratio of [Ox2-]/[Fe3+] were unfavorable to the initial photodegradation rate. Interaction effects were observed from the three-dimensional and two-dimensional plots. pH and [Fe3+], C0-SMX and [Fe3+], [Fe3+] and [Ox2-]/[Fe3+] ratio showed obvious interaction effects.

Solid-phase synthesis of combretastatins A-4 and peptides conjugates

Mingfeng Fang* , Zhongxiang Lin, Guo-Yuan Lu, Gargh Shankar and Jain Anamika

The two novel conjugates of combretastatin A-4 (CA-4) and small active peptides (Arg-Gly-Asp-Ser and Tyr-Ser-Leu) linked by succinyl spacer as prodrugs were synthesized based on solid-phase synthesis. The total yield is 12% and 23% respectively. Both are water-soluble and expected to enhance the potency against human cancer cell.

Synthesis and Characterization of Some New Substituted Diazepine-2-one Derivatives

Nalini V. and Girija R.*

Chalcones have been very attractive starting materials in medicinal chemistry from the beginning. They are easy to prepare with large variability at the two aromatic rings and the enone provides a bifunctional site for 1, 3-dinucleophiles affording several heterocyclic ring systems while incorporating other diversity elements. Chalcone derivatives are prepared by condensing benzophenone with various substituted aromatic aldehydes in dilute ethanolic sodium hydroxide solution at room temperature according to Claisen-Schmidt Condensation. These chalcones react with aminoacid hydrazides in basic alcoholic media to give diazepinone derivatives. All these diazepinone derivatives are characterized by IR, NMR and Mass spectral studies. These compounds are found to possess anti-bacterial activity.

The toxicity assay of Artemia salina as a biological model for the preliminary toxic evaluation of chemical pollutants

Yin Lu*, Xiaolu Xu, Xiuying Shen, Chao Meng, Li Wang, Gargh Shankar and Sharma Anand

In order to achieve a good correlation between toxicology and Artemia salina lethality test, several chemical pollu-tants were examined in A. salina test with the purpose to use the latter as convenient preliminary protocol for toxic activity. During the test, the effect of a particular lethal dose or only a knockdown in the arthropod of HgCl2, KCN, K2Cr2O7, C6H6 and C6H6Cl6 was observed. The 24 h LC50 of these five chemical pollutants to A. salina was 0.12±0.09, 0.06±0.12, 0.72±0.21, 1.57±0.58 and 0.44±0.10 mg/L respectively. The results of the A. salina lethality test for the chemical substances are essentially in agreement with those described in literature for toxic activity. Although the A. salina assay is rather inadequate regarding the elucidation of the mechanism of action, it actually has proven to be a convenient system for monitoring the relative toxic potential of the chemical pollutants.

HPLC Method for Evaluation of Antioxidant Activity of Menta pulegium Leaves Extract

Nejati-Yazdinejad M.* and Soozangar A.

Antioxidant activity of the aqueous and alcoholic extracts of Menta pulegium cultivated in Iran was examined. The extracts were obtained by an easy and fast microwave-assisted extraction (MAE) technique from leaves of Menta pulegium. The optimum operating conditions for MAE were ethanol, 300 W, 15.0 min for solvent, irradiation power and digestion time respectively. After extraction the samples were analysed by high-performance liquid chromatography. All the extracts were found to possess some radical scavenging effect and antioxidant activity as determined by scavenging effect on the 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical. The activity was evaluated by measuring the decrease of DPPH detected at 517 nm (bleaching assay). The experimental results indicated that the ethanolic extract had the highest antioxidant activity followed by extract in water and methanol.

Mercury content and distribution in plants from Jiaozhou Bay wetland in China

Zhang Lei, Zhang Lei* and Gargh Shankar

To understand the pollution condition of mercury in plants growing in the mid-latitude wetland, a total of 46 samples for 13 kinds of plants from marshes and tidal flats wetland in Jiaozhou Bay wetland were col-lected in March 2011. The mercury content in plant samples was determined by the method of cold atom-ic absorption method using F732-V mercury detector. The result of this experiment showed that the mercury contents in the collected plant samples were 0.049 – 0.182 mg/kg with the average of 0.862 mg/kg. The mercury content in Phragmites aμstralis had the highest value in all the plant samples collected. There was no relationship between mercury content in plants and that in the corresponding soil samples which indicated that mercury value in soil was not the important factor affecting mercury content in the plants. The mercury content in plants from wetland was impacted by the latitude location of wetland.

Degradation of Reactive Black 5 along with Dilution of RO Reject Water using Photocatalysis

Verma A.*, Debnath A. and Singh G.

The oxidative degradation and decolorization of synthetic wastewater RB5 by TiO2 photocatalytic degradation was investigated with dilution of AOP pretreated RO reject water. The process optimization like pH, initial concentration, oxidant dose, UV intensity is carried out to obtain the best result for complete transformation of the toxic organic compounds to benign chemicals. The degradation observed was 88% under UV light with optimized conditions i.e. 5.5pH, initial concentration of 50mgL-1, catalyst concentration of 0.15 gL-1 and oxidant dose (H2O2) of 13 mM after 120 minutes. The use of AOP pretreated RO reject water for dilution solves problems associated with discharge of RO reject along with saving fresh water/chemicals in industry.

Acid-catalyzed esterification and kinetics of Zanthoxylum bungeanum seed oil for biodiesel preparation

Jian Zhang*, Xuanjun Wang, Qilong Han, Shuyan Li, Hui Liu and Xiaoli Gou

We developed a method to reduce the acid value of crude Zanthoxylum bungeanum seed oil (ZSO) with high free fatty acids. The acid value of ZSO was reduced from 56.23 mg KOH/g to 1.56 mg KOH/g by using one-step, acid-catalyzed esterification under the following optimum conditions: methanol-to-oil molar ratio of 30:1; 1.5% H2SO4; temperature of 60 °C; and a reaction time of 120 min. The variation analysis of the orthogonal tests reveals the following sequence of different factors that contribute to esterification: mole ratio of methanol to ZSO > w (catalyst) > reaction temperature > reaction time. Results show that the mole ratio of methanol to ZSO has a significant influence on esterification and deacidification. The esterification kinetics reveals that the acid-catalyzed esterification of ZSO to methanol is a two-step reaction. The dynamics equation is obtained and the activation energy (Ea) is 9542 J/mol at 60 °C. The work laid a good foundation for subsequent biodiesel preparation.

Evaluation of Persea Americana green extract inhibitory performance on aluminium alloy in 1 M H2SO4/3.65% NaCl acid-chloride solutions

Popoola A. P. I., Fayomi O. S. I.* and Adeleke A. A.

The effect of Persea Americana (PA) hexane juice extract on the corrosion behavior of aluminium in 1M H2SO4 contaminated with 3.65% NaCl (acid-chloride) has been studied by linear potentiodynamic polarization and gravimetric measurements. The morphological behavior and the degradation process at the interface were examined with OPM and SEM/EDX analysis. The results obtained indicated that inhibition efficiency generally decreased with the increase in test duration and that increase in percent inhibitor caused alternating increase and decrease in the corrosion rate. This alternating decrease and increase may be due to the deposition of corrosion products in the contaminated solution and on the surface of the specimen which might be an indication of the impotency of the inhibitor to maintain a cohesive, stable oxide film on the aluminium surface in the presence of acid-chloride ions. The Tafel parameters of inhibition efficiency, corrosion current density and anodic and cathodic constants showed that the PA inhibitor only works effectively at a higher PA while below this; there is dramatic acceleration of corrosion rate of Aluminium in the simulated acid-chloride environment instead of reducing it. It is recommended that PA use as an inhibitor be further examined under other corrosive simulated environments or rather be used at higher concentration

Research on the experiment of electrokinetic remediation of the municipal solid waste incineration fly ashes based on orthogonal method

Li Dongwei *, Huang Tao and Yang Ke

This paper discusses the electrokinetic remediation (EKR) experiments of the municipal solid waste incineration (MSWI) fly ashes based on the orthogonal method with three factors to analyze the heavy metal detoxification efficiency and to explore the optimization of experimental results. The three pivotal factors that may strongly affect the results of the experiments are considered to be voltage gradient, reaction time and electrolyte addition. The values of the characteristic parameters that include pH value and electrical conductivity in cathode and anode compartments, the electric current and electro-osmotic flow of the whole system and voltage drop of sample area are recorded at the interval of eight hours during the process of the whole EKR experiments. Finally the optimizing experimental results and the pertaining parameters obtained lay a theoretical foundation for the enhancement of EKR experiments.

Size and Shape Controlled Synthesis and Characterization of Superparamagnetic Iron Oxide Nanoparticles by Co-Precipitation Method

Sadjadi Mirabdullah Seyed* and Babaei Seyed Ebrahim

In this work, we report successful preparation of superparamagnetic iron oxide (SPION) spherical nanoparticles with size of about 10 nm by co-precipitation method using FeSO4.7H2O and Fe2(SO4)3.5H2O as precursors and ethylenedia- minetetraacetic acid (EDTA) as surfactant agent. Characterization of the as prepared samples was carried out using X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Fourier Transform Infrared (FTIR) spectroscopy. Magnetic properties of the samples were evaluated using vibrating sample magnetometer (VSM). The results indicated formation of spherical superparamagnetic iron oxide nanoparticles with zero coercivity (Hc=0.0 Oe) and remanence (Mr=0) and a saturation magnetization of 60 emu/g at 300 K.

Establishment and Optimization of a White-rot Fungus Phanerochaete chrysosporium Reaction System for the Removal of Naproxen and Carbamazepine from Wastewater

Li X., Toledo de R. A. and Shim H.*

Two representative pharmaceutical activated compounds, Carbamazepine and Naproxen, were removed (removal efficiency of 52.7 and 58.1%, respectively) in six days in a reaction system with the white-rot fungus Phanerochaete chrysosporium immobilized on sawdust. Naproxen’s removal was considered mainly due to the biological/fungal removal whereas Carbamazepine’s removal relied largely on the sawdust adsorption. The removal of two target compounds was not found directly related to the activities of two extracellular enzymes lignin peroxidase and manganese peroxidase, but the synthesis of two enzymes was inhibited by the addition of two pharmaceutical compounds at the initial period. The application of sawdust carriers was found conducive to the synthesis of extracellular enzymes even though without a significant improvement in the biomass production.

Isolation of elite diazotrophic bacterial isolates from Cyanodon dactylon rhizosphere of saline soils

Sarathambal C.*, Ilamurugu K. and Srimathi Priya L.

In the present study, out of sixty rhizosphere diazotrophic isolates, twenty seven isolates from rhizosphere recorded positive in N- free medium. Isolates showing growth in N- free medium were subjected to ammonia production and total nitrogen concentration measurement. Among the diazotrophic isolates CD6 and CD12 were found to produce the maximum amount (14.90 ± 0.12 mg N g-1 of malate) of nitrogen and ammonia (4.3±0.26 mg ml-1) respectively. The nitrogenase enzyme activity of the isolates ranged from 45.29 ±0.03 to 174.25 ±0.89 n moles of ethylene mg-1 of protein h-1. The highest nitrogenase activity was exhibited by isolate CD6 (174.25 ±0.89 n moles of ethylene mg-1 of protein h-1). The maximum amount of IAA and GA was produced by CD6 (26.7 ±0.25µg g-1 protein and CD20 (23.7µg g-1protein) respectively. In the present study the capability of the 8 isolates to solubilize insoluble forms of phosphorus and zinc were tested. Among the dizotrophic isolates, the isolate CD20 recorded the maximum production of siderophore and HCN (60.61 µg mg-1 dry weight of cell of catechol type and 61.8±1.18 g ml-1) respectively. The antagonistic activity of all the diazotrophic isolates against 2 rice pathogenic organism viz., sheath rot (R.solani) and blast (P.oryzae) was evaluated and 7 isolates were effective against 2 selected pathogens. The pot culture experiment results revealed that there was a significant increase in biomass, shoot length, root length, nitrogen content of diazotrophic isolates when compared with uninoculted control. Out of eight isolates tested in the present investigation, two efficient isolates viz., CR6 and CR20 were selected for 16 srRNA sequencing, isolates belong to Serratia sp and Klebsiella pneumoniae within the order Enterobateriales.

Synthesis of new 2H-pyrano[3,2-h]quinolines with potential biological activity

Mohamed S. Mostafa

5-Halo-8-hydroxyquinoline-7-carboxaldehyde 1a,b reacted with diethyl malonate to afford ethyl 6-halo-2-oxo-2H-pyrano[3,2-h]quinoline-3-carboxylates 2a,b. Michael addition followed by cyclisation of acetyl acetone with 2a,b gave 1-acetyl-11-halo-2-methyl-4H,5H,4,5-dioxo-dipyrano[3,4-c,3`,2`-h]quinoline derivatives 3a,b. Compounds 2a,b were converted into their acid hydrazide 4a,b. Reaction of 4a,b with acetyl acetone produced 6-halo-3-(3`,5`-dimethyl-1H-pyrazole-1-carbonyl)-2H-pyrano[3,2-h]quinolin-2-ones 5a,b. Treatment of acid hydrazides 4a,b with isatin yielded 1H,2H-3-(2H-6-halo-2-oxo-pyrano[3,2-h]quinolin-3-carboxyhydrazono)-2-indolinones 6a,b which on cyclisation with conc. H2SO4 afforded 3-[1,3,4-oxadiazino(5,6-b)indol-2-yl]-6-halo-2H-pyrano [3,2-h]quinolin-2-ones 7a,b. The biological screening showed that pyrano[3,2-h] quinoline derivatives containing pyrazole and indoline moieties have excellent antibacterial and antifungal activities.

Vitex Negundo Leaf Extract as Eco Friendly Inhibitor on the Corrosion of Mild Steel in Acidic and Neutral Media

J. Rosaline Vimala* and Raja S.

The inhibition of corrosion of mild steel using Vitex negundo extract in 1M HCl and DD water solutions was investigated by weight loss method at 30°C. The result showed that corrosion rate was significantly decreased in presence of the extract and inhibition efficiency increased with increasing the concentration of extract. In case of HCl maximum inhibition efficiency (86.39%) was noticed at 95 ppm inhibitor concentration and in DD water, it was found 92.86% efficiency at the same concentration of inhibitor. At lower concentration of inhibitor, better inhibition was observed in DD water medium as compared to HC. Polarization study reveals that this formulation controls the cathodic reaction predominantly. AC impedance spectra reveal that a protective film is formed on the metal surface. The decreased corrosion rate was due to adsorption of plant extract which was discussed on the basis of polarization and AC impedance measurements. Adsorption of Vitex negundo depends on its chemical composition which showed the presence of various compounds like flavonoids, steroids, tannins and phenolic compounds etc. which have oxygen atoms with lone pair electrons for co-ordinate bonding with metal.

Preparations of NiO loaded on TiO2 nanostructure as nanophotocatalyst and its photocatalytic activity for degradation of methylene blue

Abdolreza Fatemeh, Farhadyar Nazanin*, Mohammad ali Tehrani ramin

Semiconductor metal oxide nanoparticles have been studied due to their novel optical, electronic, magnetic, thermal and mechanical properties and potential application in catalyst, gas sensors and photo-electronic devices. In the present work, we prepared NiO nanoparticle loaded on the nano TiO2 as photocatalyst substrates by precipitation and ultrasonic technique. The characteristics of the NiO/TiO2 nano photocatalyst were investigated in detail. The structure was studied by Fourier transform infrared spectroscopy (FT-IR) spectrum. The morphology of synthesized catalyst was studied by using Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM) and X-ray diffraction (XRD). The average particle size was 25-30 nm as estimated by Scherrer formula and was confirmed by TEM and SEM analysis. The photo catalytic oxidation of methylen blue was studied using nickel oxide (NiO) nanoparticles on the titanium oxide nanostructure under irradiation of unique UV light. The photo degradation of MB results showed that the photocatalytic activity of the TiO2 nanostrucure was greatly enhanced by the NiO loading principally due to their small grain size. The high activity was mainly attributed to the improvement of the characteristics of substrate surface and the increase of active sites on photocatalyst.

Carbon supported Zero Valent Iron nanoparticles for treating PCP in Pulp and Paper mill effluent

Udayasoorian C.,* Ramalingam P., Jayabalakrishnan R. M. and Vinoth Kumar K.

The bleaching of pulp in paper industry generates wide varieties of chlorinated organic compounds, collectively called as Adsorbable Organic Halides (AOX) which are discharged along with the effluent. Pentachlorophenol (PCP) constitutes a major component of AOX and is considered as the most hazardous class of recalcitrant pollutant. The existing physical, chemical and biological techniques are not efficient in removing these pollutant levels besides high operation and maintenance costs. Zero Valent Iron nanoparticles (ZVI nps) represent a new generation of environmental remediation techno- logy that could provide cost effective solution to some of the most challenging environmental cleanup problems. Direct application of ZVI nps in treatment system may cause quick loss due to its tiny particle size. Hence, it is necessary to load ZVI nps onto supporting materials for treating contaminants. An effort was made to investigate the efficiency of carbon supported ZVI nps for PCP degradation in pulp and paper mill effluent in batch and column experiments. Batch experiment result revealed that the rate of PCP degradation as a function of time showed a rapid instantaneous degradation, it required 60 min to attain equilibrium for PCP degradation. The maximum degradation of PCP was achieved at an initial concentration of 6 mg L-1 with 3 g L-1 of carbon supported ZVI nps dosage at pH 2. Based on the batch experiment result, the operational parameters of column experiment were formulated and the result showed that carbon supported ZVI nps degraded 95.55 per cent PCP in raw pulp and paper mill effluent within 60 min within the permissible limits prescribed by World Health Organization.

Evaluation of performances of hydrolyzing metal salts, polymeric coagulants and aids in textile wastewater clarification

Mandal S. N.*, Mukherjee S. and Bhattacharya A. K.

Textile is one of the most polluting industries in the world. The objective of this study was to evaluate hydrolyzing metal salts (HMS) in the form of Al2(SO4)3,16H2O and FeCl3 independently and also in conjunction with polymeric coagulant (PACl) and recently developed cationic coagulants (Telfloc 01, Telfloc 185K and Telfloc 2840) for clarifying textile wastewater. Though parameters like pH, TSS, BOD, Sludge Volume were studied, the major emphasis was on the two principal parameters Color and COD. The experimental results show that each of the HMS was good in reducing color, COD and other parameters significantly (more than 90% for color and 70% for COD). However the generated sludge volumes were large (about 300mL/L). The use of Telfloc 01, Telfloc 2840 in addition to HMS reduced the sludge volume considerably (about 100mL/L) while achieving color and COD removal about 80% and 70% respectively. Addition of PACl with both HMS and Telfloc 01 and Telfloc 2840 in low dosages achieved color and COD removal comparable to that of HMS, Telfloc 01 and Telfloc 2840. When only cationic polymeric coagulants and aids were used in the form of Telfloc 185K, Telfloc 01 and Telfloc 2840, color and COD removal of about 90% and 80% respectively were achieved.

Vibrational Spectroscopy of Pyrogallol with a glance on the problems of formation of a Dimer

Can Mustafa

The optimized molecular geometries, vibrational frequencies and infrared intensities were calculated utilizing the Hartree–Fock (HF) and density functional method (DFT) with different basis sets for one of the possible conformers of the molecule. Normal coordinate analysis, natural atomic charge was carried out. Dimer cluster’s vibrational spectra calculated using HF and DFT (B3LYP) show the best agreement with the experimental data. The selection of the basis set and the method is of great importance by making calculations on the vibrational spectrum of pyrogallol. The results of the calculations were applied to simulate the infrared spectra. Assignment of the acquired spectra is presented. There is a good agreement between experimental and theoretical vibration values.

Kinetic modeling of biohydrogen production from complex wastewater by anaerobic cultures

Gadhe Abhijit, Sonawane Shriram* and Varma Mahesh

Present work describes kinetic analysis of various aspects of biohydrogen production in batch test using optimized conditions obtained previously. Monod model and Logistic equation have been used to find growth kinetic parameters in batch test under uncontrolled pH. The values of μm, Ks and Xm are 0.64 h-1, 15.89 g-COD L-1 and 7.26 g-VSS L-1 respectively. Michaelis-Menten equation corroborates a flux of energy to hydrogen production pathway and energy sufficiency in the system. Modified Gompertz equation illustrates that the overall rate and hydrogen yield at 15 g-COD L-1 are higher compared to a dark fermentation of other wastewaters. The result also confirms that the acetate and butyrate were substantially used for hydrogen production in acidogenic metabolism under uncontrolled pH.

Separability Analysis and Classification of Rice Fields using KOMPSAT-2 High Resolution Satellite Imagery

Junho Yeom, Youkyung Han and Yongil Kim*

Global warming has become one of the world’s most serious social issues. Nitrogenous fertilizer, which is generally used for agricultural activity, is a major source of greenhouse gas in the atmosphere. Investigating the distribution of crop fields is thus essential to controlling greenhouse gases. Analyses using remotely sensed data such as aerial photos and satellite images can be more cost-effective and reliable for large agricultural areas. Classification techniques that use multi-date satellite images are efficient tools for identifying agricultural land. In this study, image co-registration between images from different dates is performed for preprocessing. The Fast Line-of-sight Atmospheric Analysis of Spectral Hypercubes (FLAASH) atmospheric correction technique is applied to convert radiance data in the satellite image to reflectance data. We then analyze and compare several vegetation indices using separability analysis. Rice fields are classified using the composition of the multi-temporal satellite image and the most efficient vegetation index. The extracted rice fields are compared with reference data derived from aerial photo interpretation. The classification results provided agricultural accuracies of approximately 90%. In addition, the extracted rice fields had acceptable producer and user accuracies of 83% and 78% respectively in Daejeon and 80% and 72% respectively in Gongju.

A rapid method for the determination of rosmarinic acid in Cordia dichotoma seeds using ultrasound-assisted extraction and high-performance liquid chromatography-tandem mass spectrometry

Feng Liu and Shuge Tian*

An ultrasound-assisted extraction (UAE) and high-performance liquid chromatography-tandem mass spectrometry (HPLC–MS/MS) method that offers good linearity, accuracy and precision was developed for the simultaneous determination of rosmarinic acid (RA) in Cordia dichotoma seeds. Single-factor and orthogonal experiments were performed to determine the appropriate range of extraction conditions and to obtain the optimum extraction conditions respectively. The optimum UAE conditions for C. dichotoma seeds were as follows: ethanol concentration of 70%, solid/liquid ratio of 1:35 g/mL, ultrasound time of 30 min and ultrasound power of 300 W. UAE is an alternative technique for the fast extraction of C. dichotoma seeds. The factors selected in this study had significant functions on the extraction of RA from C. dichotoma seeds.