Indian Journal of Chemical Technology

http://www.niscair.res.in

 

VOLUME 16

NUMBER 4

JULY 2009

CODEN:ICHTEU

ISSN:0971-457X

CONTENTS

 

Papers

 

 

 

Adsorption behaviour of Pb(II), Cd(II) and Zn(II) on NALCO plant sand

291

M Mohapatra, S Khatun & S Anand

 

 

Packed bed column studies for the removal of Acid blue 92 and Basic red 29

 

using non-conventional adsorbent

301

P Sivakumar & P N Palanisamy

 

 

 

Utilization of Erythrina variegata orientalis leaf powder for the removal of

 

cadmium

308

P Rohini Kumar, M Venkateswara Rao, N Chitti Babu, P V Ravi Kumar &

 

P Venkateswarlu

 

 

 

Enzymatic synthesis of fructose ester from mango kernel fat

317

P P Dandekar & V B Patravale

 

 

 

Mn recovery from medium grade ore using a waste cellulosic reductant

322

D Hariprasad, B Dash, M K Ghosh & S Anand

 

 

 

Corrosion inhibition and biocidal activity of a cationic surfactant

328

P Shanthy, P Rengan, A Thamarai Chelvan, K Rathika & S Rajendran

 

 

 

Corrosion inhibition of 304 stainless steel in sodium chloride by ciprofloxacin

 

and norfloxacin

334

R S Dubey & Yogesh Potdar

 

 

 

Cetyl trimethylammonium bromide as corrosion inhibitor for mild steel in

 

acidic medium

339

Mukta Sharma, Jyoti Chawla & Gurmeet Singh

 

 

 

Reversed phase thin layer chromatography of five co-administered drugs with

 

surfactant modified solvent systems

344

Ali Mohammad, Sudhanshu Sharma & Showkat Ahmad Bhawani

 

 

 

Second derivative spectrophotometry for simultaneous determination of

 

iron (II) and copper (II) using 2-ketobutyric acid thiosemicarbazone

351

 

 

Notes

 

 

 

Preparation of reusable enzyme strips using alkylamine and arylamine

 

glass beads affixed on plastic strips for urea determination

357

Minakshi Sharma, Vijay Kumar, Jitender Kumar & C S Pundir

 

 

 

Removal of fluoride from low TDS water using low grade coal

361

L Borah & N C Dey

 

 

 

Author Index

365

 

 

Keyword Index

366

 

 

Guidelines for Authors

367

 

 

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 291-300

 

 

Adsorption behaviour of Pb(II), Cd(II) and Zn(II) on NALCO plant sand

 

M Mohapatra1*, S Khatun2 & S Anand1

1Institute of Minerals and Materials Technology (IMMT), Bhubaneswar 751 013, India

2Indian Institute of Chemical Technology, Hyderabad 500 007, India

Present investigation evaluates the adsorption of Pb(II), Cd(II) and Zn(II) ions on plant sand of National Aluminum Company, Orissa, India. The XRD pattern and FTIR spectra showed goethite, alumina and silica as the major phases in the sand. Effects of various parameters such as time, pH, temperature, metal ions and adsorbent concentrations were studied. The adsorption followed pseudo second order kinetics for all the three cations. The proton stoichiometry was dependent on the nature of the metal ion showing the order Zn(II)>Cd(II)>Pb(II). The adsorption was found to be in the order Zn(II)>Cd(II)> Pb(II) with loading capacities of 47.79, 42.2 and 22.8 mg g-1 of plant sand sample. The adsorption data was fitted to various models. The thermodynamic parameters (Δ)G0, (Δ)H0 and (Δ)S0 have been evaluated. The XRD patterns of Pb(II) adsorbed plant sand sample showed that the crystallinity of silica phase was affected with the appearance of (110) plane and disappearance of (011) plane. It also disturbed the (110) plane of goethite. Cd(II) adsorbed sample showed disappearance of (011) plane of silica phase and transformation of alumina phase Al2O3 to s-Al2O3. The adsorption of Zn(II) showed prominence of (110) plane of goethite with disappearance of s-Al2O3 phase.

Keywords: Plant sand, Adsorption, Isotherms, Kinetics, Heavy metal ions, XRD

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 301-307

 

 

Packed bed column studies for the removal of Acid blue 92 and

Basic red 29 using non-conventional adsorbent

 

P Sivakumar* & P N Palanisamy

Department of Chemistry, Kongu Engineering College, Perundurai, Erode 638 052, India

Email: shivagobi@yahoo.com

 

The adsorptive removal of Acid blue 92 and Basic red 29 dyes was achieved using a packed column prepared by Euphorbia antiquorum L activated carbon. The effects of various factors like influent concentration, flow rate and bed height were analysed. The column experiments using Euphorbia antiquorum L activated carbon showed that adsorption efficiency increases with increase in the influent concentration and bed depth and decreases with increasing flow rate. Column adsorption performance was evaluated using Thomas and Yoon-Nelson kinetic models. The adsorption capacity calculated by Thomas and Yoon-Nelson models were compared with the experimental adsorption capacity. The Yoon-Nelson model describes the adsorption behaviour of the selected adsorbent-adsorbate system more reasonably than Thomas model and Basic red 29 adsorption behaviour fits exceptionally well with the Yoon-Nelson model.

Keywords: Fixed bed column, Activated carbon, Adsorption, Euphorbia antiquorum L, Acid blue 92, Basic red 29

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 308-316

 

 

Utilization of Erythrina variegata orientalis leaf powder for the removal of cadmium

P Rohini Kumar1, M Venkateswara Rao1, N Chitti Babu2, P V Ravi Kumar2 &

P Venkateswarlu2*

1Department of Chemical Engineering, RVR & JC College of Engineering, Guntur, 522 019, India

2Department of Chemical Engineering, Andhra University, Visakhapatnam, 530 003, India

Email: pvlu9@rediffmail.com

 

Removal of cadmium, a priority pollutant, is carried out by abundantly and freely available Erythrina variegata orientalis (Indian coral tree) leaf powder. The extent of removal depends on initial concentration of cadmium in the solution, pH of the solution, temperature, etc. A significant increase in percentage removal of cadmium is observed as pH is increased from 2 to 4. The percentage removal of cadmium increases marginally for pH of 4 to 7. As the initial concentration of cadmium is increased from 23 to 188 mg/L, the % removal is decreased from 98.8 to 86.1%. Freundlich and Langmuir isotherm models well describe the data indicating favourable biosorption. The biosorption is endothermic, irreversible and follows pseudo-second-order kinetics, and rate constant is 0.23 g/(mg-min) for a dosage of 40 g/L. The equilibrium agitation time is 50 min.

Keywords: Biosorption, Cadmium, Erythrina variegata orientalis, Thermodynamics

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 317-321

 

 

Enzymatic synthesis of fructose ester from mango kernel fat

P P Dandekar & V B Patravale*

Department of Pharmaceutical Sciences and Technology, Institute of Chemical Technology,
N.P. Marg, Matunga, Mumbai 400 019, India

Email: vbp_muict@yahoo.co.in

 

 

Fructose ester as a biosurfactant was successfully synthesized from the fatty acid fraction (olein fraction) of Mango Kernel Fat (MKF). The synthesis was carried out by reaction of sugar and fatty acid fraction in presence of the enzyme lipase from Candida rugosa which acted as a biocatalyst. Phosphate buffer (pH 7.0) was used as the reaction medium to realise maximum enzymatic action. The product was separated from the reaction medium by liquid- liquid extraction. Maximum conversion (36.52 %) was achieved at fructose to olein fraction molar ratio of 1 : 10 (mol/L), with the lipase concentration of 4g/L, at a temperature of 30oC at the end of 3 days. The presence of an ester band in the synthesized ester was confirmed by Fourier Transform Infrared (FTIR) analysis. Identity of the product was further confirmed by NMR studies and a colour identity test for the ester group.

Keywords: Biosurfactant, Fructose ester, Mangifera indica, Mango kernel fat (MKF), Candida rugosa

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 322-327

 

 

Mn recovery from medium grade ore using a waste cellulosic reductant

D Hariprasad, B Dash, M K Ghosh* & S Anand

Institute of Minerals and Materials Technology, Bhubaneswar 751 013, India

Email: m_k_ghosh@yahoo.com

 

Medium grade siliceous manganese ore containing 38.22% Mn was leached in sulphuric acid medium using shredded newspaper as reducing agent. Objective of the present study was to investigate the effectiveness of ligno-cellulosic base wastes such as used newspaper as a reducing agent. The experimental parameters chosen for this study were: H2SO4 concentration (2-5% v/v), temperature (60-900C), reductant to ore ratio (0.4-1) and ore particle size (57 274 m). Optimum conditions for >90% extraction were: 900C, 5% H2SO4 (v/v), reductant to ore ratio 0.5, 8 h, 10% pulp density and ore particle size -100 m. Newspaper was found to be equally effective as a reducing agent for low grade ore (15.83% Mn) also wherein the amount of reductant and acid needed were proportional to Mn content of the ore. The leach solution was enriched to 87 g/L by recycling process. The enriched solution was purified by pH adjustment to 4.7 using 20% lime slurry. MnSO4.H2O was crystallized from purified solution. A schematic flow-sheet has been included.

Keywords: Manganese ore, Leaching, Cellulosic reductant, Waste newspaper

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 328-333

 

 

Corrosion inhibition and biocidal activity of a cationic surfactant

P Shanthya, P Rengana, A Thamarai Chelvanb, K Rathikac & S Rajendranc*

aDepartment of Chemistry, Yadava College, Madurai, India

bPG and Research Department of Chemistry, Thiagarajar College, Madurai, India

cCorrosion Research Centre, PG and Research Department of Chemistry, GTN Arts College, Dindigul, India

Email: srmjoany@sify.com

 

The inhibition efficiency (IE) of CTAB - Zn2+ system in controlling corrosion of carbon steel in well water has been evaluated by weight loss method. Enumeration of microorganisms from well water and biocidal efficiency of inhibitor system (CTAB-Zn2+) were also determined by serial dilution technique and spread plate method. The formulation consisting of 200 ppm of CTAB and 5 ppm of Zn2+ shows an IE of 98%. Potentiodynamic polarization curves indicate that the CTAB Zn2+ system functions as anodic inhibitor. AC impedance spectra reveal that a protective film is formed on the metal surface. FTIR spectra suggest that the protective film consists of Fe2+- CTAB complex and Zn(OH)2. The optimum concentration of CTAB for destroying the bacterias viz. E.coli, Salmonella and Shigella is 25 ppm. At 25 ppm of CTAB, it shows 100% biocidal efficiency in well water containing 5 ppm of Zn2+.

Keywords: Corrosion inhibition, Carbon steel, Biocidal activity, N-Cetyl-N,N,N-trimethyl ammonium bromide (CTAB), CTAB-Zn2+ system

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 334-338

 

 

Corrosion inhibition of 304 stainless steel in sodium chloride by ciprofloxacin and norfloxacin

R S Dubey* & Yogesh Potdar

Chemistry Research Laboratory, Department of Chemistry, R J College (University of Mumbai),
Ghatkopar (W), Mumbai 400 086, India

Email:dubeyrps@rediffmail.com

 

Heterocyclic organic compounds namely ciprofloxacin and norfloxacin were used as corrosion inhibitor for protection of 304 stainless steel in 1.5 percent NaCl solution. The inhibition effect of these compounds was investigated by using electrochemical techniques such as open circuit potential (OCP) and potentiodynamic polarization. The results obtained reveal that these compounds are very good corrosion inhibitors and show their best performance at a concentration of 1800 ppb. Potentiodynamic curves indicate that these compounds are anodic type of inhibitors.

Keywords: Corrosion inhibition, 304 Stainless steel, Ciprofloxacin, Norfloxacin, Potentiodynamic polarization

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 339-343

 

 

Cetyl trimethylammonium bromide as corrosion inhibitor for mild steel
in acidic medium

Mukta Sharma1*, Jyoti Chawla1 & Gurmeet Singh2

1Department of Applied Sciences & Humanities, Career Institute of Technology and Management,

Faridabad 121 001, India

2Department of Chemistry, Delhi University, Delhi 110 007, India

Email: muktapragya@gmail.com; chem_jyoti@yahoo.com

 

The inhibitive effect of cetyl trimethylammonium bromide (CTAB) on acid corrosion of mild steel in sulphuric acid at different temperatures has been investigated. Galvanostatic and potentiostatic studies were performed to determine the corrosion current, inhibition efficiency, passivation current and passivation potential range. The parameters so obtained were used to explain the effectiveness of inhibitor when present in different concentrations. Scanning Electron Microscopic (SEM) studies also help to understand the changes that take place on the surface layer with respect to change in CTAB concentration. The extent of corrosion inhibition has also been evaluated by comparing the micrographs obtained from SEM. The results obtained are in direct agreement with the electrochemical studies.

Keywords: Corrosion inhibitors, Surfactants, Mild steel, Adsorption

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 344-350

 

 

Reversed phase thin layer chromatography of five co-administered drugs with surfactant modified solvent systems

Ali Mohammad*, Sudhanshu Sharma & Showkat Ahmad Bhawani

Department of Applied Chemistry, Faculty of Engineering & Technology, Aligarh Muslim University,

Aligarh 202 002, India

Email: mohammadali4u@rediffmail.com

 

The chromatography of five co-administered drugs i.e. paracetamol, ibuprofen, diclofenac sodium, aspirin and ascorbic acid was performed on various reversed phase layers. The surfactant mediated solvent systems were used with various impregnated silica gel H layers for the chromatography of these five drugs. The various experimental conditions were optimized for the selection of optimum concentration of impregnants. The mutual separation of a mixture of paracetamol, diclofenac sodium and ibuprofen; and paracetamol, aspirin and ascorbic acid are achieved on various impregnated silica gel H layers, using surfactant mediated solvent systems containing n-hexane: 1% CTAB in MeOH: ethyl acetate: acetic acid, (13:1:4:2, v/v) and toluene: 1% CTAB in MeOH: n-propanol: formic acid, (14:1:3:2, v/v) respectively.

Keywords: Thin layer chromatography, Paracetamol, Diclofenac sodium, Ibuprofen, Aspirin, Ascorbic acid

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 351-356

 

 

Second derivative spectrophotometry for simultaneous determination of
iron (II) and copper (II) using 2-ketobutyric acid thiosemicarbazone

L E Attah

Department of Chemical Sciences, Cross River University of Technology, P O Box 2113, Calabar, Nigeria

Email: louattah@yahoo.com

 

A new chromophoric reagent, 2-ketobutyric acid thiosemicarbazone (KBAT) has been used for the simultaneous determination of iron, copper and vanadium. KBAT forms yellowish-green and blue complexes with iron (II) and copper (II) respectively at pH 6.5 and a yellow complex with vanadium (V) at pH 5.5. Calibration graphs for the individual determinations by second derivative spectrophotometry were obtained. The derivative amplitudes obeyed Beers law at 387.2 nm for copper (II), 440 nm for iron (II) and 400 nm for vanadium (V), in the concentration ranges 0.30-2.40, 0.20-2.280 and 0.25-2.56 mg mL-1 respectively. Zero crossing method using the second derivative mode at the selected wavelengths was employed in the simultaneous determinations. The accuracy and reproducibility of the determination methods on known amounts of iron, copper, and vanadium in their binary mixtures were tested. The effects of foreign ions on the determinations of the metals were also studied. The recommended procedure was applied to the analysis of ferro-vanadium alloy, phosphor bronze, rice and groundnut.

Keywords: Derivative spectrophotometry, Zero crossing, Iron, Copper, Vanadium, 2-Ketobutyric acid thiosemicarbazone

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 357-360

 

 

Preparation of reusable enzyme strips using alkylamine and arylamine glass beads affixed on plastic strips for urea determination

Minakshi Sharma, Vijay Kumar, Jitender Kumar & C S Pundir*

Biochemistry Research Laboratory, Department of Biochemistry & Genetics, M D University, Rohtak 124 001, India

Email: pundircs@rediffmail.com

 

Reusable strips of urease were prepared by covalently immobilizing it onto alkyl and arylamine glass beads, affixed on a plastic strip with a non-reactive adhesive. The immobilized urease retained its initial activity, prior to immobilization about 56% on alkylamine and 33.3% on arylamine. Maximum activity of alkylamine conjugated urease was attained at pH 6.5, 25C for 1 min, while arylamine conjugated urease showed maximum activity at pH 7.0, 40oC, 15 min. The Km for urea was 4.65 and 16.66 mM, for alkyl and arylamine conjugated urease respectively. A method for determination of serum urea developed using these strips is based on measurement of NH3 generated with Nesslers reagent. The minimum detection limit permitted by the method was 10 and 5 mg/dL using alkyl and arylamine conjugated urease, respectively. Urea value in serum of healthy persons determined by this method, was in the range of 5-55 mg/dL with a mean of 26 mg/dL. The recovery of added urea was 82% for alkylamine and 85% for arylamine glass beads. A fair correlation (r=0.821) was found between urea values obtained by the standard urease kit and the present method. The alkylamine and arylamine conjugated urease stored at 4C in 0.02 M potassium phosphate buffer pH 7.0 were reused 100 and 90 times respectively, during the span of one month. The method offers advantage of enormous ease in handling of immobilized urease.

Keywords: Urea, Urease, Serum, Alkyl and arylamine glass, Immobilization

 

 

Indian Journal of Chemical Technology

Vol. 16, July 2009, pp. 361-363

 

 

Removal of fluoride from low TDS water using low grade coal

L Borah* & N C Dey

Analytical Chemistry Division, North East Institute of Science & Technology, Jorhat, India

Email: laxmi.bh@rediffmail.com; ncdey49@yahoo.co.in

 

Defluoridation of ground water using low grade Assam coal as an adsorbent is studied by batch sorption experiments. Effect of the variables, like quantity of adsorbent, contact time, particle size of the adsorbent are examined to establish the optimum conditions. The results show that the low grade Assam coal, collected from Tirap colliery of the North Eastern coalfield, after pretreatment, can be used as an effective adsorbent in removing fluoride from ground water. The optimum conditions for the efficient removal of fluoride are observed to be (i) quantity of adsorbent = 1.25 g in 100 mL water, (ii) contact time = 60 min, (iii) particle size of adsorbent = ─72 BSS or lower.

Keywords: Defluoridation, Fluoride, Adsorption, Low grade coal, Fluorosis