Pakistan Journal of Scientific and Industrial Research Vol. 48, No. 6 Contents November - December 2005

Physical Sciences

Electrochemical Reduction of 4-(3-Pyridylazo)-3-Amino-2-Pyrazolin-5-OneRefat Abdel-Hamid, Mostafa K. M. Rabia and Nadia A. Abdalla 7046-SB 371

Catalytic Transfer Reduction of Electron Deficient Alkenes and an Imine Using PotassiumFormate and Catalytic Palladium AcetateMd Mosharef Hossain Bhuiyan 7082-SAN 377

Synthesis and Characterization of Dimethyltin(IV) Complex with 2-Methylpyridyl-benzhydrazone (AcPyBzh): Crystal Structure of [Me2SnCl (AcPyBzh)]M. A. Affan, Fasihuddin B. Ahmad, Ramli B. Hitam, Mustafa B. Shamsuddin andBohari M. Yamin 6923-GH 381

Mass Fragmentation Pattern of Some Mono- and Di-Substituted Formamidines. Part-1.Mass Pattern of 1-ArylformamidinesM. Umar Ali, M. Zahurul Haque, M. Abdullah Al-Maruf and M. Abdullah As-Saki 7049-SB 386

Intramolecular Fatty Acids Distribution in the Triglycerides of Hordeum vulgareSalma Rahman and Tanveer Ahmad Chaudri 6929-GQ 389

A Comparative Study on the Determination of Fe in Groundwater by Different MethodsM. R. Zaman, R. A. Banu and A. Yousuf 7013-SB 393

Concentration and Distribution of Some Heavy Metals in Urban Soils of Ibadan, NigeriaI. U. Umoren and P. C. Onianwa 7053-SB 397

Biological Sciences

Effects of Physical and Chemical Treatments on the Enzymatic Activities of Rice Bran LipasesM. Zahurul Haque, Nurul Absar and M. A. Jalil 7031-GQ 402

Rose Bengal and Mercaptoethanol Tests for the Diagnosis of Brucella abortus Biotype-1Infection in Sprague-Dawley RatsM. S. Rahman and B. K. Baek 7007-GQ 407

Prevalence of Onchocerciasis Syndrome in Ise-Orun Local Government Area of Ekiti State,NigeriaL. K. Olofintoye, S. O. Adewole, F. B. Erinle and A. I. Ajayi 7063-SAN 412

Incorporation of Button Mushrooms in Pakistani DishesTasnim Kausar and Rukhsana Bajwa 7174-SB 417

Seasonal Incidence and Extent of Damage Caused by Citrus Leaf Miner, Phyllocnistis citrellaStainton Infesting LemonHabibur Rahman, Khandakar Shariful Islam and Mahbuba Jahan 6858-GQ 422

Technology

Chromate Coating of Zinc-Aluminum Plating on Mild SteelInam-ul-Haque, Asim Khan and Nadeem Ahmad 7096-SB 426

Short Communications

Spectroscopic and Dyeing Characteristics of the Yellow Dye from Morinda lucida(Brimstone Tree)A. O. Adetuyi, L. Lajide and A. V. Popoola 6979-SB 430

Analysis and Purification of Nkalagu (Nigeria) Limestone and Poultry Eggshells for theProduction of Paint Grade Calcium CarbonateE. Osabohien, E. O. Adaikpoh and F. I. Nwabue 7055-SB 433

Review

Fundamental Concepts and Mechanisms in the Metal Biosorption Technology for theTreatment of Industrial WastewatersAsma Saeed, Asia Aslam and Muhammed Iqbal 7218-SI 436

IntroductionNumerous azo compounds find important applications in thefield of medicine (Jisun et al., 2002; Netto et al., 2001; Ragehet al., 1999; Garg and Singh, 1970; Modest et al., 1957). Theelectrochemical behaviour of these compounds plays animportant role in their biological activity (Bourbonnais et al.,1998; Leontievsky et al., 1997; Solomon et al., 1996). A lite-rature survey reveals that only little work has been carried outon the electorochemical behaviour of heterocyclic azo com-pounds, such as arylazopyrazolones (Shawali et al., 1992;Abdel-Hamid, 1986; Jain, 1984; Ravindranath et al., 1983),and pyridylazophenol (Al Obaidi et al., 1987; Florence et al.,1974 ). The objective of the present investigation was to studythe electrochemical reduction of 4-(3-pyridylazo)-3-amino-2-pyrazolin-5-one in universal buffer solutions at different pHvalues ranging between 2.18 - 10.75. The study was carriedout using two electrochemical techniques, namely, cyclicvoltammetry and digital simulation, so that the mechanism forthe electrochemical reduction of 4-(3-pyridylazo)-3-amino-2-pyrozolin-5-one could be formulated. The behaviour of theelectrochemical reduction was investigated at 298 K and aschematic mechanism, consistent with the experimental results,has been proposed. The mechanism was further confirmed andfully characterized by cyclic voltammetric simulation analy-sis making use of computer programmes CVSIM and CVFIT(Dario et al., 1998; Gosser and Zhang, 1991).

Materials and MethodsFor the present electrochemical studies on heterocyclic azocompounds, 4-(3-pyridylazo)-3-amino-2-pyrazolin-5-one was

prepared according to the method reported earlier (Fahmyet al., 1990; Elnagdi and Abd Allah, 1973). The prepared com-pound was recrystallised from ethanol and characterized byelemental analysis and IR spectra. Stock solution (5.0 x 10-3

mol dm-3) of the azo compound under study was prepared in50% aqueous ethanol mixture. Brritton-Robinson modifieduniversal buffers in the pH range of 2.18 - 10.75 were pre-pared in distilled water using analytical reagent grade che-micals (citric acid, boric acid, phasphoric acid and sodiumhydroxide) with ionic strength of 0.4 mol dm-3 and were usedas the supporting electrolytes (Brritton, 1956). Solutions forcyclic voltammetry measurements were prepared by mixing1.0 ml of stock solution of the azo compound and 9.0 ml ofthe appropriate buffer solution. Dissolved Oxygen was removedfrom these solutions by flushing nitrogen gas for about 15 min.The pH of the buffers was checked with an Orion researchmodel 601A/digital ionalyzer, using combined electrode.

Cyclic voltammograms were recorded using an EG&G PARmodel 264 A polarographic analyzer. The measurements werecarried out with a conventional three-electrode configuration.An EG&G PAR model SMDE 303A mercury-drop system insmall dropping mode was used as the working electrode. Theelectrode area was 1.05 x 10-2 cm-2. The reference electrodewas an Ag/AgCl electrode. A 1.0 cm2 platinum foil was usedas auxiliary electrode throughout the experimental work.Solutions were purged with pure nitrogen before the measure-ments were done, and an atmosphere of nitrogen was main-tained above the working solutions. All experiments wereperformed at 298 K.

Eversince the pioneering work of Feldberg (Feldberg, 1969),digital simulation techniques have played an important role

Pak. J. Sci. Ind. Res. 2005 48(6) 371-376

*Author for correspondence;E-mail: nadiaahmed20032003@yahoo.com

Electrochemical Reduction of 4-(3-Pyridylazo)-3-Amino-2-Pyrazolin-5-One

Refat Abdel-Hamida, Mostafa K. M. Rabiaa and Nadia A. Abdalla*b

aDepartment of Chemistry, Faculty of Science, Sohag, EgyptbDepartment of Chemistry, Faculty of Science, Aswan, Egypt

(received May 28, 2004; revised August 25, 2005; accepted August 27, 2005)

Abstract. The electrochemical reduction of 4-(3-pyridylazo)-3-amino-2-pyrazolin-5-one in universal buffer solutions ofdifferent pH values was studied at 268 K. From the results obtained, it was concluded that the azo compound was reducedvia an ECEC mechanism (two-electron and two-proton mechanism). The mechanism was confirmed by digital simulation.The heterogeneous electron transfer and homogeneous protonation follow-up reaction parameters were evaluated and theelectrode mechanism is discussed.

Keywords: electrochemical reduction, ECEC mechanism, aminopyrazoline, 4-(3-pyridylazo)-3-amino-2-pyrazolin-5-one,cyclic voltammetry, azo compounds

371

IntroductionHomogeneous hydrogenation of unsaturated compoundswith transition-metal complexes proceeds in a stepwise man-ner via metal hydride species. Molecular hydrogen readilyreacts with various transition-metal complexes resulting inmetal monohydrides or dihydrides. Chemoselective hydroge-nation of carbon-carbon multiple bonds in conjugated carbo-nyl functions has been a long desired synthetic transforma-tion. In terms of chemoselectivity and regio- and stereocontrol,transition-metal hydrides offer a number of advantages overthe more traditional methods of catalytic hydrogenation(Augustin, 1965) and dissolving metal reduction methods(House, 1972). Despite the bewildering variety of reducingagents available for synthetic chemistry, new and ever moreselective reductants are in constant demand. In many cases,the carbon-carbon multiple bonds can be carried out bymeans of a hydrogen donor. This process is termed as cata-lytic transfer hydrogenation (Zassinovich et al., 1992). Thetransition-metal catalyzed hydrogen transfer reaction, withthe aid of hydrogen donors such as trialkylammonium for-mate (Cortese and Heck, 1978), n-Bu3SnH (Keinan and Gleiz,1982), Ph2SiH2/ZnCl2.H2O (Keinan and Greenspoon, 1986),triethoxysilane and H2O (Tour et al., 1990), and NaH2PO2/H2O (Sala et al., 1984) are some of the examples employedfor selective conjugate reduction. Sodium salts of formic acid,phosphinic acid and phosphorous acid have also been reportedas hydrogen donors in catalytic transfer hydrogenation(Johnstone et al., 1985). Conjugate reduction of α, β-unsatu-rated cyano esters to the corresponding saturated cyanoesters in the presence of HCOOK/Pd(OAc)2 has been recentlyreported by research group of the present author (Basu et al.,2003a). That line of research was further investigated byusing a new series of electron deficient alkenes, which pos-

sessed other sensitive functional groups and an imine, theresults of which study are reported here.

Materials and MethodsThe 1H- and 13C-NMR were measured on Bruker AC 200 spec-trometer using CDCl3 as the solvent, and chemical shifts wereexpressed as ‘δ’ values in ppm against TMS as an internalstandard. Silica gel thin layer chromatography was routinelyused to check the purity of the compounds. The TLC spotswere exposed in iodine vapours for visualization.

General method for the preparation of compound 2 (unsa-turated stannyl esters). Unsaturated cyanoesters (compound1, 5 mmol) and bis-tri-n-butyltin oxide (5 mmol) in toluene(40 ml) was refluxed for 12-14 h. The solvent was then evapo-rated in vacuo and the crude product was purified by columnchromatography.

Tri-n-butylstannyl 2-cyano-3-(4-methoxyphenyl)acrylate,compound 2a. Viscous liquid; yield: 84%. 1H NMR (CDCl3):δ 7.88 (s, 1H), 7.71 (d, 2H, J = 6.6 Hz), 6.8 (d, 2H, J = 6.6Hz), 3.62 (s, 3H), 1.69 (m, 6H), 1.35 (m, 12H), 0.95 (t, 9H, J= 6.6 Hz).

Tri-n-butylstannyl 2-cyano-3-(4-hydroxyphenyl)acrylate,compound 2b. Viscous liquid; yield: 80%. 1H NMR (CDCl3):δ 8.12 (s, 1H), 7.90 (d, 2H, J = 8.73 Hz), 6.99 (d, 2H, J = 8.73Hz), 1.70 (m, 6H), 1.37 (m, 12H), 0.92 (t, 9H, J = 6.6 Hz).

Tri-n-butylstannyl 2-cyano-3-(4-chlorophenyl)acrylate,compound 2c. Viscous liquid; yield: 75%. 1H NMR (CDCl3):δ 8.21 (s, 1H), 7.74 (d, 2H, J = 8.6 Hz), 7.49 (d, 2H, J = 8.6Hz), 1.71 (m, 6H), 1.39 (m, 12H), 1.00 (t, 9H, J = 6.6 Hz).

Tri-n-butylstannyl 2-cyano-3-(furan-2-yl)acrylate, com-pound 2d. Viscous liquid; yield: 76%. 1H NMR (CDCl3): δ

Catalytic Transfer Reduction of Electron Deficient Alkenes andan Imine Using Potassium Formate and Catalytic Palladium Acetate

Md Mosharef Hossain BhuiyanDepartment of Chemistry, University of Chittagong, Chittagong-4331, Bangladesh

(received August 23, 2004; revised November 17, 2005; accepted November 18, 2005)

Pak. J. Sci. Ind. Res. 2005 48(6) 377-380

Abstract. Chemoselective reduction of α, β-unsaturated cyanostannyl esters, ketones and an imine with potassium for-mate as hydrogen donor and palladium acetate as homogeneous catalyst in DMF was observed to proceed readily withsaturation of C-C and C-N double bonds, without any concomitant reduction of cyano, carboxylate, halogen or carbonylgroups and demetallation.

Keywords: catalytic transfer hydrogenation, potassium formate, palladium acetate, electron deficient alkenes, catalytictransfer, catalytic reduction, chemoselective hydrogenation, transition metal-hydrides

377

Synthesis and Characterization of Dimethyltin(IV) Complex with2-Methylpyridylbenzhydrazone (AcPyBzh): Crystal Structure of

[Me2SnCl (AcPyBzh)]

M. A. Affan*a, Fasihuddin B. Ahmada, Ramli B. Hitamb, Mustafa B. Shamsuddinb and Bohari M. Yaminc

aResource Chemistry, Faculty of Resource Science and Technology, Universiti Malaysia Sarawak,94300-Kota Samarahan, Sarawak, Malaysia

bDepartment of Chemistry, Faculty of Science, University Technology Malaysia, 81310-UTM Skudai,Johor Darul Takzim, Malaysia

cSchool of Chemical Sciences, Universiti Kebangsaan Malaysia, 43600-Bangi, Selangor, Malaysia

(received July 23, 2003; revised August 31, 2005; accepted September 1, 2005)

Abstract. The reaction of dimethyltin(IV) dihalide with 2-methylpyridylbenzhydrazone (AcPyBzh) afforded the com-plex compound [Me2SnCl(AcPyBzh)]. The complex was characterized by IR, 1H and 13C-{1H} NMR spectroscopictechniques and elemental analyses. The crystal structure of [Me2SnCl(AcPyBzh)] has been determined. The AcPyBzhanion in this complex acts as a monobasic NNO bidentate ligand, the tin(IV) lying in an elongated distrorted trigonalbipyramidal environment where the azomethine nitrogen and amidate oxygen, together with the two-methyl carbons,are in the equatorial plane, whereas the chloride is the apical ligand. The crystal is monoclinic, space group P2(I)/n,with a = 12.0945 (3), b = 7.5167 (2), c = 19.9795 (4) Å, α = 90°, β = 105.85°, γ = 90°.

Keywords: organotin(IV) complexes; crystal structure; 2-methylpyridylbenzhydrazone ligand, dimethyltin(IV)complex

Pak. J. Sci. Ind. Res. 2005 48(6) 381-385

*Author for correspondence; E-mail: affan62@hotmail.com;maaffan@frst.unimas.my

IntroductionThe chemistry of hydrazones has been intensively investigatedin recent years owing to their coordination capabilities. Theymay coordinate to central metal ion or atom, either in the ketoor in the anionic (enol) form via loss of the “amide” hydrogen.It is becoming increasingly apparent that the coordination chem-istry of the organotin(IV) is of relevance in a wide variety ofbiological and potential pharmaceutical applications, such asanti-tumour agents (Yin et al., 2004; Haiduc et al., 2001; Jancsoet al., 2001). The coordination chemistry of tridentate acylhydrazones derived from 2(α)-N-heterocyclic aldehydes orketones (compound 1; Fig.1) has been studied extensively, anda series of transition and non-transition metal complexes havebeen isolated and characterized (Bacchi et al., 1996; Dutta andHossain, 1984; Domiano et al., 1979). The structure of thecopper(II) complex Cu(HL)(L)ClO4.C2H5OH, containing bothneutral (HL) and deprotonated (L) ligands (R1 = H; R2 = o-OHC6H4), has also been described (Domiano et al., 1979). Theonly isolated inorganic tin(IV) complex was with tridentateligand (compound 1; Fig. 1) (R1 = R2 = C6H5) and trans-diiodobridged dimeric structure (SnI2L)2 has been proposed forthis complex (Dutta and Hossain, 1984). Khalil et al. (1994)

described the mode of complexation of monoorganotin(IV)chloride and diorganotin(IV) dichloride with N(2-pyridinylme-thylene)benzhydrazone (R1 = H, R2 = C6H5) and proposed asix-coordinated complex. However, owing to the insolubilityof this diorganotin(IV) complex in common polar and non-polar organic solvents, its structural characterization by X-raycrystallography could not be carried out. The related hydra-zone ligand (2) (R1 = CH3, R2 = C6H5; Fig. 1), is expected toyield organotin(IV) complexes with increased solubility inorganic solvents. Therefore, it was thought that it might bepossible to grow single crystals of some of these complexesand study them by X-ray diffraction. The present report is asystematic study of organotin(IV) complexes of the hydrazoneligand formed by the condensation of 2-acetylpyridine withbenzhydrazide. As a part of the investigation is reported thesynthesis and characterization of this hydrazone ligand and itsdimethyltin(IV) (complex 3; Fig.1), together with the X-raysingle-crystal structure determination of the [Me2SnCl(AcPyBzh)] complex (3).

Materials and MethodsReagents. All chemicals were procured from Fluka (FlukaChemie GmbH, Industriestrasse 35, CH-9471 Buchs, Swit-zerland) and were used without further purification. Metha-

381

Pak. J. Sci. Ind. Res. 2005 48(6) 386-388

Mass Fragmentation Pattern of Some Mono- and Di-SubstitutedFormamidines. Part-1. Mass Pattern of 1-Arylformamidines

M. Umar Alia, M. Zahurul Haque*b, M. Abdullah Al-Maruf a and M. Abdullah As-Sakia

a Department of Chemistry, Rajshahi University, Rajshahi-6205, BangladeshbBCSIR Laboratories, Rajshahi-6206, Bangladesh

(received May 20, 2004; revised February 26, 2005; accepted March 31, 2005)

Abstract. Some 1-arylformamidines were prepared by the Raney nickel (W-2) desulphuration of some 1-arylthioureas inanhydrous boiling benzene medium. Mass fragmentation patterns of the products were ascertained from the mass spectraldata.

Keywords: Raney nickel, thiourea, desulphuration, mass fragmentation, 1-arylformamidines, mass pattern, nickel sulphide

IntroductionStudies on the Raney nickel (nickel sulphide) desulphurationof organosulphur compounds are well documented.Monoarylthiocarbamides are used as starting materials forthe synthesis of various substituted dithiobiurets,dithiazolidines and and S-triazines (Ali et al., 2001). Thesetypes of arylthiocarbamides find various industrial and bio-logical uses (Haque et al., 2003). Among the various as-pects of studies on organic nitrogen and sulphur com-pounds, the Raney nickel desulphuration process and thechemistry of thioureas are of significant importance. Thedesulphuration process involving the Raney nickel has beenapplied in a large number of complicated syntheses. Purelyas a synthetic tool, the Raney nickel desulphuration pro-cess has been used to advantage in the total synthesis ofcantharidine, plumbagin, some deoxypentose and hexosederivatives, and some of their pyrimidine or purine glyco-sides. This catalyst, furthermore, has been employed in thestructural elucidation of many complicated synthetic andnatural products, such as penicillin, biotin and several othersimilar compounds. It has been also used in the selectivedesulphuration of steroid derivatives, without affecting theirpoints of unsaturation. Raney nickel desulphuration of cer-tain 1-arylthioureas in boiling benzene and ethanolic mediahas been investigated earlier (Ali and Paranjpe,1984). Thepresent study describes the probable mass spectral analy-sis of some 1-substituted arylformamidines.

Materials and MethodsPreparation of Raney nickel (W-2). To an aqueous solutionof caustic soda (128.0 g in 750.0 ml), powdered Ni-Al alloy(100.0 g) was added in small portions, and the system was

stirred using mechanical stirrer for a period of about 30 min.The temperature of the reaction was maintained at about 25 °Cduring the addition of the alloy. The system was then heatedover a steambath for 5-6 h. The aqueous sodium aluminatethus formed was decanted off and the resultant Raney nickelwas washed twice with water. It was again treated with a freshsolution of caustic soda (200.0 ml, 10%), and thus freed fromany traces of aluminum in the form of sodium aluminate. Theaqueous filtrate was decanted off and the Raney nickel soprepared was washed repeatedly with water to remove anylast traces of caustic soda. It was then washed for 3-4 timeswith rectified spirit and was stored in the same solvent in astoppered glass bottle (yield, 50.0 g).

Raney nickel desulphuration of 1-chlorophenylthiourea inboiling benzene: formation of 1-p-chlorophenylformamidine.To a benzene suspension of the Raney nickel (W-2; 24.0 g in150.0 ml) in a three necked 500.0 ml round bottomed flask,fitted with a mechanical stirrer, a reflux condenser and a drop-ping funnel, hot benzene suspension of 1-p-chloropheny-lthiourea (Ia, Fig.1: 9.3 g, 0.05 mol in 50.0 ml) was added. Thereaction mixture was heated gently to reflux, with continuousstirring for 150 min and then filtered hot to remove wastedRaney nickel (nickel sulphide). The solvent was distilled offfrom the filtrate and a reddish-brown solid (IIa, Fig. 1: 4.0 g;yield 52%) was isolated. It was washed carefully with ethanoland crystallised from a mixture of benzene-petroleum ether(1:1), m. p. 183 °C. From the elemental analysis, its molecularformula was indicated as C7H7ClN2 (determined: C = 53.20, H =4.81; N = 17.65; the expected calculated values for C7H7ClN2:C= 54.04, H = 4.53, N = 18.12%).

The product was moderately soluble in cold ethanol and chlo-roform but highly soluble when these solvents were hot. It*Author for correspondence; E-mail: mdzahurulhaque@yahoo.com

386

Intramolecular Fatty Acids Distribution in the Triglycerides ofHordeum vulgare

Salma Rahman* and Tanveer Ahmad ChaudriApplied Chemistry Research Centre, PCSIR Laboratories Complex, Lahore, Pakistan

(received August 20, 2003; revised September 10, 2005; accepted September 13, 2005)

Pak. J. Sci. Ind. Res. 2005 48(6) 389-392

Abstract. Triglycerides of a local variety of Hordeum vulgare, ‘jao-87,’ were separated from the lipids by columnchromatography, purified on plain thin layer chromatography plates, and then fractionated by silver nitrate impregnatedthin layer chromatography. Fatty acids composition of these fractions was verified by gas chromatography after theirmethylation. The distribution of fatty acids, attached at α, α’- and β-positions of the triglycerides and their fractions, wasdetermined by lipolytic hydrolysis and subsequent gas chromatographic analysis of the 2-monoglycerides. The β-positionwas usually occupied by oleic, linoleic and linolenic acids, depending upon the comparative high percentage of therespective fatty acid in that triglyceride fraction.

Keywords: lipids, fatty acids, triglycerides, barley, Hordeum vulgare

IntroductionHordeum vulgare (barley; ‘vern. jao’), Family Gramineae, isa cereal of significant importance. Besides its use as foodfor human beings and feed for animals, it is a raw material forthe malting and brewing industries. Barley contains about3% lipids, in addition to starch, sugars, pectin, cellulose,proteins, lignin and tannins (Jones and Amos, 1957). Lipidsare important nutritional components in cereal grains, as theycontain higher energy than carbohydrates and proteins. Theysolubilize vitamins A, D, E and K, which are necessary forthe proper maintenance of health and are a source of essen-tial fatty acids, thus contributing to several metabolic func-tions (Gunstone et al., 1986). Barley lipids are rich in linoleicacid, an essential fatty acid. γ-Linoleic acid is the first inter-mediate in the bioconversion of linoleic to arachidonic acid,which is known to have therapeutic properties, being a pre-cursor of prostaglandins, thromboxanes and leukotrienes(Gunstone et al., 1986).

There has been increasing interest in cereal lipids, as theseare a potential source of significant amounts of dietary poly-unsaturated fatty acids. Very little work has been done on thelipids of barley keeping in view these aspects. Most of thestudies have been devoted to the identification and charac-terization of lipids, their fatty acids composition (Parsons andPrice, 1974; Price and Parsons, 1974), and changes in lipidscomposition during malting and brewing processes (Priceand Parsons, 1975; Walsh et al., 1965). Lipids of barley con-tain a number of neutral and polar constituents of which trig-lycerides is the major class comprising more than 50% of the

total lipids content. Fatty acids composition includes palm-itic, oleic and linoleic acids as the major fatty acids, whereaslauric, myristic, palmitoleic, stearic, linolenic and arachidic acidsare also present, though in smaller quantities (Salma et al.,2004). Knowledge of the composition and structure of triglyc-erides of barley is important for the understanding of its nutri-tional aspects,oil stability, and possible physiologicaleffects.The fatty acids in a triglyceride molecule are distrib-uted at α, α’- and β-positions. The present study reports forthe first time the distribution pattern of fatty acids at α, α’-and β-positions in the triglycerides of barley. For this pur-pose, triglycerides and their fractions, obtained by argentationthin layer chromatography, were hydrolyzed selectively at α,α’-positions (Conacher et al.,1970; Subbaram and Youngs,1964; Mattson and Volpenhein, 1961), whereas unhydrolizedβ-monoglycerides were separated by thin layer technique (Tho-mas et al., 1965). The fatty acids attached at the β-positionswere identified after methylation by comparative gas chroma-tography. The distribution of fatty acids in the triglyceridemolecules ranged from C12:0- C20:0 and the β-position was usu-ally occupied by oleic and linoleic acids. The survey of litera-ture reveals a usual distribution of oleic, linoleic and linolenicacids at the β-position in edible vegetable oils (Gunstone etal., 1965; Mattson and Volpenhein, 1961).

Materials and MethodsBarley variety ‘jao-87’ was obtained from the AgriculturalResearch Institute, Faisalabad, Pakistan. Whole grains werecrushed and lipids extracted in chloroform : methanol : watermixture as described by Price and Parsons (1974). Triglycer-ides (2 g), were separated from the total lipids by column chro-*Author for correspondence; E-mail: ha_sr@hotmail.com

389

A Comparative Study on the Determination of Fe in Groundwaterby Different Methods

M. R. Zaman*a, R. A. Banub and A. Yousuf a

a Department of Applied Chemistry and Chemical Technology, Rajshahi University, Rajshahi-6205, BangladeshbDepartment of Chemistry, Rajshahi College, Rajshahi, Bangladesh

(recieved March 11, 2004; revised September 24, 2005; accepted September 28, 2005)

Pak. J. Sci. Ind. Res. 2005 48(6) 393-396

Abstract. Three different experimental methods were used to analyse iron content in groundwater samples drawn fromvarious spots of Mirzapur, a southeastern part of Rajshahi City, Bangladesh. These included UV-visible spectrophoto-metry, atomic absorption spectrophotometry, and titrimetric methods. As many as 20 water samples were collectedfrom randomly selected domestic water supply tubewells throughout the area. Iron content was found to range between0.052 - 5.890 ppm, 0.060 - 6.060 ppm, and 0.139 - 5.584 ppm by the spectrophotometric, atomic absorption spectro-photometric, and titrimetric methods, respectively. The values obtained with the three different methods were, fairlycomparable and lie within the fringe of experimental deviations.

Keywords: drinking water, Fe determination, metal contamination, toxic effect, groundwater iron

*Author for correspondence; E-mail: drmrzaman@yahoo.com

IntroductionIron is an essential mineral for living beings. The total ironcontent of a normal adult body is about 4 to 5 g. The primaryfunction of iron is to form haemoglobin, which carries oxygenin the blood in the form of oxyhaemoglobin. Myoglobin is aniron containing chromoprotein, like haemoglobin, which com-bines with oxygen and acts as an oxygen store for muscles. Itis also involved in the process of cellular respiration.

The probability of changes in the groundwater quality, parti-cularly with respect to heavy metal contamination, has incre-ased significantly during the recent years. Iron, among theheavy metals, may be present in concentrations that may beeither in the beneficial or the toxic range. As per internationalstandards, the permissible limit of Fe in drinking water is 0.3mg/l, while 1.0 mg/l is rated as excessive (WHO, 1971). The USpublic health safety standards specify 0.3 mg/l of iron(USEPA, 1979). Groundwater in the excessive rainfall areascontains iron in toxic amounts. In deep tubewells, iron existsas ferrous ion, which on coming in contact with air rapidlychanges to light yellow-orange colour due to oxidation andprecipitates as ferric hydroxide. Such waters are extremelyharmful for drinking.

Some recent studies carried out in Bangladesh have indicatediron contamination in groundwater (Khan et al., 2003; Samadet al., 2003; Tareq and Rahman, 2002). Rahman et al. (2000)studied the underground-water quality of Tongi, GazipurDistrict, Bangladesh. The study reported that Fe contamina-tion was within the permissible limit. Alam and Anam (1991)

have studied the chemical characteristics of groundwatersamples collected from some deep and hand-operated tube-wells around Dhaka City, Bangladesh. Water available inGorakhpur, India is moderately hard and contains appreciablecontent of Fe (Srivastava et al., 2001). Raveendran and Ismail(1991) have studied the quality of groundwater in Bahrain.Recently, Chilton (2003) reported that underground aquifersare the major sources of municipal and industrial water sup-plies. Some of the world’s largest cities (Beijing, Buenos Aires,Dhaka, Lima, Mexico City) draw heavily from them, whilesome of the fastest growing cities are completely dependenton groundwater. Groundwater from aquifers beneath or closeto Mexico City, for example, provides the city with more than3.2 billion litres per day. However, as the groundwater pum-ping increases to meet the growing water demand, it canexceed the rates at which the aquifers are replenished. In fact,water level of several urban aquifers have shown long-termdecline. Since Fe is an important water mineral, the presentstudy was carried out to compare three different methods,namely, spectrophotometric, atomic absorption photometry,and titrimetry for proper assessment of the quality of ground-water with respect to this important water constituent.

Materials and MethodsTwenty groundwater samples were collected from hand-ope-rated tubewells of Mirzapur area of Rajshahi City, duringOctober-November, 2002 (Fig.1). For the purpose, those wellswere selected that were under constant use and were freefrom external pollution. The samples were collected in plasticcontainers during running condition of the wells. These tube-

393

Concentration and Distribution of Some Heavy Metals in Urban Soils ofIbadan, Nigeria

I. U. Umoren*ab and P. C. Onianwaa

aDepartment of Chemistry, University of Ibadan, Ibadan, NigeriaaDepartment of Chemistry, University of Uyo, PMB-1017, Uyo, Nigeria

(received June 18, 2004; revised March 1, 2005; accepted March 15, 2005)

Pak. J. Sci. Ind. Res. 2005 48(6) 397-401

Abstract. Concentrations and distribution of seven heavy metals, namely, Pb, Cd, Zn, Cr, Co, Ni and Cu in the soil samplescollected from 38 different sites from Ibadan Metropolis and its suburbs were investigated. The metals were extracted fromthe soil with HNO3-HClO4-HF combination for the elemental analysis using flame atomic absorption spectrophotometer.The results obtained for all locations indicated (μg g-1 dry weight): Pb (150±143); Cd (4.2±4.4); Zn (213±213); Cr(131±96); Co (38±19); Ni (79±56); and Cu (40±36). Zonal average of metal concentrations indicated the highest metalload in the environment of the urban high traffic (UHT) zone followed by the refuse dump sites. Interelemental associationin the UHT-zone showed significant correlation between the pairs Pb-Cd (r = 0.521), Pb-Cu (r=0.412), Zn-Cr (r = 0.603),Zn-Cu (r = 0.334), Ni-Cr (r = 0.749), Ni-Co (r =0.324), and Cd-Cu (r = 0.408).

Keywords: heavy metals, environment pollution, metal contamination, metal-polluted soil

IntroductionHeavy metals are natural components of the environment.However, their pressence is a serious problem as they pollutethe soil, water and air. Environmental contamination with toxicheavy metals has become an issue of global concern owing totheir multiple effects on the ecosystem (Nriagu, 1990). Heavymetals may accumulate in rural and urban soils due to a vari-ety of human activities. Potential pathways include municipalincinerators, metal processing industries, automobile exhausts,application of phosphate fertilizers to agricultural farmland,application of sewage sludge and animal manure (often highin copper) to agricultural land, and the deposition of paintflakes from buildings (Alan, 1993; Alloway, 1990; Ward et al.,1977; Lagerweff and Specht, 1970).

Automobile exhausts account for about 80% of the air pollu-tion by heavy metals in Nigeria (Onianwa and Egunyomi, 1983).The market share of leaded gasoline in Nigeria is still 100%,which is known to have a very high lead content of 0.66 gper litre (WRI, 2000). Cadmium is released into the air as aresult of incineration or disposal of Cd-containing products,such as rubber tyres, plastic containers and the wear of break-linings (David and Wiliiams, 1975). In non-polluted soils, thecadmium concentration is generally less than 1.0 mg kg-1.Recently, Onianwa (2001) has reported a study on the levelsof Pb, Zn, Cd, Cu, Cr, Co, and Ni in the roadside topsoils inlbadan. Variations in the levels of lead in the roadside soilsand vegetation were attributed to the traffic volume. It has

been reported that the level of soil lead increased as the trafficvolume increased, and decreased significantly as the distancefrom the highway increased (Xiong, 1998; Onianwa andAdoghe, 1997; Olajire and Ayodele, 1997; Zupancic, 1997;Fergusson, 1990; Garcia and Millan, 1988; Ward et al., 1977).Widespread use of Zn in galvanized products have also con-tributed to the contamination of soils with cadmium and zinc(Kabata-Pendias and Pendias, 1992).

Studies of various environmental media in lbadan, Nigeria, havehighlighted the growing hazards of the heavy meta-lrelatedpollution load (Onianwa, 2001; Onianwa and Fakayode, 2000;Onianwa and Adoghe, 1997; Onianwa and Egunyomi, 1983).The present study aims at further assessing the level of heavymetal load due to the increased traffic volume with the growingpopulation and to identify the other major anthropogenicsources of these heavy metals in the environment.

Materials and MethodsSoil samples were taken from 38 sites from the Ibadan Me-tropolis and its suburbs during the dry season, November2001-January 2002 (Fig. 1). For effective sampling, the citywas subdivided into five zones: urban industrial ((UI); ur-ban high traffic (UHT), urban low traffic (ULT), refuse dumpsites (RDS), and rural zones (RZ). The samples were col-lected in polyethylene bags from 0-5 cm depth (topsoil),with a stainless steel hand trowel. Samples were air-dried atambient temperature for four days in the laboratory and thenground in a porcelain mortar and passed through a 0.5 mmnylon sieve.

*Author for correspondence; E-mail: innihobongumoren @yahoo.comapresent address:

397

Effects of Physical and Chemical Treatments on the Enzymatic Activities ofRice Bran Lipases

M. Zahurul Haque*a, Nurul Absarb and M. A. Jalila

aBCSIR Laboratories, Rajshahi-6206, Bangladesh

bDepartment of Biochemistry, University of Rajshahi, Bangladesh

(received May 10, 2004; revised September 1, 2005; accepted October 25, 2005)

Abstract. The lipolytic activities of lipases lip-I, lip-II and lip-III, purified from rice bran variety Paijam, wereinvestigated after physical and chemical treatments. The purified lipases had pH optima of 7.3-8.0 and temperatureoptima of 34-40 °C. The results indicated that lip-I was more stable than lip-II and lip-III. The lipases isolated from ricebran, variety Paijam, belong to the category of alkaline lipases. Bile salts were found to be weak activators for theactivation of lipases, while maximum activities were obtained with deoxycholate. The activities of rice bran lipases wereenhanced by the presence of Ca++ upto certain concentrations, while EDTA application strongly inhibited the lipolyticactivities. Rice bran lipases were more sensitive to the denaturing agent guanidine-HCl than urea. The presence of heavymetal ions, such as Cu++, Hg++, Zn++, Fe++, strongly inhibited activities of the lipases, while such metals as Ba++, Mg++

and Mn++ slightly increased the activities of lipases.

Keywords: lipolytic activities, rice bran lipases, bile salts, olive oil, heavy metals, rice variety Paijam

Pak. J. Sci. Ind. Res. 2005 48(6) 402-406

IntroductionRice bran is a valuable by-product of the rice milling industry.It is the most important part of the rice grain as it containsproteins, minerals and vitamins. It is also considered to be agood source of oil, containing 16-22% oil (Ali et al., 1999). Itsonly utility in Bangladesh, however, is its input as an ingredi-ent in the livestock feedstuffs (Ali et al., 2000). Beriberi is avery common and fatal disease in Bangladesh, which is linkedto B1 deficiency in the diet. The poorer classes of Bangladeshare the main victims of the disease, who live on a diet, defi-cient in vitamin B1. Rice bran is a rich source of anti-neuriticvitamin B1. After extraction of the oil, the left-over bran cakemay also be used to increase the fertility of soil, as it containsimportant ingredients such as nitrogen, phosphorous andsulphur.

Lipases are an important class of enzymes which play a vitalrole in the digestion of fats and oils present in food materials(Hussain et al., 1995). Although known for a long time, ricebran lipases have not been the subject of much work as com-pared with the lipases from other sources such as pancreas,castor bean and wheat germ (Shastry and Rao, 1971). Much ofthe earlier work on this enzyme pertains to its inactivation inorder to ‘stabilize’ the bran and oil (Aizono et al., 1976; Funatsuet al., 1971). The lipase activity is known to persist in thewhole rice grains (paddy) for as long as 15 years. Recently,

some work has been conducted on the purification and prop-erties of this enzyme (Absar et al., 1999).

The present study reports the purification of lipases fromrice bran, variety Paijam, grown in Bangladesh. The puri-fied lipases were subjected to various physical and chemi-cal treatments, and the effects of these treatments on thelipolytic activities were also investigated. The study wasexpected to yield the useful information regarding someof the physicochemical properties, such as pH optimumand pH stability, temperature optimum and thermostabil-ity, the stability of lipases towards denaturating agents,and the enzymic activities in the presence of metallic salts.The experimental findings are expected to be helpful inestablishing the conditions for chemical modifications ofthe lipases and in understanding the relationship betweentheir structure and function.

Materials and MethodsChemicals used and purification of lipases. Rice bran ofvariety Paijam was procured from Noor-Habib Auto Rice Mills,Rajshahi. Chemicals used in the study were bile salts and urea(BDH), guanidine-HC1 (Bio-Rad Laboratories, Richmond,California, USA), and miscellanceous other reagents used wereall of analytical reagent grade.

The rice bran lipases (lip-I, lip-II and lip-III) were purified, inbiologically active form, by gel filtration of 85% ammoniumsulphate-saturated crude extract on Sephadex G-75, followed*Author for correspondence; E-mail: mdzahurulhaque@yahoo.com

402

Rose Bengal and Mercaptoethanol Tests for the Diagnosis of Brucellaabortus Biotype-1 Infection in Sprague-Dawley Rats

M. S. Rahman*ab and B. K. Baeka

aCollege of Veterinary Medicine, Chonbuk National University, Jeonju 561 756, South KoreabDepartment of Medicine, Faculty of Veterinary Science, Bangladesh Agricultural University, Mymensingh-2202, Bangladesh

(received March 26, 2005; revised September 12, 2005; accepted October 15, 2005)

IntroductionBrucellosis is an economically important disease of domes-tic and pet animals. Methods for its diagnosis have been ex-tensively investigated (Baek et al., 2003; Kakoma et al.,2003; Plommet and Fensterbank, 1984). Although wild andlaboratory animals are crucial in the economy of developingcountries, studies on the prevalence of brucellosis in theseanimals have received comparatively little attention. Withrespect to serological diagnosis, studies have been carriedout on conventional tests using whole cell antigens andcomplement fixation test (CFT), as well as agar immunodif-fusion tests using uncharacterized trichloroacetic acid orsonic extracts (Diaz-Aparicio et al., 1994; Waghela et al.,1980; Falade, 1978; Bell et al., 1976). Brucella abortus bio-type-1 has been isolated from cattle from different provincesof South Korea and studied extensively (Rahman, 2003; Baeket al., 2001; Park et al., 1998; Chung et al., 1988). Purposeof the present study was to investigate the Rose Bengal test(RBT) and mercaptoethanol test (MET) for the diagnosis ofB. abortus biotype-1 infection in Sprague-Dawley (S-D) ratsusing whole cell antigen of B. abortus strain 1119-3 (S1119-3). Such studies, using rat sera from brucellosis infected, ornon-infected rats, have not been performed preveously. Thepresent study, therefore, is an attempt to establish the actualdiagnostic value of these tests, not reported so far, for prac-tical applications.

Materials and MethodsCulture of Brucella abortus. Brucella abortus biotype-1,isolated in South Korea, was used in this study forexperimentally induced brucellosis infection in rats. For thepreparation of antigens for RBT and MET, S1119-3 strain ofB. abortus was used. B. abortus biotype-1 was cultured inBrucella broth (Difco Co., USA) for 48 h at 37 ºC with 5% CO2.The master inoculum of S1119-3 was grown on Brucella agar(Difco Co., USA) for 72 h at 37 ºC, followed by growth inBrucella broth in a rotary shaking incubator at 180 rpm at 37 ºC.After 30 h incubation, the cell culture was inactivated by heatingat 95 ºC for 1 h, washed with physiological saline 3 times, andkept suspended in the physiological saline until use.

Experimental design. Healthy and disease-free, 6 to 10month old female S-D rats (n = 45), weighing 200 - 250 gwith no history of previous exposure to Brucella species wereused in the present investigations. Rats were classified intobrucellosis infected (n = 27) and control groups (n = 18).The infected group was equally divided into nine sub-groups,each comprising three animals, for 0, 1, 2, 4, 8, 12, 16, 20and 24 weeks of post-infection studies. Similar sub-group-ings were followed for the control group, however, eachsub-group consisted of 2 rats. The rats were maintainedunder hygienic conditions and were fed on commercial feedand water ad libitum. 500 μl suspension, containing 1.0×109

colony forming unit (cfu) of B. abortus biotype-1, suspendedin physiological saline solution, was injected subcutaneouslyto each of the 27 rats. Eighteen rats were sub-cutaneously

Pak. J. Sci. Ind. Res. 2005 48(6) 407-411

*Author for correspondence; E-mail: prithul02@yahoo.co.ukbpresent address:

Abstract. Rose Bengal test (RBT) and mercaptoethanol test (MET) were conducted for the diagnosis of Brucellaabortus biotype-1 infection. For this purpose, female Sprague-Dawley (S-D) rats were subcutaneously infected at thedose rate of 1.0×109 colony forming unit suspension of B. abortus in physiological saline. The S-D rats were monitoredat regular intervals using serological and bacteriological methods. The reciprocal antibody titer after the first week was1: 800 with RBT, whereas it was 1: 400 with MET. The reciprocal antibody titer of 1: 25 through RBT and 1:100through MET, respectively, were noted in infected rats of 24 weeks post-infection. Bacteremia was detected untill 24weeks post-infection. RBT, using B. abortus strain S1119-3 whole cell antigen, appears to be a potential candidate, asa useful diagnostic method, for brucellosis detection in rats.

Keywords: brucellosis, Brucella abortus biotype-1, Sprague-Dawley rats, Rose Bengal test, mercaptoethanol test

407

Prevalence of Onchocerciasis Syndrome in Ise-Orun Local GovernmentArea of Ekiti State, Nigeria

L. K. Olofintoye*, S. O. Adewole, F. B. Erinle and A. I. AjayiZoology Department, University of Ado-Ekiti, PMB 5363, Ado-Ekiti, Nigeria

(received July 16, 2004; revised June 2, 2005; accepted June 15, 2005)

Abstract. Twenty seven towns and villages in the Ise-Orun local government area of Ekiti State, Nigeria are in the grip ofonchocerciasis. Out of the 2045 subjects examined, 1131 (55.3% at 95% confidence interval- CI, 0.53-0.57) were found to beinfected by the disease. The prevalence of onchocerciasis varied from one town or village to the other in the area of study. The peakprevalence (80.5% at 95% CI, 0.73-0.89) was recorded in the village Temidire. The people aged 50-59 years accounted for peakprevalence (72.0% at 95% CI, 0.63-0.81). Out of the total 2045 subjects examined, 51.0, 26.8,19.2 and 3.0% were, respectively,found to be suffering from craw-craw, leopard skin, nodules, and partial blindness.

Keywords: dermatology, onchocerciasis infection, Onchocerca volvulus, craw-craw disease, leopard skin disease

IntroductionOnchocerca volvulus causes one of the most disabling anddebilitating diseases known to man (Braide et al., 1982).The disease caused by O. volvulus, however, is non-peri-odic, unlike some forms of filarias, which are either noctur-nal or diurnal in periodicity (Branin, 1990). The activity ofthis microfilarial worm results in to dermatological, lym-phatic and opthalmological conditions, which can begrouped together as onchocerciasis syndrome (Hagon,1998). Dermatological manifestations of onchocerciasishave also been noted to be associated with changes in theskin (Kale, 1998; Murdoch, 1993; Hay, 1989). Apart from itsmedical importance, onchocerciasis has been identified asan important factor in the economy of Tropical Africa, as itincapacitates a large segment of adult population, thuspreventing them to achieve their maximum productivecapacity. The disease has, in the past as well as at present,prompted some communities to abandon their fertile landfor less productive areas in order to save themselves fromthe ravages of the onchocerciasis disease (Newoke, 1990).The present study was, therefore, aimed at investigatingthe rate of overall dermatological and clinical manifesta-tions of onchocerciasis in the Ise-Orun local governmentarea in the Ekiti State, Nigeria.

Materials and MethodsStudy area. This study was carried out in 27 towns andvillages in the Ise-Orun local government area of the EkitiState (Fig. 1). The inhabitants of these towns and villages aremostly farmers, cultivating yam, cassava, maize and cocoa,

while some are fishermen. They are mostly indigenous to thesetowns and villages, except for a few health workers, artisansand civil servants working as temporery residents. The roadsleading to these towns and villages are bad, almost not

* Author for correspondence; E-mail: toyetalk@yahoo.com

Pak. J. Sci. Ind. Res. 2005 48(6) 412-416

Fig. 1. Map of Ekiti State showing sampling towns andvillages of the Ise-Orun local government areastudied for the prevalence of onchocerciasissyndrome.

NIGERIA

EKITI STATE

4 45’E 5 00’ 5 15’ 5 30’ 5 45’E0 15’N8 15’N

8 00’

7 15’

7 30’

7 15’N4 45’ 5 00’ 5 15’ 5 30’ 5 45’E

7 15’N

7 30’

7 15’

8 00’

KWARA STATE

KOOISTATE

STATEONDO

Otun

MOBA

IJERO

Ijero

IlejemejeIYE

EKITIWEST

AramokeEFON

Efon-Alaaye

EKITI SOUTH WEST

Ilawe

Ikere

IKERE

ADO

AdoAdo

IREPODUN/IFELODUN

Igede

IDO/OSI

Ido

OYE

Oye IKOLE

Ikole

GBONYIN

Ode

EMURE

Emure

Omuo

EKITI EAST

KEY

0 200 400 600 800KmState Boundory

Local Govt. Boundory

State Capital

Local Govt. Capitals

The Study Area

ISE/ORUN

Ise

N

412

Incorporation of Button Mushrooms in Pakistani Dishes

Tasnim Kausar*a and Rukhsana Bajwab

a Food Research Centre, PCSIR Laboratories Complex, Jamrud Road, Peshawar, Pakistanb Department of Plant Pathology, Punjab University, New Campus, Lahore, Pakistan

(received February 21, 2005; revised October 13, 2005; accepted October 15, 2005)

Pak. J. Sci. Ind. Res. 2005 48(6) 417-421

Abstract. Button mushrooms (Agaricus bisporus) were incorporated into six table delicacies and six traditional Pakistanidishes. Protein content of the mushroom-fortified dishes increased from 8.44% to 67.50%. Organoleptic evaluationsshowed that all the mushroom-fortified table delicacies and traditional dishes showed significant improvement in theiracceptability.

Keywords: button mushrooms, anti-nutritive factors, toxins and allergents, Agaricus bisporus, table delicacies, Pakistani dishes

*Author for correspondence

IntroductionThe widening gap between supply and demand of proteincan be bridged by supplementing the existing sources withunconventional sources of protein, such as plant leaves,oilseed cakes and edible mushrooms. Unlike plant leavesand oilseed cakes, edible mushrooms are free from anti-nutritive factors, toxins and allergents (Falanghe, 1976). Theproduction of mushrooms as a source of fungal proteins, oras flavouring agents, has the most attractive prospect. Abreakthrough for cultivation of mushrooms in Pakistan hasalready been achieved by researchers of Agricultural Uni-versity, Faisalabad, and PCSIR Laboratories Complex,Lahore, by optimization of conditions for the cultivation ofoyster and button mushrooms (Kausar et al., 2003; Kausarand Zafar, 2002; 1999; Khan and Siddique, 1987).

Mushrooms are regarded highly both as nutritious foodsand delicacies. They are gaining popularity in over-popu-lated areas of the world as they can provide adequate amountof texture protein in the diet. Mushrooms contain 35-45%protein on a dry matter basis, with the amino acid profile thatis better than many vegetables and fruits (Jaindak and Kapoor,1976; Bano and Srivastava, 1962). They are also a rich sourceof minerals and vitamins, and their digestibility is better thanmeat (Anonymous, 1999; Garcha, 1976). The Food Develop-ment Authority in 1994 awarded mushrooms the status of‘Healthy Foods’ (Ananymous, 1999). Mushrooms are not astaple food by themselves but can be regarded as importantdiet supplements. Vegetable proteins, such as leaf proteinand mustard protein concentrates have been incorporated innormal dishes of India, Nigeria, Jamaica, and Pakistan (Shah,1984; Olatubosum et al., 1972).

The present study reports the incorporation of button mush-rooms (Agaricus bisporus) in some traditional Pakistanidishes and table food delicacies so that the protein contentsand acceptability of the so fortified commonly consumed fooddishes is improved significantly.

Materials and MethodsFresh mushrooms (Agaricus bisporus) were washed withwater to remove any sticking soil. Excessive moisture wasreduced by pressing them gently between folds of filter papersheets. Mushrooms were chopped into slices and added todifferent table delicacies and traditional Pakistani dishes withthe objective of improving their culinary values, such as taste,flavour, and acceptability (Table1).

The recipes and procedures for the preparation of differentmushroom-fortified table delicacies and traditional Pakistanidishes are detailed below; ts = tablespoon, wheneverreferred.

Mushroom delicacies(i) Mushroom soup

Fresh mushrooms (0.5 x 0.5 cm pieces) = 100 gOnions = 50 gBeef (dry, crushed) = 2 tsCornflour = 1 tsSalt = ¼ tsBlack pepper = ¼ ts

Finely chopped onions were fried in butter to which were addedsliced mushrooms, sprinkled with 25 ml water, and cooked atrelatively low heat for 10 min. The remaining ingredients werethen mixed to the mushroom and onion slurry and boiled for2-3 min before serving.

417

IntroductionThe citrus leaf miner, Phyllocnistis citrella Stainton, is oneof the most destructive microlepidopteran pests of citrus(Patel and Patel, 2001). It causes considerable economicdamage to various citrus plants in the South and SoutheastAsian countries (Hill, 1987; Atwal, 1976; Vevai, 1969; Alam,1962). The leaf miner has been reported to attack citrusplants in different parts of Bangladesh (Ali, 1989). The lar-vae after hatching, penetrate through the cuticle layer of theleaf tissue and mine the adaxial and abaxial surface of thenewly formed leaf causing the leaves to crumble. The zigzagsilvery galleries made in the leaves reduce the photosynthe-tic activity and thus the crop vigour, which encourage thedevelopment of citrus cankers (Patel and Patel, 2001; Prodhan,1992; Shevale and Pokharkar, 1992). The leaf miner, being aninternal feeder, is difficult to control. Within this context,knowledge related to the peak periods of incidence of thepest is important for its successful management. Seasonalincidence of this pest has been studied by several authors intheir respective native areas (Patel and Patel, 2001; Batraet al., 1998; Lara et al., 1998; Pena et al., 1996; Shevale andPokharkar, 1992). As the information in this regard is notavailable for Bangladesh, an attempt was made to study theseasonal incidence and the extent of damage caused byP. citrella during different months of the year.

Pak. J. Sci. Ind. Res. 2005 48(6) 422-425

Materials and MethodsThe study was conducted in a citrus orchard, located atMadhukhali, District Faridpur, Bangladesh, during Januaryto December, 2002. The seasonal incidence and the damagecaused by the leaf miner was investigated on lemon, Citruslimon Burm. Studies on the seasonal incidence of the pestwere confined to the larval stage. The layout plan of the studywas randomized complete block design, with five replicationsconsidering a single plant as a replicate. Four-year old lemonplants, having uniform vigour, were selected. The plants werefree from any insecticide applications. Obser-vations weremade in the middle of each month throughout the year. Ateach observation, tender twigs were randomly selected fromall over the periphery of the plant canopy. Data were recordedin terms of the number of larvae per infested leaf, percentageof leaf infestation, percentage area of leaf infestation, andlength of mine per leaf.

Larvae of different instar(s) of P. citrella, including the pre-pupal stage, were observed every month on 15 infested leavesper plant under a magnifying glass, and recorded as the meannumber of larvae per infested leaf. The number of healthy(larvae-free) and infested leaves were counted from eachselected twig (approx 15 leaves on the twig). The countingwas done from the apex and percentage of leaf infestationwas recorded. The percentage area of leaf infestation of 15infested leaves per plant was recorded, which was measuredgraphically by considering a single leaf as 100% area. The*Author for correspondence; E-mail: mjahan@bangla.net

Seasonal Incidence and Extent of Damage Caused by Citrus Leaf Miner,Phyllocnistis citrella Stainton Infesting Lemon

Habibur Rahman, Khandakar Shariful Islam and Mahbuba Jahan*Department of Entomology, Bangladesh Agricultural University, Mymensingh-2202, Bangladesh

(received April 14, 2003; revised November 17, 2005; accepted November 23, 2005)

Abstract. The seasonal incidence and extent of damage caused by citrus leaf miner, Phyllocnistis citrella Stainton (Lepi-doptera : Gracillariidae) were investigated during a styudy carried out in a citrus orchard at Faridpur, Bangladesh. The leafminer was active throughout the year, and its incidence and extent of damage varied significantly in different months. Itwas observed that the trend of rising and falling of the pest level occurred twice in a year, with two peak populations in themonths of April and September. The minimum incidence was found in January and July. The extent of damage in respectof percentage of leaf infestation, area of leaf infestation and the mine length per leaf were, respectively, 80%, 60% and12.8 cm in April, and 64.9%, 50.06% and 10.4 cm in September. The environmental temperature and relative humidity ofspring and autumn influenced the incidence of citrus leaf miner resulting in higher pest population and plant damage. Thelow environmental temperature in the winter months and excessive rainfall in the monsoon season adversely affected thepest in the field. The moderate environmental conditions of spring and autumn were, therefore, the most favourableperiods for P. citrella in Bangladesh.

Keywords: Phyllocnistis citrella, citrus damage, citrus leaf miner, lemon infestation

422

Chromate Coating of Zinc-Aluminum Plating on Mild Steel

Inam-ul-Haque*ab, Asim Khana and Nadeem Ahmada

aDepartment of Chemistry, University of Engineering and Technology, Lahore-54890, PakistanbPresent address: J-263, Defence Housing Authority, Lahore-54792, Pakistan

(received September 17, 2004; revised June 15, 2005; accepted September 9, 2005)

Abstract. The chromate coating on zinc-aluminum deposits has been studied. Zinc-aluminum deposition from non-cyanide bath was carried out at current density 3-3.5 A/dm2, plating voltage ~ 1.25 V, temperature 18-20 oC, for 15 min.The effect of aluminum chloride on the rest potentials of golden, colourless and non-chromated zinc-aluminum alloydeposits was observed. It was found that rest potential was slightly increased with the increase in the concentration ofaluminum chloride, only in the case of golden chromating. The rest potential of colourless chromated zinc-aluminumdeposits on mild steel were observed to have no correlation with aluminum chloride concentration. The abrasionresistance of colourless chromating was better than golden chromating.

Keywords: zinc-aluminum deposition, chromating, rest potential, chromate coating, mild steel chromating

Pak. J. Sci. Ind. Res. 2005 48(6) 426-429

building materials and for electrical appliances (Yamaji et al.,1997).

The durability of passivation in zinc electroplating has beenstudied using weak acid zinc bath free from cyanide andammonia for zinc plating, and yellow and non-coloured pas-sivating solutions for passivation process. At the runningvoltage of 1.1 V, amperage of 1 A, pH 5-5.4, at room tempera-ture, best plating results were obtained from the zinc bath.The plated sample was washed in distilled water and thendipped in dilute HNO3 for two seconds to make the zincplated surface active toward accepting final passivating film.The sample was then dipped in passivating solutions. Chro-mate film developed on the zinc surface, which protected itagainst corrosion, as well as gave it an attractive appear-ance. It was found that yellow passivation at the dippingtime of one min at room temperature with the passivatingsolution composition of CrO3, 50g/l; H2SO4, 1 ml/l; HNO3, 3ml/l gives best corrosion resistance, but had weak abrasionresistance. On the other hand, colourless passivating solu-tion comprising CrO3, 2 g/l; KF, 4 g/l; HNO3, 3 ml/l givesgood abrasion resistance with weak corrosion resistance(Haque et al., 2003a). Electrodeposition of zinc is done oniron to provide protection against corrosion and to enhanceappearance. Colouring of zinc-electroplates throughchromating has been reviewed (Haque et al.,2003b).

Materials and MethodsChemicals. The chemicals used with their sources included:zinc chloride (Qingadao Sunchiment, China), aluminum chlo-ride and potassium dichromate (Riedel-de Haën, Germany),

IntroductionSteel sheets coated with zinc or aluminum alloy are succes-sively coated with a metal layer containing iron, cobalt andnickel at 0.1-10 mg/m2 and a chromate layer containing > 25mg (as chromium) Cr +6/m3 at 10-150 mg/m2. The coated steelsheets so obtained have good adhering property (Tomiyasuand Ikishima, 2000).

The aqueous bath for chromating of zinc or zinc-alloy surfacecontains Cr6+ ions, Cr3+ ions, and nitrate ions at the chromiumion/nitrate molar ratio of 2.1-5.5, and cations of nickel, cobalt,zinc and aluminum at the cations/nitrate molar ratio of 0.05-1.The chromating bath preferably contains the Cr3+/Cr6+ molarratio of 0.25-0.67, and optionally includes minor phosphateions and fluoride-containing anions. The conversion bath issuitable for chromating of zinc-coated steel sheets at 10-100mg chromium/m2 for resistance to darkening and white corro-sion, as well as for the similar coating on zinc-aluminum alloysurface without pretreatment by metal flash coating. The wetchromate coating is dried without rinsing. The typical aque-ous bath for chromating includes zinc nitrate at nitrate/totalchromium molar ratio of 5.5, and is suitable for chromating ofgalvanized steel sheets, or of zinc-55% aluminum alloy coat-ing (Matsubara and Kato, 1999).

Steel sheets coated with a zinc-(25-75%) aluminum alloy arecoated with a chromating compound and dried without wash-ing with water to form a chromate film. The film contains 10-40mg chromium/m² and 1.0-3.0 g organic resin/m² and has a phos-phate/chromium ratio of 0.5-4.0. The sheets are suitable as

*Author for correspondence; E-mail: namihaque@yahoo.com,haque51@hotmail.com

426

Spectroscopic and Dyeing Characteristics of the Yellow Dye fromMorinda lucida (Brimstone Tree)

A. O. Adetuyi*, L. Lajide and A. V. PopoolaDepartment of Industrial Chemistry, Federal University of Technology, Akure, Ondo State, Nigeria

(received December 11, 2003; revised October 10, 2005; accepted October 15, 2005)

Abstract. The yellow dye obtained from Morinda lucida plant, yield 16.5%, melting point 108-110 °C, showedabsorption in the visible range 400-450 nm. Four major functional groups were identified at λmax of 435 nm. The IR and1H-NMR spectra exhibited absorptions consistent with a conjugated polyfunctional structure. The yellow morinda dyeis tentatively proposed as 4-benzoyl-2-amino acetaldehyde. The pigment imparted its brilliant yellow hue on the dyedcellulosic yarn and fabric with moderate fastness ratings to washing, perspiration, hot-pressing, however, having poorstability to high energy radiation.

Keywords: brimstone tree, Morinda lucida, yellow hue, equilibrium dye uptake, initial modulus, yellow morinda dye

Morinda lucida plant (brimstone tree), Family Rubiaceae, is soldin the Southern Nigerian markets for its medicinal uses (Burkill,1985). Adesogan (1973) isolated oruwal as anthraquinols andoruwalol, as 5- or 8-hydroxyl derivatives of oruwal, and 10anthraquinones from the stem of the plant. The plant is a yellowwood when fresh, which however darkens on exposure, becom-ing dark-brown with lighter yellowish-brown sapwood. It islocally called ‘orowo’ or ‘awopa’ in Southern Nigeria. It is alsoused, like the teak tree (Tectona grandis), for household con-struction in Western Africa and Southern Nigeria. A yellow dyeis associated with all parts of this plant, and the dye extractionand purification from the bark of the plant has been reportedearlier (Adetuyi et al., 2002). The present study attempts toelucidate the structure of the yellow morinda dye, using spectro-scopic methods, such as UV-visible and nfra-red (IR), andproton-nuclear magnetic resonance (1H-NMR). The studyfurther reports its dyeing properties on cellulosic fibres.

Scoured and bleached white cellulosic fibres (yarn andfabric) were used for studies on the dyeing characteristics ofmorinda yellow pigment without prior application of amordant. The dyeing was done at two different depths, 2%and 5% for cotton yarn and fabric, respectively, in an infinitedyebath in which the concentration of the colourant wasmaintained constant (Giles, 1974).

Two dyebaths, each containing 4 g/l of the yellow morindadye extract (2.5 ml) and dye assistants: 30% sodium chloride(5 ml) and 3% sodium hydroxide (10 ml) in a liquid-to-goodsratio of 100 : 1, and a blank bath of the same liquor ratiohaving the same contents but without the addition of pigment

were prepared for 2% dyeing of 500 mg cotton yarn (Giles,1974). The dilution factor for the dye stock was 20. Onedyebath served as the standard solution from which variousaliquots were taken for serial dilutions. Their optical densitywas measured on Biochron-4060 spectrophotometer at λmax

402 nm of the pure dyestuff solution. The dyeing was done ina single-bath dyeing machine MBMK II at temperatures of60 °C and 80 °C. Sampling of the spent dye-liquor, about 2ml, was taken at intervals of 30 min for a period of 3 h. Thedyed yarns were removed from the dye-liquor prior to sam-pling. Equivalent aliquot from the blank liquor was introducedinto the dye liquor to replace the dye assistants (which wereadded to the pigment to aid dye solubilization and dyeing),that had been removed by the dyed yarn. The dyed yarns werereturned and the dyeing was continued till the next samplingperiod. The sampled solutions were diluted and their opticaldensity was measured. The dye-uptakes were determinedusing the following formula:

1000 x CDf (1) WDf

where:

WDf = weight of the dyed cellulosic yarn (0.5 g)

CDf = the percent concentration of dye in yarn (w/v), whichwas calculated as follows:

CDf = 0.02 - CDs (2)

where:

0.02% (%w/v) = a constant (initial concentration of dye-liquor)

Pak. J. Sci. Ind. Res. 2005 48(6) 430-432

Short Communication

*Author for correspondence; E-mail: yomiadetuyi2002@yahoo.com

430

Analysis and Purification of Nkalagu (Nigeria) Limestone and PoultryEggshells for the Production of Paint Grade Calcium Carbonate

E. Osabohien*a, E. O. Adaikpohb and F. I. Nwabuec

a Department of Chemistry, Delta State University, Abraka, Nigeriab Department of Geology, Delta State University, Abraka, Nigeria

c Coal Mine, Enugu, Nigeria

(received June 30, 2004; revised September 30, 2005; accepted October 3, 2005)

Pak. J. Sci. Ind. Res. 2005 48(6) 433-435

Abstract. The local limestone (Nkalagu, Nigeria) and poultry eggshells were collected and analysed using gravimetric andspectrophotometric methods. The parameters determined were: moisture content, loss on ignition, impure silica, combinedoxides such as CaO, MgO, Fe2O3, Na2O and K2O. The carbonate contents fell short of that required (> 95%) for paintmanufacture. The non-carbonate matters, regarded as impurities, were removed or reduced by chemical processes, whichinvolved acid digestion through carbonation of the resultant filtrates. The purified CaCO3 grades from both these sampleswere compared with the commercially available grades. The purified grades showed improved whiting and fineness,indicating their usefulness for paints and other CaCO3 applications.

Keywords: limestone, Nigeria (Nkalagu), poultry eggshells, calcium trioxocarbonate, gravimetric limestone analysis,spectrophotometric limestone analysis

*Author for correspondence;E-mail: osabohieneemma@yahoo.com

Limestone, consisting mainly of Ca and Mg, abounds widelyin the earth’s crust, most commonly occurring as their carbon-ates in the rock. Impurities in the limestone include silica, alu-mina, oxides of Fe, Na, K, and organic matter. Other minorimpurities, such as P, Ti, Mn and S may also exist. It is a natu-rally occurring sedimentary rock, with CaCO3 content greaterthan 70% (or CaO > 40%). When CaCO3 and MgCO3 occur inapproximately equimolar concentrations in the rock, it is calleddolomite (Greensmith, 1978).

The naturally occurring limestones, used in the chemical pro-cess industries, contain a minimum of 95% carbonate content(Mark et al., 1967). Other sources of CaCO3 include chalk,marble, oolite, calcareous marl, corals, pearls and shells.Eggshells of birds are composed mainly of CaCO3 and smallquantities of MgCO3, CaPO4, and organic matter (Thorpe andWhiteley, 1949). The most common sources of calcium in poul-try rations are ground limestone and marine shells (Card andNesheim, 1972).

The limestone, eggshells and other sources of CaCO3 are of-ten contaminated with impurities, which can be removed bychemical processes, resulting in the precipitated forms, usu-ally marketed as chalk, whitings, ground limestones, or marbledust containing 96-99% of CaCO3. The precipitated types havefiner particle size, best for the hiding power of paints (Ritter,1963). The industrial production of precipitated CaCO3

is done

by different methods, which include carbonation, calcium chlo-ride procedure, or the recovery as a by-product, all startingwith the calcination of natural limestones in kilns (Myers andLong, 1975). A different method of limestone purification wasdeveloped at Conshohocher by Valley Forge Cement Com-pany. In this method, the froth formed from the lime slurry incells, mixed with fatty acids and a frothing agent (alcohol), issubjected to a cationic cell separation which then classifiesthe grains of CaCO3 (Bogue, 1955).

Calcium carbonate belongs to the group of pigments knownas “extenders”, which mainly add to the bulk and other desir-able physical properties of paints with a consequent reduc-tion in the cost of production. They are deficient in both colourand opacity or hiding power (Mark et al., 1968). The types ofpaints that employ large volumes of extenders are architec-tural and maintenance finishes, particularly used as interior orflat wall paints where hiding is not as critical as uniform cover-ing (GoodHart-Willcox, 1975).

The limestone and eggshells were, respectively, collected fromNkalagu, Ebonyi State, and Abraka, Delta State, Nigeria. Thesamples were dried, pulverized and stored. Each sample (1.0g) was analyzed for the moisture content, loss on ignition,silica, combined oxides, calcium oxide, and magnesium oxidecontents gravimetrically, in accordance with standard meth-ods (AOAC, 1970; Palmer, 1965; Bisque, 1961; Vogel, 1954).The Al2O3 and Fe2O3 contents were determined spectropho-tometrically, while the Na2O and K2O contents were obtainedby flame photometry (Gary, 1980).

Short Communication

433

Fundamental Concepts and Mechanisms in the Metal BiosorptionTechnology for the Treatment of Industrial Wastewaters

Asma Saeed*, Asia Aslam and Muhammed IqbalEnvironment Biotechnology Group, Biotechnology and Food Research Centre, PCSIR Laboratories Complex,

Lahore-54600, Pakistan

(received May 17, 2005; revised November 28, 2005; accepted November 30, 2005)

Abstract. The review deals with the need to treat industrial effluents before their discharge into open water bodies. Thetechnical and economical problems associated with conventional water treatment procedures have been pointed out.Biosorption, as an alternative technology for metal remediation of wastewaters is discussed. A detailed description of thetheoretical basis, fundamental concepts and mechanisms involved in the adsorption of metals has been given. The validityof biosorption data as determined by the fit on the mathematical models of Freundlich and Langmuir adsorption isothermshas been described. The ion exchange mechanism, its differences with the Langmuir adsorption isotherms mechanism, andthe advantages of one mechanism over the other in understanding the concepts of the biosorption process have beenconsidered.

Keywords: toxic metal remediation, effluent treatment, metal biosorption, Langmuir/Freundlich adsorption isotherms, ionexchange, biosorption technology

The ecological impact of heavy metals. Enhanced industrialactivity during recent decades has led to the discharge ofunprecedented volumes of wastewaters. As a result, environ-ment is being heavily polluted with pesticides, fertilizers, met-als, and miscellaneous toxic materials (Travieso et al., 1999).Of the various activities associated with environmental pollu-tion, mining operations, ore-processing and smelting, urban-ization, metal-plating, tanneries, and agriculture-related pur-suits are directly related to metal pollution (Pagnanelli et al.,2002; Puranik and Paknikar, 1997). Unlike most organic wastesand the microbial load in aquatic bodies, furthermore, metalcontaminants are not biodegradable, tending to accumulatein living organisms, becoming a permanent burden on theecosystem (Bailey et al., 1999). Their presence in the environ-ment, even at low concentrations, has therefore the potentialof becoming a cause of toxicity to humans and other forms oflife (Gupta et al., 2001; Volesky, 2001). Industrial effluents anddrinking water loaded with metals is thus a serious publichealth problem (Chiron et al., 2003).

Although several metals have a physiological role as pros-thetic groups in metalloproteins, and as constituents of en-zymes, coenzymes and cofactors in metabolic pathways(Lehninger et al., 1993), their presence in excessive amounts inthe food chain leads to toxicity symptoms, to disorders in thecellular functions, and eventually death (Volesky, 1990). Over-abundance of the essential trace elements and particularly theirsubstitution by non-essential ones, such as Cd, Ni, Ag, can

also cause toxicity symptoms. Furthermore, when a metal withno known biological function competes with, or replaces a func-tional metal, toxicity results (Hughes and Poole, 1989).

In addition to the direct entry of toxic metals into the humanbody, such as through inhalation of metallic dust or ingestionof food contacted with metalware, food chain in the ecosystemis the major indirect contributor. Metals assimilated by microbesand plants, tend to accumulate as they move through the foodchain (Yetis et al., 1998; Matheickal and Yu, 1996), which leadsto food chain enrichment in metal- polluted environments. Thelevels of certain metals are frequently higher in older individu-als than in juveniles, which is in accordance with the generalprinciple of bioaccumulation. From the ecotoxicological pointof view, metals such as Cd, Hg, and Pb, the so-called family of‘big three’, are highly toxic and are included in the ‘Red List’ ofpriority pollutants published by the Department of the Envi-ronment, UK, and in ‘List I’ of EEC Dangerous SubstancesDirective (Volesky and Schiewer, 1999; Aderhold et al., 1996).The same directive lists Cu, Ni, Sn and Cr in ‘List II’, whichcontains pollutants of less toxicity. These metals, nevertheless,create environmental pollution problems since, although notnecessarily toxic at low concentrations, they accumulate in thefood chain and upon entry into human body are not excreted.Therefore, from the environmental and human safety points ofview, it is of the utmost importance that metal contaminants areremoved from industrial wastewaters before their release intonatural water bodies or open landscapes. The environmentalimpact due to their toxicity has led to the enforcement of strin-*Author for correspondence; E-mail: asmadr@wol.net.pk

Pak. J. Sci. Ind. Res. 2005 48(6) 436-447

436

ii

Contents of Pak. J. Sci. Ind. Res. 2005, 48(1-6)

Vol. 48(1), January - Feburary 2005

Physical Sciences

Mass Transfer Rates and Column Heights in Reactive Extraction ProcessesMuhammad Tariq Saeed, Razia Khanam and Muhammad Yar Shaheen 1

Humidity Effect on the Disintegrant Property of ααααα-Cellulose and the Implication forDissolution Rates in Paracetamol TabletsMichael U. Uhumwangho and Roland S. Okor 8

Proximate, Mineral and Phytate Profiles of Some Selected Spices Found in NigeriaE. I. Adeyeye and E. D. Fagbohun 14

Effects of Exposures to Cement Dust and Powder on Workers in Cement Distribution/RetailOutlets in Benin City, NigeriaIfeyinwa Flossy Obuekwe and Lovette Isioma Okoh 23

Determination and Seasonal Variation of Heavy Metals in Algae and Sediments in Sewersfrom Industrial Areas in Lagos State, NigeriaO. R. Awofolu 28

Short Communication

Screening of Fused Pyrimidines as Antimicrobial Agents: Inhibitory Activities of SomeTetrahydrobenzothieno-PyrimidinesM. M. H. Bhuiyan and M. Fakruddin 37

Biological Sciences

Determination of Trace Metals in Silver Cat Fish (Chryssichthys nigrodigitatus) Associatedwith Water and Soil Sediments from Beach-Line Fish PondsO. O. Ayejuyo, O. G. Raimi and O. R. Moisili 39

Development of a High Yielding Wheat Variety “Bahawalpur-97” for Southern Punjab,PakistanMushtaq Ahmad, Lal Hussain Akhtar, S. Z. Siddiqi, Manzoor Hussain, A. Rashid,Ghulam Hussain, M. Aslam, M. Safdar, M. Masood Akhtar, M. Arshad and A. H. Tariq 42

Studies on the Lipolytic Enzymes of Carica papaya Seed PowderM. Akhtar Javed, Muhammad Naeem and Rana Amjad 47

Characterisation of Amidohydrolytic Activity of Bacillus megaterium in SubmergedFermentationQuratulain Syed, Nasira Bashir and Muhammad Akram Kashmiri 51

Pak. J. Sci. Ind. Res. 2005, Vol. 48(6)

iii

Short Communications

Mechanism of Monocarpic Senescence of Momordica dioica: Source - SinkRegulation by Reproductive OrgansAshis Ghosh 55

Status of Grain Smut Sphacelotheca sorghi and Long Smut Tolyposporium ehrenbergiiof Sorghum in Sindh and Balochistan, PakistanA. A. Hakro and A. Khan 57

Technology

The Dyeability Potential of Cellulosic Fibres Using African Yellow Wood(Enantia chlorantha)A. O. Adetuyi, A. V. Popoola, L. Lajide and M. O. Oladimeji 59

The Effect of Local Materials (Fillers) on the Crosslink Density, Hardness, Resilience andHysteresis of Natural RubberB. F. Adeosun and O. Olaofe 63

Preparation and Characterisation of Alkyd Resins Using Crude and Refined Rubber SeedOilE. U. Ikhuoria and F. E. Okieimen 68

Erratum 74

Vol. 48(2), March - April 2005

Physical Sciences

The Impact Parameters of the Broadening and Shift of Spectral LinesM. S. Helmi and G. D. Roston 75

Isomerization of 1,5-Hexadiene Catalyzed by Bis-(Cyclopentadienyl) Lanthanide SchiffBase/NaH Systems; Ln = Sm, Dy, Y, ErMuhammad Yousaf, Yanlong Qian and Muhammad Khalid Saeed 81

Beneficiation Studies on the Low-Grade Chromite of Muslim Bagh, Balochistan, PakistanS. Atiq, Irfan Hafeez, K. Khan and M.A. Malik 86

Studies on the Adsorption of Copper (II) by Activated Charcoal and its Application in theTreatment of Textile Industry EffluentsHajira Tahir, M. Nasiruddin Khan and Anila Sarwar 90

Biomagnification of Some Heavy and Essential Metals in Sediments, Fishes and Crayfishfrom Ondo State Coastal Region, NigeriaS. S. Asaolu and O. Olaofe 96

Pak. J. Sci. Ind. Res. 2005, Vol. 48(6)

iv

Indoor NO2 Sampling in a Large University Campus in Benin City, Southern Nigeria,Using Palmes Diffusion TubesE. E. Ukpebor, Y. T. Sadiku and S. I. Ahonkhai 103

Short Communications

Quantitative Determination of Sinensetin in Orthosiphon stamineus Leaves by Thin-LayerChromatography and Imaging DensitometryM. Amzad Hossain, Zakri Zakaria and Zhari Ismail 108

Effect of Storage on the Physicochemical Properties of Palm OilF. O. Abulude, M. O. Ogunkoya and O. S. Eluyode 110

Biological Sciences

Hybridization Studies in Normal and Cracked-Skull Diseased African Catfish,Clarias gariepinusO. Fagbuaro, J. I. Awopetu, M. A. Faluyi and P. O. Aluko 113

A Comparative Study of the Food and Feeding Habits of Chrysichthys nigrodigitatus andBrycinus nurse in a Tropical RiverC. G. Oronsaye and F. A. Nakpodia 118

Biological Evaluation of Extracts and Triterpenoids of Euphorbia hirtaM. Abu-Sayeed, M. Abbas Ali, P. K. Bhattacharjee, Anwarul Islam, G. R. M. Astaq,Mohal Khan and Sharmina Yeasmin 122

Short Communications

Blood Clotting Effect of Leaf Extracts of Bryophyllum pinnatumJ. M. Okuo and I. M. Ejimadu 126

Development of Stabilized Vegetable Amylases for Enzymatic Desizing of Woven Fabric withStarch Containing SizesS. Ishrat Ali and A. Farhan Khan 128

Technology

Effect of Part Replacement of Mercaptobenzothiazole with Locust Bean Cake on the Thermaland Electrical Conductivities of Natural Rubber VulcanizatesB. F. Adeosun, A. E. Oyeleke and E. G. Olumayede 131

Factors Affecting the Geometric and Tensile Properties of Stretch-Knitted Cotton FabricsS. Muhammad Nawaz, Assad Farooq, Babar Shahbaz and Ghulam Murtza 135

Pak. J. Sci. Ind. Res. 2005, Vol. 48(6)

v

Review

Castor Oil: A Vital Industrial Raw MaterialD. S. Ogunniyi 143

Vol. 48(3), May - June 2005

Physical Sciences

A Class of Algorithms for Zeros of PolynomialsStephen Ehidiamhen Uwamusi 149

The Nature of Aquifers in the Crystalline Basement Rocks of Ado-Ekiti, Igede-Ekiti andIgbara-Odo Areas, Southwestern NigeriaAkindele O. Oyinloye and Oladimeji L. Ademilua 154

Studies on Ion-Solvent and Ion-Ion Interactions and Adiabatic Compressibilities of SomeBromide Salts in Methanol at Different TemperaturesAnkan Choudhury and Mahendra Nath Roy 162

Viscometric Study of Interactions of Poly(Vinyl Alcohol) with Different Solvents atVarious TemperaturesRehana Saeed, Fahim Uddin and Gulnaz Hameed Khan 167

Studies on the Chemistry Control of Some Selected Drinking and Industrial WatersRiaz Ahmed 174

Phytochemical Studies on Adhatoda vasicaNighat Sultana, Muhammad Aijaz Anwar, Yousuf Ali and Nighat Afza 180

Synthesis of New 2-Derivatives of 3-(5,6,7,8-Tetrahydronaphthalen-2-yl)QuinoxalineM. M. Kamel, M. I. El-Zahar and M. M. Anwar 184

Studies on the Chemical Modification of Rice Bran Lipase-1M. Zahurul Haque, Nurul Absar, M. A. Jalil and M. L. Rahman 190

Variations of Heavy Metals in Green Seaweeds from Karachi Coast of PakistanRashida Qari and Sardar Alam Siddiqui 195

Precision and Accuracy in Elemental Determination in Environmental Samples UsingInstrumental Neutron Activation AnalysisShamshad Begum Quraishi and Chung Yong-Sam 202

Short Communication

Impact of Sugarcane Industry on EnvironmentSajid Farid, Musa Kaleem Baloch, Ahtsham Razaque and Syed Amjad Ahmad 209

Pak. J. Sci. Ind. Res. 2005, Vol. 48(6)

vi

Biological Sciences

Phytochemical Screening and Cytotoxicity of Root Extracts of Eupatorium odoratumAgainst the Shrimp Nauplii of Artemia salinaS. Amatya and S. M. Tuladhar 212

Estimation of Induced Secondary Metabolites in Carrot Tissues in Response to ElicitorPreparations from SeaweedsFatima Bi and Seema Iqbal 216

Short Communication

Occurrence of Fusarium Head Scab in International and National Wheat Breeding MaterialsSyed Jawad Ahmad Shah, F. Azam, I. Ali and T. Mohmmad 220

Vol. 48(4), July - August 2005

Physical Sciences

Some Common Fixed Point Theorems in Fuzzy 2-Metric SpacesSushil Sharma and Jayesh Kumar Tiwari 223

The Fe-Gd Phase DiagramS. Atiq, R. D. Rawlings and D. R. F. West 231

Effect of Sodium Chloride on Dissolution of Galena in Aqueous Acid SolutionAbdul Khalique, Adnan Akram, A. S. Ahmed and Nusrat Hamid 236

Separation of Close Boiling Acidic Isomers by Dissociation ExtractionA. S. Ahmed, M. B. Bhatty, M. T. Saeed and M. P. I. Qazi 240

Determination of the Level of PCBs in Small Fishes from Three DifferentCoastal Areas of Karachi, PakistanA. B. Munshi, A. S. Hina and T. H. Usmani 247

Biological Sciences

Laboratory Evaluation of Plant Extracts as Antifeedant Against the Lesser Mealworm,Alphitobius diaperinus and Rice Weevil, Sitophilus oryzaeM. Kamruzzaman, M. Shahjahan and M. L. R. Mollah 252

Quantification of Bactericidal Action of the Ethanolic Extract of Garcinia kola SeedsAlone, and in Combination with the Branded Antibiotic Septrin, on the CultureIsolates from Throat Irritation Patients by Bacterial Growth KineticsV. A. Ajibade, I. G. Adanlawo and T. T. Akande 257

Pak. J. Sci. Ind. Res. 2005, Vol. 48(6)

vii

Assessment of the Safety of Wild Strains of Lactobacillus as Probiotics OrogastricallyAdministered to RatsV. O. Oyetayo 263

Restriction of Root and Shoot Growth Limits Their Growth Rates and Changes theMorphology of Cotton Seedlings During EmergenceGhulam Nabi and C. E. Mullins 268

Evaluation of Nutritive Properties of the Large African Cricket (Gryllidae sp)Yemisi A. Adebowale, Kayode O. Adebowale and Michael O. Oguntokun 274

Prevalence of Intestinal Helminth Parasites of Dogs in Lagos, NigeriaComfort Adejoke Ibidapo 279

Correlation and Path Analysis in Candidate Bread Wheat (Triticum aestivum) LinesEvaluated in Micro-Plot Test TrialTila Mohammad, Sajjad Haidar, M. Jamil Qureshi, Abdul Jabbar Khan and Roshan Zamir 284

Short Communication

Studies on the Utilization of Oscillatoria thiebautii as Food Source for Artemia sp CultureS. G. Abbas Shah, Razia Sultana and Abid Askari 289

Technology

Isolation, Determination and Characterization of Taro (Colocasia esculenta) StarchFeroz A. Jaffery, Abid Hasnain, Khalid Jamil and Tahir Abbas

292

Vol. 48(5), September - October 2005

Physical Sciences

On Methods Derived from Hansen-Patrick Formula for Refining Zeros of PolynominalEquationStephen Uwamusi 297

Studies of Molecular Interactions of ααααα-Amino Acids in Aqueous and Cationic SurfactantSystems Investigated from Their Densities and Apparent Molal Volumes at 283.15,288.15 and 293.15 KMan Singh 303

Liquid-Liquid Equilibrium Data of Ternary Systems of Water, Acetic Acid and Alkanols(1-Butanol, 1-Pentanol and 1-Hexanol)M. A. Rahman, M. S. Rahman, M. N. Nabi and M. A. K. Azad 312

Synthesis and Antimicrobial Activity of Some Heterocycles: Part-VM. M. H. Bhuiyan, Khandker M. M. Rahman, M. K. Hossain and M. A. Rahim 318

Pak. J. Sci. Ind. Res. 2005, Vol. 48(6)

viii

Combined Aerobic and Physicochemical Treatment of Pharmaceutical Industry SludgeI. O. Asia and C. M. A. Ademoroti 322

Essential Oil Composition of Green Peel of the Inter-Varietal Mandarin Hybrid, KinnowOrangeShahid Mahmud, Amran Waheed, Tanzeela Nazir and Razia Khanum 329

Biological Sciences

Biochemical Changes Induced in Some Rabbit Tissues on the Administration of anAntimalaria Drug, FansidarO. I. Oloyede and M. F. Asaolu 334

Interspecific Variations in the Fecundity of Some Dominant Fish Populations inIkpoba River, NigeriaL. I. N. Ezemonye and F. A. Osiezaghe 338

Numerical Taxonomy of Two New Mite Species of the Genus Caloglyphus Berlese(Acaridae) from PakistanMuhammad Sarwar, Muhammad Ashfaq and Shamshad Akbar 345

Cause and Effect Relationship for Some Biometric Traits in Bread WheatNazar Muhammad Cheema, Muhammad Ashraf Mian, Muhammad Ihsan,Muhammad Azeem Tariq, Ghulam Rabbani and Abid Mahmood 354

Combining Ability Analysis of Seed Cotton Yield and its Components in Cotton(Gossypium hirsutum)Muhammad Tehseen Azhar and Asif Ali Khan 358

Effect of Storage Fungi on the Seed Quality Parameters of Different Mustard VarietiesTamoor Khan, K. Khan and Muhammad Zahoor ul Haq 362

Short Communications

Evaluation of Commercial and Candidate Bread Wheat Varieties for Durable Resistance toRusts in PakistanSyed Jawad Ahmad Shah, Tila Muhammad and Farooq-e-Azam 366

Multiple Shoot Bud Formation and Plantlet Regeneration from in vitro Cultured Pistacia veraSeedsShaista Jabeen and Nasreen Zaidi 368

Vol. 48(6), November - December 2005

Physical Sciences

Electrochemical Reduction of 4-(3-Pyridylazo)-3-Amino-2-Pyrazolin-5-OneRefat Abdel-Hamid, Mostafa K. M. Rabia and Nadia A. Abdalla 371

Pak. J. Sci. Ind. Res. 2005, Vol. 48(6)

ix

Catalytic Transfer Reduction of Electron Deficient Alkenes and an Imine Using PotassiumFormate and Catalytic Palladium AcetateMd Mosharef Hossain Bhuiyan 377

Synthesis and Characterization of Dimethyltin(IV) Complex with 2-Methylpyridyl-benzhydrazone (AcPyBzh): Crystal Structure of [Me2SnCl (AcPyBzh)]M. A. Affan, Fasihuddin B. Ahmad, Ramli B. Hitam, Mustafa B. Shamsuddin andBohari M. Yamin 381

Mass Fragmentation Pattern of Some Mono- and Di-Substituted Formamidines. Part-1.Mass Pattern of 1-ArylformamidinesM. Umar Ali, M. Zahurul Haque, M. Abdullah Al-Maruf and M. Abdullah As-Saki 386

Intramolecular Fatty Acids Distribution in the Triglycerides of Hordeum vulgareSalma Rahman and Tanveer Ahmad Chaudri 389

A Comparative Study on the Determination of Fe in Groundwater by Different MethodsM. R. Zaman, R. A. Banu and A. Yousuf 393

Concentration and Distribution of Some Heavy Metals in Urban Soils of Ibadan, NigeriaI. U. Umoren and P. C. Onianwa 397

Biological Sciences

Effects of Physical and Chemical Treatments on the Enzymatic Activities of Rice Bran LipasesM. Zahurul Haque, Nurul Absar and M. A. Jalil 402

Rose Bengal and Mercaptoethanol Tests for the Diagnosis of Brucella abortus Biotype-1Infection in Sprague-Dawley RatsM. S. Rahman and B. K. Baek 407

Prevalence of Onchocerciasis Syndrome in Ise-Orun Local Government Area of Ekiti State,NigeriaL. K. Olofintoye, S. O. Adewole, F. B. Erinle and A. I. Ajayi 412

Incorporation of Button Mushrooms in Pakistani DishesTasnim Kausar and Rukhsana Bajwa 417

Seasonal Incidence and Extent of Damage Caused by Citrus Leaf Miner, Phyllocnistis citrellaStainton Infesting LemonHabibur Rahman, Khandakar Shariful Islam and Mahbuba Jahan 422

Technology

Chromate Coating of Zinc-Aluminum Plating on Mild SteelInam-ul-Haque, Asim Khan and Nadeem Ahmad 426

Pak. J. Sci. Ind. Res. 2005, Vol. 48(6)

x

Short Communication

Spectroscopic and Dyeing Characteristics of the Yellow Dye from Morinda lucida(Brimstone Tree)A. O. Adetuyi, L. Lajide and A. V. Popoola 430

Analysis and Purification of Nkalagu (Nigeria) Limestone and Poultry Eggshells for theProduction of Paint Grade Calcium CarbonateE. Osabohien, E. O. Adaikpoh and F. I. Nwabue 433

Review

Fundamental Concepts and Mechanisms in the Metal Biosorption Technology for theTreatment of Industrial WastewatersAsma Saeed, Asia Aslam and Muhammed Iqbal 436

Pak. J. Sci. Ind. Res. 2005, Vol. 48(6)

AUTHOR INDEX TO VOLUME 48Pak. J. Sci. Ind. Res. 2005, Vol.48(6) Author index

Abbas, T. 292Abdalla, N. A. 371Absar, N. 190, 402Abulude, F. O. 110Abu-Sayeed, M. 122Adaikpoh, E. O. 433Adanlawo, I. G. 257Adebowale, K O. 274Adebowale, Y. A. 274Ademilua, O. L. 154Ademoroti, C. M. A. 322Adeosun, B. F. 63, 131Adetuyi, A. O. 59, 430Adewole, S. O. 412Adeyeye, E. I. 14Affan, M. A. 381Afza, N. 180Ahmad, F. B. 381Ahmad, M. 42Ahmad, N. 426Ahmad, S. A. 209Ahmed, A. S. 236, 240Ahmed, R. 174Ahonkhai, S. I. 103Ajayi, A.I. 412Ajibade, V. A. 257Akande, T. T. 257Akbar, S. 345Akhtar, L. H. 42Akhtar, M. M. 42Akram, A. 236Ali, I. 220Ali, M. A. 112Ali, M. U. 386Ali, S. I. 128Ali, Y. 180Al-Maruf, M. A. 386Aluko, P. O. 113Amatya, S. 212Amjad, R. 47Anwar, M. A. 180Anwar, M. M. 184Arshad, M. 42Asaolu, M. F. 334Asaolu, S. S. 96Ashfaq, M. 345Asia, I. O. 322Askari, A. 289Aslam, A. 436Aslam, M. 42

As-Saki, M. A. 386Astaq, G. R. M. 122Atiq, S. 86, 231Awofolu, O. R. 28Awopetu, J. I. 113Ayejuyo, O. O. 39Azad, M. A. K. 312Azam, F. 220, 366Azhar, M. T. 358

Baek, B. K. 407Bajwa, R. 417Baloch, M. K. 209Banu, R. A. 393Bashir, N. 51Bhattacharjee, P. K. 112Bhatty, M. B. 240Bhuiyan, M. M. H. 37, 318, 377Bi, F. 216

Chaudri, T. A. 389Cheema, N. M. 354Choudhury, A. 162

Ejimadu, I. M. 126Eluyode, O. S. 110El-Zahar, M. I. 184Erinle, F. B. 412Ezemonye, L. I. N. 338

Fagbohun, E. D. 14Fagbuaro, O. 113Fakruddin, M. 37Faluyi, M. A. 113Farid, S. 209Farooq, A. 135

Ghosh, A. 55

Hafeez, I. 86Haidar, S. 284Hakro, A. A. 57Hamid, N. 236Hamid, R. A. 371Haq, M. Z. 362Haque, I. U. 426Haque, M. Z. 190, 386, 402Hasnain, A. 292Helmi, M. S. 75Hina, A. S. 247

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Hitam, R. B. 381Hossain, M. A 108Hossain, M. K. 318Hussain, G. 42Hussain, M. 42

Ibidapo, C. A. 279Ihsan, M. 354Ikhuoria, E. U. 68Iqbal, M. 436Iqbal, S. 216Islam, A. 122Islam, K. S. 422Ismail, Z. 108

Jabeen, S. 368Jaffery, F. A. 292Jahan, M. 422Jalil, M. A. 190, 402Jamil, K. 292Javed, M. A. 47

Kamel, M. M. 184Kamruzzaman, M. 252Kashmiri, M. A. 51Kausar, T. 417Khalique, A. 236Khan, A. A. 358Khan, A. F. 128Khan, A. J. 284Khan, A. 57Khan, A. 426Khan, G. H. 167Khan, K. 86, 362Khan, M. N. 90Khan, M. 122Khan, T. 362Khanam, R. 1, 329

Lajide, L. 59, 430

Mahmood, A. 354Mahmud, S. 329Malik, M. A. 86Mian, M. A. 354Mohammad, T. 220, 284Moisili, O. R. 39Mollah, M. L. R. 252Muhammad, T. 366Mullins, C. E. 268

Munshi, A. B. 247Murtza, G. 135

Nabi, G. 268Nabi, M. N. 312Naeem, M. 47Nakpodia, F. A. 118Nawaz, S. M. 135Nazir, T. 329Nwabue, F. I. 433

Obuekwe, I. F. 23Ogunkoya, M. O. 110Ogunniyi, D. S. 143Oguntokun, M. O. 274Okieimen, F. E. 68Okoh, L. I. 23Okor, R. S. 8Okuo, J. M. 126Oladimeji, M. O. 59Olaofe, O. 63, 96Olofintoye, L. K. 412Oloyede, O. I. 334Olumayede, E. G. 131Onianwa, P. C. 397Oronsaye, C. G. 118Osabohien, E. 433Osiezaghe, F. A. 338Oyeleke, A. E. 131Oyetayo, V. O. 263Oyinloye, A. O. 154

Popoola, A. V. 59, 430

Qari, R. 195Qazi, M. P. I. 240Qian, Y. 81Quraishi, S. B. 202Qureshi, M. J. 284

Rabbani, G. 354Rabia, M. K. M. 371Rahim, M. A. 318Rahman, H. 422Rahman, K. M. M. 318Rahman, M. A. 312Rahman, M. L. 190Rahman, M. S. 312, 407Rahman, S. 389Raimi, O. G. 39

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Rashid, A. 42Rawlings, R. D. 231Razaque, A. 209Roston, G. D. 75Roy, M. N. 162

Sadiku, Y. T. 103Saeed, A. 436Saeed, M. K. 81Saeed, M. T. 1, 240Saeed, R. 167Safdar, M. 42Sarwar, A. 90Sarwar, M. 345Shah, S. G. A. 289Shah, S. J. A. 209, 220Shahbaz, B. 135Shaheen, M. Y. 1Shahjahan, M. 252Shamsuddin, M. B. 381Sharma, S. 223Siddiqi, S. Z. 42Siddiqui, S. A. 195Singh, M. 303Sultana, N. 180Sultana, R. 289Syed, Q. 51

Tahir, H. 90Tariq, A. H. 42Tariq, M. A. 354Tiwari, J. K. 223Tuladhar, S. M. 212

Uddin, F. 167Uhumwangho, M. U. 8Ukpebor, E. E. 103Umoren, I. U. 397Usmani, T. H. 247Uwamusi, S. 149, 297

Waheed, A. 329West, D. R. F. 231

Yamin, B. M. 381Yeasmin, S. 122Yong-Sam, C. 202Yousaf, M. 81Yousuf, A. 393

Zakaria, Z. 108Zaidi, N. 368Zaman, M. R. 393Zamir, R. 284

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