Synthesis of high acidity nanocrystalline γγγγ-Al 2O3 by...

J. Indian Chem. Soc.,

Vol. 90, September 2013, pp. 1285-1291

Synthesis of high acidity nanocrystalline γγγγ-Al2O3 by sonochemical method

Hosein Nazarpour*, Omid Rahmanpour and Mohammad Reza Khosravi Niku

Gas Engineering Department, Petroleum Universi ty of Technology, Ahwaz, Iran

E-mail : [email protected], [email protected], [email protected]

Manuscript received online 24 August 2012, revised 17 October 2012, accepted 01 November 2012

Abstract : Effect s of ult ras onic i rrad iation on the catalyt ic ac id ity and morphology of γγγγ -Al2O 3

catalyst we re studied. XRD, N2 ads orption-des orption (BET) , SEM and NH3 -T PD tests were use d to

c haracte rize the s amples. Accord ing to the XRD res ult, ult ras ound di d not dest roy the c atal yst ’ s

s t ructure. T he SEM microg raph of cata lyst synthesize d unde r ul trasonic irrad iation (U-s) s ho we d

s mal le r partic les s i ze than othe rs s amples indicat i ng t hat s onoc hemic al method has a major impact on t he morpholog y of γγγγ -Al2O3 . Also NH3 -TPD test indicate d that ultrasound irrad iat ion i nc rease d acidity

of γγγγ -Al2O3 nanoc atalyst f ro m 0 .491 to 1 .139. Accord ing to the expe rimental res ults , the c atal yst

pre pared using sonoc he mical method s ho we d bette r pe rformance compared with those pre pared by

othe r met hods. Keywords : γγγγ -Al2 O3 , ul t ras ound, morpholog y, acid ity.


Vol. 90, September 2013, pp. 1293-1300

Solvent effect on protonation equilibria of 2,3-dihydroxybenzoic acid and malonic acid

Belete Yilma Hirpaye and Gollapall i Nageswara Rao*

Department of Inorganic and Analytical Chemi stry, School of Chemistry, Andhra University,

Visakhapatnam-530 003, Andhra Pradesh, India, E-mail : [email protected]

Manuscript received online 12 October 2012, accepted 01 November 2012

Abstract : T he protonat ion c ons tants of 2 , 3-dihydrox ybe nzoic ac id and malonic acid at 303 .0 ± 0 .1 K and 0 .16 mol dm– 3 ionic stre ngth in 0–60% v/v diox an-wate r mixtures we re determined by the pH-

metric me thod us ing MI NIQUAD75 c omput er prog ra m. Selection of the bes t f it c he mic al model of the

protonat ion equil ibria i s based on s tanda rd deviat ion i n protonat ion constants and res idual anal ys is

using c rystal log raphic R-factor and s um of squares of res iduals in a ll mass balance equati ons. Line a r

variati on of protonat ion constants with inve rse of die lectric cons tants of t he s olve nt mixture has bee n

att ribute d to the domi nance of the e lectrost at ic forc es. Distributions of s pecies, protonat io n

equili bria and ef fect of influe ntial para mete rs on the prot onation c ons tants have a ls o bee n d isc usse d. Keywords : 2, 3 -Dihydrox ybe nzoic ac id, malonic ac id, protonati on cons tants, diox an, MINIQUAD75.


Vol. 90, September 2013, pp. 1301-1309

Structural and spectroscopic aspects of 2,3-butanedionemonoxime- monohydrazone : Theory and experiment

Jnan Prakash Naskara*, Bhargab Guhathakurtaa , Liping Lub , Miaoli Zhub* and Rahul Bhattacharyac

aDepartment of Chemistry, Inorganic Chemistry Section, Jadavpur University, Kolkata-700

032, India, E-mail : jpnaskar@rediffmai l.com

b Insti tute of Molecular Science, Key Laboratory of Chemical Biology and Molecular

Engineering of the Education Ministry, Shanxi University, 92 Wucheng Road, Taiyuan, Shanxi

030006, P. R. China

c Indian Chemical Society, 92, Acharya Prafulla Chandra Road, Kolkata-700 009, India

E-mail : drrahulchem@rediffmail .com


Abstract : 2 ,3 -B utane dionemonox ime-mono hydra zone (B DMMH) (1), a 1 : 1 Schi ff base conde ns ate of 2 , 3-butane di one monoxime with hydrazine hydrate , was s ynthes ized i n methanol . Compound 1 has

bee n c haracte rize d by C, H and N mic roanalyses, FT -I R, 1H NM R and UV-Vis s pect ra. The so li d state

s tructure of i t has bee n de te rmine d throug h X-ray c rystal log raphy. T he compound c rystal li zes in the

monocl inic s pace g ro up with a = 6 .440(4), b = 4 .256(3), c = 10 .703(7) Å, ββββ = 94.102(7), V = 292 .6(3) Å3

and Z = 2 . The c ompound is in the syn-methyl and sy n-methyl conformation. Calculat ions at the le vel

of De nsi ty Funct ional T he ory (DFT) we re a ls o pe rforme d to c orroborate the s ol id s tate structure.

Compute d I R s pectrum of 1 was compa re d with the experi me nt al val ues. A Molec ular Orbita l (MO)

level of anal ysis was als o undert ake n to s ubstanti ate the UV-Vis spectra l f i ndings. 1 H NM R c he mic al s hi f ts of 1 in the TM S sca le in CDCl3 is in s at i sfact ory harmony with the calc ul ate d c he mic al s hi f ts

based on Gauge-I nde pende nt Atomic Orbita l (GI AO) approac h. Keywords : Sc hif f base , ox ime, X-ray c rysta l st ructure, DFT calc ulations.


Vol. 90, September 2013, pp. 1311-1317

Synthesis, crystallographic characterization and DNA binding properties of a manganese(II) complex containing 1,10-phenanthroline ligand

Bhaskar Biswasa*, Partha Mitrab and Rajarshi Ghoshc*

aDepartment of Chemi stry, Raghunathpur College, Purulia-723 133, West Bengal, India

E-mail : [email protected]

bDepartment of Inorganic Chemistry, Indian Association for the Cultivation of Science,

Kolkata-700 032, India

cDepartment of Chemistry, The University of Burdwan, Burdwan-713 104, West Bengal, India


Manuscript received online 03 November 2012, accepted 14 November 2012

Abstract : A mononuc lear mang anese(I I ) complex [M n( phe n)2 (OH2 )2 ][M n(phe n)2 (OH2 )Cl] (NO3 ) 3 (1 )

conta ining 1, 10-phe nanthrol ine [phe n=1,10-phe nanthrol ine] l igand has bee n s ynthesize d and

c rystal lographic al ly c haracte rize d. The oxidat i on leve l of the manganese at oms in two asymmetric

uni ts was dete rmine d by bond vale nce s um c alc ulat ion (B VS). T he DNA b indi ng s tudy has bee n

explore d by spectrophot omet ric and s pectrofluo rimetric meas ure me nts. Keywords : Mang anese(I I ), BVS calc ulat ion, s upra molec ular inte ract ion, DNA bind ing study.


Vol. 90, September 2013, pp. 1319-1325

Synthesis of hydroxyapatite by sol-gel combustion method using tricarboxylic acid and diamide as a mixed fuel

Swamiappan Sasikumar

Centre for Excel lence in Nanomaterials, School of Advanced Sciences, VIT University,

Vellore-632 014, Tamilnadu, India, E-mail : [email protected]

Manuscript received online 13 March 2012, revised 03 November 2012, accepted 20 November 2012

Abstract : Calcium hydrox yapatite was s ynthes ize d by s ol -gel combust ion method by e mployi ng ure a

and ci t ric aci d as a mixe d fuel. Nitric acid was used as an oxi di zer; c alc ium nitrate and di-ammonium

hydroge n phosphate we re take n as the c alc ium and phos phate precurs or re spect ive ly. The inf lue nce of

metal ion to fue l rat io on the phase e volution and morphology was studied. The s ynt hes ized po wde rs

we re c haracteri zed by powder X-ray di ff ractomete r for phase evolution and Fourie r t ransfor m

i nf rared s pectrometer was use d to f ind out the c arbonate s ubs ti tution in hydrox yl and phosphate

s ites. T he rmal analys is was carrie d out to ve ri fy the phase t ransi t ions and the rmal s tabil i ty o f the

products. The re s ult s ho ws the influe nce of ratio of f uels on the auto ignit ion te mperature as the auto

igni t ion te mpe rature of urea dec reases by t he addit ion of c i t ric acid. I n addit ion, t he phase formatio n

i s found to vary with the me ta l ion to fuel rat i o, irrespe ct ive of the i ni tia l metal i on to phos phate

rati o. Keywords : Biomate rials , se lf -propagati ng synthe sis , phase t ransformation, X-ray di f f ract ion.


Vol. 90, September 2013, pp. 1327-1333

Synthesis, characterization, thermal, electrical conductivity and biological studies of Schiff base metal complexes

N. J. Suryawanshia , G. B. Pethe, S. G. Bhadangeb and A. S. Aswar*

Department of Chemistry, Sant Gadge Baba Amravati University, Amravati-444 602,

Maharashtra, India, E-mail : aswar2341@rediffmail .com

aDepartment of Industrial Chemistry, Arts, Science and Commerce College, Chikhaldara-444

807, Maharashtra, India

bDepartment of Chemi stry, Shri Shivaji College, Akola-444 001, Maharashtra, India

Manuscript received online 25 Apri l 2012, revised 28 August 2012, accepted 22 November 2012

Abstract : The c oord ination c omplexes of M nI I , CoI I , NiI I , CuI I , Ti I I I , CrI I I , Fe I I I , ZrIV and UO 2V I

wi th new Sc hif f base de rived from 3-acety l-6-met hyl-2H -pyran-2 ,4(3H)-d ione (de hydroacetic acid)

and thiocarbohydrazide have bee n synthesize d. T hese c om plexes have bee n c ha rac te rized on the basis

of ele me ntal analys is , I R and elect ronic spectra, mag net ic mome nt and the rmog ravimet ric analysis .

T he c omplexes are c olore d and s table in air. The ligand ac ts as d ibasic tetrade nt ate nature and forms

1 : 1 (metal : l igand) c omplexes with the metal i on. The the rmal be havior of me ta l c omplexes s ho w

t hat the hydrate d c omplexes l ose molec ules of hydrat ion f irst; fo ll owe d by decompos iti on of l igand molec ules in the s ubsequent s te ps. The s ol id- state electric al c onductivi ty of lig and and its c omplexes

have bee n meas ure d ove r a wide range of te mpe rature in thei r c omp re ssed pellet form and the

complexes are found to be of se mic onduct ing in nature. T he lig and and i ts complexes have als o bee n

tested for their ant i mic robia l be havior agains t vari ous microo rg anis ms and al l c omplexes s ho w a

good act ivity. Keywords : Hydra zone Schif f base complexes, IR spectra, DC c onduc tivity, TGA, ant imic rob ia l act iv ity.


Vol. 90, September 2013, pp. 1335-1339

A new method for on-line dissolution and determination of trace impurities in high silica material using inductively coupled plasma atomic emission spectrometry

S. S. Mukhopadhyay and Dipal i Kundu*

Analytical Chemistry Section, Central Glass and Ceramic Research Institute, Kolkata-700 032,

India, E-mail : [email protected]. in Fax : 91-33-24730957

Manuscript received online 01 June 2012, revi sed 22 November 2012, accepted 26 November 2012

Abstract : A si mple and rap id me thod has bee n de vel oped for online dis so lution of hig h si l ic a materi al fol lowe d by the determinat ion of t race i mpuri t ies in I CP-AES. Hi gh sil ic a materi al was

placed in a mixture of HF and wate r (1 : 2 ) inside a polypropyle ne bott le . Afte r cappi ng the l id, the

bottle was kept at room te mperature (25 ± 5) ºC for 45 mi n with occ asional ma nual s ha king. The

res ultant s olut ion in HF was tes ted for me ta ll ic t race imp urit ies directl y in I CP-AE S. The test res ul t

of the rap id diss olut ion tec hnique was c hec ke d with those obta ine d by conve ntional diss o lution of the

materi al in s upra pure HF. T he res ult s obtai ne d by two di ff erent sample dis sol uti on techniques we re

i n ve ry g ood ag ree me nt . Acc uracy of the me thod has bee n ve ri f ie d by anal yzi ng ce rt ifie d refe re nce

hig h si lic a mate ria ls li ke quartz, SAB, SARM 49 and hig h puri ty sil ic a, B CS-CRM.313/1 . Keywords : Hig h si l ic a mate ria ls , acid diss olution, po lypro pyle ne bot t le , ICP- AES.


Vol. 90, September 2013, pp. 1341-1346

Mixed ligand complex equilibria and coordination tendencies of CoII, NiII, CuII and ZnII with L-glutamine/L-citrulline and uracil

Divya Bartariaa , Moni ka Singh and V. Krishna

Department of Chemistry, University of Allahabad, Al lahabad-211 002, Uttar Pradesh, India

aUnited Institute of Technology, Naini, Allahabad-211 002, Uttar Pradesh, India


Manuscript received online 27 October 2012, revised 16 November 2012, accepted 30 November 2012

Abstract : The s peciati on, plausi ble e qui l ibrium and s oluti on structural study of mixe d-l igand

complexes of L-g lut amine/ L- ci t rul l ine and urac il has bee n invest igated by pote nt i ome try i nvolving

Cu I I , ZnI I , NiI I and CoI I metal ions. T he ove rall stab il i ty constants of te rna ry complexes have bee n dete rmine d in bi ol og ical l y relevant c ond iti ons and at ionic stre ngt h of 0 .1 M NaNO 3 . The models

conta ining di ffe re nt numbe rs of s pecies we re ref i ne d by using the c ompute r prog ram SCOG S. The

s tabi l ity c ons tants and complex at ion e quil ibria for the bes t-fi t c hemic al models we re arri ve d at base d

on stat is t ica l paramete rs. The tre nd i n variation of stabil ity c onstants of 1 : 1 : 1 L-Gln/L-Cit(A) :

M I I : uraci l(B) e vide nce d as ACuI IB > AZn I IB > ANiI IB > ACoI IB; is attributed to the electros tat ic

and non-elect rostat ic forces. Keywords : Glutamine, uracil, c it rul l i ne , mixe d ligand complex .


Vol. 90, September 2013, pp. 1347-1352

Ho3+-PVC membrane potentiometric electrochemical sensor based on 2-acetylfurane thiosemicarbazone as an ionophore

Hassan Ali Zamania*, Azadeh Tadjarodib and Saeedeh Eslaminezhadb

aDepartment of Applied Chemistry, Mashhad Branch, Islamic Azad Universi ty, Mashhad, Iran


bDepartment of Chemi stry, Iran University of Science and Technology, Tehran, Iran

Manuscript received online 15 June 2012, revi sed 30 November 2012, accepted 06 December 2012

Abstract : A highly se lect i ve and se nsit ive p lastic i zed me mbra ne se ns or for holmium( I I I ) ions, base d on 2-acetylfurane thiose mic arbazone (AFT) as me mb rane carrie r, was pre pare d. The se ns or s hows a

l ine ar dynamic range of 1. 0 × 10 –6 to 1. 0 × 10 – 2 M , wi th a Ne rnst ian slope of 19 . 8 ± 0 .3 mV pe r

decade, and a detect ion l imit o f 5 .5 × 10 – 7 M . It has a fas t res ponse time of ~5 s and could be use d in a

pH range of 2 .3–7 .8 . The propose d sensor re ve ale d very good se lectivi ties with res pect to mos t of the

common me ta l i ons i nclud ing Yb, Sm, P r, G d, Er, T m, Cr, Fe, Na, K , Ca, Cd, Ni and P b ions. The

prac tic al ut il i ty of the se ns or has been de mo nst rated by us ing it as an indic ator e lectrode in the

pote nt iome tric t it rat ion of HoI I I wi th E DT A, dete rmi nation of fluo ride i ons in two mo uth was h

pre parati ons and als o to the dete rmi nati on of HoI I I ions in tap wate r and ri ver wate r samples. Keywords : Pote ntiometry, ion-select ive e lectrode, P VC me mbra ne, sens or.


Vol. 90, September 2013, pp. 1353-1360

Studies on magnetic behavior of the yttrium barium copper oxide sample obtained from polymeric precursor technique

Aloke Chattopadhyay

Department of Chemistry, S. B. College, Bagati , Mogra, Hooghly-712 148, West Bengal, India

E-mail : aloke.chat [email protected]

Manuscript received online 24 September 2012, revised 30 November 2012, accepted 22 December

2012

Abstract : It was poss ible to achie ve yttrium barium coppe r ox ide (Y1B a2 Cu4O8 ) by polyme ric

prec urs or t ec hnique using s odi um polyac ryl ate . I n this prese nt investig at ion, mate rial obtained by

polyme ric prec urs or t ec hnique, is was he d wit h dist il led wate r for seve ral t ime s, dried and mag net ic

me as ure me nts have bee n c arried out. It has bee n found that fe rromag net ic be havior is ind icate d at 77 K and XRD study indicates prese nce of Y 1Ba2 Cu2 . 8 4 O6 . 5 8 with some impuri ty. Mome nt vs

t empe rature plot s ho ws magnet ic nature eve n ne ar about at 300 K . So the mate rial may be useful. Y 1Ba2 Cu2 . 8 4O6 . 5 8 in t he materi al is expected to c ontribute in mag net ic behavior. SEM image ind ic ates

di ffe re nt phases. Che mical analysis has bee n done by EDS which ind icates prese nce of Y , Ba, Cu, O

and ve ry lit t le amo unt of Na. Keywords : Polyme ric prec urs or, polyvalent metal ion, X-ray dif f ract ion study, mag net ic mate rial .


Vol. 90, September 2013, pp. 1361-1366

Application of 1-(1,3-dioxoisoindolin-2-yl)-3-phenylurea as a sensing material in construction of Tm3+-ion selective electrochemical sensor

Mahmoud Ebrahimi and Hassan Ali Zamani*

Department of Appl ied Chemi stry, Mashhad Branch, Islamic Azad University, Mashhad, Iran


Manuscript received online 06 August 2012, accepted 23 December 2012

Abstract : A Tm3 + -PVC me mbrane ion-selective e lect rode has bee n fabri cated based on 1- (1, 3-dioxois oindol in-2-yl)-3-phenylure a (IPU) as a s uitable se nsing mate rial. T he sensor ex hi bi ts a line a r

dynamic range of 1 .0 × 10 –6 –1.0 × 10– 2 M with a Ne rns tian slope of 20 .8 ± 0 .4 mV pe r dec ade of

t huli um conce nt rati on and a detect ion l i mit of 6 .3 × 10– 7 M . A quic k res ponse time for t he se ns or

( s mal le r tha n 10 s) was obse rve d, and the e lectrode was found to work in the pH range of 2 .4–9 .8 . The

rec omme nde d se ns or reve ale d c omparative ly g ood se lectivit y with respect to mos t a lkal i, a lka l ine

earth, some trans i tion and he avy metal ions. T o assess its analytic al appl ic abi lity the proposed T m3 +

s ens or was s uccessful ly e mploye d as an indic at or e lect ro de in the tit ration of Tm3 + ion with EDTA

and the T m3 + dete rmination in b inary mixtures. Keywords : PVC me mbra ne, se ns or, pote nt iometry , ion-se lective e lectrode.


Vol. 90, September 2013, pp. 1367-1378

Spectrophotometric microdetermination of gadolinium(III) and terbium(III) with xylenol orange in presence of cationic cetylpyridinium bromide as a surfactant

A. B. Zadea* and A. S. Dhepeb

aDepartment of Chemi stry, Laxminarayan Insti tute of Technology, R. T. M. Nagpur

University, Nagpur-440 010, Maharashtra, India

E-mail : [email protected] Fax : 91-712-2561107

bDepartment of Applied Chemistry, Smt. Radhikatai Pandav College of Engineering, Nagpur-

411 204, Maharashtra, India, E-mail : [email protected]

Manuscript received online 04 December 2012, revised 28 December 2012, accepted 30 December 2012

Abstract : Xyle nol orange (XO ) has bee n reporte d earlie r to f orm v iolet c ol ored binary c omplexes

with se ve ral lanthanides and used for the dete rminat ion of se ve ral meta l ions. The additi on of cati onic s urfactant, cetyl pyrid inium bro mide (CPB) to the colored s olution of xy le nol orange res ulte d

i nt o d isc oloration at s pecific pH values whic h is due to the i nteract ion of anionic XO with cationic

CPB. The add it ion of s peci f ic meta l ions to this deco lori ze d s olution re s ulted into format ion of deep ly

colored wate r s olub le stable te rna ry c omplexes with a large bathochro mic s hi ft of 42 nm wit h

i nc re ase in abs orbance at s hifte d wave le ngth. Stoic hiometric c ompos i tion of 1 : 2 : 4 ( e .g . Gd I I I-XO-

CPB) has bee n obse rved by Job’s met hod of cont inuous variat ion. T he val ues of log K for bot h binary

and te rnary c omplexes have bee n c alc ul ated. The te rnary complexes we re formed in wide r pH ra nge

with increase in st abil ity and ex hibite d absorpt ion ma xima at 612 nm for both the me ta l ions

unders tudy. Various analyt ical para mete rs l ike orde r of addition of re actants, eff ect of t i me and

tempe rature, effect o f re age nt concentration, Beer’ s l aw, photometri c ranges, Sandell ’s se nsit i vity

and molar abs orpt ivity have a ls o bee n calculate d and compared. T he ef fects of inte rfe ring i ons o n

dete rmination of both the met al ions we re studied. A sim ple, rapid and highly se nsi ti ve met hod fo r

t he dete rmi nati on of Gd I I I and T bI I I wi th xy le nol orange i s propose d. Keywords : Spectrophotometry, xyle nol ora nge (XO) , cetylpyrid inium bro mide (CP B) , gadol inium (Gd), te rbium (Tb) .


Vol. 90, September 2013, pp. 1379-1382

The determination of pharmaceutically important ibuprofen by non-aqueous potentiometric titration method

Vaishali R. Patil and Pradip P. Deohate*

Department of Chemistry, Shri Radhakisan Laxminarayan Toshniwal College of Science,

Akola-444 001, Maharashtra, India, E-mail : [email protected]. in

Manuscript received online 05 December 2012, revised 26 December 2012, accepted 30 December 2012

Abstract : The dete rmi nat ion of pharmace utic al ly important ibuprofe n by no n-aque ous pote nt iome tric ti t rat ion method using is opropyl alc ohol as t he so lve nt and KOH in is opropyl alc ohol

as the tit ra nt has been est ab li s he d. The study of ef fect of s ol vent and c once ntration on potenti omet ric

dete rmination of ibuprofe n has bee n carrie d out fol lowe d by the est imat i on of ibuprofe n in sing le

component t ablets . The t it rat ions we re carrie d out us ing a pair of g lass and ca lomel e lectrode. The

method was found to be precise for ass ay of ibuprofe n and res ults obta ine d are c omparab le with those

obta ine d by I .P. method. Keywords : Ibup rofe n, non-aqueous, pote nt iometri c tit ration.


Vol. 90, September 2013, pp. 1383-1393

Comparative studies on the efficiency of filters of different brands of cigarettes in reducing nicotine and other hazardous chemicals from smoke condensates – A gas chromatography-mass spectrometry study

Ashutosh Chakraborttya and Sujit Chandra Lahiri*

Central Forensic Science Laboratory, 30, Gorachand Road, Kolkata-700 014, India

E-mail : [email protected], c.ashu@rediffmai l.com


Abstract : Smo king of c ig aret tes, a tobacco product has be e n found to be haza rdous to the cons ume rs due to the pre se nce of addict ive and tox ic c hemical nicoti ne and a l arge numbe r of haza rdous

c he micals li ke carbo nmo nox ide, hydroc yanic ac id, po lyaro matic hydroc arbon (PAH) etc . in c ig are tte

s moke conde ns ates. The compounds are res ponsible for heart diseases and c ance rs. However,

manufacture of c igare ttes i s as s oci ated with e mpl oyme nt, tax ge ne rat ion and prof it . At tempts have

bee n made to produce f ilte r t ippe d c igaret tes with s uit able ads orbe nts of ha zardous c hemic als to

make c igare tte s moki ng ple as ant and less injurious to health.

Comparat ive studies on the cons tit ue nts of fi l te rs of dif f e rent ma ke s and their e ffective ness in

reducing injurious const i tue nts of s mo ke conde ns ates of dif fe re nt c igarettes had bee n made.

Chloroform is use d as s olve nt and g as c hro matog raphy-mass s pectro metry (GC-M S) was use d for the

ide nti f ic ation of the c he mic al c onstitue nts of fi l te rs and abs orbed c he mic als f rom s mo ke conde ns ates.

T riace tin wth c it rof lex based and triaceti n with d ipropyle ne (d iethyle ne ) g lycobe nzoate we re f ound to

be mos t effect ive to arrest t he most haza rdous c ompound nic otine and othe r c he mic als. Ads orptio n

capaci ties o f f il te rs use d in low price d counte rfe it c ig aret tes was lo w and a ls o c ont ai n haza rdous

c he mical di butyl phthalate . More works are nee ded to have a better picture. Keywords : Chloroform, c igarette , filt ers, gas c hromatog ra phy-mass spectro metry (G C-MS), nicot i ne, s mo ke conde nsates, tobacc o.


Vol. 90, September 2013, pp. 1395-1401

Studies on the kinetics of tetrahexylammonium bromochromate oxidation of methionine in various percentage of acetic acid + N,N-dimethylformamide mixture

S. Sheik Mansoora* and Basim H. Asgharb

aPost Graduate and Research Department of Chemistry, C. Abdul Hakeem College,

Melvisharam-632 509, Tamilnadu, India, E-mail : [email protected]. in

bDepartment of Chemistry, Faculty of Applied Sciences, Umm Al-Qura University, Makkah,

Saudi Arabia

Manuscript received online 21 October 2012, revised 18 November 2012, accepted 19 November 2012

Abstract : Methioni ne (Met ) is a natural ly occ urring s ulphur c ontaining ami no acid. T he ki net ics of ox idation of met hi onine by tetra hexylammonium bro moc hromate (THex ABC) in various pe rce ntage of

acetic acid + N, N-dimethylforma mide mixture (AcOH + DMF) leads to the formation of corres ponding

s ulphoxide. The re action is f irst order eac h in Met, THex ABC and [H+ ] . T he react ion is catal ysed by

hydroge n ions . The react ion rate have bee n de te rmi ne d at di ffe re nt pe rce nt age of AcOH + DMF

mixtures at di f fe re nt te mpe ratures and activat ion paramete rs calculate d. The re act ion does not

i nduce polyme rizat ion of ac ry loni tri le . A s uit able mec ha nis m has bee n propose d. Keywords : Met hi onine, tetrahex ylammonium bro mochro mate, kine tics , ox idation.


Vol. 90, September 2013, pp. 1403-1409

Assessment of ground water pollution using multivariate statistical techniques in and around Municipal Solid Waste dumpsite : A case study from Autonagar, Hyderabad, Andhra Pradesh, India

Izhar Ahmeda*, M. A. Malika , T. V. D. Prasad Raob and M. Satyanarayananc

aDeccan College of Engineering and Technology, Hyderabad-500 007, India

E-mail : [email protected], [email protected]

bDepartment of Chemi stry, Osmania University, Hyderabad-500 007, India


cNational Geophysical Research Institute, Hyderabad-500 007, India


Manuscript received online 27 July 2012, revised 15 November 2012, accepted 26 November 2012

Abstract : Applic ation of dif fe re nt mult ivariate st at istic a l approac hes for the inte rpre tation of data during mo nitoring of groundwater near the MSW dumpsi te in Autonag ar are a, Hyde rabad i s

pre se nte d in this study. A numbe r of physic o-c he mi cal c haracte rist ics of g round wate r sample around

t he dumpsite we re analyze d s o as to asce rtain the exte nt o f g round wate r pol lution by le ac hates f ro m

MSW. Data set thus obtai ned was t re ated using R-Mode Factor Analysis (F A) and P rinc ipal

Compone nt Analys is (P CA) using IBM SP SS20 Statist i cs Sof tware. FA ide ntif ied three factors

res pons ib le for data struct ure ex plaining 65. 4% of total variance and was c ompare d with the B ure a u

of I nd ian Standards for drinki ng wate r. This allowed g rouping of se lecte d para mete r acc ord ing to

common features and leading to the explanation of geoge ni c pol lut ion. Keywords : M unicipal sol id waste (MSW) dumps ite , groundwate r, multi variate analysis , factor analys is .


Vol. 90, September 2013, pp. 1411-1420

Study of adsorption of methylene blue on TiO2 in the aqueous solution

containing salts of magnesium and calcium at high concentration

Yuping Jianga , b and Daiqi Yea*

aCollege of Environmental Science and Engineering, South China University of Technology,

Guangzhou 510006, P. R. China, E-mail : [email protected]

bCollege of Chemistry & Biology, Uni versity of Electronic Science and Technology of China,

Zhongshan Institute, Zhongshan Ci ty 512000, Guangdong Province, P. R. China

Manuscript received online 10 August 2012, revised 05 December 2012, accepted 06 December 2012

Abstract : The ads orption of pol lutants onto anatase TiO2 i s a ke y stage i n the photodeg radatio n

process and shows di ffe re nt effects unde r various c ondit ions. The ads orpt ion of methylene b lue (MB ) onto T iO2 was invest ig ated us ing TiO2 part ic le s uspe nsi ons containing hig h sa lt conce ntrati ons. The

i nte nsi ty of the MB ads orption and ionic ass ociation were dete rmi ne d via tota l organic carbon (TOC)

and molar conduct i vity meas ure me nts, res pectively. UV-Vis spectro metry experi me nts sho wed that t he part ic les we re nanosized anatase TiO2 in t he s uspe nsion. Ads orption inc rease d the quant i ty of the

MB dime r and the MB s us pe ns ion was st able whe n the s al t concentration was equal t o or gre ate r t ha n

0 . 5 M , whic h als o s howe d that t he expe rime ntal re s ul ts we re independe nt of agg reg at ion. Al l of the

adsorpt ion tre nds i ni tial ly inc re ase d to a max imum value; the n, the ads orpt ion sl ig htl y dec re ased for

a fe w minutes before re ac hing e qui l ibrium. Ho we ve r, di ffe re nces ex iste d for the d iffe re nt s al t

conce ntrat ion ra nges. F rom 1–3 M , i nc re as ing the te mpe rature dec re ased the e quil ibri um ti me; beyond 3 M , the adsorpt ion c apabi li ty s lig htly inc rease d; f rom 3–5 M , the adsorpt ion rate decre ase d

m uc h fas te r than in the othe r ranges, and a hinde ring ads orption effect was obse rved in the fol lowi ng

orde r : Mg 2 + > Ca2 + . The mec hanis m is a ls o disc usse d in de tai l . Keywords : MB, TiO 2 , adsorpt ion, sa lt conce nt rati on, UV-Vis spectroscopy.


Vol. 90, September 2013, pp. 1421-1424

Effect of solvent on anodization of Zr-4 in L-ascorbic acid – SEM studies

V. Jeevana Jyothia* and Ch. Anjaneyulub

aDepartment of Chemistry, R.B.V.R.R. Women’s Col lege, Narayanguda, Hyderabad-500 029,

India, E-mail : [email protected]

bDepartment of Chemistry, University College for Women, Osmania University, Hyderabad-

500 007, India

Manuscript received online 08 November 2012, accepted 10 December 2012

Abstract : Anodization of Zirc aloy-4 in 0 .1 M L-ascorb ic acid has bee n carrie d out. K inet ics o f anod ic ox idation of Zirca loy-4 has bee n s tud ied at a constant curre nt de ns i ty of 8 mA.c m– 2 and at roo m

tempe rature. T he plots o f formation voltage vs t ime, rec iproc al c apaci tance vs time and rec iproc al

capaci tance vs format ion vol tage we re dra wn. F ro m thes e plots, formation rate , curre nt e ffic ie nc y

and di ffe re nt ial f ie ld we re c alc ulate d. T he addit ion of s olve nt (ethyle ne g lyc ol ) s howe d bet te r kinet ic

res ult s for 20, 40, 60 and 80% aquo-g lyc ol ic me dia, the d ie lectric constant values are low leading to

t he marke d imp rove me nt in the kinet ics. The s urface mo rphology of the anod ic f ilms was a ls o stud ied by Scanning E lectron Mic rographs (SEM).

Keywords : Anodi zat ion, formation rate , curre nt effic ienc y , dif fe re nti al fie l d, Zi rcal oy-4 , SEM.


Vol. 90, September 2013, pp. 1425-1430

Ultrasonic studies on the molecular interactions of gadolinium soaps in benzene-dimethylformamide mixture

Seema Agrawala* and S. K. Upadhyaya

P.G. Department of Chemistry, S. S. L. Jain College, Vidisha-464 001, Madhya Pradesh, India

aDepartment of Chemi stry, Christian Eminent College, Indore, Madhya Pradesh, India


Manuscript received online 05 October 2012, revised 07 November 2012, accepted 26 December 2012

Abstract : The ul trasonic meas ure me nts of t he so lutions of gadolinium c aprylate and l aurate in a mixture of 50 /50 be nze ne-di methyl formamide (v/ v) have bee n use d to e valuate c rit ic al micel la r

conce ntrat ion, ul t ras onic ve loc i ty and various ac ous tic al pe rame te rs at 303 , 308, 313 and 318 K. The

t rends in ac oust ic al pe ra mete rs indic ates that the re are sig nif icant molec ule r inte rac ti on betwee n

s oap and s ol ve nt molecules . The values of c mc increase wi th the rise i n te mperature and molec ules of

gadol inium s oaps do not agg reg ate appreciably in dil ute s oap s ol uti on below the c mc. Keywords : Ultras ound, c ompressi bil i ty, gadolinium s oaps, cmc.


Vol. 90, September 2013, pp. 1431-1439

Pedogenesis in rice growing hydric soils of Majuli river island, Assam, India

B. P. Bhaskar*, Dipak Sarkar and U. Baruah

Division of Soil Resource Studies, National Bureau of Soil Survey and Land Use Planning,

Amravati Road, Nagpur-440 033, Maharashtra, India

Manuscript received online 06 November 2012, revised 15 December 2012, accepted 26 December 2012

Abstract : The e le mental compos iti on of f our re presentati ve rice gro wing hydric s oil s in wetlands of

Majuli i s lands we re stud ie d in relation to morphology and part ic le si ze by de velopi ng co lour ind ices

and ele me nt to c lay rat io method. T he se textural ly c ontrast and ne utra l to slightl y a lkal ine rice

g ro wi ng s oi ls s howe d stri king dif fe re nce in dis tri but ion of tot al c alc ium and low conte nts with se rious

loss of tota l iro n and manganese in c hannel fi ll s and old f l oodplains due to prolonged s aturat ion. The

c hange of s oi l moisture reg ime in a lluv ial plains, accele rates the le aching and loss of iro n and

mang anese ox ides f rom s urface hori zons and dec rease in c lay by la te ra l move me nt and fe rrol ys is

processes that have favoured formation of iro n-e nri che d s ubs urface horizo ns in paddy so il s . An

ave rage l inkage met hod was e mploye d to wo rkout che mical aff inity and variabi li ty of s oil propert ies

among cluste rs. The c luste r data s howe d that clay and bulk de nsity are leas t vari able whe reas K , Ca,

Fe and M n are highly variable among cluste rs ind icating the use fulness in del ineat i ng bounda ries

ac ross landscapes of f loodplai n wet lands in the rive r i s land . Keywords : Geoc he mistry , Majuli ri ver is land, hydric so ils , e leme nt to c l ay rati o.


Vol. 90, September 2013, pp. 1441-1446

Syntheses of 1,5-benzothiazepines. Part XL : Syntheses and antimicrobial studies of 10-substituted-6a,7-dihydro-6-(4-methoxyphenyl/phenyl)-7-(3-nitrophenyl)-6H-[1]benzopyrano[3,4-c][1,5]benzothiazepines

Seema Pant*, Dharmveer and Deepika Saxena

Department of Chemistry, LBS Government PG College, Kotputli-303 108, Jaipur, Rajasthan,

India, E-mail : [email protected]

Manuscript received 24 May 2011, revised 16 July 2012, accepted 03 October 2012

Abstract : T he re actions of exoc ycl ic αααα , ββββ -unsaturate d ke tones, the be nzyl i de ne flavano ne s, 3- (3-nit robe nzyl ide ne)-4 ′′′′ -methoxyfl avanone and 3-(3-ni trobenzylide ne)flavanone, with 5-s ubstitute d-2-

ami nobe nze nethio ls , the s ubs ti tue nts being haloge no, al kyl and al kox yl, have bee n c arried out in dry

ethanol wit h cata lytic amounts of t ri f luoroacetic acid. The twelve ne w compounds, 10-s ubst ituted-

6a ,7 -dihydro-6-(4- methoxyphe nyl/ phe nyl) -7- (3-ni trophe nyl )-6H-[1 ]be nzopyrano[3 ,4-

c ] [1 ,5 ]benzothiaze pi nes, we re synthesize d and c haracteri zed by mic roest imat i ons for C, H, N and S

and I R, NM R and mass s pectra l stud ies. The s ynt he sized c ompounds we re sc ree ne d for anti mic robi al

acti vi ty ag ainst t he Gram-posit ive bacte ria, Staphylococcus aure us and Gra m-negati ve bacteri a,

Enterobactor cloacae , Pseudomonas aeruginosa and the fung us , Candida alb icans , with re fe re nce

drugs, Vanc omicin, Cefope ra zone/ Sulbactam, Me ropene m and Fluc onazole , res pecti vel y. Most of the

compounds s howe d pro mising bioactiv ity. Keywords : Exoc ycl ic , be nzylide ne flavanone, Staphyl ococcus aureus , Enterobactor cloacae , Pseudomonas

aerugi nosa , Candi da al bi cans.


Vol. 90, September 2013, pp. 1447-1459

Synthesis of both kinetically and thermodynamically controlled diastereomeric pairs of bis-isoxazolidines from dibenzylideneacetone : Their reactivity and biological activity

Bhaswati Bhattacharyyaa, Arijit Kundub, Kaliprasanna Dharac*, Nikhil Guchhaitc , Bijan K. Palc , Sudipta Hazrad, Sukalyani Debnathd , Banasri Hazrad and Amarendra Patrac

aDepartment of Chemi stry, Hooghly Mohsin College, Hooghly-712 101, West Bengal, India

bDepartment of Chemi stry, Darjeeling Government College, Darjeeling-734 101, West Bengal

cDepartment of Chemistry, University College of Science and Technology, University of

Calcutta, Kolkata-700 009, India, E-mail : kal [email protected]

dDepartment of Pharmaceutical Technology, Jadavpur University, Jadavpur, Kolkata-700 032,

India

Manuscript received 19 September 2012, accepted 03 October 2012

Abstract : React ions of C -aryl -N-phe nyl -ni trones with dibe nzyl ide ne acet one yie lde d pai rs of diaste re ome ric bis-i s ox azolidines in g ood to mode rate yie lds. Both t ypes of cyc loadducts possesse d

ide ntical regi o- and stereo-select iv ity. Molec ular model ing studies re vealed s mal l di ffe re nce i n e ne rg y

between the two i somers. Les s stable is ome r was conve rte d to more s table one via parti al

cycloreve rs ion fol lowe d by re-c ycloaddition pathway. Zinc medi ated ac id cata lyze d c ycl ore ve rsio n

was obse rved for more stab le di astere ome r whe re as less stable one y ie lded corres ponding bis-1 ,3-

ami noalcohols in s i milar c ondit ion. Some cyc loadducts were scree ne d for antic ance r and antibacteri al

acti vi ty. Keywords : Nitro ne, dibe nzyl ide ne acetone, bis-i s ox azolidines, diaste re ome ris m, cyc lore versi on, molec ular mode ling , antic ancer, ant ibacteri al .


Vol. 90, September 2013, pp. 1461-1466

Synthesis of 3-[5-(morpholinomethyl/piperidinomethyl/pyrrolidinemethyl)-1,2,4-oxadiazol-3-yl]-4H-chromones

Chunduru Srinivasa Rao, Ch. Venkata Ramana Reddy, C. Jyotsna and Shakil S. Sait*

Department of Chemistry, JNTU, Kukatpally, Hyderabad-500 085, India

Dr. Reddy Laboratories, Bachupally, Hyderabad-500 090, E-mail : [email protected]

Manuscript received online 04 November 2012, revised 05 December 2012, accepted 30 December 2012

Abstract : 5 -(Chl oromethyl) -3-(4H -c hro me n-3-yl) -1 ,2 , 4-oxad iazole (1a-e) re act with pyrroli di ne (6) to

g ive 3-(4H-c hromen-3-y l)-5- (pyrrol idin-1-ylmethyl)-1, 2, 4-oxad iazole (7a-e), (1a-e ) react with

pipe ridine (4) to g ive 1-{[3-(4H- c hrome n-3-yl )-1 ,2 ,4 -oxad iazol -5-yl ]me thyl}p ipe ridi ne (5a-e) and (1 a-

e) re act with morphol ine (2) to g ive 4 -{[3- (4H-c hrome n-3-yl) -1 ,2 ,4 -oxad iazol -5-y l]methyl}morphol ine

(3a-e) . Keywords : Pyrrolidine, pipe rid ine, morphol ine, 5 -(c hloro methyl)-3- (4H-c hro me n-3-yl )-1 ,2 ,4 -oxadi azole .


Vol. 90, September 2013, pp. 1467-1471

Metal elements analysis of fruits using inductively coupled plasma atomic emission spectrometry coupled with microwave digestion

Li Yanga ,c*, Yongtao Liub, Jianwei Zhanga, Yingyi ng Gaoa and Guoxi Xic

aDepartment of Experimental Center, Henan Institute of Science and Technology, Xinxiang

Henan 453003, P. R. China, E-mail : [email protected] Fax : 86-373-3040015

bDepartment of Li fe Science and Technology, Xinxiang Medical University, Xinxiang Henan

453003, P. R. China

cSchool of Environment, Henan Normal University, Xinxiang Henan 453003, P. R. China

Manuscript received online 04 August 2012, revised 25 December 2012, accepted 26 December 2012

Abstract : T he objective of this work was to develop a met hod to de te rmine the metal c onte nt i n f rui t s amples f rom Xinx iang in China. Se ve n samples o f f ruit avail able i n the s upe rma rke t we re analyzed

for the met als Mg, Ca, Fe, Cu, Zn, Al, B, Ni by inductively c oup led p las ma atomic emiss ion

s pectrome try (I CP-AES) coupled wi th micro wave digest ion. The Mg, Ca, Fe, Cu, Zn, Al , B, Ni

conce ntrat ions we re bet ween 1182–3754, 1023–4100, 58.6–146 , 15 .6–32.7, 17.9–92. 9, 26. 7–100 , 34.9–

190 and 6 .9–53.4 mg/ kg, res pect ively. T he me thod was prec ise (with RSD < 4. 24% ) and se nsit ive (LOD

range d betwee n 0 .0075 and 0 .0652 µµµµg/mL).

Keywords : Metal e le me nts, f ruit s ample s, mic ro wave d igestion, ICP-AES.


Vol. 90, September 2013, pp. 1473-1488

Reactions of the allylic substrate at a glance

Tridib Tripathya , Haradhan Kol yaa and B. R. Deb*

aDepartment of Chemi stry, Midnapore College, Midnapore, Paschim Medinipur-721 101,

West Bengal, India

bDepartment of Chemi stry, Vidyasagar University, Midnapore, Paschim Medinipur-721 102,

West Bengal, India, E-mail : [email protected]

Manuscript received 18 October 2012, accepted 02 November 2012

Abstract : The c he mis try of the a l lyl ic compounds ha s pl aye d, an important part in organic c he mis try. Re arrange me nts i n the al ly lic s ubstrate have be e n long kno wn. All yl ic re arrange me nts are ofte n observed in b imolec ular (SN2 ) as we l l as in uni molec ul ar s ubst itution (SN 1 ) process. Many

appare ntly s pontaneous is omeri c rearra nge me nts of a llyl ic compounds are als o kno wn. Bec ause of the

res onance st abil ization of the al lyl c arboc at ion nucleophilic s ubsti tuti on of the al ly lic s ubstrate by SN 1 pathway is e as y to occ ur. It is als o obse rve d that b imolec ular nuc leophil ic s ubst itution (SN2 ) a ls o

occ urs at a fas te r rate than the corres ponding s aturated analogues. SN 1 ′′′′ , SN 2 ′′′′ , SN i ′′′′ mec hanis ms are

als o ope rated only to the a ll yl ic s ubstrate .

Res onance s tab ilizat ion of the a llyl radic al le ads to the subst ituti on at the all yl posit ion v ia

rad ica l pathway a ls o. During add it ion of HX to the double bond of the al lyl ha li des, regi oselective

products are obtaine d, the produc t distribut ion i s c ond ition depe nde nt. [3 ,3 ]- and [2 ,3]-sig matropic

re arra nge me nts are als o found to occ ur.

Because of the versat i le reacti ons of the a llyl ic substra te , it is c hose n to disc uss it s various re actions with possible mec hani stic exp lanat ions in detai l i n the prese nt art ic le .

Keywords : Reac tions, a ll yl ic compounds, mec hanis m.


Vol. 90, September 2013, pp. 1489-1492

Synthesis and characterization of glycine substituted cyclotriphosphazenide

Santosh Kumar Singh and S. P. S. Jadon*

Department of Chemistry, S. V. Col lege, Aligarh-202 001, Uttar Pradesh, India


Manuscript received 07 June 2011, revised 25 September 2012, accepted 10 October 2012

Abstract : G lyc ine s ubst ituted adduct of (P NCl2 )3 was synthesize d and c haracteri zed on the basis of

qual itati ve , quanti tative , TL C, FTI R and mass spectra l analysis . T he c he mic al data assig ned as (P3 N3 )2 H2 (NH2 CH2 COO)8 NHCH2 COO, having NHC H2 COO-bridgi ng bet wee n two (P3 N3 ) rings along

with othe r g lycinic g roup l inked to P atom of P3N3 rings.

Keywords : Phospha ze nides , amino acid, g lycine.


Vol. 90, September 2013, pp. 1493-1496

Synthesis and characterization of meso-substituted triazonoporphyrins

Ranjan K. Bhatt, Dileep Kumar Singh and Mahendra Nath*

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

E-mail : [email protected]. in Fax : 91-11-27666605

Manuscript received 17 October 2011, revised 03 September 2012, accepted 03 October 2012

Abstract : A si mple one-pot three -compone nt synthetic protoc ol for the construction of novel meso -s ubs tit ute d porphyri n- triazone conjug ates has bee n de veloped. T he re action of 5- (4-aminophe nyl)-

10 ,15,20-tri phe nyl porphy rin with formalde hyde and N, N ′′′′ -dis ubstitute d ure a or thiourea de rivatives

i n THF at ref lux te mpe rature afforded the corres ponding ne w tri azo noporphyri ns in mode rate yiel ds.

All the pre pare d products we re c harac te rized by I R, 1 H NMR and mass spectrome try.

Keywords : Synthe sis , t riazonoporphy rins, ure a, thiourea, one -pot react i on.


Vol. 90, September 2013, pp. 1497-1499

DABCO-catalysed one-pot synthesis of furo[3,2-c]coumarin from 3-halochromone

Sourav Maitia , Jaydip Ghosha , Tapas Sarkarb and Chandrakanta Bandyopadhyaya*

aDepartment of Chemi stry, R. K. Mission Vivekananda Centenary College, Rahara, Kolkata-

700 118, India, E-mail : [email protected]

bChemistry Division, CSIR-Indian Institute of Chemical Biology, Jadavpur-700 032, India

Manuscript received 29 February 2012, revised 18 June 2012, accepted 05 October 2012

Abstract : A highly eff ic ie nt s ynthes is of furo[3 ,2-c ] couma rins have bee n ac hieve d by a DABCO-catalyse d react ion of 3 -haloc hro mones wit h 4-hydroxyc ouma rin. DABCO was found to be the most

ef fic ie nt catalys t among the d iff ere nt bases use d for this reacti on.

Keywords : Chromone, 3- haloc hro mo ne, DABCO, furo[3 ,2-c ]couma rin, 1 -be nzopyran.

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