Pakistan Journal of Scientific and Industrial Research

Series A: Physical Sciences

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Dr. Shoukat Parvez
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 Pakistan Journal of Scientific and Industrial Research
Series A: Physical Sciences
Vol. 56, No.1, January-February, 2013

Contents
FTIR - A Didactic Approach for the Study of Humic Acid - Chromium
Chelation During the Environmental Remediation
Zakiuddin Ahmed, Syed Arif Kazmi, Mateen Muhammad Khan, Gulzar Hussain Jhatial
and Nadir Buksh 1

Characteristics Assessment of Cooking Oil and Vanaspati Ghee

Aftab Ahmed Kandhro, Razia Sultana, Rubina Saleem, Ambrat Lal and Arfa Yasmin 6

Density Functional Theory Studies on Electronic Properties of Thiophene S-oxides

as Aromatic Dienophiles for Reactivity Prediction in Diels-Alder Reactions
Semire Banjo 14

Studies on the Composition of Effulent Wastes of Kot Lukh-pat Industrial Estate

(0-400 M), Pakistan
Muhammad Tariq, Tahira Shafiq, Ghulam Rabbani Khan, Muhammad Sajjad and
Muhammad Hammad Khan 19

Forbidden Transitions for Low-Lying Levels in Atomic Boron

Glay Gnday Konan, Betl Karaoban, Gldem rer, Leyla zdemir and Osman A ar 24

Synthesis and Thermopower of Vanadium-Doped Bismuth-Based (Bi-2223)

High-Tc Superconductors
Muhammad Abid 30

Investigation of Flash Cure Process for Finishing Cotton

Iram Abdullah, Syed Qummer Zia Gilani and Aula Khan 34

Effect of Fibre Length on the Physical and Mechanical Properties of Sisal /

Polyethylene Composites
Abdullahi Danladi and Abiodun Suleiman Tunde 42

Comparative Study of D-Slot and Straight Slot in Compact Spinning System

under Mechanical Variables
Nasir Mahmood, Muhammad Qamar Tusief, Ghulam Murtaza, Rashid Kanwar and
Mahmood Ahmed Khan 47
Short Communications

Synthesis and Photochromic Activity of a New Diarylethene Bearing Benzo [b]

Thiophene Unit
Mohammed Kamrul Hossain, Abul Fazal Mohammad Sanaullah and Mohammad
Helal Uddin 54

Alkyd Resin from Ipomoea batatas Lam.

Peter Abimbola Oluyori, Gabriel Ademola Olatunji and Olubunmi Atolani 57
Pak. j. sci. ind. res. Ser. A: phys. sci. 2013 56 (1) 1-5

FTIR - A Didactic Approach for the Study of Humic Acid - Chromium

Chelation During the Environmental Remediation
Zakiuddin Ahmeda*, Syed Arif Kazmib, Mateen Muhammad Khana,
Gulzar Hussain Jhatiala and Nadir Buksha
a
Fuel Research Centre - PCSIR, Off University Road, Karachi-75280, Pakistan
b
Department of Chemistry, University of Karachi, Karachi-75270, Pakistan
(received December 15, 2011; revised April 12, 2012; accepted May 17, 2012)

Abstract. The present study uses infra-red spectroscopy as a didactic approach to characterize the chromium-
humic acid interaction. Shifts of the characteristic carboxylate peaks in the IR spectrum of humic acid
upon its interaction with chromium are noted. These changes have been interpreted to conclude that binding
of chromium to humic acid is through these groups. An analytical grade humic acid was used for this study.
It was also concluded that at the moderate pH i.e 8.5 all the waste chromium ions were cleared from waste
water controlling the water pH.
Keywords: IR study, humic acid, chelation, chromium binding

Introduction stability of ECP-metal complexes followed the order

Humic acids (HA) isolated from coals using an alkaline
solution, are very complexed organic macromolecules
with acid functional groups, primarily carboxylic acids
and phenols as well as carbonyls, amines, aromatic and
aliphatic carbons. Humic acid binds heavy metals due
to its higher content of oxygen-containing functional
groups (Casas and Martin, 1997), which can form stable
complexes with metals as Cu(II), Hg(II), Cd(II), Cr(III)
etc. This binding capacity has been demonstrated in
several studies (Yasser et al., 2011; Dragan and Fitch,
1998). It is found that humic substances can reduce the
concentration of free metals ions in waters (Stackhouse
and Benson, 1989).
In a reported experiment (Holman et al., 2002), the lead
complex band shift for C=O from 1670 cm-1 for the
free ligand to 1537 cm-1 and another similar experiment
(Tharanitharan and Srinivasan, 2009) was designed in
which the FTIR spectrum of free EDTA was compared
with that of lead EDTA identifying the changes in C=O
produced by EDTA-lead complexation. Many more
experiments involving the synthesis and study of the
FTIR spectra of carbonylcontaining organometallic
compounds are now proposed as laboratory experiments.
The binding sites for Cu, Cd, and Pb are strongly related
to the humic substance content of extracellular polymers
(ECP) in activated sludge (Guibaud et al., 2003). The
*Author for correspondence; E-mail: frc_pcsir@hotmail.com
1
Cd > Pb ~ Cu and the metallic ions are bonded to acidic
groups of humic acid (Boyd et al., 1981). In that way,
carboxylate has been identified as the group mainly
responsible for chelation between humic substances
and metallic ions (Holman et al., 2002). This is because
lone-electron pairs on the oxygen atom can produce a
coordinate bond with the empty d-orbitals in heavy
metals. This chelation produces changes in position and
intensity of the characteristic IR absorption bands in
the ranges around 1700 cm-1 and 1600 cm-1.
Complexes between 2,5-dihydroxybenzoate and heavy
metals including Cd(II) using IR and electronic spectroscopy
showed octahedral coordination with the heavy metal bound
to two monodenate carboxylate groups in the trans position
and 4 water molecules (Micera and Erre, 1992). On the
basis of the latter, one hypothesis that can be established is
that carboxyl and carboxylate groups in the humic material
are responsible for Cd complexation, which is evidenced
by displacements of the symmetric and asymmetric stretching
vibration of the COOH and COO-groups.
A better understanding of interaction between metal-
organic ligand is one of the key issues in soil science today.
Advanced analytical techniques, such as atomic
absorption spectrometry alone cannot play proper role
in the study of heavy metal interactions with coal
constituents. Therefore, infrared studies may support
in the understanding and reviewing of interior of
Pak. j. sci. ind. res. Ser. A: phys. sci. 2013 56 (1) 6-13

Characteristics Assessment of Cooking Oil and Vanaspati Ghee

Aftab Ahmed Kandhro*, Razia Sultana, Rubina Saleem, Ambrat Lal and Arfa Yasmin

ACRC- PCSIR Laboratories Complex, Shahrah-e-Dr. Salimuzzaman Siddiqui, Karachi-75280, Pakistan

(received February 27, 2012; revised June 26, 2012; accepted July 4, 2012)

Abstract. Various physico-chemical characteristics of commercial cooking oil and vanaspati ghee of
different brands collected from local market have been analyzed. All the characteristic parameters were
analyzed using AOCS method, while fatty acids composition of samples were determined using gas
chromatography (GC) coupled with flame ionization detector (FID). Physico-chemical characteristics of
all cooking oils seem comparable with each other, however, vanaspati ghee samples showed different
physico-chemical characteristics due to presence of high amount of trans fat. There is direct relation
between physico-chemical characteristics such as moisture and impurities, iodine value, unsaponifiable
matter, saponification value, refractive index, density and colour.
Keywords: physico-chemical parameters, fatty acid composition, GC-FID, cooking oil

Introduction flavour, texture and mouth feel to the food (Shahidi

Vegetables oils are derived from plant sources like
soybeans, palm, corn, melon, groundnut, sheabutter,
cocnut, etc. Some of these vegetable oils are used for
domestic (edible) and industrial purposes (oleo
chemicals) (Hui, 1996).
Many oilseed crops are grown in Pakistan as a source
of vegetable oil. These crops are grouped in two
categories viz. conventional and non-conventional
oilseed crops. Rapeseed-mustard, groundnut and sesame
are conventional crops and are being grown in the
country for a long period. Sunflower, soybean and
safflower are non-conventional crops. There are also
some oilseed crops, which are mainly used for industrial
purposes, such as linseed and castor.
The quality of fats plays very important role in food
processing technology. Oxidation of fat is the main
reason of deterioration in the quality of foods and can
directly affect many quality characteristics such as
flavour, colour, texture, nutritive value, and safety of
the food. The quality and dietary character of the edible
oil have been a topic of concern among food scientists,
nutritionists and consumers (Kandhro et al., 2008a).
Lipids provide a concentrated source of energy and
essential fatty acids through dietary intake. They also
serve as important constituents of cell walls and carrier
of fat-soluble vitamins. In addition, lipids provide
*Author for correspondence; E-mail: chemist_afi@yahoo.com
6
et al., 1997). Vegetable oils, made up of lipids, are very
common commodities in our daily life (Mikuma and
Kaneko, 2010).
A variety of fats and oils are widely available for
consumption in the form of cooking oil, health products
and food ingredients, as well as for the manufacture of
cosmetics, soap and surfactants (Kandhro et al., 2010b).
Chemical composition of fats and oils and their specific
properties have allowed them to be used as foods, fuels
and lubricants. Fats and oils are naturally occurring
substances that consist predominantly of mixtures of
fatty acid esters of glycerol (Pitts and Thomson, 2003;
Coulombe, 2002). Fatty acids (FA) in food and biological
samples are commonly analysed by gas chromatography
(GC) (James and Martin, 1952). Characterization and
determination of various kinds of saturated, mono and
polyunsaturated fatty acids together with their positional
and geometrical isomers have been studied using GC-
FID and GC-MS methods (Kandhro et al., 2010a; 2010b;
Kandhro 2008a; 2008b).
Naturally obtained animal fats and vegetable oils contain
not only the content of triacylglycerols, also containing
several groups of accompanying substances which may
be useful as nutrients, but at the same time they are
either objectionable from the point of view of sensory
value such that they affect the taste, odour, colour,
appearance and functional properties (Cmolk and
Pokorny, 2000).
Pak. j. sci. ind. res. Ser. A: phys. sci. 2013 56 (1) 14-18

Density Functional Theory Studies on Electronic Properties of

Thiophene S-oxides as Aromatic Dienophiles for Reactivity
Prediction in Diels-Alder Reactions
Semire Banjo
Department of Pure and Applied Chemistry, Ladoke Akintola University of Technology, Ogbomoso, Nigeria

(received May 30, 2011; revised November 30, 2011; accepted December 27, 2011)

Abstract. The reactivity of thiophene S-oxides was discussed with special emphasis on the use of thiophene
S-oxides as dienophiles in Diels-Alder type reactions. The w values obtained for thiophene S-oxide (TO)
with electron-donating group (-CH3) increased the nucleophilicity power whereas substitution with electron-
withdrawing groups (such as -NO2 and -CO2CH2CH3) increased the electrophilicity power, indicating an
increase of reactivity towards a nucleophiles. The higher the value of Dw the more favourable the D-A
process, therefore apart from (4+2) addition reactions of these TO as diene with the typical dienophiles
like 1,2-dicyanoethene and 1,2-dicyanoethne, it could be possible for TO with strong electron withdrawing
substituents to serve as dienophile, e.g. heterocycles 1e and 1f. Also, from the value of Dw heterocycle
1d could involve in (4+2) addition reactions with heterocycles 1e and 1f.
Keywords: thiophene S-oxide, reactivity, global properties, density functional theory

Introduction butable to a slight but continued deoxygenation of the

Thiophene S-oxide have remained an elusive species
until fairly recent times; although thiophene S,
S-dioxides are well-known compounds. They are
viewed as building blocks with the proviso that they
could be synthesized from thiophenes directly and
would prove suitable cyclic dienes for cycloaddition
reactions that would lead to multi-functionalized
arenas (Thiemann et al., 2009). Furthermore, thiophene
S-oxides have been found to exhibit a wealth of
interesting reactivity (Fujii et al., 2002; Furukawa
et al., 1998; 1997; Pouzet, 1997; 1995), as good dienes
in Diels-Alder type reactions and add stereoselec-
tively to a row of dienophiles (Thiemann et al., 2003;
2000a; Ho et al., 1998), however, this depends on the
substituents on the frame of the thiophene-S-oxide
and also on the nature of the dienophile present in these
reactions (Fujii et al., 2002).
In solution and upon exposure to light, e.g. daylight,
thiophene-S-oxides enjoy a much shorter lifetime and
appreciable amount of thiophenes can be isolated from
the ensuing mixtures (Ohira et al., 2005). Thiophene-
S-oxides have been found to be active against a number
of cancer cell strains. Whether this activity is attri-
E-mail: semireban@yahoo.com
14
compounds is still under study (Fujii et al., 2002). The
use of aromatic compounds as dienes has been widely
studied in D-A reactions (Thiemann et al., 2003; 2000a;
2000b; Lautens and Fillion, 1996; Paquette et al., 1982),
however, their use as dienophiles is a new and interesting
branch that allows to state large and versatile synthetic
sequences.
Moreover, nowadays, computational chemistry methods
offer a unique ability for organic chemists to generate
optimal geometry structures, the structural and electronic
properties of reactants and products make decisions
as to which of the chemical trans-formations will
occur in reactions. From the theoretical point, the
differences in the stability of heterocycles are explained
in terms of aromaticity and delocalization of electron
densities on p molecular orbitals. For the stable
compounds, a high p molecular orbital delocalization
established between two aromatic rings, which may
not be presented in the less stable isomers. It is evident
that the aromaticity correlates with the thermodynamic
stability of a system, and also is relationship between
hardness and stability. Bird (1997), Chamizo et al.
(1993) Zhou and Navangul (1990) and Parr and
Pearson (1983) had reported the principle of maximum
Pak. j. sci. ind. res. Ser. A: phys. sci. 2013 56 (1) 19-23

Studies on the Composition of Effluent Wastes of Kot Lukh-pat

Industrial Estate (0-400 M), Pakistan
Muhammad Tariqa, Tahira Shafiqa, Ghulam Rabbani Khanb, Muhammad Sajjadb and
Muhammad Hammad Khana*
a
Center for Environmental Protection Studies (CEPS), PCSIR Laboratories Complex, Lahore-54600, Pakistan
b
Department of Chemistry, Division of Science and Technology, University of Education, Township Campus
Lahore, Pakistan

(received October 2, 2010; revised June 7, 2011; accepted June 9, 2011)

Abstract. The quality of wastewater effluents in the Kot Lukh-pat Industrial Estate main drain, stretched
from 0 to 1.1 km ahead was studied. Samples were collected during June and September, 2008 along first
400 m and quality parameters like pH, conductance, TSS, TDS, COD, BOD, chlorides and sulphides were
determined. In most of the samples COD, BOD and S2- remained above the recommended limits of National
Environmental Quality Standards (NEQS) of Pakistan, while chlorides and TSS were found to be below
the limits. The effect of temperature and pH on the quality of wastewater was noted in most of the samples
because, it affects the solubility of oxygen, volatile compounds and growth of microbes. The decrease in
oxygen content caused by high temperature can shift the microbial community from aerobic to anaerobic
and also causes life threatening conditions for the aquatic life in the water body that receives the wastewater.
Increase in pH causes the increased efficiency of microbes which consume the organic compounds in
wastewater. This study pointed out the alarming condition of the wastewater.
Keywords: wastewater, environmental management, Kot Lakh-pat Industrial drain, COD, BOD

Introduction 1997; Ghafoor et al., 1994). Industrial water pollutants

Municipal wastewater is a combination of domestic
wastewater, small amount of industrial and agro-zoo-
technical wastewater, storm water, drain water, surface
infiltration, and ground water (Ausubel, 1999). When
this drain of a municipal wastewater enters an industrial
area, a number of pollutants are expected to be added
in it, most of them are toxic in nature. However, city
authorities should know the characteristics of the
wastewater, the ability of sewage system to handle
them, and the effects of the wastewater upon all
components of the city disposal system before receiving
the wastewater into drain.
Industrial discharge is one of the major sources of water
pollution. Each industry has certain pollutants in its
wastewater. The physico-chemical properties of a
wastewater can be divided into the following categories;
diseases causing agents, oxygen consuming agents,
plant nutrients, suspended solids and sediments,
dissolved solids, toxic substances, thermal pollution,
oil, grease and acids (Girard, 2007; Kahloon et al.,
2003; Kaul and Ashutosh, 2002; Hassan and Bhutta,
*Author for correspondence; E-mail: jawad_frc@hotmail.com
19
such as organic and inorganic compounds, metals and
dissolved solids can have serious impacts on environ-
mental quality, depending upon their characteristics and
concentration (Qadir et al., 2010; Miller et al., 2009;
Sultan, 1995; Trivedi and Gurdeep, 1992). The textile
industry is not only one of the biggest water consumers,
but also a great user of chemical products (Soares et
al., 2007).
The toxic water pollutant can enter the food chain
through crop irrigation and the contamination of aquatic
life (Berlin and Briggs, 2005; Boyd et al., 2003). These
pollutants cause wastewater borne diseases due to lack
of adequate finances for wastewater treatment. The
nutrients in the wastewater along with soluble salts and
heavy metals ultimately reach into water bodies e.g.,
lakes, river stream, and ultimately ocean. These are
consumed by the organisms like algae, causing an
excessive growth e.g., red-tide. When these algae die
and decay, they quickly deplete the dissolved oxygen
in the water body causing life threatening condition for
the aquatic life (Ausubel, 1999; Benka-Coker and Ojior,
1995). Appearance and odour are direct indicators of
wastewater pollution. Wastewater may be coloured or
Pak. j. sci. ind. res. Ser. A: phys. sci. 2013 56 (1) 24-29

Forbidden Transitions for Low-Lying Levels in Atomic Boron

Glay Gnday Konana, Betl Karaoban a, Gldem rer a, Leyla zdemir a* and Osman A ar b
a
Department of Physics, Sakarya University, Sakarya, Turkey
bDepartment of Physics, Karamanoglu Mehmetbey University, Karaman, Turkey

(received October 18, 2011; revised April 30, 2012; accepted May 2, 2012)

Abstract. The multiconfiguration Hartree-Fock in the framework of the Breit-Pauli Hamiltonian (MCHF+BP),
relativistic Hartree-Fock (HFR), and multiconfiguration Dirac-Fock (MCDF) calculations of the wavelengths,
oscillator strengths, and transition probabilities for the magnetic dipole (M1) and electric quadrupole (E2)
forbidden transitions between low-lying levels in the atomic boron have been performed. The data for the
analysis of forbidden lines in the spectrum is important for the study of the plasma in astrophysical objects
and fusion devices. The data for forbidden transitions obtained from this study have been compared with
experimental and other theoretical data available in the literature. Moreover, a discussion of these calculations
for the boron atom (B I) has been given in view of the MCHF+BP, HFR and MCDF methods.
Keywords: boron, forbidden transitions, transition probabilities, oscillator strengths

Introduction using an extended version of MCHF method which

The data of electric quadrupole (E2) and magnetic
dipole (M1) transitions among the levels of the ground
configuration can be used for diagnostics of thermo-
nuclear plasmas or for the estimation of the radiative
losses in plasmas (Karwowski and Martin, 1991). The
boron atom (B I) is an ideal system to be studied. The
ground electronic configuration is 1s22s22p with three
electrons outside a compact k-shell core. The small
numbers of electrons make theoretical calculations
simple for the accuracy of results. Astrophysical scientists
have focused their attention on identifying the B I lines
in the sun spectrum and the solar abundance of B I. As
we know, accurate solar abundance determination is
based on precise values of transition probabilities (rates)
and oscillator strengths. There are many theoretical
methods developed to obtain the energy levels and
transition probabilities of atoms and ions. Among all
the methods, MCHF method or MCHF combined with
Breit-Pauli approximation are the ones that are most
widely used in calculating energy levels and transition
probabilities of atomic boron.
Analysis of boron spectrum was greatly extended by
many other studies (these data can be found from NIST
website). The electric dipole (E1) and quadrupole (E2),
and magnetic dipole(M1) transition parameters for
first-row atoms and their isoelectronic ions using
multiconfiguration Dirac-Fock programme of Desclaux
were performed (Cheng et al., 1979). E2 and M1
transition probabilities for boron were calculated by
*Author for correspondence; E-mail: lozdemir@sakarya.edu.tr
includes relativistic effects in the Breit-Pauli approxi-
mation (Fischer, 1983). Other interesting comparative
data have been published as a part of the IRON project.
Galavis et al. (1998) studied the radiative rates for
transitions within n=2 complex in several ions of boron
isoelectronic sequence (6 < Z < 28). The forbidden
emission coefficients for intraconfiguration transitions
2p3/22p1/2 along the boron sequence using the rela-
tivistic quantum defect orbital (RQDO) method were
reported by Charro et al. (2001). Verhey et al. (1987)
performed relativistic calculations of the M1 transition
between the 2P3, 2 levels of the ground-state boron
isoelectronic sequence using the multiconfigurational
Dirac-Fock extended average level (MCDF-EAL)
method. Mina et al. (1981) calculated relativistic of E1
and M1 transitions between the J = 1/2 and 3/2 levels
of the ground state in the boron isoelectronic sequence.
Energy levels, lifetimes, and transition probabilities
for transitions between computed levels were reported
for the Be-like (Z = 4-12) to Ne-like (Z = 10-24)
sequences (Fischer and Tachiev, 2004). In their work,
several forbidden transitions (M1, E2, and M2) were
also presented in addition to allowed (E1) transitions.
Moreover, in our earlier work we presented an investi-
gation including the level energies and electric dipole
transitions for neutral boron (Karaoban et al., 2011).
In this work, transition parameters have been presented
such as wavelengths, oscillator strengths, and transition
probabilities (or rates) for magnetic dipole (M1) and
electric quadrupole (E2) transitions of low-lying levels

24
Pak. j. sci. ind. res. Ser. A: phys. sci. 2013 56 (1) 30-33

Synthesis and Thermopower of Vanadium-Doped Bismuth-Based

(Bi-2223) High-Tc Superconductors
Muhammad Abid
a
Department of Physics, Quaid-i-Azam University, Islamabad, Pakistan

(received June 6, 2011; revised August 15, 2012; accepted September 5, 2012)

Abstract. A superconducting sample with nominal composition of Bi1.3Pb0.4V0.3Sr2Ca2Cu3Od prepared by

using solid-state reaction method. DC electrical resistivity of the sample determined by using a standard
four-probe technique within a temperature range of 77-300 K. Zero electrical resistivity of the sample was
found at a critical temperature (Tc,zero) of 108 1 K. Whereas, the onset temperature (Tc,onset) was observed
at 122 1 K. Temperature dependent thermoelectric power (Seebeck coefficient) of the superconducting
sample was measured with a newly developed and calibrated apparatus.

Keywords: Bi1.3Pb0.4V0.3Sr2Ca2Cu3Od superconductors, vanadium doping, thermoelectric power, electrical

resistivity

Introduction properties. The presence of high valence cations V5+,

The Bismuth Strontium Calcium Copper Oxide
(BSCCO) ceramic system is known to have large
number of existing or co-existing crystal structures or
phases. Among the cuprate high-T c materials, the
Bi(Pb)-Sr-Cu-O are considered to be the most
promising candidates for various reasons, in particular
for their rather high critical temperature Tc, high critical
current density Jc and power transmission in electric
cables at liquid nitrogen temperatures. A large amount
of work has been done on this system in order to make
technical applications possible (Kaiser, 1997; Awana
et al., 1992). It is known that the Bi-(2223) phase is
stable within a narrow temperature range and exhibits
phase-equilibrium with only a few of the compounds
existing in this system (Larbalestier et al., 2001). Two
major issues seemed to make the development of the
Bi-(2223) phase complicated are its stabilization in a
very narrow temperature range and that the kinetics
of its formation are so slow that it is almost impossible
to obtain the pure Bi-(2223) phase material (Zhang
et al., 1990). The doping materials like Al, La, Sb, Pb
have been attempted by different authors in Bi-based
superconductors (Sugai and Soto, 1989). Substitution
may play an important role on the properties of high
temperature superconducting materials. The existence
of doping element in substitution lattice sites lead to
the formation of a superconductor with altered
E-mail: m.abid@ciitsahiwal.edu.pk
30
Nb5+ and Ta5+ in the stoichiometry can sufficiently
enhance the formation of high-Tc Bi-(2223) phase
(Kazin et al., 1990). In this work, the effect of
Vanadium doping on thermoelectric power and
resistivity of Bi 1.3 Pb 0.4 V 0.3 Sr 2 Ca 2 Cu 3 O d super-
conducting sample are presented as a function of
temperature in a range of 77 to 300 K.
Materials and Methods
Sample preparation. The specimen was prepared from
99.9 % pure powders of Bi2O3, V2O5, PbO, SrCO3,
CaCO 3 and CuO. The powders were mixed and
thoroughly grinded in an agate mortar to give a
homogeneous composition of Bi1.3Pb0.4V0.3Sr2Ca2Cu3Od.
The grind powder was calcined for 24 h in open air at
800 C (by using a tube furnace, open at its both ends
to the atmosphere for better oxidation process of the
sample powder). The prepared pellet was given a
controlled heating and cooling in air by using a horizontal
tube furnace. Poly vinyl alcohol (PVA) was used as
binder in the sample. PVA is one of the few high
molecular weight commercial polymers, which is water-
soluble and is dry solid, commercially available in
granular and powdered form. The properties of poly
vinyl alcohol vary according to the molecular weight
of the parent poly vinyl acetate and the degree of
hydrolysis. Fully hydrolyzed form with medium viscosity
grade PVA was used in our case. Sample was in the
shape of cylindrical disks having diameter of 25 mm
Pak. j. sci. ind. res. Ser. A: phys. sci. 2013 56 (1) 34-41

Investigation of Flash Cure Process for Finishing Cotton

Iram Abdullah *, Syed Qummer Zia Gilani and Aula Khan
ab b c

a
University of Leeds, Leeds, UK
b
Department of Textile Chemistry, National Textile University, Faisalabad-37610, Pakistan
c
Masood Textile Mills Limited, Sheikupura Road, Faisalabad, Pakistan

(received May 24, 2011; revised February 28, 2012; accepted March 7, 2012)

Abstract. Easy-care performance is imparted to cotton fabric by the formation of crosslinks between the
adjacent cellulose chains. The most widely accepted crosslinking method is treatment with N-methylol
resins using sequential pad-dry-cure technique. Flash cure technique is also used to complete the crosslinking
by single stage dry/cure cycle. As a result better tear and tensile properties are attained without the
undesirable effect on crease recovery property. Such a curing system can be used for energy conservation
or to reduce energy consumption in resin finishing of cotton fabrics.
Keywords: crosslinking, N-methylol, flash curing, easy-care properties

Introduction pad-dry-cured fabrics (Wright, 1981). Since then

Pad-dry-cure is the conventional procedure for imparting
durable crease recovery properties to the cotton fabrics.
The industrial pad-dry-cure procedure consists of
impregnating the fabric with the aqueous solution of
the crosslinking agents along with a suitable catalyst
system, pre-drying, drying and then a subsequent curing
step either on a stenter frame or drying on rollers and
then curing in a stenter frame or on a semi-contact
curing oven, after washing in one or more open width
wash boxes. Finally, drying is done on drying rollers.
High energy consumption occur during drying and
curing operations and more energy is required for heavy
weight fabrics. The common approach in textile industry
to conserve energy is to complete drying and curing
stage in a stenter frame. The afterwash, in many cases,
is also omitted to save energy.
In 1980s the low wet pick-up techniques such as lick
roller (Rowland et al., 1983a), transfer pad-cure
(Varghese and Doshi, 1982) and foaming techniques
(Gonzales and Reinhardt, 1986; Rowland et al., 1983b;
Namboodri and Duke, 1979) were investigated to
reduce the energy consumption in drying. The results
were comparable to conventional pad-dry-cure system.
However, commercially 35% wet pick-up was required
to eliminate the pre-drying step. Furthermore, more
than 20% reduction in resin add-on produced fabrics
with lower durable press properties compared with
*Author for correspondence; E-mail: i_tayyab@hotmail.com
34
industry has made significant advances in developing
special finishing effects such as water repellency
(Wadsworth and Wey, 1988), water proofing
(Mukhopadhyay and Midha, 2008), fire retardency
(Wadsworth and Wey, 1988) and garment finishing
(Lambert and Harper, 1990) via foam application of
finishing chemicals. The ultraviolet radiation was also
investigated to cure fabrics. The radiation times were
too long for commercial use and sophisticated safety
equipment was required for workers for eye protection
(Ferrero et al., 2008; Millington, 1998; Reinhardt and
Harris, 1980).
Performing drying and curing in a single stage can
conserve significant amount of energy, though very
little information is available on single stage curing
procedure. Pensa and Sello (1982) cured cotton fabric
at 160 C/30 sec and indicated that high concentration
of an active catalyst system is required to resin finish
light to medium fabrics. The low wet pick-up technique
was combined with a highly active catalyst system to
perform the single stage curing of heavy drill fabrics
at 170/min (Varghese and Doshi, 1982).
The present work aims at finishing cotton fabric with
most widely used N-methylol crosslinking agents using
flash cure: a single stage curing procedure and conven-
tional pad-dry-cure procedure. In this study flash/single
stage curing technique has been compared with
conventional pad-dry-cure technique. The treatment
parameters of concentration of resin and catalyst, wet
Pak. j. sci. ind. res. Ser. A: phys. sci. 2013 56 (1) 42-46

Effect of Fibre Length on the Physical and Mechanical Properties

of Sisal / Polyethylene Composites
Abdullahi Danladi* and Abiodun Suleiman Tunde
Department of Textile Science and Technology, Ahmadu Bello University, Zaria, Nigeria

(received April 4, 2011; revised November 30, 2011; accepted December 30, 2011)

Abstract. Composites of sisal fibres with polyethylene polymer chips were prepared at 50% fibre weight
with varying lengths of the sisal fibres and the physical and mechanical properties of the composites were
determined. The results of the physical properties show that moisture uptake of the composites initially
increases from 0 to 60% as the fibre length increased from 0 to 5 mm and there after remained about the
same. Density was observed to decrease initially at 5 mm and then steadily increased. The hardness and
thickness was increased with increase in fibre length. Youngs modulus, breaking load and breaking
extension increased as the length of fibres in composite increased from 10 mm length, while work of
rupture increased with increase in fibre length from about 5 mm.
Keywords: composites, sisal fibre, fibre length, physical properties, mechanical properties.

Introduction manila (obtained from the abaca plant, Musa taxtilis)

The interest in ligno cellulosic fibres has increased
dramatically in the past few years and these fibres are
now in great demand because of their attractive
properties. They have become the focus of attention
to scientists worldwide as they exhibit a combination
of high strength with low specific gravity. Plant fibre
reinforced composites prove that it is possible to
construct high-performance materials with environment
friendly resources. Research reported by Rowell (1998)
reflects that composite materials have shown
outstanding durability, corrosion resistance, lower
maintenance and replacement cost, low investment in
fabrication equipment, high strength to weight ratio,
light weight and exceptional high formability, even at
continuous high operating temperature up to 200 C.
Composite materials have gained popularity in high
performance products such as aerospace components
(wings, tails, fuselages, and propeller), boat and scull
hulls, bicycle frames and race car bodies. More uses
include fishing rods and storage tanks.
Danladi (2008) reported that sisal fibre is obtained from
the leaves of the plant called Sisalana (Agave sisalana),
which originated from Mexico and is cultivated in East
Africa, Brazil, Haiti, India, Indonesia and can also be
found dispersed in Nigeria. It is grouped into the broad
heading of hard fibres among which sisal is second to
*Author for correspondence; E-mail: adanladi08@gmail.com
in durability and strength. It is one of the most
extensively cultivated plants for fibres, easily cultivated
in all kind of environments. The diameter of the fibre
varies from 100 to 300 . Sisal fibre is extracted from
the leaf either by scraping or retting, followed by
scraping or by mechanical means i.e. decorticators.
Hawe et al. (1984) have reported the use of polyethylene
for composites applications. Kumar and Sabu (1994)
studied the effect of fibre length on the properties of
short fibre composites and have argued that if the fibres
are longer than the critical length, the strength in the
composite will depend on the stressibility of the matrix
or fibres. Since composite properties are affected by
fibre length among other factor, this work is intended
to study the effect of fibre length on the physical and
mechanical properties of sisal / polyethylene composites.
Materials and Methods
Fibre extraction. The leaves from the sisal plant were
crushed between pair of anvil rollers under pressure to
remove the water and other liquid contents from its
leaves. The remains of the crushed leaves were scraped
gently with blunt knife to remove the remaining fleshy
pulp. The fibres left behind were washed several times
with water until a clean state was achieved, then treated
in a mild solution of 0.5% caustic soda solution at a
temperature of 40 C and finally dried. With the help
of a ruler and clamp, the fibres were straightened without

42
Pak. j. sci. ind. res. Ser. A: phys. sci. 2013 56 (1) 47-53

Comparative Study of D-Slot and Straight Slot in Compact

Spinning System under Mechanical Variables
Nasir Mahmooda*, Muhammad Qamar Tusief a, Ghulam Murtazaa, Rashid Kanwarb
and Mahmood Ahmed Khanc
a
Department of Fibre & Textile Technology, Universiy of Agriculture Faisalabad, Faisalabad, Pakistan
bDepartment of Physics, University of Agriculture Faisalabad, Faisalabad, Pakistan
c
Department of Math and Statistics, University of Agriculture Faisalabad, Faisalabad, Pakistan

(received October 31, 2011; revised September 5, 2012; accepted September 12, 2012)

Abstract. The present research study was planned, to appraise the quality and properties of the compact
yarn as influenced by hank roving, type of suction slots, spindle speed and spacer size. The basic properties
of the compact yarn such as strength, elongation, unevenness and hairiness were analyzed as a function
of compact spinning to control those protruding fibres which become the part of the yarn but have no role
in the yarn formation and ultimately no contribution to yarn strength.
Keywords: suction straight and D slots, spindle speed, hank roving, spacers

Introduction
Although the first industrial compact spinning frame
was launched at ITMA (International Textile Market
Association) in 1995, yet investigations on compact
yarns were carried out since 1993. It is generally known
that the compact spinning method is certainly an
excellent substitute for conventional yarn spinning,
since it minimizes the hairiness of single yarns. This
can reduce the twisting angle and develop yarn quality.
The properties of compact yarn are better than con-
ventional ring spun yarn. Compact spinning gives the
potential to generate a near-perfect yarn structure by
applying air suction to compact the fibre stream in the
main drafting zone, thereby virtually reducing the
spinning triangle. There are many new schemes offered
to deal with the present yarn quality/production speed
difficulty on traditional ring systems and compact yarn
spinning is one of these schemes. Although this system
uses the main components of a traditional ring spinning
system, it is also considered to be a new spinning system
by some researchers (Tyagi and Kumar, 2009). The
compact spinning systems are mostly used for spinning
of combed yarn, however, many attempts have been
made to use the compact system for spinning carded
yarns. Recently, D-type slot compact system has been
introduced for producing carded compact yarn. D-slot
has more slot length than straight slot. In straight slot
compacting system, the compactness is achieved by
fibre transport through the perforated lattice and air
drawn through inclined slots in compact spinning system.
*Author for correspondence
E-mail: nasirmahmood23uaf@yahoo.com
47
D-slot has delta shape at the entry point which helps
the shorter fibres to compact in a better manner, resulting
in better utilization of short fibres. In compact spinning,
tension differences between fibres during the twist
insertion are smaller than those in ring spinning due to
the elimination of the spinning triangle (Loganathan
et al., 2009).
The pressure between the aprons in the drafting zone
is controlled by spinning spacer; in turn it governs the
degree of control exercised on the floating fibres and
as such would have influence over the drafting irre-
gularities. It is often necessary to use a wider spacer
for a coarser count however, if there are un drafted
places in the yarn when it leaves the front rollers, the
break draft should be increased. Spacer should be
increased only if the draft results remain unsatisfactory
after the break draft has been increased (Kumar et al.,
2006). The drafting quality at the compact frames is
governed by apron spacing and twist in the input roving.
The yarn quality is also affected by the input hank
roving. Control over the fibres in top arm drafting is
critically influenced by the apron spacing. Reduction
of apron spacing improves the control over the fibres,
but settings below a certain level lead to frequent drafting
faults and therefore to more irregular yarn. Apron
spacing influence upon the yarn imperfection, count
upon yarn evenness. Optimum apron spacing is depen-
dent upon top-roller loading and lies at a lower level at
higher load. Apron spacing has also a significant effect
on the nep count in the yarn, closer spacing leading to
less neps.
Pak. j. sci. ind. res. Ser. A: phys. sci. 2013 56 (1) 54-56

Short Communication
Synthesis and Photochromic Activity of a New Diarylethene
Bearing Benzo[b]Thiophene Unit
Mohammed Kamrul Hossain*, Abul Fazal Mohammad Sanaullah
and Mohammad Helal Uddin
Department of Chemistry, University of Chittagong, Chittagong - 4331, Bangladesh

(received May 5, 2011; revised July 15, 2011; accepted September 26, 2011)

Abstract. The synthesis of new photochromic compound 3-[2-(3,5-bis methoxymethoxymethylthiophene-

2-yl)-3,3,4,4,5,5-hexafluorocyclopent-1-enyl]-2-methyl-benzo[b]thiophene is reported. In multistep synthesis
from 2,4-dibromothiophene, benzo[b]thiophene was synthesized. This product exhibited photochromic
properties upon irradiation with ultraviolet and visible light.
Keywords: photochromism, photomemory, photocyclization, coupling reaction

Photochromism is the term used for a reversible photo
induced transformation of a molecule between two
isomers whose absorption spectra are distinguishably
different (Drr and Bouas-Laurent, 1990). The chemical
bond reconstruction via photo excitation induces not
only the change of absorption spectra but also refractive
indices, fluorescence spectra, oxidation/reduction
potentials, chiral properties and so on (Irie and Uchida,
1998). The quick change of these properties induced
by the photoexcitation has been attracting much atten-
tion (Hossain et al., 2005a; 2005b; de Jong et al., 2003;
Myles and Branda, 2002; Delaire and Nakatani, 2000;
Matsuda and Irie, 2000; Hanazawa et al., 1992) from
the view points of the application to optoelectronic
devices such as memories and switches.
In this study novel photochromic compound 3-[2-(3,5-
bis-methoxy-methoxymethylthiophene-2-yl)-3,3,4,
4,5,5-hexafluoro-cyclopent-1-enyl]-2-methylbenzo[b]
thiophene (9) has been designed and synthesized. It
shows unique photochromic behaviours upon irradiation
with UV light.
Absorption spectra were measured with an absorption
spectrophotometer (Hitachi, U-3310). 1H-NMR spectra
were recorded on a FT-NMR, JEOL-AL300, spectro-
meter at 270 MHz. All chemical shifts are given in ppm
relative. IR spectra were recorded with a FT-IR, 2000,
Perkin-Elmer spectrometer. Mass spectra were taken
on JEOL JMS-GCMATE II (EI, 70 ev). Photo irradiation
was carried out by using a 500 W super high pressure
mercury lamp and monochromic light was obtained by
*Author for correspondence; E-mail: mkhossain73@yahoo.com
passing it through a monochromator (JOBIN YVON).
The samples were not degassed.
The newly synthesized compound 3-[2-(3,5-bis-
methoxymethoxymethylthiophene-2-yl)-3,3,4,4,5,5-
hexafluorocyclopent-1-enyl]-2-methyl benzo[b]
thiophene (9) is shown in (Scheme 1). Compound (9)
was prepared in five steps from the commercially
available 2, 4-dibromothiophene (1). Compound (2)
and (3) have been synthesized according to the known
procedure (Mitsumori et al., 1995).
2, 4-Diformylthiophene (2). To a solution of 1.45 g of
2,4-dibromo thiophene (1) (6.06 mmol) in 300 mL of
ether was added dropwise 25.2 mL of a solution of tert-
butyllithium in hexane (1.7 M) at -78 C. The mixture
was stirred for 10 min and then 4.7 mL of N,N-dimethyl
formamide was added. After stirring for 1 h, dry/acetone
bath was removed and the reaction mixture was allowed
to warm gradually to room temperature. A yellow oil
obtained by usual work-up was purified by silica gel
column chromatography (n hexane:ethyl acetate = 3:1)
to afford 0.69 g of white solid of 2,4-diformylthiophene
2 (81% yield). m.p 79-80 C. IR (KBr): 1688, 1658 cm-1.
1
H-NMR (270 MHz, CDCl3) 9.98 (d, 1H), 9.95(s, 1H),
8.45 (dd, 1H), 8.17 (d, 1H) Anal calcd for C6H4O2S: C;
51.42; H; 2.88; S; 22.88, Found: C, 51.66, H, 3.17, S,
22.94.
2,4-dihydroxymethylthiophene (3). A mixture of
0.68 g of 2,4-diformylthiophene (2) (4.73 mmol) in
15 mL of EtOH was added to 0.4 g of NaBH 4
(11.7 mmol) in an ice bath. After stirring for 3 h, ice
bath was removed and the reaction mixture was allowed

54
Pak. j. sci. ind. res. Ser. A: phys. sci. 2013 56 (1) 57-58

Short Communication
Alkyd Resin from Ipomoea batatas Lam.
Peter Abimbola Oluyoria*, Gabriel Ademola Olatunjia and Olubunmi Atolanib
a
Department of Chemistry, University of Ilorin, PMB 1515, Ilorin, Nigeria
b Department of Chemical Sciences, Redeemers University, PMB 3005, Redemption City,
Mowe, Ogun State, Nigeria

(received March 21, 2012; revised May 9, 2012; accepted May 16, 2012)

Abstract. A new alkyd resin has been isolated from the hexane extract of powdered sweet potato (Ipomoea
batatas Lam.) peels. The proposed structure of the compound was established to be Poly 3-(2,4-
dihydroxyphenyl) butanoate by means of data obtained from the FTIR, 1H-NMR and 13C-NMR spectra.
Keywords: Ipomoea batatas, Poly 3-(2,4-dihydroxyphenyl) butanoate, alkyd resin, renewable resin

Sweet potato (Ipomoea batatas Lam.) is a member of
the Convolvulaceae family which originated from south
Mexico and Central America. It is considered to be the
seventh most important crop worldwide (Woolfe, 1992).
It is a cheap and readily available staple food in Nigeria,
with promising nutritional attributes rich in vitamin B6,
vitamin C, manganese, copper, potassium and iron
(Antia et al., 2006). The colour of the flesh of the root
vegetable ranges from white to yellow, orange, red or
purple depending on the variety (Wood and Young,
1974). Leaves are rich in protein, minerals and vitamins
(Ishida et al., 2000).
Antioxidant activity of sweet potato peel is due to the
presence of phenolic acids (Oyeneho and Hettiardichy,
1993). Furthermore, sweet potato peel extracts possess
great antioxidant potency (Rajini and Nandita, 2004)
and have been ultilised as natural antioxidants in
soybean oil and can be used safely instead of synthetic
antioxidants (Zia-ur-Rahman et al., 2004). Potato peel
also has some medicinal applications as studied by
Majorie (2000); Subrahmanyam (1996) and Aakanksha
and Keswani (1985). Although Oyeneho and Hettiarachchy
(1993) had found some polyphenolic compounds in
potato peels, no such work has been reported on sweet
potato peels in our environment.
Fatty acids with potential for conversion to alkyd resins
have been obtained from various plants as reported by
Emelugo et al. (2011); Ogunniyi and Odetoye (2008);
Banerjee (2005) and Akintayo (2004). Alkyd resin plays
an important role in the paint, coating and surfactant
industries. Soya bean oil is used as a source of alkyd
resin with good success (Kharkate et al., 2005) and
more renewable sources need to be sorted. Since there
*Author for correspondence; E-mail: oluyoripeter@yahoo.com
is constant demand for biodegradable polymeric resin
for both food and non-food products, presence of an
alkyd resin from Ipomoea batatas has been investigated.
The aim of this work therefore, was to isolate and
determine the chemical constituents of sweet potato
peels to promote its new uses.
Twenty tubers of white skinned variety of sweet potato
(I. batatas Lam.) were obtained from a local market in
Ilorin, Nigeria and identified by a taxonomist at the
herbarium of Biological Department of the University
of Ilorin, Ilorin, Nigeria. The peels were carefully
removed, air-dried at room temperature and stored in
a cool dark place until further analysis. The peels
unavoidably contained minute sweet potato tissues.
Extraction. The peel (221 g) was dried, pulverized and
extracted with hexane using Soxhlet extractor for 6 h.
The extract was concentrated in vacuo to yield (8.6 g)
thick blackish syrup.
Thin layer chromatography (TLC). The TLC was
carried out on a precoated aluminium plates (Silica gel
GF254, 0.25 mm Merck W. Germany). Spots were detected
under ultraviolet/visible light (254 and 366 nm) before
spraying with vanillin spray reagent followed by heating
the plate at 110 C for about 5 min.
Column chromatography. The crude extract was
fractionated using silica gel column chromatography
(column diameter 4.2 cm, height 35 cm) into its chemical
constituents using a solvent system: hexane/diethyl
ether; 2:1. Thirty six fractions were obtained. The column
chromatography (CC) was monitored with TLC and
the fractions were combined as appropriate. Combined
fractions 4-12 afforded the alkyd resin, which was
further subjected to PTLC.

57