Indian Journal of
Chemical Technology
Volume 9 Number 3 May 2002
CODEN:ICHTEU 9(3)
179-278 ISSN:
0971-457X
CONTENTS
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Research Articles |
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New rodent repellent and UV resistant nylon tapes for aircraft
arrester net |
185 |
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K Ganesan, Santosh Kumar, D K Dubey, Shri Prakash,
Jagat Singh, |
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Utilisation of Jatropha
seed oil in the stabilisation of poly (vinly chloride) against thermal
degradation |
188 |
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Role of Zn2+ in
the inhibition of corrosion of mild steel by 1-hydroxyethane-1,1-diphosphoric
acid |
197 |
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Basic dye adsorption on a
low cost carbonaceous sorbent – kinetic and equilibrium studies |
201 |
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Kinetic studies on the photocatalytic
decolourisation of water-soluble crown dyes using Fe° and Zn° catalysts |
209 |
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Thermodynamic dissociation
constants of glycine and dl-alanine
in water-ethanol mixtures |
212 |
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Galactose oxidase
immobilised on Ocimum sanctum seeds
for the enzymatic preparations of L-glucose, L-galactose and L-xylose |
218 |
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Study on the formation of
dinitramide using mixed acid nitrating agents |
223 |
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Scale-up and optimization
studies on lignin biodegradation of rice straw using Phanerochaete chrysosporium |
227 |
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Pressure mediated reduction
of nitro to amino functionality with FeSO4/NH3/H2O/EtOH
system |
235 |
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Retention behaviour of
metal ions on calcium sulphate layers: Separation of mercury |
239 |
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Contd. |
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Sorption aided process for
the removal and recovery of Zinc(II) using salicylaldoxime immobilised silica
gel |
245 |
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The phosphine oxides
Cyanex-921, Cyanex-923 and Cyanex-925 as extractants for Pb(II) from aqueous
media |
251 |
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|
|
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Ion-exchange kinetics on styrene
supported zirconium(IV) tungstophosphate: An organic-inorganic type cation
exchanger |
256 |
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Notes |
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An efficient route for the
synthesis of chloroaceticanhydride and benzyl mercaptan |
261 |
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Educator
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The history of bromine
from discovery to commodity |
263 |
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Chem-Tech Scan
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272 |
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Announcement
|
276 |
Indian Journal
of Chemical Technology
New rodent repellent and UV
resistant nylon tapes for aircraft arrester net
K Ganesana, Santosh Kumara, D K Dubeya, Shri Prakasha, Jagat Singhb, J K Tyagib & M P KaushikaT
Received 2 August 2001; revised received 11 February 2002; accepted 6 March 2002
A new rodent repellent and UV resistant nylon tape for the fabrication of fighter aircraft arrester net has been developed. Oleoresin, a sensory irritant from natural sources has been used along with black carbon and butyl recinoleate. These tapes have been found to be effective against rodents under laboratory conditions
Indian Journal
of Chemical Technology
Utilisation of Jatropha seed oil in
the stabilisation of poly (vinyl chloride)
against thermal degradation
F E Okieimen
Received 5 March 2001; revised received 4 January 2002; accepted 14 February 2002
Jatropha
seed meal was extracted with n-hexane
and the oil obtained was found to have iodine value 157.37, acid value 5.61 and
free fatty acid 2.70. The fatty acid profile of the oil showed that oleic acid
(31.35%), palmitic acid (20.9%) stearic acid (15.68%) and caprylic acid
(10.45%) were the major fatty acid components. The seed oil was epoxidised at
29°C using peracetic acid produced in
situ by reacting hydrogen peroxide (30% v/v)
with various amounts of glacial acetic acid. Barium, cadmium, lead and zinc
soaps of the oils were prepared by metathesis in alcohol solution. Thermal
degradation studies on poly (vinyl chloride) in the presence of Jatropha seed
oil, the epoxidised oil and the metal soaps of the oils were carried out at
various temperatures (170, 180 and 190°C) under oxidative and non-oxidative conditions. Changes in
intrinsic viscosity and levels of unsaturation in the degraded polymer samples
together with kinetic data (rate measurements at 1% conversion) were used to
evaluate the relative stabilising effect of the additives on the thermal
degradation of poly (vinyl chloride). It was found that although the values of
the rate of dehydrochlorination were of about the same order of magnitude (10-2%
min-1), the rates were relatively lower, and the time at which
degradation reached 1% conversion considerably higher than the corresponding
values obtained in the absence of the additives. The data from solution
viscosity measurements and from estimates of the level of unsaturation in the
degraded polymer samples indicate that metal soaps of the oil exert stabilising
effect on the oxidative and monoxidative thermal degradation of poly (vinyl
chloride).
Indian Journal of Chemical Technology
Role of Zn2+ in the inhibition of
corrosion of mild steel by
1-hydroxyethane-1, 1-diphosphonic acid
Susai Rajendrana*,
R Maria Joanyb, B V Apparaoc & N Palaniswamyd
Received 22 May 2001; revised
received 7 February 2002; accepted 19 March 2002
50
ppm sodium salt of 1-hydroxyethane-1, 1-diphosphonic acid (HEDP) offered only
11% inhibition efficiency (IE) to corrosion of mild steel immersed in neutral
aqueous environment containing 60 ppm chloride. When 50 ppm Zn2+ is
added to 50 ppm HEDP, the IE increased to 98%. The influence of Zn2+
on the corrosion -inhibition by HEDP is discussed based on the results obtained
from UV-visible, FTIR and luminescence spectra. Presence of Zn2+
facilitates the transport of HEDP from the bulk of the solution to the metal
surface; both the anodic reaction and cathodic reaction are controlled
effectively.
Indian Journal
of Chemical Technology
Vol. 9, May 2002, pp. 201-208
Basic dye adsorption on a low cost
carbonaceous sorbent – Kinetic and equilibrium studies
B Stephen Inbaraj & N Sulochana*
Received 5 March 2001; revised received 17 March 2002; accepted 20 March 2002
A carbonaceous sorbent prepared from an indigenous
agricultural waste, jack fruit peel, by acid treatment was tested for its
efficiency in removing basic dyes. Malachite green, a common basic dyestuff of
triphenyl methane series used for dyeing silk and wool directly and cotton
mordanted with tannin to deep green, was chosen for investigation. The process
parameters studied include agitation time, initial dye concentration, carbon
dose, pH and temperature. The
adsorption followed first order reaction equation and the rate is mainly
controlled by intraparticle diffusion. Freundlich, Langmuir and
Redlich-Peterson isotherm models were applied to the equilibrium data. The
adsorption capacity (Qo)
obtained from the Langmuir isotherm plot was 166.37 mg g-1 at an initial pH of 6.0
and at 32 ± 0.5°C. The influence of pH on
dye removal was not significant and the adsorption capacity increased with
increase in temperature. A portion of the dye was recovered from the spent
carbon using 50% acetic acid (v/v).
Indian Journal
of Chemical Technology
Kinetic studies on the
photocatalytic decolourisation of water-soluble crown dyes using Feo
and Zno catalysts
Y K Agrawal*, B R Pandya & S K Menon
Received 5 March 2001; revised received 27 January 2002; accepted 14 February 2002
Photodecolourisation
of crown dyes with Feo and Zno as catalysts is discussed.
Effects of pH and concentration of
catalyst on the decolourisation and kinetics for degradation etc have been
studied.
Indian Journal of Chemical Technology
Thermodynamic dissociation constants of glycine
and dl-alanine in
water - ethanol mixtures
M Ashfaqur Rahman*, A R Chowdhury & M R Zaman**
Received 12 June 2001; revised received 10 January 2002; accepted 7 February 2002
The thermodynamic dissociation
constants of glycine and dl-alanine
in 0, 20, 40, 60 and 80% (w/w) water
- ethanol mixtures at 30°C and at a constant ionic strength, Is = 0.1 M KNO3 have
been measured pH-metrically using
Irving and Rossotti technique. pK1
and pK2 values in aqueous
medium have been found to agree well with previously reported ones. It is observed
that the pK1 values of
these acids increase regularly with the increase of ethanol contents in the
mixtures while pK2 values
show distinct minima ca. at 40% (w/w) ethanol content. The variation in pK values with the solvent composition
is discussed in terms of the free energy transfer from water to ethanol-water
mixtures. It is concluded that the specific solute-solvent interactions play a
vital role in changing the pK values
in ethanol-water mixtures.
Indian Journal
of Chemical Technology
Galactose oxidase immobilised on Ocimum sanctum seeds for the enzymatic
preparations of L-glucose, L-galactose and L-xylose
K K Yadav, S K Vernwal, Z Afaq & K D S Yadav*
Received 4 July 2001; revised received 28 February 2002; accepted 20 March 2002
Galactose oxidase has been immobilised on a solid support developed
by modification and activation of surface of Ocimum sanctum seeds. The conversions of xylitol to L-xylose;
galactitol to L-galactose and D-sorbitol to L-glucose using the above
immobilised enzyme preparation have been shown. Galactose oxidase
co-immobilised with catalase increases the conversion yields. Conversion of
D-sorbitol to L-glucose using the immobilised galactose oxidase in a mini flow
bed reactor has been demonstrated.
Indian Journal
of Chemical Technology
Study on the formation of
dinitramide using mixed acid nitrating agents
G Santhosh, S Venkatachalam*, M Kanakavel & K N Ninan
Received 9 August 2001; revised received 27 February 2002; accepted 21 March 2002
Nitration
of ammonium sulphamate was carried out using a mixture of sulphuric acid and
nitric acid at -30 to –40°C. The mole ratio of sulphuric acid to nitric acid was varied from 0
to 4 and the extent of formation of ammonium dinitramide (ADN) was measured.
The initial yield of ADN increases with increase of sulphuric acid content in
the acid mixture and starts decreasing as the reaction time is increased. The
variation of product yield with change in reaction time and total acid
concentration was studied.
Indian
Journal of Chemical Technology
Scale-up
and optimization studies on lignin biodegradation of rice straw using Phanerochaete chrysosporium
Sk Masud Hossaina*, Manas Dasb & S H
Ibrahimc
Received 19 February 2001; revised received 28 January 2002; accepted 10 March 2002
An
effective batch aerobic study on lignin biodegradation with Phanerochaete chrysosporium is performed
and process parameters are optimized. The optimum time is 14 days for lignin
biodegradation of rice straw. At the optimum time, 2 percent glucose (carbon
source) and 0.20 percent L-asparagine (nitrogen source) calculated on raw
material, can degrade maximum lignin. The percent of lignin degradation at
optimum GNC dose is 47.38 with lowest kappa number (k) value 23.58 with optimum
inoculum concentration 20 percent (v/v) and optimum age of inoculum 7 days
with pH 4.5. The minimum COD and BOD
values for optimum GNC Dose treated effluents after 14 days digestion are 1,050
mg/L and 625 mg/L respectively. The optimum GNC Dose treated effluents having
colour (OD at 465 nm) is 0.20 which is minimum.
Indian
Journal of Chemical Technology
Pressure mediated reduction of nitro to amino
functionality with
FeSO4/NH3/H2O/EtOH
system
Hari Sankar Kakati & Dibakar Chandra Deka*
Received 8
August 2001; revised received 11 February 2002; accepted 20 March 2002
Pressure
mediated reduction of nitro to amino group by FeSO4/NH3/H2O/EtOH
system has been carried out. Moderate nitrogen pressure (1.1 MPa at reaction
temperature) at 100o C for 4 h has almost doubled the yield to 70.7%
from 39.7% when no pressure is applied. Functional groups like chloro and olefinic
double bond remain intact but esters are incompatible.
Indian Journal of Chemical Technology
Retention behaviour of metal ions on calcium sulphate
layers: Separation of mercury
Aditya K Misra* & Sonu Pachauree
Received 16 December 2000; revised received 27 March 2002; accepted 1 April 2002
Calcium sulphate static phase thin layer chromatography
(TLC) has been performed in eight pure and mixed solvent systems containing
acetonitrile and dioxane. Separations of Pb2+ from Hg2+,
Bi3+ and UO22+; UO22+
from VO2+; Ni2+ from Cr3+; Ag+ from
Bi3+; Ce4+ from Ce3+; Hg2+ from Cd2+;
Zn2+ from Hg2+ have been achieved successfully. Rapid
quantitative separation of mercury (2-20 mg)
from binary, ternary and multicomponent mixtures containing several metal ions
has also been successfully achieved.
Indian Journal of Chemical
Technology
Sorption aided process for the removal and recovery of
Zinc (II) using salicylaldoxime immobilised silica gel
Mitali Sarkar* & Pradip Kumar Datta
Received 27 April 2001; revised received 3 January 2002; accepted 6 March 2002
Salicylaldoxime
immobilised silica gel was used as an effective solid phase surface, for the
preconcentration, removal or recovery of zinc ion from aqueous phase. The
efficiency was tested by the equilibrium sorption study both in batch and
column operations. The efficiency increases with the shaking period, agitation
speed, adsorbent dose, temperature and flow rate but is independent on the
volume of the solution. Maximum adsorption was found to occur at pH 5.5. Alkali metal, alkaline earth
metal and ammonium salts do not influence the adsorption process. Heavy metal
ions viz. Cu(II), Ni(II), Co(II) and Fe(III) get adsorbed by the said process
but at much different pH values.
Complexing ligands like EDTA and cyanide markedly decrease the adsorption of
Zn(II) by the said procedure. The adsorption data fits well the Langmuir
adsorption isotherm model. The negative free energy change indicates that the
process is favourable as well as spontaneous. The merit of the process lies
with its high preconcentration factor.
Indian Journal of Chemical Technology
The phosphine oxides Cyanex-921,
Cyanex-923 and Cyanex-925 as
extractants for Pb(II) from aqueous media
J N Iyer, S D Pawar & P M Dhadke*
Received 19 June 2001; revised received 27 January 2002; accepted 1 March 2002
The behaviour of neutral phosphine oxides Cyanex-921, Cyanex-923 and
Cyanex-925 in the extraction of Pb(II) from nitrate media is described. The
extraction of Pb(II) was found to be quantitative in the pH range 8.0-9.0 with these extractants. From the metal loaded
organic phases for these extractants, Pb(II) was stripped back with 0.5 M H2SO4.
The effects of pH, temperature,
equilibrium time, diluents, diverse ions and stripping ability using various
acids on the extraction of Pb(II) have been studied. The methods are also
extended for the analysis of real samples.
Indian Journal of Chemical
Technology
Vol. 9, May 2002, pp. 256-260
Ion-exchange kinetics on styrene supported zirconium(IV)
tungstophosphate:
An organic-inorganic type cation exchanger
A A Khan*, R
Niwas & M M Alam
Received 25
November 2000; revised received 15 January 2002; accepted 19 March 2002
Kinetics of exchange reaction of Mg2+, Ca2+, Sr2+,
Ba2+, Cu2+, Mn2+, Ni2+ and Zn2+
on styrene supported zirconium (IV) tungstophosphate cation exchanger has been
studied at 25, 33, 50 and 65oC. The rate of exchange is found to be
particle diffusion controlled at a metal ion concentration ³ 0.02 M in aqueous medium. Various kinetic parameters such as
self-diffusion coefficient, D0 , energy of activation, Ea, and entropy of activation, DS*, have been calculated.
Indian Journal of Chemical Technology
Note
An efficient route for the synthesis
of chloroaceticanhydride and benzyl mercaptan
R L Jagadish*a, T R Vijayakumar & K M Lokanatha Raib
Received 20 September 2001; revised received 21 February 2002; accepted 21 March 2002
An efficient and cost saving procedure for the synthesis of chloroacetic anhydride and benzyl mercaptan is discussed here.
Indian Journal of Chemical Technology
The history of bromine from
discovery to commodity
Jaime Wisniak*
The discovery of bromine represents one of the first experimental evidences
that elements could be grouped in families of similar properties.
Transformation of the new element and its derivatives into a commercial reality
had to wait until automobiles begun to be mass-produced. The pattern end use of
bromine has reflected the changes in social appreciation of environmental
protection and safety. From a strong initial use as gasoline additive and
agricultural chemical, the end uses are changing drastically into
flame-retardants and sanitary uses. From a strictly initial European industrial
activity it has turned into an important chemical activity for the United
States, Jordan, and Israel.