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International Journal of
Chemical Synthesis and Chemical
Reactions
IJCSCR
Jan – June 2016
Mechanical Engineering
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Ahmedabad, India
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Kangra, Himachal Pradesh, India
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Saud University, Riyadh, Saudi Arabia
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Commerce & Science College, Jalagaon, Mumbai, India
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Chennai, India
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India
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Vishnupuri, Nanded MS, India
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India
Dr. Hitesh D PatelGujarat University, India
Kasim Mohammed HelloAl-Muthanna University, Iraq
Dr. Krishna Namdev AlasundkarGovernment College of Engineering, Karad
Shivaji University, Kolhapur, India
Dr. Lakhwinder SinghDepartment of Applied Science, CGC College
of Engineering, Mohali, Punjab, India
Dr. M. R. JayapalNarasaraopeta Engineering College,
Narasaraopeta, Guntur, India
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of Engineering, King Saud University,Saudi Arabia
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India
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(Manipal), India
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Technology, India
EDITORIAL BOARD MEMBERS
Dr. Pradeep Kumar RanaDepartment of BSH, GIET, Gunupur, Odisha,
India
Dr. R. P. BadoniCollege of Engineering Studies, University of
Petroleum & Energy Studies, India
Dr. Rajeev SinghDepartment of Chemistry, ARSD, University of
Delhi, India
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Uttarakhand, India
Ramakrishna RaoDepartment of Chemistry, GITAM School of Technology, GITAM University, Bangalore,
India
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Dr. Someshwar Dagduappa DindulkarDepartment of Bioscience and Biotechnology, Konkuk University, Global hall 413, Konkuk
University, 1 Hwayang-dong, Gwangin-gu, Seoul, South Korea
Dr. Sudalai Kumar SFrancis Xavier Engineering College,
Vannarpet Tirunelveli, Tamil Nadu, India
Dr. Suryya K RanaDungarpur College of Engineering &
Technology, Dungarpur, Rajasthan, India
Dr. Tanveer AlamUniversity of Nizwa, Birkat Al Mouz, Nizwa,
Sultanate of Oman, Oman
Dr. V. ChristopherDepartment of Organic Chemistry, Andhra
University, Visakhapatnam, India
Dr. Vajjiravel MurugesanDepartment of Chemistry, B. S. Abdur Rahman
University, Vandalur, Chennai, Tamil Nadu, India
Prof. Velluru SrideviDepartment of Chemical Engineering,A. U. College of Engineering, Andhra
University, Visakhapatnam, Andhra Pradesh, India
Dr. Wilson Mbiti NjueDepartment of Chemistry, Kenyatta University,
Nairobi Kenya, Kenya
From the Editor's Desk
Dear Readers,
We would like to present, with great pleasure, the inaugural volume of a new scholarly
journal, International Journal of Chemical Synthesis and Chemical Reactions. This
journal is part of the Applied Sciences, and is devoted to the scope of present chemical
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This new journal was planned and established to represent the growing needs of Chemical Synthesis
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International Journal of Chemical Synthesis and Chemical Reactions focuses on original high-quality
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mechanism, Kinetic analysis, Combustion, and many more.
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Many scientists and researchers have contributed to the creation and the success of the chemical synthesis
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editorial staff of JournalsPub, who supported us at every stage of the project.
It is our hope that this fine collection of articles will be a valuable resource for chemistry readers and will
stimulate further research into the vibrant area of chemical synthesis and reactions.
Puneet Mehrotra
Managing Director
1. Synthesis and Characterization of Cadmium-Exchanged Sodalite A.V. Borhade, S.G. Wakchaure 1
2. Elucidation of Synthetic Mechanism Involved in the Conversion of Zwitterionic Clonixin to Carboxamide Side-Product S. Sudalai Kumar, N. Ramkumar, D. Kodimunthiri 6
3. Ultrasonic Study of Binary Liquid Mixtures of Triethyl Amine With Primary Alcohols at 303.15 KDhirendra Kumar Sharma 12
4. Preparation and Characterization of Ce-Si-SBA-15 Modified With IronK.J. Rose Philo, M.A. Rahana, S. Sugunan 17
5. Studies on Zirconium(IV) Telluroiodate: A New Heteropolyacid Based Inorganic Ion Exchange MaterialPremvir Singh 26
Contents
IJCSCR (2016) 1–5 © JournalsPub 2016. All Rights Reserved Page 1
International Journal of Chemical Synthesis & Chemical Reactions Vol. 2: Issue 1
www.journalspub.com
Synthesis and Characterization of Cadmium-Exchanged Sodalite
A.V. Borhade1, S.G. Wakchaure
2*
1Research Centre, Department of Chemistry, HPT Arts and RYK Science College, Nashik, India
2Department of Chemistry, PVG’s College of Engineering, Nashik, India
Abstract
Cadmium derivative of chloro-sodalite has been synthesized at low temperature by
hydrothermal method. The sodalite is characterized by IR, X-ray powder diffraction, and
SEM. The Cd derivative was obtained by facile exchange of cadmium for sodium in chloro-
sodalite using a solution of cadmium nitrate in Teflon autoclaves at 100°C. The IR spectra of
parent gallo silicate chloro-sodalite and cadmium-exchanged chloro-sodalites show three
kinds of IR vibrations, νas (Al–O–Si) (asymmetric stretching vibrations), νs (Al–O–Si)
(symmetric stretching vibrations), and δ (O–T–O) (bending vibration). Introduction of non-
tetrahedral cations into sodalite framework changes the IR spectra in the range of pseudo-
lattice vibrations located at about 700–500 cm1
. Parent chloro-sodalite and its cadmium
derivative shows cubic symmetry in a space group P 4 3n. The crystal structures were refined
by Rietveld refinement method. A considerable change is observed in cell parameters for the
cadmium derivative. Cell expansion is accompanied with slight increase in T–O bond
distances and T–O–T bond angles. The framework expansion takes place due to introduction
of non-framework cadmium ion. The unit cell parameter (a) is 8.9502 Å for chloro-sodalite
and it is found to be 9.0001 Å for cadmium sodalite. SEM pictures of cadmium derivative
shows slight deposition of particles on the crystal surfaces.
Keywords: cadmium, derivative, gallosilicate, sodalite
INTRODUCTION
Waste water discharged by industries
processing ores and concentrates of
nonferrous metals are usually polluted
with heavy metals, such water contains
toxic heavy metals which discharged into
the environment as industrial wastes
causing soil and water pollution.[1]
Constant trapping of heavy metal ions in
the zeolite framework structure is one of
the possible way of cation exchange and
making them harmless.
Pb+2
, Cu+2
and Cd+2
are the common heavy
metals which tend to accumulate in
organisms and cause serious diseases and
disorders.[2]
They are also the commonly
found ground water contaminants both at
industrial and military installations.
Several methods are available for removal
of dissolved heavy metals, like ion
exchange, precipitation, ultrafiltration,
reverse osmosis, and electrodialysis.[3–6]
Activated carbon adsorption is also
effective process for the removal of heavy
metals at trace quantities,[7]
but it is not
suitable due to high cost associated with
production and generation of spent
carbon.[8]
The use of alternative low cost
material as potential sorbents for removal
of heavy metals has recently been
emphasized. Among various available
techniques, ion exchange is considered to
IJCSCR (2016) 6–11 © JournalsPub 2016. All Rights Reserved Page 6
International Journal of Chemical Synthesis & Chemical Reactions
Vol. 2: Issue 1
www.journalspub.com
Elucidation of Synthetic Mechanism Involved in the Conversion
of Zwitterionic Clonixin to Carboxamide Side-Product
S. Sudalai Kumar1,2*
, N. Ramkumar2, D. Kodimunthiri
1
1Department of Science and Humanities, Francis Xavier Engineering College, SCAD Group of Institutions,
Tirunelveli, Tamil Nadu, India 2School of Chemistry, University of Hyderabad, Hyderabad, Telangana, India
Abstract
N-(3-Chloro-2-methylphenyl)-2-oxo-1,2-dihydropyridine-3-carboxamide is obtained as a by-
product during the synthesis and crystallization of Clonixin (2-(3-chloro-2-
methylanilino)nicotinic acid) and its polymorphs, respectively. This conversion was
unexpected and it changed the usual investigation path way enabling the formation of neutral
and zwitterionic polymorphs in our study on Clonixin in contrary to studies of 2-(p-
tolylamino) nicotinic acid investigation. The same conversion is checked in the other
synthesized analogs such as 2-(phenylamino)nicotinic acid (PNA), 2-
(methyl(phenyl)amino)nicotinic acid (MPNA), 2-(p-tolylamino)nicotinic acid (TNA) and 2-
(methyl(p-tolyl)amino)nicotinic acid (MTNA) but they were all not going to any other side
product formation like Clonixin. These ampholites were synthesized by the aromatic
nucleophilic substitution reactions of respective aryl amines and 2-chloronicotinic acid in the
presence of p-tolylsulfonic acid and pyridine in this report. However, the side product was
separated from the crystallization of Clonixin in acetic acid during polymorph hunt. All other
analogs were failed in giving this side product as those crystal structures of compounds were
analyzed thoroughly by single crystal X-ray determination method. On comparison of this
molecule with other ampholites, a new mechanism was proposed for the conversion of
Clonixin to this by product in this study and the other molecules are under investigation for
no conversion even though they are similar in structures.
INTRODUCTION
Arylamino nicotinic acids are the organic
compounds which has many medicinal
applications especially they all exhibit
anti-inflammatory drug properties.[1,2]
Based on their importance in medical field,
many arylamino nicotinic acids were
synthesized by different research groups in
different occasions.[3,4]
Recently these
molecules have some immense interest in
solid state chemistry corresponding to the
polymorph investigations. They have been
proven in many studies that they were
more prone to be polymorphic.
Tetramorphs and trimorphs were reported
for these molecules by Li and coworkers.[4]
Some of the neutral and zwitterionic
crystal structures were also reported by
Kumar and Nangia.[5]
Molecular
complexes for these molecules was also
investigated by Kumar.[6]
All these
molecules fell in the category of
ampholites in which they show acidic and
basic behavior and exist as zwitterion in
certain pH ranges. Li and coworkers[7]
reported already the crystal structure of
this N-(3-chloro-2-methylphenyl)-2-oxo-
1,2-dihydropyridine – 3 - carboxamide
compound while in synthesis of Clonixin
(Scheme 1). The same product was also
IJCSCR (2016) 12–16 © JournalsPub 2016. All Rights Reserved Page 12
International Journal of Chemical Synthesis & Chemical Reactions Vol. 2: Issue 1
www.journalspub.com
Ultrasonic Study of Binary Liquid Mixtures of Triethyl Amine
With Primary Alcohols at 303.15 K
Dhirendra Kumar Sharma
Department of Chemistry, Bundelkhand University, Jhansi, UP, India
INTRODUCTION
Most of the physical properties change
whenever there is a change in the
composition and structure of the liquid
mixture. Then non-linear dependence of
the physical–chemical properties with
composition has been attributed to the size,
shape, and polarity of the molecules.
Ultrasonic velocity is one such property
which is very important for the study of
molecular interactions in solution. It gives
information about the extent of interaction
and some other parameters such as
adiabatic compressibility and free
lengthy.[1]
Velocity determination of
ultrasound waves enables us to study the
properties of the medium, in which it
travels, owing to the important of
ultrasound velocity in the investigation of
molecular interaction in solutions, its
measurements have been carried out in the
different binary liquid mixture studies in
the present work.[2]
ULTRASONIC AND ULTRASOUND
The term, ultrasonic, refers to the science
and technology dealing with acoustic
waves of frequency higher than the
nominal limit of audibility by the human
ear. It must be called nominal limit, since
it is not definable in exact terms, but only
on some statistical basis, because it also
depends on sex and age and varies
considerably from person to person. Sound
waves can be classified into three types
viz. infrasonic waves, audible or sound
waves, and ultrasonic waves.[3–5]
The longitudinal waves whose frequency
lies below 20 Hz (cycle per second) are
called infrasonic waves. Human ear is not
sensitive to these waves. The waves are
produced by large vibrating bodies such as
during an earthquake. Audible or sound
waves are those longitudinal waves whose
frequency range produce the sensation of
sound when enter into human ear. Thus,
these waves are called either audible or
sound waves. Audible waves are produced
by vibrating bodies that includes vocal
cords of humans and animals, stretched
strings of musical instruments like guitar
and violin, stretched membranes (e.g.,
drum, loudspeaker), air columns (flute),
and by irregular motions of bodies (e.g.,
tree leaves, doors, etc.). Those audible
waves which are produced by regular
periodic motions of definite frequencies
given pleasing effects on the ear and are
called “musical sound waves.” On the
other hand, those waves which reproduced
by irregular non-periodic disturbances of
bodies produced an irritating effect on the
ear and are called “noise waves.”
The longitudinal waves whose frequency
lies between 20,000 and 5 × 108 Hz are
“ultrasonic waves.” The ultrasonic range
of full acoustic spectrum is broken down
into three subsections, such as low
frequency/airborne, conventional/
industrial, and high frequency/acoustic
microscopy as shown in Figure 1. Human
ear is not sensitive to these waves. This
types of waves can be produced either by
the high frequency vibration of a quartz
crystal under an alternating eclectic field
or by the vibration of a ferromagnetic rod
IJCSCR (2016) 17–25 © JournalsPub 2016. All Rights Reserved Page 17
International Journal of Chemical Synthesis & Chemical Reactions Vol. 2: Issue 1
www.journalspub.com
Preparation and Characterization of Ce-Si-SBA-15 Modified
With Iron
K.J. Rose Philo1*, M.A. Rahana
1, S. Sugunan
2
1Department of Chemistry, St. Paul’s College, Kalamassery, India
2Department of Applied Chemistry, Cochin University of Science and Technology, Cochin, India
Abstract
Recently environmental concerns have driven the development of specialized catalysts to
prevent polluting substances from being released into the environment. New technologies
have improvised our understanding of catalytic functions as well as selectivity in order to
save the energy and chemicals. Today, catalysis is the workhorse in the chemical industry
with approximately >90% of the products produced in catalytic processes. In addition, life
cannot exist without catalysis, as virtually all biochemical processes that sustain life are
reliant on enzymes, nature’s own catalysts. Mixed metal oxides are multimetal multiphase
oxides which typically contain one or more transition metal oxide and exhibit significant
chemical and structural complexity. In recent years porous materials attract the attention of
researchers and material scientists due to commercial interest in their applications in various
fields especially in heterogeneous catalysis. Among the variety of catalysts, cerium oxide
(CeO2) plays an important role in emerging technologies for environmental and energy-
related applications. Also many efforts have been made to investigate the pore structure of
SBA-15 and utilize SBA-15 as templates for preparing nano-structured materials.
Incorporation of transition metals into the SBA-15 silica framework is still a challenge in the
field of mesoporous material synthesis. Only few reports are available that has successfully
demonstrated the modification. Mesoporous ceria catalyst was prepared by the soft template
method using the neutral surfactant hexadecyl amine (HDA). It is mixed with 15 and 20%
SBA-15 prepared by surfactant assisted method using Pluronic-123. The prepared samples
were modified with 10% Fe. A detailed investigation of physico-chemical characterization of
the catalytic systems was performed by techniques such as wide and low angle XRD, BET
surface area by sorption studies of nitrogen gas, SEM, TEM, TG/DTA and FT-IR.
Keywords: hexadecyl amine, iron doping, mesoporous ceria, neutral surfactant, SBA-15
INTRODUCTION
In the chemical industry and industrial
research, catalysis plays an important role.
Different catalysts are in constant
development to fulfil economic, political
and environmental demands. When using a
catalyst it is possible to replace a polluting
chemical reaction with a more
environmentally friendly alternative. In the
start only pure components were used as
catalysts, but after the year 1900
multicomponent catalysts were studied and
are now commonly used in the industry.[1–
8]
Typical industrial catalysts, however,
consist of several components and phases.
Supported catalysts play a significant role
in many industrial processes. The support
provides high surface area and stabilizes
-
IJCSCR (2016) 26–33 © JournalsPub 2016. All Rights Reserved Page 26
International Journal of Chemical Synthesis and Chemical Reactions Vol. 2: Issue 1
www.journalspub.com
Studies on Zirconium(IV) Telluroiodate: A New Heteropolyacid
Based Inorganic Ion Exchange Material
Premvir Singh* Analytical Research Laboratory, Chemistry Department, Aligarh Muslim University, Aligarh, India
Abstract
Zirconium (IV) telluroiodate has been synthesized as a new inorganic cation exchanger by
adding a mixture of aqueous solution of 0.1 M potassium iodate and 0.1 M sodium tellurite to
aqueous solution of 0.1 M zirconium (IV) oxychloride under varying mixing ratios at pH 1.
Its ion exchange capacity for Na+ was found to be 1.85 meqg
1 of dry exchanger. The
material has been characterized on the basis of chemical composition, FTIR, TGA, SEM and
XRD. The chemical stability and thermal stability of the exchange material have also been
studied. Further, various ion exchange studies such as pH titration, determination of ion
exchange capacities for various metal ions and distribution behavior have been performed on
this material.
Keywords: cation exchanger, characterization, heteropolyacidic salt, synthesis, zirconium
(IV) telluroiodate
INTRODUCTION
Synthesis of new inorganic ion exchangers
is always of interest. Since, they are
specific in nature and can solve diverse
problems of environmental and analytical
chemistries.[1–3]
These materials have also
been employed in treatment of radioactive
nuclear effluent, to remove toxic
substances from aqueous effluent,[4,5]
pre-
concentration and recovery of a number of
ionic species from aqueous and non-
aqueous system. These materials have also
been employed in the development of
chemical sensor and ion exchange
membrane.[6,7]
Advancement in inorganic
ion exchanger is not only due to the high
thermal stability and resistivity towards
radiation field but also for usual selectivity
for ionic species and versatility in
separation. Synthetic inorganic ion
exchangers based on tetravalent metal acid
(TMA) salt often show much better ion
exchange behavior as compared with
single salt thus, such materials have been
the object of considerable studies due to
their intercalation properties, higher ion
exchange capacity, stability and selectivity
towards certain metal ions.[8–22]
In continuation of our work based on
zirconium (IV) based heteropolyacid
salts[23,24]
ion exchangers, here we have
synthesized a new heteropolyacidic salt i.e.
zirconium (IV) telluroiodate, as per
literature no information has been found
on this material as ion exchanger. This
paper presents the synthesis,
characterization and ion exchange
behavior of zirconium (IV) telluroiodate.
EXPERIMENTAL SECTION
Reagents and Chemicals
Zirconium oxychloride (CDH), sodium
tellurite (S. D. Fine Chem.) and potassium
iodate (E Merck, India) were used for the
synthesis of ion-exchangers. All other
International Journal of
Chemical Synthesis and Chemical
Reactions
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Jan – June 2016
Mechanical Engineering
Electronics and Telecommunication Chemical Engineering
Architecture
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