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International Journal of
Chemical Synthesis
and Chemical
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IJCSCR
Jan – June 2016
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From the Editor's Desk
Dear Readers,
We would like to present, with great pleasure, the inaugural volume of a new scholarly
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journal is part of the Applied Sciences, and is devoted to the scope of present chemical
synthesis and chemical reactions issues, from theoretical aspects to application-dependent
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ManagingDirector
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 K
Dhirendra Kumar Sharma 12
4. Preparation and Characterization of Ce-Si-SBA-15 Modified With Iron
K.J. Rose Philo, M.A. Rahana, S. Sugunan 17
5. Studies on Zirconium(IV) Telluroiodate: A New Heteropolyacid Based Inorganic Ion Exchange Material
Premvir 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. Wakchaure2*
1
Research Centre, Department of Chemistry, HPT Arts and RYK Science College, Nashik, India
2
Department 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 cm1
. Parent chloro-sodalite and its cadmium
derivative shows cubic symmetry in a space group P43n. 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. Kodimunthiri1
1
Department of Science and Humanities, Francis Xavier Engineering College, SCAD Group of Institutions,
Tirunelveli, Tamil Nadu, India
2
School 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. Rahana1
, S. Sugunan2
1
Department of Chemistry, St. Paul’s College, Kalamassery, India
2
Department 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
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International Journal of Chemical Synthesis and Chemical Reactions vol 2 issue 1

  • 1. International Journal of Chemical Synthesis and Chemical Reactions IJCSCR Jan – June 2016 Mechanical Engineering Electronics and Telecommunication Chemical Engineering Architecture Office No-4, 1 Floor, CSC, Pocket-E, Mayur Vihar, Phase-2, New Delhi-110091, India E-mail: info@journalspub.com ¬ International Journal of Thermal Energy and Applications ¬ International Journal of Production Engineering ¬ International Journal of Industrial Engineering and Design ¬ International Journal of Manufacturing and Materials Processing ¬ International Journal of Mechanical Handling and Automation « International Journal of Radio Frequency Design « International Journal of VLSI Design and Technology « International Journal of Embedded Systems and Emerging Technologies « International Journal of Digital Electronics « International Journal of Digital Communication and Analog Signals « International Journal of Housing and Human Settlement Planning « International Journal of Architecture and Infrastructure Planning « International Journal of Rural and Regional Planning Development « International Journal of Town Planning and Management Applied Mechanics 5 more... 1 more... 2 more... 2 more... 5 more... Computer Science and Engineering « International Journal of Wireless Network Security « International Journal of Algorithms Design and Analysis « International Journal of Mobile Computing Devices « International Journal of Software Computing and Testing « International Journal of Data Structures and Algorithms Nanotechnology « International Journal of Applied Nanotechnology « International Journal of Nanomaterials and Nanostructures « International Journals of Nanobiotechnology « International Journal of Solid State Materials « International Journal of Optical Sciences Physics « International Journal of Renewable Energy and its Commercialization « International Journal of Environmental Chemistry « International Journal of Agrochemistry « International Journal of Prevention and Control of Industrial Pollution Civil Engineering « International Journal of Water Resources Engineering « International Journal of Concrete Technology « International Journal of Structural Engineering and Analysis « International Journal of Construction Engineering and Planning Electrical Engineering « International Journal of Analog Integrated Circuits « International Journal of Automatic Control System « International Journal of Electrical Machines & Drives « International Journal of Electrical Communication Engineering « International Journal of Integrated Electronics Systems and Circuits Material Sciences and Engineering « International Journal of Energetic Materials « International Journal of Bionics and Bio-Materials « International Journal of Ceramics and Ceramic Technology « International Journal of Bio-Materials and Biomedical Engineering Chemistry « International Journal of Photochemistry « International Journal of Analytical and Applied Chemistry « International Journal of Green Chemistry « International Journal of Chemical and Molecular Engineering « International Journal of Electro Mechanics and Mechanical Behaviour « International Journal of Machine Design and Manufacturing « International Journal of Mechanical Dynamics and Analysis « International Journal of Fracture and damage Mechanics « International Journal of Structural Mechanics and Finite Elements 5 more... 4 more... 3 more... Biotechnology « International Journal of Industrial Biotechnology and Biomaterials « International Journal of Plant Biotechnology « International Journal of Molecular Biotechnology « International Journal of Biochemistry and Biomolecules « International Journal of Animal Biotechnology and Applications 3 more... Nursing « International Journal of Immunological Nursing « International Journal of Cardiovascular Nursing « International Journal of Neurological Nursing « International Journal of Orthopedic Nursing « International Journal of Oncological Nursing 5 more... 4 more... Subm it Your A rticle2016 www.journalspub.com
  • 2. International Journals Publisher JournalsPub is a multi-disciplinary international journal boosting innovative & eminence research work by Division of Dhruv Infosystems Pvt. Ltd. Launched in 2014 under the support and guidance by our Honorable EditorialBoard Members from renownedinstitutes. ObjectivesofJournalsPub üJournalsPub is international scholarly journal that publishes peer reviewed journal in the frontier areas of AppliedSciences,MedicalandEngineering. üJournalsPub publishes Original Research Papers, Review Papers, Popular Articles, Short Communications&CaseStudy. üPublishingspecialissues on Proceedingsof Conferences,SeminarsandSymposia. üJournalsPub Publishes issues twice a year (bi-annually) in English-language which is available online (openaccess)andinprintedversionwithagoaltopromoteanextensiveacademicawareness. üJournalsPub desires to set a good benchmark in the publishing industry by launching more than 100+ new International Journals to help the scientific community to enhance communication within the research communities and maintain a balance between the existing and emerging interdisciplinary technologies. üJournalsPub aims to provide quality research articles for Academic Researchers, Industrial Professionals, Engineers, Scientists, Professors, etc. working in the areas of Applied Sciences, Medical andEngineeringtocontributeandcommunicateinnovativework. SalientFeatures üAn umbrellaof 100+ journalsthatcoversAppliedSciences,MedialandEngineeringArena. üThe first and one of the rapidly emerging publication website in Country as well as overseas for its excellenceandexposure. üUniversaltransmissionandreflectivity. üARigorous, Fast andConstructivePeerReviewProcess üSpeedyPublicationof Manuscripts üEminentEditorialBoardMembersfromrenownedorganizations. üFreeRegistration,OnlineSubmission, Processing, Publication&OnlineAccessofManuscripts. üThejournalpublishesnovelresearcharticleswithemphasison theoreticalandexperimentalwork. International Journal of Chemical Synthesis and Chemical Reactions
  • 3. JournalsPub (Division of Dhruv Infosystem Private Ltd.) having its Marketing office located at Office No. 4, First Floor, CSC pocket E Market, Mayur Vihar Phase II, New Delhi-110091, India is the Publisher of Journals. Statements and opinionsexpressedintheJournalreflecttheviews oftheAuthor(s) andarenottheopinionofJournalsPub unless so stated. Subscription Information and Order Cost of Journal National Subscription ?Rs. 3000/-perJournal(includes2 printissues), SingleIssue copypurchaseRs.1800/copy International Subscription ?OnlineOnly- $99, PrintOnly-$149 (includes2printissues) ?Online+ Print-$199(includes2printissues +onlineaccessof publishedbackvolumes) To purchaseprintcompilationof backissues pleasesendyourqueryatinfo@journalspub.com Subscription must be prepaid. Rates outside the India include speed delivery charges. Prices subject to change without notice. Mode of Payment:At par cheque, Demand draft, and RTGS (payment to be made in favor of Dhruv Infosystem Pvt. ltd., payableatDelhi/NewDelhi. OnlineAccess Policy A). ForAuthors: In order to provide maximum citation and wide publicity to the authors work, JournalsPub also have OpenAccess Policy; Authors who would like to get their work open access can opt for Optional Open Access publication at nominal cost as follows: India,SARC andAfricanCountries:INR 1500 includingsinglehardcopyofAuthor's Journal. OtherCountries:USD 200includingsinglehardcopyofAuthor's Journal. B.) ForSubscribers: Online access will be activated within 72 hours of receipt of the payment (working days), subject to receipt of correct informationonuser details/StaticIPaddress of thesubscriber. The accesswillbeblocked: If the user requests for the same and furnishes valid reasons for blocking due to technical issue. Misuse of the access rights as pertheaccesspolicy. Advertising and Commercial Reprint Inquiries: JournalsPub with wide circulation and visibility offer an excellent media for showcasing/promotion of your products/services and the events-namely, Conferences, Symposia/Seminars etc.These journals have very high potential to deliver the message across the targeted audience regularly with each published issue. The advertisements on bulk subscriptions, gift subscriptions or reprint purchases for distribution etc. are also very welcome. LostIssue Claims:Pleasenotethefollowingwhen applyingfor lostor missingissues: Claims for print copies lost will be honored only after 45 days of the dispatch date and before publication of the next issue as perthefrequency. Tracking id for the speed post will be provided to all our subscribers and the claims for the missing Journals will be entertainedonlywiththeproofs whichwillbeverifiedatboththeends. Claimsfiledduetoinsufficient(or nonotice)ofchangeof address willnotbehonored. Change ofAddress of Dispatch should be intimated to JournalsPub at least 2 months prior to the dispatch schedule as per thefrequencyby mentioningsubscriberID andthesubscriptionID. Refundrequestswillnotbeentertained. LegalDisputes AllthelegaldisputesaresubjectedtoDelhiJurisdictiononly. If you haveanyquestions,pleasecontactthePublicationManagementTeam: info@journalspub.com;Tel:+910120-4347644.
  • 4. International Journal of Chemical Synthesis and Chemical Reactions International Journal of Chemical Synthesis and Chemical Reactions, focuses on the material synthesis, mass balance, kinetic analysis and other related fields of chemical synthesis process and chemical reactions. Journalacceptsbothexperimentalandtheoreticalpapersthatfallunderthescopeof thejournal. Focus andScopeoftheJournal ! Chemical engineering ! Electro synthesis ! Methods in organic synthesis ! Organic synthesis ! Peptide synthesis ! Reaction mechanism ! Kinetic analysis ! Combustion ! Mass balance ! Emerging reactor technologies ! Materials synthesis and processing International Journal of Chemical Synthesis and Chemical Reactions is published twice a year (bi-annual) by JournalsPub- is an imprint of Dhruv Infosystems Pvt. Ltd., India.The outlooks stated in the articles do not essentially reflect of the publisher. The publisher does not endorse the quality or value of the advertised/sponsored products described therein. Please consult full prescribing information before issuing aprescriptionfor anyproductsmentionedinthispublication. No part of this publication may be reproduced, stored in retrieval or transmitted in any form without written permissiontothepublisher. To cite any of the material contained in this journal, in English or translation, please use the full English reference at the beginning of each article. To reuse any of the material, please contact JournalsPub (info@journalspub.com).
  • 5. PUBLICATION MANAGEMENT TEAM INTERNAL MEMBERS Associate Manager Chairman Mr. Puneet Mehrotra Managing Director, JournalsPub, New Delhi Hidam Renubala Ankita Singh Akanksha Marwah Deepika Bhadauria Commissioning Editors Priyanka Garg Chhavi Goel Shrawani Verma
  • 6. EDITORIAL BOARD MEMBERS Dr. A. Thirupathaiah Department of Chemistry, Chaitanya Degree & PG Colleges, Hanmakonda, Warangal, India Dr. Ahmad Reza Massah Department of Chemistry, School of Basic Sciences, Islamic Azad University, Shahreza, Isfahan, Iran Dr. Ajit Manharlal Bhavsar Dishman Pharmaceuticals and Chemicals Ltd., Ahmedabad, India Dr. Anuja Chauhan Arni University, Kangra, Himachal Pradesh, India Dr. Asif Mahmood Department of Chemical Engineering, King Saud University, Riyadh, Saudi Arabia Dr. Avinash Sonar Department of Chemistry, VSN Arts, Commerce & Science College, Jalagaon, Mumbai, India Dr. C Jaya Kumar Department of Chemical Engineering, A. C. Technology, Anna University, Chennai, India Dr. Chennamsetty Subramanyam Bapatla Engineering College, Bapatla, India Dr. Dnyaneshwar Wankhede Swami Ramanand Tirth Marathwada University, Vishnupuri, Nanded MS, India Dr. Faiyazalam Mahmadsaiyad Shaikh Navnirman Science College, Surat, Gujarat, India Dr. Hitesh D Patel Gujarat University, India Kasim Mohammed Hello Al-Muthanna University, Iraq Dr. Krishna Namdev Alasundkar Government College of Engineering, Karad Shivaji University, Kolhapur, India Dr. Lakhwinder Singh Department of Applied Science, CGC College of Engineering, Mohali, Punjab, India Dr. M. R. Jayapal Narasaraopeta Engineering College, Narasaraopeta, Guntur, India Dr. Mohamed Abashar Department of Chemical Engineering, College of Engineering, King Saud University, Saudi Arabia Dr. Mohammed Shaheer Malik CSIR-Indian Institute of Chemical Technology, India Dr. Nandkumar M. Patil Wockhardt R & D Center, Aurangabad, India Dr. Nitinkumar S. Shetty Department of Organic Chemistry, Manipal Institute of Technology, Manipal University (Manipal), India Dr. Perumal Ramachandran Kongunadu College of Engineering and Technology, India
  • 7. EDITORIAL BOARD MEMBERS Dr. Pradeep Kumar Rana Department of BSH, GIET, Gunupur, Odisha, India Dr. R. P. Badoni College of Engineering Studies, University of Petroleum & Energy Studies, India Dr. Rajeev Singh Department of Chemistry, ARSD, University of Delhi, India Prof. Rajneesh Dutt Kaushik Gurukul Kangri University, Haridwar, Uttarakhand, India Ramakrishna Rao Department of Chemistry, GITAM School of Technology, GITAM University, Bangalore, India Dr. Rekha Lagarkha Department of Chemistry, Bundelkhand University, Jhansi, Uttar Pradesh, India Dr. Saeed Khodabakhshi Nanotechnology Research Center, Research Institute of Petroleum Industry, Tehran, Iran Dr. Sameena Bano Jamia Hamdard, India Dr. Samson Maria Louis N Sri Ramakrishna Institute of Technology, Coimbatore, Chennai, India Dr. Shubha Jain School of Studies in Chemistry & Biochemistry, Vikram University, Ujjain, Madhya Pradesh, India Dr. Someshwar Dagduappa Dindulkar Department of Bioscience and Biotechnology, Konkuk University, Global hall 413, Konkuk University, 1 Hwayang-dong, Gwangin-gu, Seoul, South Korea Dr. Sudalai Kumar S Francis Xavier Engineering College, Vannarpet Tirunelveli, Tamil Nadu, India Dr. Suryya K Rana Dungarpur College of Engineering & Technology, Dungarpur, Rajasthan, India Dr. Tanveer Alam University of Nizwa, Birkat Al Mouz, Nizwa, Sultanate of Oman, Oman Dr. V. Christopher Department of Organic Chemistry, Andhra University, Visakhapatnam, India Dr. Vajjiravel Murugesan Department of Chemistry, B. S. Abdur Rahman University, Vandalur, Chennai, Tamil Nadu, India Prof. Velluru Sridevi Department of Chemical Engineering, A. U. College of Engineering, Andhra University, Visakhapatnam, Andhra Pradesh, India Dr. Wilson Mbiti Njue Department of Chemistry, Kenyatta University, Nairobi Kenya, Kenya
  • 8. 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 synthesis and chemical reactions issues, from theoretical aspects to application-dependent studiesand thevalidationofemergingtechnologies. This new journal was planned and established to represent the growing needs of Chemical Synthesis Reactions as an emerging and increasingly vital field, now widely recognized as an integral part of scientific and technical investigations. Its mission is to become a voice of the chemical synthesis reactions Science community,addressing researchersandpractitionersinthisarea. The core vision of International Journal of Chemical Synthesis and Chemical Reactions in Journals Pub is to propagate novel awareness and know-how for the profit of mankind ranging from the academic and professional research societies to industry practitioners in a range of topics in chemical reactions in general. Journals Pub acts as a pathfinder for the scientific community to published their papers at excellently,well-time&successfully. International Journal of Chemical Synthesis and Chemical Reactions focuses on original high-quality research in the realm of Electrosynthesis, Methods in organic synthesis, Peptide synthesis, Reaction mechanism,Kineticanalysis,Combustion, andmanymore. The Journal is intended as a forum for practitioners and researchers to share the techniques of chemical synthesisreactionsand solutionsinthearea. Many scientists and researchers have contributed to the creation and the success of the chemical synthesis reactions community. We are very thankful to everybody within that community who supported the idea of creating an innovative platform. We are certain that this issue will be followed by many others, reporting newdevelopmentsinthefieldofchemicalsynthesisreactions. This issue would not have been possible without the great support of the Editorial Board members, and we would like to express our sincere thanks to all of them. We would also like to express our gratitude to the editorialstaffofJournalsPub,who supported us ateverystageoftheproject. It is our hope that this fine collection of articles will be a valuable resource for chemistry readers and will stimulatefurtherresearchintothevibrantareaofchemicalsynthesisandreactions. PuneetMehrotra ManagingDirector
  • 9. 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 K Dhirendra Kumar Sharma 12 4. Preparation and Characterization of Ce-Si-SBA-15 Modified With Iron K.J. Rose Philo, M.A. Rahana, S. Sugunan 17 5. Studies on Zirconium(IV) Telluroiodate: A New Heteropolyacid Based Inorganic Ion Exchange Material Premvir Singh 26 Contents
  • 10. 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. Wakchaure2* 1 Research Centre, Department of Chemistry, HPT Arts and RYK Science College, Nashik, India 2 Department 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 cm1 . Parent chloro-sodalite and its cadmium derivative shows cubic symmetry in a space group P43n. 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
  • 11. 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. Kodimunthiri1 1 Department of Science and Humanities, Francis Xavier Engineering College, SCAD Group of Institutions, Tirunelveli, Tamil Nadu, India 2 School 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
  • 12. 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
  • 13. 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. Rahana1 , S. Sugunan2 1 Department of Chemistry, St. Paul’s College, Kalamassery, India 2 Department 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
  • 14. - 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
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