Indian Journal of Chemistry

Sect. A: Inorganic, Bio-inorganic, Physical, Theoretical & Analytical

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VOLUME 51A

NUMBER 6

JUNE 2012

 

CONTENTS

 

 

791

 

Catalytic performance of acidic ionic liquid in esterification of benzyl alcohol with butyric acid

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Xiaodan Wu, Xiaoxiang Han, Lingxiao Zhou &
Ang Li
*

 

 

 

Synthesis of benzyl butyrate is optimized by response surface methodology using SO3H-functionalized Brønsted acidic ionic liquids as catalysts. A Box-Behnken model has been applied
to obtain the optimal conditions (R2 = 0.9907). Under the optimized conditions, the yield of benzyl butyrate reaches 99.4 %.
[HSO3-pmim]HSO4 shows high stability and catalytic activity for the esterification.

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

800

 

Novel Fe encapsulated montmorillonite K10 clay for photo-Fenton mineralization of Acid Yellow 17

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

I Muthuvel, B Krishnakumar & M Swaminathan*

 

 

 

Solid hetero-Fenton catalyst with 26 % ferric nitrate loading
is found to be most efficient in the degradation of Acid Yellow 17.  While its activity is significant up to pH 7, the catalyst exhibits the best photocatalytic activity at pH 3.

 

 

 

Notes

 
807

 

CdO and CdS nanoparticles from pyrolytic method: Preparation, characterization and photocatalytic activity

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Sandip Mondal, Tanmay Chattopadhyay*,
Sudhanshu Das, Sankar Roy Maulik, Swarup Neogi &
Debasis Das

 

 

 

 

 

 

 

 

 

 

812

 

Intercalation of biologically important iminodiacetato-chromium(III) ion in the interlayer of ZnAl-layered double hydroxide

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

R Sahu, B S Mohanta & N N Das*

 

 

 

Intercalation of the biologically important bis-iminodiacetato-chromium(III) ion, [Cr(ida)2]¯, in the interlayer of ZnAl-layered double hydroxide through rehydration of ZnAl(O) mixed oxide, and, its characterization by XRD, TG-DTA, FT-IR and
UV-vis-DRS is described.

 

 

 

 

816


2,7-Diferrocenyl-3,6-diazaocta-2,6-diene: A highly selective dual fluorescent sensor for Zn2+ and Ag+ and electrochemical sensor for Zn2+

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Kaku Dutta & Diganta Kumar Das*

 

 

 

2,7-Diferrocenyl-3,6-diazaocta-2,6-diene acts as a fluorescent sensor for Zn2+ ion by “switch on” mode and as a fluorescent sensor for Ag+ by “switch off” mode.

 

 

 

 

 

821


Microwave synthesis of polymer coated silver nanoparticles by glucose as reducing agent

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Jolly Pal & Manas Kanti Deb*

 

 

 

Silver nanoparticles (~ 11 nm) are prepared by a simple method employing silver nitrate as precursor, glucose as reducing agent and PVP as stabilizing agent.

 

 

 

30 nm

 

 

 

 

825


Cold induced aggregation microextraction with an ionic liquid for trace determination of cadmium and lead in water samples

 

 

 

 

 

 

 

 

 

 

 

 

 

Mojtaba Shamsipur*, Majid Ramezani,
Ali Akbar Miran Beigi & Tahereh Poursaberi

 

 

 

Cold induced aggregation microextraction with an ionic liquid, [C6MIM][PF6], is used as a rapid and simple method for determination of trace amounts of cadmium and lead by sequential analysis with flame atomic absorption spectroscopy.

 

 

 

 

 

 

 

830

 

Announcement

Electronic supplementary data

 

 

 

 

 

Authors for correspondence are indicated by (*)

 

 

 

 

 

Indian Journal of Chemistry

Vol. 51A, June 2012, pp. 791-799

 

Catalytic performance of acidic ionic liquid in esterification of benzyl alcohol with butyric acid

Xiaodan Wu, Xiaoxiang Han, Lingxiao Zhou & Ang Li*

Department of Applied Chemistry, Food Science & Biotechnology Engineering,
Zhejiang Gongshang University, Hangzhou, 310035, PR China

Email: hxx74@126.com/ liang7422@163.com

Received 22 December 2011; revised and accepted 17 May 2012

Response surface methodology is successfully applied to optimize esterification of benzyl alcohol with butyric acid by an ionic liquid viz., [HSO3-pmim]HSO4. The effects of various reaction conditions, including reaction time, alcohol/acid molar ratio, the amount of water carrying agent and ionic liquid are investigated. A Box–Behnken experimental design has been employed to search for the optimal yield of benzyl butyrate. The analysis confirms that the relationship between the amount of water carrying agent and the amount of ionic liquid is the most significant parameters affecting the yield of benzyl butyrate. The coefficient of determination of this model is 0.9907. The optimum reaction conditions are established and verified experimental trial performed for validating the obtained results. Under the optimum conditions, the yield of benzyl butyrate reaches 99.4 %. The ionic liquid could be reused five times without noticeable drop in activity.

Keywords: Ionic liquids, Esterification, Benzyl butyrate, Response surface methodology, Brønsted acidity

 

Indian Journal of Chemistry

Vol. 51A, June 2012, pp. 800-806

 

Novel Fe encapsulated montmorillonite K10 clay for photo-Fenton mineralization of Acid Yellow 17

I Muthuvel, B Krishnakumar & M Swaminathan*

Department of Chemistry, Annamalai University, Annamalainagar 608 002, India

Email: chemres50@gmail.com

Received 1 January 2012; revised and accepted 7 May 2012

A novel Fe encapsulated montmorillonite K10 clay has been prepared by solid state dispersion method and characterized by FT-IR, SEM-EDS, ICP-AES and BET surface area measurements. XRD analysis suggests that iron in the catalyst exists as FeOOH. ICP-AES analysis shows increase in Fe(III) concentration from 35 to 457 ppm on immobilization of Fe on montmorillonite K10 clay. EDS analysis of SEM images also confirm the presence of Fe in the catalyst. The catalyst has been applied for photodegradation of Acid Yellow 17 in the presence of H2O2 under UV light. Effect of pH on mineralization of the dye has been studied in detail. The initial pH influences not only the photocatalytic activity of the catalyst but also the Fe leaching from the catalyst. Unlike homo-Fenton catalysts, the proposed catalyst exhibits good activity and stability even at neutral pH 7 (75 % at 60 min irradiation). Further, lowest leaching of Fe(III) at pH 7 makes the catalyst suitable for dye wastewater treatment at neutral pH.

Keywords: Photochemistry, Photodegradation, Photocatalysts, Dye degradation, Hetero-Fenton degradation, Azo dyes, Acid Yellow 17, Montmorillonite K10 clay, Wastewater treatment

 

Indian Journal of Chemistry

Vol. 51A, June 2012, pp. 807-811

 

CdO and CdS nanoparticles from pyrolytic method: Preparation, characterization and photocatalytic activity

Sandip Mondala, Tanmay Chattopadhyayb, *, Sudhanshu Dasa, Sankar Roy Maulikc, Swarup Neogid
&
Debasis Dasa, *

aDepartment of Chemistry, University of Calcutta, Kolkata 700 009, India

Email: dasdebasis2001@yahoo.com

bDepartment of Chemistry, Panchakot Mahavidyalya, Sarbari, Purulia 723 121, India
Email: tanmayc2003@gmail.com.

cDepartment of Silpa Sadana, Visva-Bharati University, Sriniketan, 731 236, India

dDepartment of Physics, University of Calcutta, Kolkata, 700 009, India

Received 29 November 2011; revised and accepted 26 April 2012

CdO and CdS nanocrystals have been prepared via simple thermal treatment of coordination polymers, viz., [Cd(dca)2(Mim)2]n and [Cd(SCN)2(Bim)2]n (where Bim and Mim are benzimidazole and
1-methylimidazole respectively) as
precursors at 600–650 °C in air for 2 h. A variety of techniques like infrared spectroscopy, X-ray diffraction, scanning electron microscopy and thermal gravimetric analysis have been employed to carry out structural characterization of these nanoparticles. The optical band gap of these materials, estimated to be about 2.43 and 2.50 eV respectively, establish a relationship between energy band gap of bulk and nanomaterials. Photocatalytic reactivity of these nanomaterials are evaluated by studying the degradation of C. I. Reactive Yellow 84, a popular and widely used reactive dye in cotton industry.

Keywords: Coordination polymers, Nanoparticles, Semiconductors, Photocatalytic activity, Pyrolytic technique, Cadmium oxide, Cadmium sulphide

 

Indian Journal of Chemistry

Vol. 51A, June 2012, pp. 812-815

 

Intercalation of biologically important iminodiacetatochromium(III) ion in the interlayer of ZnAl-layered double hydroxide

R Sahu, B S Mohanta & N N Das*

PG Department of Chemistry, North Orissa University, Baripada 757 003, Orissa, India

Email: dasnn64@rediffmail.com

Received 19 January 2012; revised and accepted 22 May 2012

The intercalation of bis-iminodiacetatochromium(III) ion, [Cr(ida)2]-, in the interlayer of ZnAl-layered double hydroxide (LDH) through rehydration of ZnAl(O) mixed oxide and its characterization by XRD, TG-DTA, FT-IR and UV-vis-DRS is described. X-ray diffraction studies reveal the increase of basal spacing in the ZnAl-LDH–Cr(ida) hybrid from 7.69 Å to 12.55 Å due to intercalation of [Cr(ida)2]-, which is also evident from FT-IR and UV-vis-DR spectra. Thermogravimetric analyses show a marginal increase in the decomposition temperature for the [Cr(ida)2]- moiety with exothermic peaks in the LDH–Cr(ida) hybrid, indicating enhanced thermal stability of the [Cr(ida)2]- ion in the LDH interlayer. This method may be useful for intercalation of other anionic Cr(III) complexes of biological importance.

Keywords: Intercalation, Layered double hydroxides, Layered double hydroxide hybrids, Chromium, Iminodiacetate

 

Indian Journal of Chemistry

Vol. 51A, June 2012, pp. 816-820

 

2,7-Diferrocenyl-3,6-diazaocta-2,6-diene: A highly selective dual fluorescent sensor for Zn2+ and Ag+ and electrochemical sensor for Zn2+

Kaku Dutta & Diganta Kumar Das*

Department of Chemistry

Gauhati University, Guwahati 781 014, Assam, India

Email: digantakdas@gmail.com

Received 23 May 2011; revised and accepted 15 May 2012

2,7-Diferrocenyl-3,6-diazaocta-2,6-diene (DFDD), obtained by condensation reaction of acetylferrocene and ethylenediamine, exhibits Zn2+ ion-induced enhancement of fluorescence intensity and Ag+ ion-induced quenching of fluorescence intensity. The Zn2+ ion shifts the redox potential of DFDD from +0.660 V ± 0.005 V to + 0.615 ± 0.005 V as observed by cyclic voltammetry and square wave voltammetry. Ca2+, Mg2+, Mn2+, Fe2+, Co2+, Ni2+, Cu2+, Cd2+, Pb2+ and Hg2+ have very little effect on fluorescence intensity of DFDD. These metal ions together with Ag+ ion have no effect on the electrochemistry of DFDD. Both, fluorescence and UV-visible spectroscopic data show a 1:1 interaction between DFDD and Zn2+ with binding constant 75 M -1. The applicability of DFDD as fluorescence sensor for Zn2+ ion has been shown in its estimation in commercial tablets.

Keywords: Sensors, Electrochemical  sensors,  Fluorescent sensors, Fluorescence, Cyclic voltammetry, Square wave voltammetry, Zinc, Silver

 

Indian Journal of Chemistry

Vol. 51, June 2012, pp. 821-824


Microwave synthesis of polymer coated silver nanoparticles by glucose as reducing agent

Jolly Pal & Manas Kanti Deb*

School of Studies in Chemistry, Pt. Ravishankar Shukla University, Raipur 492 010, Chhattisgarh, India

Email: debmanas@yahoo.com

Received 22 August 2011; revised and accepted 21 May 2012

Silver nanoparticles have been prepared by the reduction of silver nitrate using glucose as reducing agent and polyvinylpyrrolidone as stabilizing agent and characterized by transmission electron microscopy and UV-visible spectroscopy. TEM images show the average size of silver nanoparticles to be 11 nm. Various optimizing parameters such as effects of silver nitrate concentration, glucose concentration and microwave irradiation time are also described.

Keywords: Silver nanoparticles, Microwave synthesis, Glucose, Nanoparticles, Polyvinylpyrrolidone, Polymer coated nanoparticles

 

Indian Journal of Chemistry

Vol. 51A, June 2012, pp. 825-829

 

Cold induced aggregation microextraction with an ionic liquid for trace determination of cadmium and lead in water samples

Mojtaba Shamsipura, *, Majid Ramezanib, Ali Akbar Miran Beigic & Tahereh Poursaberid

aDepartment of Chemistry, Razi University, Kermanshah, Iran

Email: mshamsipur@yahoo.com

b Department of Chemistry, Faculty of Science, Islamic Azad University –Arak branch, Arak, Iran

c Oil Refining Research Division, Research Institute of Petroleum Industry, Tehran, Iran

dInstrumental Analyses Department, Research Institute of Petroleum Industry, Tehran, Iran

Received 7 March 2012; revised and accepted 28 May 2012

Cold induced aggregation microextraction (CIAME) with an ionic liquid has been used as a rapid and simple method for determination of trace amounts of cadmium and lead by sequential analysis with flame atomic absorption spectrometry. In this study, cadmium and lead have been complexed with
O, O-diethyldithiophosphate as chelating agent in a solution containing Triton X-114 and sodium hexafluorophosphate
, and then extracted into an ionic liquid. The effect of various parameters on extraction efficiency such as amounts of [C6MIM][PF6] and NaPF6, pH of solution, extraction time, temperature and complexing agent concentration have been optimized. Under the optimized conditions, the detection limits are 0.12 µg L-1 and 1.61µg L-1, relative standard deviation 2.4 % and 2.7 % and enrichment factor 70 and 67 for cadmium and lead, respectively. The proposed method has been successfully applied for analysis of cadmium and lead in certified reference material and various water samples.

Keywords: Analytical chemistry, Extraction, Microextraction, Cold induced aggregation microextraction, Flame atomic absorption spectrometry, Ionic liquids, Imidazolium ionic liquids, Hexafluorophosphates, Cadmium, Lead, Water analysis