Indian Journal of Chemistry

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

http://www.niscair.res.in; http://nopr.niscair.res.in

Total visitors: 292 since 13-04-2017

CODEN: ICACEC; ISSN: 0376-4710 (Print), 0975-0975 (Online)

 

 

 

 

VOLUME 56A

NUMBER 4

APRIL 2017

 

CONTENTS

 

 

365

 

Graphene oxide-supported gold nanocomposites for highly sensitive sandwich immunosensor for α-fetoprotein detection

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Pengjun Li, Juanhua Lai & Ping Qiu*

 

 

 

A graphene oxide-Au NPs sensor platform combined with a multiple-enzyme labeled antibody-carbon sphere bioconjugate as the basis for an ultrasensitive electrochemical immunosensor for detection of the cancer biomarker, α-fetoprotein, is described. After a sandwich immunoreaction, the Ab2-HRP-Au-PDA-carbon sphere captured onto the electrode surface produces an amplified electrocatalytic response due to the reduction of the enzymatically oxidized thionine in presence of hydrogen peroxide. The increase in response current is proportional to the AFP concentration in the range of 0.01-20 ng/mL with a detection limit of 3 pg/mL.

 

 

 

 

373

 

Microwave assisted transesterification of waste cooking oil over modified forms of zirconia coated on honeycomb monolith

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

V T Vasantha, S Z Mohamed Shamshuddin *,
Reena Saritha Serrao & Joyce Queeny D’Souza

 

 

 

Biodiesel has been effectively synthesized from waste cooking oil over honeycomb coated with modified form of zirconia such as MgO/ZrO2 via microwave-assisted transesterification.

 

 

 

 

379

 

Catalytic activity of niobia supported graphene oxide for esterification of oleic acid

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

S Kanimozhi, A Pandurangan* & P Hemalatha

 

 

 

Niobia loaded GO has been used as catalyst for esterification of oleic acid. In this reaction, 96.4% of methyl oleate is obtained under the reaction conditions of 150 °C for 4 h reaction time. This novel niobia loaded GO as heterogeneous catalyst shows excellent catalytic activity and reusability in esterification of oleic acid.

 

 

 

Notes

 

387

 

On the syntheses and structures of two calcium coordination polymers containing terminal amide ligands

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Bikshandarkoil R Srinivasan* & Kiran T Dhavskar

 

 

 

The syntheses and crystal structures of two calcium coordination polymers, viz., [Ca(NMF)2(4-nba)2] (4-nba = 4-nitrobenzoate;
NMF = N-methylformamide) and [Ca(BA)2(4-nba)2] (BA =  benzamide) are reported. A unique μ2-
h1: h1 bridging bidentate
4-nba ligand links the hexacoordinated Ca(II) ions situated on a special position in both compounds into a one-dimensional chain with Ca···Ca separations of 5.561 and 5.482 respectively.

 

 

 

 

393

 

One pot non-emulsion based hydrothermal synthesis of urchin-shaped hydroxy sodalite using waste coal fly ash

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Rituparna Das, Subhajit Aich & Milan Kanti Naskar*

 

 

 

Urchin-shaped hydroxy sodalite particles are synthesized by one pot non-emulsion based hydrothermal conversion of coal fly ash at
100 °C for 96 h in the absence of any surfactants. BET surface areas of the particles are found to be 193, 197, 82 and 44 m2 g-1 for the reaction time of 24 h, 48 h, 72 h and 96 h, respectively. FESEM images reveal that the thread-ball-like particles are converted into urchin-shaped hydroxy sodalite on increasing reaction time from 24 h to 96 h at 100 °C. EDX analysis indicates Si/Al and Na/Al ratios of 1.28 and 1.03, respectively, which are close to the stoichiometric composition of hydroxy sodalite.

 

 

 

 

399

 

Solubility and transfer Gibbs free energetics of glycine, DL-alanine, DL-nor-valine and DL-serine in aqueous sodium fluoride and potassium fluoride solutions at 298.15 K

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Sanjay Roy*, Partha Sarathi Guin, Kalachand Mahali & Bijoy Krishna Dolui*

 

 

 

The amino acids, glycine, DL-alanine, DL-nor-valine and
DL-serine, show salting-in effect in aqueous-KF, whereas in aqueous NaF solutions, only glycine and DL-serine show salting-in effect. DL-serine shows the highest stability in both KF and NaF solutions. The values of Gibbs free energy due to
acid-base, hydrogen bonding, and dispersion types of interactions show that all the amino acids are more stable in aqueous KF rather than in aqueous NaF solutions. K+ imparts stronger dispersion interaction as compared to Na+ to stabilise larger amino acids.

 

Fig. 2.TIF

 

 

 

407

 

Effect of hydroxyl alkyl amines on the solubility behavior of calcium sulphate dihydrate (gypsum) in the aqueous sodium chloride system at 35 °C

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Jignesh Shukla & Arvind Kumar*

 

 

 

Addition of hydroxyl alkyl amines (ethanolamine, diethanolamine and triethanolamine) at 35 °C alters the solubility of CaSO4·2H2O in NaCl solutions significantly. At any equal concentration of hydroxyl alkyl amines in the solution, the order of CaSO4·2H2O solubility enhancement is: EA < DEA < TEA. The addition of hydroxyl alkyl amines shifts the solubility maximum of CaSO4·2H2O towards higher concentration of NaCl in solution.

 

IJCA-1348_GA.tif

 

 

 

Authors for correspondence are indicated by (*)

 

 

 

 

 


Now Subscription

Payment Made Easy

 

Indian Journal of Chemistry, Sec A Subscribers

You can now pay through

ECS /NEFT /RTGS

 

Following are the details:

 

Bank Name: SYNDICATE BANK

Address: PUSA CAMPUS, IARI, NEW DELHI 110 012

Branch: PUSA CAMPUS, IARI, NEW DELHI

A/C No.: 90292160000079

A/C Name: NISCAIR, NEW DELHI 110 012

IFSC Code: SYNB0009029

MICR Code: 110025041

Branch Code: 9029

SWIFT Code: SYNBINBB019

 

Please send UTR no. with full postal address by e-mail

after payment through ECS/NEFT/RTGS to:

sales@niscair.res.in

 

Indian Journal of Chemistry

Vol. 56A, April 2017, pp. 365-372

 

 

Graphene oxide-supported gold nanocomposites for highly sensitive sandwich immunosensor for α-fetoprotein detection

Pengjun Lia, Juanhua Laib & Ping Qiua, *

aDepartment of Chemistry, Nanchang University, Nanchang 330031, China

Email: pingqiu@ncu.edu.cn

bJiangxi medical device testing center, Nanchang 330047, China

Received 18 September 2016; revised and accepted 14 March 2017

A graphene oxide-Au NPs sensor platform combined with a multiple-enzyme labeled detection antibody-carbon sphere bioconjugate has been used as the basis for an ultrasensitive electrochemical immunosensor to detect the cancer biomarker, α-fetoprotein (AFP). Greatly enhanced sensitivity has been achieved by using the bioconjugates featuring horseradish peroxidase (HRP) and Ab2 linked to carbon nanospheres (Ab2-HRP-Au-PDA-carbon sphere) at a high ratio of HRP/Ab2. After a sandwich immunoreaction, the Ab2-HRP-Au-PDA-carbon sphere captured onto the electrode surface produces an amplified electrocatalytic response due to the reduction of enzymatically oxidized thionine in the presence of hydrogen peroxide. The increase of response current is proportional to the AFP concentration in the range of 0.01-20 ng/mL, with the detection limit of
3 pg/mL. This amplification strategy is a promising platform for detection of other proteins and clinical applications.

Keywords: Nanocomposites, Immunosensors, Gold nanoparticles, Sandwich immunosensors, Graphene oxide,
α-Fetoprotein

 

Indian Journal of Chemistry

Vol. 56A, April 2017, pp. 373-378

 

 

Microwave assisted transesterification of waste cooking oil over
modified forms of zirconia coated on honeycomb monolith

V T Vasanthaa, c, S Z Mohamed Shamshuddina, c, *, Reena Saritha Serraoa & Joyce Queeny D’Souzab, c

aChemistry Research Laboratory, HMS Institute of Technology, NH4, Kyathasandra, Tumakuru, Karnataka, India

bDepartment of Chemistry, St. Joseph’s College, Langford Road, Bengaluru, Karnataka, India

cRegional Research Center, Visweswaraya Technological University, Bengaluru Region, Belagavi, Karnataka, India

Email: mohamed.shamshuddin@gmail.com

Received 16 January 2017; revised and accepted 28 March 2017

Microwave assisted transesterification of waste cooking oil over honeycomb monoliths coated with zirconia based catalysts such as MgO/ZrO2 and CaO/ZrO2 to synthesize biodiesel is reported. For comparison, biodiesel synthesis via transesterification using conventional heating method has also been carried out. The solid acid Al2O3/ZrO2 coated on a honeycomb has also been used as a catalyst to reduce the percentage of free fatty acid in waste cooking oil via esterification using conventional heating. The honeycomb monoliths have been coated with solid bases and characterized for their physico-chemical properties such as surface acidity, surface basicity, crystalinity and morphology using suitable techniques. The honeycomb monoliths coated with solid catalysts are found to be highly efficient and reusable in the process of synthesizing biodiesel from waste cooking oil. A maximum yield of biodiesel (98%) is obtained at 60 °C in 10 min by keeping the molar ratio of oil:methanol ratio at 1:6 under microwave irradiation.

Keywords: Catalysts, Modified catalysts, Biodiesel synthesis, Transesterification, Microwave, Waste cooking oil, Honeycomb monoliths, Zirconia catalysts, MgO/ZrO2, CaO/ZrO2

 

 

 

Indian Journal of Chemistry

Vol. 56A, April 2017, pp. 379-386

 

 

Catalytic activity of niobia supported graphene oxide for
esterification of oleic acid

S Kanimozhi, A Pandurangan* & P Hemalatha

Department of Chemistry, Anna University, Chennai-600 025, India,

Email: pandurangan_a@yahoo.com

Received 29 September 2016; revised and accepted 21 March 2017

Biodiesel has been obtained from esterification of oleic acid with methanol using niobia loaded graphene oxide (GO). Different weight percentages of niobia (1, 3, 5 and 7 wt.%) have been loaded on GO by the wet impregnation method. The synthesized materials have been characterized by XRD, FT-IR, Raman spectroscopy, TGA, BET surface area, NH3-TPD, ICP-OES, SEM and HR-TEM studies. The catalytic activity of niobia supported on GO has been tested for esterification of oleic acid with methanol for biodiesel production. The maximum yield of methyl oleate (96.4%) is obtained at the reaction conditions of 150 °C, 0.5 g of 5 wt% of niobia on GO catalyst, 1:9 molar ratio of oleic acid:methanol and time 4 h. Influence of solvents (ethanol, propanol, butanol) has been tested for comparative study with same reaction conditions. Based on the catalytic studies, niobia supported GO has good catalytic activity for esterification of oleic acid reaction with good reusability.

Keywords: Catalysts, Graphene oxide, Niobia loaded GO, Esterification, Methyl oleate, Biodiesel

 

Indian Journal of Chemistry

Vol. 56A, April 2017, pp. 387-393

 

 

On the syntheses and structures of two calcium coordination polymers
containing terminal amide ligands

Bikshandarkoil R Srinivasan* & Kiran T Dhavskar

Department of Chemistry, Goa University, Goa 403 206, India

Email: srini@unigoa.ac.in

Received 20 December 2016; accepted 20 March 2017

The syntheses and crystal structure of the calcium coordination polymers [Ca(NMF)2(4-nba)2] 1 (4-nba =
4-nitrobenzoate; NMF=N-methylformamide) and [Ca(BA)2(4-nba)2] 2 (BA= benzamide) is reported. A unique μ2-
h1: h1 bridging bidentate 4-nba ligand links the hexacoordinated Ca(II) ions situated on a special position in both compounds into a one-dimensional (1-D) chain with Ca···Ca separations of 5.561 and 5.482 respectively. Each Ca(II) in the chain is bonded to a pair of symmetry related terminal amide ligands (NMF in 1; BA in 2) which are disposed trans to each other. A comparative study of several 4-nitrobenzoates of calcium is described.

Keywords: Coordination chemistry, Coordination polymers, Calcium, 4-Nitrobenzoate, Methylformamide, Benzamide

 

Indian Journal of Chemistry

Vol. 56A, April 2017, pp. 394-398

 

 

One pot non-emulsion based hydrothermal synthesis of urchin-shaped hydroxy sodalite using waste coal fly ash

Rituparna Das, Subhajit Aich & Milan Kanti Naskar*

Sol-Gel Division, CSIR-Central Glass & Ceramic Research Institute, Kolkata 700 032, India

Email: milan@cgcri.res.in

Received 15 February 2017; revised and accepted 23 March 2017

Urchin-shaped hydroxy sodalite particles have been synthesized by one pot non-emulsion based hydrothermal conversion of coal fly ash at 100 °C for 96 h in the absence of any surfactants. Crystallization behavior of the particles has been studied by X-ray diffraction, and the characteristic vibration bands of hydroxy sodalite were confirmed by FTIR spectroscopy. BET surface area of the particles are found to be 193, 197, 82 and 44 m2 g-1 for the reaction time of 24 h, 48 h, 72 h and 96 h, respectively. FESEM images revealed that the
thread-ball-like particles are converted into urchin-shaped hydroxy sodalite with increasing reaction time from 24 h to 96 h at 100 °C. The elemental analysis of the product studied by EDX indicates the Si/Al and Na/Al ratios of 1.28 and 1.03, respectively which is close to the stoichiometric composition of hydroxy sodalite.

Keywords: Hydrothermal synthesis, Aluminosilicates, Sodalite, Hydroxy sodalite, Fly ash, Coal fly ash, Crystallization

 

Indian Journal of Chemistry

Vol. 56A, April 2017, pp. 399-406

 

 

Solubility and transfer Gibbs free energetics of glycine, DL-alanine,
DL-nor-valine and DL-serine in aqueous sodium fluoride
and potassium fluoride solutions at 298.15 K

Sanjay Roya, *, Partha Sarathi Guina, Kalachand Mahalib & Bijoy Krishna Doluic, *

aDepartment of Chemistry, Shibpur Dinobundhoo Institution (College), Howrah, 711102, West Bengal, India

Email: sanjayroyp@gmail.com

bDepartment of Chemistry, University of Kalyani, Nadia, 741235, West Bengal, India

cDepartment of Chemistry, Visva-Bharati, Santiniketan, Birbhum, 731235, West Bengal, India

Email: bijoy_dolui@yahoo.co.in

Received 14 September 2016; re-revised and accepted 14 March 2017

The experimental saturated solubilities of glycine, DL-alanine, DL-nor-valine and DL-serine in aqueous mixtures of NaF and KF solutions at 298.15 K are measured by using an analytical ‘formol titrimetry’ method. Subsequently, the standard transfer Gibbs free energy, enthalpy for cavity formation, Gibbs free energy for cavity formation and Gibbs free energy for dipole-dipole interaction have been computed. The chemical contribution for the standard transfer Gibbs free energies for the experimental amino acids have been obtained by subtracting the cavity effects and dipole-dipole interaction effects from the total standard transfer Gibbs free energy (  (i)). The stability of the studied amino acids in aqueous NaF and KF in terms of thermodynamic parameters are discussed and compared.

Keywords: Solution chemistry, Thermodynamics, Solubility, Amino acids, Electrolytes, Transfer energetics, Formol titrimetry

 

Indian Journal of Chemistry

Vol. 56A, April 2017, pp. 407-413

 

 

Effect of hydroxyl alkyl amines on the solubility behavior of
c
alcium sulphate dihydrate (gypsum) in the aqueous sodium
chloride system at 35 °C

Jignesh Shukla & Arvind Kumar*

Salt and Marine Chemicals Division, CSIR-Central Salt and Marine Chemicals Research Institute,
Council of Scientific and Industrial Research, GB Marg, Bhavnagar 364 002, India

Email: arvind@csmcri.org

Received 28 December 2016; revised and accepted 31 March 2017

 

The solubility behavior of calcium sulphate dihydrate (gypsum, CaSO4·2H2O) in aqueous NaCl solutions upon addition of hydroxyl alkyl amines, such as, ethanolamine (EA), diethanolamine (DEA), or triethanolamine (TEA) at 35 °C is reported.  The addition of hydroxyl alkyl amines alters the solubility of CaSO4·2H2O in NaCl solutions significantly. At any equal concentration of hydroxyl alkyl amines in the solution, the order of CaSO4·2H2O solubility enhancement is found to be: EA < DEA < TEA. A three-fold increase in CaSO4·2H2O solubility maximum is observed in the solutions containing 15 wt% TEA. The addition of hydroxyl alkyl amines shifts the solubility maximum of CaSO4·2H2O towards higher concentration of NaCl in solution. Solution properties such as density (ρ) and speed of sound (u) data have been measured for the quaternary systems (CaSO4·2H2O+NaCl+hydroxyl alkyl amines+H2O). All the measurements have been carried out at 35 °C under atmospheric pressure. Solution isentropic compressibility (κS) values have been derived from u and ρ  data. Solubility, density, speed of sound, and isentropic compressibility data have been fitted with suitable polynomial equations in these systems.

 

Keywords: Solution chemistry, Solubility, Density, Compressibility, Calcium sulphate, Gypsum,
H
ydroxyl alkyl amines