Indian Journal of Chemical Technology

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VOLUME 16

NUMBER 2

MARCH 2009

CODEN : ICHTEU

 

ISSN : 0971-457X

 

CONTENTS    

Papers

 

 

Aerial oxidation of coal- analytical methods, instrumental technique and test

103

methods: A survey

 

            Raja Sen, Sunil K Srivastava & Madan Mohan Singh

 

 

 

Arsenic(III) removal from aqueous solutions by mixed adsorbent

136

            A P Singh, K K Srivastava & H Sekhar

 

 

 

Jackfruit (Artocarpus heterophyllus) leaf powder: An effective adsorbent for removal of methylene blue from aqueous solutions

142

            Md. Tamez Uddin , Md. Rukanuzzaman , Md. Maksudur Rahman Khan &

 

            Md. Akhtarul Islam

 

 

 

Synergic extraction of copper with N- phenylbenzohydroxamic acid and

150

tri-n-octyl phosphinoxide or tributylphosphate

 

            N Dallali , J Ghiasi & Y K Agrawal

 

 

 

Effectiveness of thermoil granodine against the corrosion of aluminium and

155

Al-Cu alloy in chloride solutions

 

            B V Ram Kumar, G V S Sarma , C Bhaskara Sarma & G M J Raju

 

 

 

Corrosion inhibition of mild steel in acid media by quinolinyl thiopropano

162

hydrazone

 

            Ramesh Saliyan V & Airody Vasudeva Adhikari

 

 

 

Effect of calcination temperature of TiO2-Al2O3 mixed oxides on hydride-

175

sulphurization performance of Au-Pd catalysts

 

            Zhonghua Gu, Laitao Luo & Sufen Chen

 

 

 

Comparative study on hydrogen peroxide bleaching of soda-organosolv and

181

kraft rice straw pulps

 

            Y Ziaie-shirkolaee

 

 

 

Notes

 

 

 

[Cu(NH3)4]2+SnP as a catalyst

188

            Chithra P G, Nisha J Tharayil & Beena B

 

 

 

Utilization of aleuritic acid free gummy mass- an industrial by-product for

192

making particle board

 

            K P Sao & S K Pandey

 

 

 

Free radical cross-linking copolymerization of acrylamide and N, N’ methylene- bis-

196

acrylamide by using Fe(III)/ thiourea and Ce(IV)/ thiourea redox initiator systems

 

            Bidyut Debnath, Goutam Bit & Swapan K Saha

 

 

 

Author Index

201

 

 

Keyword Index

202

 

 

Guidelines for Authors

203

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 16, March 2009, pp. 103-135

 

 

Aerial oxidation of coal-analytical methods, instrumental techniques and test methods: A survey

Raja Sen, Sunil K Srivastava* & Madan Mohan Singha

Central Institute of Mining & Fuel Research, Digwadih Campus, P.O.- F.R.I., Dhanbad 828108, India

aDepartment of Applied Chemistry, Institute of Technology, Banaras Hindu University, Varanasi 221005, India

Email: sukusri1@rediffmail.com

 

Aerial oxidation of coal particularly atmospheric oxidation of coal is mainly responsible for self heating of coal and deterioration of most of its useful technological properties like calorific value, floatability and caking properties. A lot of work has been done over the years to understand the exact mechanism of the processes responsible for this phenomenon. This literature survey attempts to list and describe various analytical techniques, both chemical and instrumental, standard tests and novel experimental procedures applied by various authors to study the different aspects of this phenomenon.

Keywords: Coal oxidation, Weathering, CPT, FTIR, PyMs, NMR, XPS

 

 

Indian Journal of Chemical Technology

Vol. 16, March 2009, pp. 136-141

 

 

Arsenic (III) removal from aqueous solutions by mixed adsorbent

 

A P Singh, K K Srivastava & H Shekhar*

*Department of Chemistry, VKS University, Ara 802 301, India

Department of Chemical Engineering and Technology, Institute of Technology, Banaras Hindu University,

Varanasi 221 005, India

 

The removal of As(III) from its aqueous solutions by adsorption on homogeneous mixture of china clay and fly ash in equal proportions has been found to be dependent on various operating parameters such as concentration, temperature and pH. The As(III) removal is favourable at low concentration, high temperature and slightly basic condition at pH 8.0. The applicability of Langmuir isotherm in present system suggests the formation of monolayer coverage of As(III) molecules at the outer surface of the adsorbent. Thermodynamic parameters indicate the spontaneous and endothermic nature of the process. Adsorption kinetics studied using the model suggested by Lagergren infers a first order rate expression.

Keywords: As(III) adsorption, Adsorption kinetics, China clay, Fly ash, Langmuir isotherm

 

 

Indian Journal of Chemical Technology

Vol. 16, March 2009, pp. 142-149

 

 

Jackfruit (Artocarpus heterophyllus) leaf powder: An effective adsorbent for removal of methylene blue from aqueous solutions

 

Md. Tamez Uddin, Md. Rukanuzzaman, Md. Maksudur Rahman Khan & Md. Akhtarul Islam

Department of Chemical Engineering and Polymer Science, Shahjalal University of Science and Technology,

Sylhet-3114, Bangladesh

Email: mtuddin_cep@yahoo.com; mtuddin-cep@sust.edu

 

Batch sorption experiments were carried out using jackfruit leaf powder (JLP), for the removal of methylene blue (MB) from aqueous solutions. Effects of process parameters pH, adsorbent mass, concentration and contact time were studied. The amount of MB adsorbed per unit weight of the adsorbent increased with the increase of pH, concentration and contact time. The pH at the point of zero charge (pHPZC) of the adsorbent was found to be 3.9. Adsorption of MB was found highly pH dependent. The FTIR of the adsorbent was done to find the potential adsorption sites for interaction with the cationic MB dye. Equilibrium data were fitted to Langmuir and Freundlich isotherms. The equilibrium data were best represented by both the isotherms. Maximum dye uptake was found to be 326.32 mg/g, indicating that JLP can be used as an excellent low-cost adsorbent for removal of MB dye. From experimental data it was found that adsorption of MB onto JLP followed pseudo second order kinetics. The desorption studies showed that most of the MB can be recovered by decreasing the pH of the solution. The experimental result inferred that electrostatic attraction between the surface and the dye is one of the major adsorption mechanisms for binding MB to JLP surface.

Keywords: Jackfruit leaf powder, Methylene blue, Adsorption, Isotherms, Kinetics

 

 

Indian Journal of Chemical Technology

Vol. 16, March 2009, pp. 150-154

 

 

Synergic extraction of copper with N-phenylbenzohydroxamic acid and
tri-n-octyl phosphinoxide or tributylphosphate

 

N Dallali1, J Ghiasi1 & Y K Agrawal2*

1 Department of Chemistry, Faculty of Sciences, Zanjan University, Zanjan 45195-313, Iran

2 Institute of pharmacy, Nirma University of Science and Technology,
Sarkej-Gandhinagar Highway, Ahmedabad 382 481, India

Email: drykagrawal@yahoo.com

 

The synergic extraction of copper(II) with N-phenylbenzohydroxamic acid (PBHA) and tri-n-octyl phosphinoxide (TOPO) or tributyl phosphate (TBP) was investigated in chloroform. The synergic effect found in presence of neutral ligand is due to the formation of the adduct Cu(PBHA)2S in chloroform (S denotes TOPO or TBP). The synergic coefficients (SC) were determined which have higher value in presence of TOPO than TBP, since TOPO has the higher basicity then TBP.

Keywords:   Copper, Synergic extraction, PBHA, TOPO

 

 

Indian Journal of Chemical Technology

Vol. 16, March 2009, pp. 155-161

 

 

Effectiveness of thermoil granodine against the corrosion of aluminum and Al-Cu alloy in chloride solutions

B V Ram Kumar, G V S Sarma, C Bhaskara Sarma* & G M J Raju

Department of Chemical Engineering, AU College of Engineering (A), Andhra University, Visakhapatnam 530 003, India

Email: bhaskaraidg@yahoo.co.in

 

The corrosion of aluminum and aluminum-copper alloy in 0.1 N NaCl solution has been studied by linear polarization technique. Current-potential data were obtained from which Icorr values and corrosion rates were estimated using Stern-Geary equation and Faraday’s laws. The phosphatizing chemical, thermoil granodine (trade name) was used as the inhibitor to study the effect of inhibitor on the corrosion of Al and 4 % Cu – Al alloy in chloride solutions. The optimum inhibitor concentration for maximum inhibition was determined and the effectiveness of the inhibitor was evaluated. The inhibition efficiency ranged from 40 to 65% for pure aluminum and 70 to 96% for aluminum-copper alloy.

Keywords:  Linear polarization, Current-potential data, Thermoil granodine, Phosphatizing, Corrosion  inhibition

 

 

Indian Journal of Chemical Technology

Vol. 16, March 2009, pp. 162-174

 

 

Corrosion inhibition of mild steel in acid media by quinolinyl thiopropano hydrazone

Ramesh Saliyan V & Airody Vasudeva Adhikari*

Department of Chemistry, National Institute of Technology Karnataka, Surathkal, Mangalore 575 025, India

Email: avchem@nitk.ac.in; avadhikari123@yahoo.co.in

 

3-{[8-(trifluoromethyl)quinolin-4-yl]thio}-N'-(2,3,4-trihydroxybenzylidene)propano hydrazide (TQTHBH) was synthesized, characterized and tested as a corrosion inhibitor for mild steel in HCl and H2SO4 solutions using weight loss method, electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization methods. The corrosion inhibition efficiency results obtained by all the above three techniques were in good agreement with each other. Scanning electron microscopy (SEM) technique is used to confirm the effectiveness of inhibition of mild steel corrosion in acid media. The results showed that TQTHBH is a good inhibitor for mild steel in acid media. The inhibition efficiency of TQTHBH in different media was in the following order: 2 M HCl < 1 M H2SO4 < 1 M HCl < 0.5 M H2SO4. The inhibition was assumed to occur via adsorption of the inhibitor molecule on the metal surface. The adsorption follows Langmuir isotherm. TQTHBH acts as an anodic inhibitor. The protection efficiency increased with increasing inhibitor concentration in the range 0.222 x 10-4 – 11.086 x 10-4 M, also slightly increased with increasing temperature. Chemisorption mechanism is proposed. The apparent activation energies and enthalpies for the adsorption process were determined. The fundamental thermodynamic functions were used to gain information about TQTHBH inhibitory behaviour.

Keywords: Mild steel, Quinoline, Corrosion inhibition, Adsorption, Scanning electron microscopy

 

 

Indian Journal of Chemical Technology

Vol. 16, March 2009, pp. 175-180

 

 

Effect of calcination temperature of TiO2-Al2O3 mixed oxides on hydrodesulphurization performance of Au-Pd catalysts

Zhonghua Gu, Laitao Luo* & Sufen Chen

Institute of Applied Chemistry, Nanchang University, Nanchang 330 031, China

Email: luolaitao@yahoo.com

 

A series of TiO2-Al2O3 mixed oxides calcined at different temperatures was prepared by the sol-gel method. The influence of calcination temperature of TiO2-Al2O3 on Au-Pd catalysts was investigated in the hydrodesulphurization of thiophene. The structural and surface properties of the samples were analyzed by nitrogen adsorption, X-ray diffraction, temperature-programmed desorption, temperature-programmed reduction and infrared spectroscopy techniques. The results showed that the prepared TiO2-Al2O3 mixed oxides had mesoporous structure. The TiO2-Al2O3 mixed oxide calcined at 773 K exhibited larger BET surface area, pore volume and more acid sites than the samples calcined among 873-1073 K. All the Au-Pd catalysts supported TiO2-Al2O3 calcined at different temperature had higher catalytic activity towards the hydrodesulphurization of thiophene, and the catalytic activity of Au-Pd/TiO2-Al2O3 (773 K) was better than that of other samples in hydrodesulphurization reaction. This was explained in terms of their structure: interaction between Au-Pd and TiO2-Al2O3, dispersion, apparent activation energy, the number of AuxPdy alloy particles and acid sites.

Keywords: Calcination effect, Mixed oxides, Au-Pd catalysts, Hydrodesulphurization

 

 

Indian Journal of Chemical Technology

Vol. 16, March 2009, pp. 181-187

 

 

Comparative study on hydrogen peroxide bleaching of soda-organosolv and Kraft rice straw pulps

 

Y Ziaie-Shirkolaee1,2*

1Department of Chemical Engineering, Faculty of Engineering, Tehran University, P.O. Box, 11365/4563 Tehran, Iran

2Research Center for New Technologies in Life Science Engineering, University of Tehran, P.O.Box: 11365/4563, Tehran, Iran

Email: ya_ziaee@yahoo.com

 

Rice straw was cooked with three levels of alkali content (12, 14 and 16%) in cooking liquor by soda-organosolv (ethanol, diethylene glycol, dimethyl formamide) process. The effect of alkali addition on yield, kappa number, brightness and viscosity of organosolv unbleached pulps was studied. The TCF bleachability of these organosolv pulps and kraft pulp was carried out using a simple three stage peroxide bleaching sequence without oxygen pre-bleaching. All tested pulps were bleached under identical conditions during each stage. After full peroxide bleaching sequences of three alkali-organosolv pulps, some similarity in behaviour of brightness and peroxide consumption for each alkali percentage was observed. The final brightness of 63-70% ISO was attained for all tested pulps. The chemical charge required to reach this level of brightness varied for different pulps (despite the equal initial content of the residual lignin), which was directly related to starting brightness values. The high bleached yield for organosolv pulps (approximately, in range of 90–91% o.d.p) indicates to the limited organosolv carbohydrate degradation during peroxide bleaching. The strength properties of bleached organosolv pulps were higher than kraft pulp. No relation was found between improvement in brightness and lignin removal during hydrogen peroxide bleaching.

Keywords: Hydrogen peroxide, Bleaching, Kraft, Rice straw

 

 

Indian Journal of Chemical Technology

Vol. 16, March 2009, pp. 188-191

 

 

[Cu(NH3)4]2+ SnP as a catalyst

 

Chithra P G1, Nisha J Tharayil2 & Beena B3

1Department of Chemistry, S N College, Punalur, Kollam, India

2Department of Physics, S N College for Women, Kollam, India

3Department of Chemistry, DB College, Sasthamkottah,
Kollam, India

 

The complex cation [Cu(NH3)4]2+ has been sorbed onto tin phosphate (SnP) support and the product has been characterized by elemental analysis. The catalytic activity of the [Cu(NH3)4]2+ sorbed SnP support has been studied through the decomposition of hydrogen peroxide. The kinetic data and calculated energy of activation show that the new catalyst system exhibits good catalytic activity.

Keyword:    Catalyst, Tin phosphate, Copper-ammonium complex cation, Ion exchanger

 

 

Indian Journal of Chemical Technology

Vol. 16, March 2009, pp. 192-195

 

 

Utilization of aleuritic acid free gummy mass - an industrial by-product for making particle board

 

K P Sao* & S K Pandey

Processing & Product Development Division

Indian Institute of Natural Resins & Gums, Namkum, Ranchi 834010, India

Email: sao_kp@hotmail.com

 

Aleuritic acid free gummy mass, a by-product obtained during the preparation of aleuritic acid from lac resin has been used in conjunction with lac resin for making medium density particle board from the particles of arhar (Cajanus cajan) plant stalk. The proportion of gummy mass and lac in the binder composition has been optimized. Influence of various parameters such as the amount of binder, time and temperature of hot press and particle size on the impact strength of the particle board was studied. The other mechanical properties namely water absorption, thickness swelling, modulus of rupture, tensile strength perpendicular to surface of board, and screw withdrawal forces of the particle board of dimensions 120x120x12 mm indicate that these boards can be used for interior applications.

Keywords: Aleuritic acid free gummy mass, Hydrolyzed lac, Particle board, Shellac, Sticklac, Cajanus cajan

 

 

Indian Journal of Chemical Technology

Vol. 16, March 2009, pp. 196-199

 

 

Free radical cross-linking copolymerization of acrylamide and N,N/ methylene-bis-acrylamide by using Fe(III)/thiourea and Ce(IV)/thiourea redox initiator systems

Bidyut Debnath, Goutam Bit & Swapan K Saha*

Department of Chemistry, University of North Bengal,
Darjeeling 734 013, India

Email: ssahanbu@hotmail.com

 

Acrylamide (AM) and N,N/ methylene-bis-acrylamide (Bis) copolymerization in water has been investigated at a total monomer concentration (AM + Bis) of 0.4 M. Extent of conversion of monomer into polymer was measured as a function of the reaction time upto the onset of macrogelation (gelation observed visually). The critical conversion at the gel point shows a minimum at ~5.7 mol% Bis concentration for Fe(III)/thiourea (TU) redox system whereas for Ce(IV)/TU redox system it occurs at ~2.6 mol% Bis concentration. It was found that polymer formed after gel points with different Bis% were not soluble in water, acetic acid, toluene or chloroform. In the copolymerization reaction involving Fe(III)/TU redox initiator system, no induction period is observed at 50°C. In the case of Ce(IV)/TU redox initiator system, however, a significant induction period is observed at 40°C, which depends upon the Bis% in the monomer mixture. Unlike Fe(III)/TU, the reaction takes only a few minutes to complete for Ce(IV)/TU redox initiator system after the induction period is over.

Keywords: Acrylamide, N,N/-Methylene-bis-acrylamide, Copolymerization, Polyacrylamide gel, Redox system