α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εF ο υο υο υο υο υ n δ εδ εδ εδ εδ ε r ’ s δ α ψ δ α ψ δ α ψ δ α ψ δ α ψ S ρ ερ ερ ερ ερ ε c i ααααα l I s s u εεεεε

I S S U E N O . 3 0 9 • O C T O B E R 2 0 0 9 • 349

S T U D I E S O N S Q U A R E W A V E A N O D I C S T R I P P I N G

V O LT A M M E T R Y F O R D E T E R M I N A T I O N O F T R A C E L E V E L S

O F G A L L I U M E M P L O Y I N G B I - F I L M E L E C T R O D E

J . V. K a m a t , N . G o p i n a t h , H . S . S h a r m a a n d S . K . A g g a r w a l

F u e l C h e m i s t r y D i v i s i o n

Introduction

Anodic Stripping Voltammetry is an established

electrochemical method and has been exploited in

the past, for estimation of metallic impurities at trace

as well as sub trace levels, employing mercury-drop

electrode [1,2]. However, because of the toxicity of

mercury, alternative electrode material, such as Bi-

film is being explored, for trace determination.

Recently, Wang et al have adopted Bi-film electrode

for electroanalytical determination of trace metals [3].

Bi-films can be formed on different carbonaceous

substrates such as carbon fibers [4, 5], printed inks

[6], carbon paste [7] or glassy carbon [8]. In this

communication, we present Square Wave Anodic

Stripping Voltammetric (SWASV) studies, on the

determination of Gallium at microgram levels,

employing Bi-Film on Gc electrode in acetate buffer.

Experimental

All voltammetric experiments were performed with

Autolab PGSTAT30 / General-Purpose Electrochemical

System. A three electrode voltammetric cell having a

GC disc of 3 mm diameter as the working electrode,

GC rod as a counter electrode and Ag/AgCl (3M NaCl)

as reference electrode was employed and 10 mL of

acetate buffer (pH = 4 .6) was used, as a supporting

electrolyte in the present studies. The GC working

electrode was polished with 0.05 mM alumina slurry

on a felt pad, prior to each new set of SWASV

experiment. The standard gallium stock solution was

prepared, by dissolving high purity gallium metal in

AR grade concentrated HCl, under reflux conditions

and stocked in a standard glass flask. The test solutions

were prepared from this standard Ga solution prior to

carrying out SWASV experiments.

Preparation of Bi-film on GC surface

Bi-film on polished GC electrode was prepared by

electrodeposition of Bi at -1.1 V from 1mM Bi (III)

solution in acetate buffer under stirring conditions.

The deposited bismuth was then stripped by sweeping

the potential of the electrode from -1.1V to + 0.4V

and a stripping peak of Bi was observed at –0.028 V.

On the basis of these investigations, a conditioning

potential of +0.4V was applied to remove Bi-film from

GC surface, prior to each new SWASV experiment.

Results and Discussion

In situ deposition of the Bi film and Ga was carried

out on the GC surface, by spiking the acetate buffer

with 1μg of Bi (III) and 0.8 μg of Ga. The stripping

voltammogram was recorded by scanning the

electrode between -1.1V and -0.5V, applying square

wave waveform which resulted in the sharp undistorted

T h i s p a p e r w a s c o n f e r r e d t h e B e s t P a p e r A w a r d ( 2 nd p r i z e ) i n t h e

P o s t e r S e s s i o n a t t h e D i s c u s s i o n m e e t o n E l e c t r o n a l y t i c a l Te c h n o l o g i e s

D M - E L A N T E - 2 0 0 8 a t M u n n a r, K e r a l a , h e l d d u r i n g F e b r u a r y 2 5 - 2 8 , 2 0 0 8

350 • I S S U E N O . 3 0 9 • O C T O B E R 2 0 0 9

α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εD R . H O M I B H A B H A C E N T E N A R Y Y E A R

stripping peak of Ga at -0.9V. Further studies were

carried out to optimize experimental parameters,

conditioning time (Tc), deposition potential (E

d),

deposition time (Td), SW frequency and SW amplitude.

Renewal of GC surface is an essential requirement for

obtaining reproducible values of peak current. SWASV

experiments were therefore carried out, to optimize

the conditioning time for the removal of the Bi-film

and target metal from GC surface. It is obvious from

Fig.1, that 120 s of conditioning time, is optimum for

the removal of the film. Next experiments were

performed by varying deposition potential from

-1.0 V to -1.5 V. In Fig. 2 SWASV peak current of Ga

is plotted as a function of deposition potential. It is

seen from the figure, that peak current Ipa increases

initially with Ed,

up to -1.1 V and then levels off at

higher values of Ed. This shows that a deposition

potential of -1.1 V is most optimum for

preconcentration of gallium. In Fig. 3, effect of

deposition time (Td) on the SWASV peak current is

presented. It can be seen that peak current, increases

linearly with deposition time from 60 s to 180 s and

at higher Td, Ip

levels off. This shows, that deposition

time of 180 s is optimum. In the next course of

investigation, the effect of SW modulation amplitude

(DE) on Ip was studied and the results are presented in

Fig. 4. It is seen from the figure, that Ip attains a

maximum value at 60 mV amplitude, which is

optimum for further studies. On the basis of above

Fig.1: SWASV peak current ( Ip

) as a function ofconditioning time ( T

c) for the removal of Bi-film from

GC surface at

the conditioning potential +0.4 V

Fig.2: Ip as a function of deposition potential (E

d). Test

solution 1μM Ga, deposition time 180 s, equilibrationperiod 30 s, SW frequency 25 Hz, SW modulationamplitude 60 mV, step potential 5mV, scan potentialrange –1.1V to - 0.5V.

Fig. 3: Ip as

a function of deposition time (Td), under the

experimental conditions as shown in Fig. 2 anddeposition potential of -1.1V.

mentioned studies, further SWASV experiments were

carried out with the optimized parameters; Ed

-1.1V, Tc 120 s, T

d 180 s, SW frequency 25 Hz, SW

amplitude 60 mV.

Validation of optimized experimental parameters was

evaluated, by performing ten individual SWASV

experiments at 1mg level of Ga. The relative standard

deviation was found to be better than

α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εF ο υο υο υο υο υ n δ εδ εδ εδ εδ ε r ’ s δ α ψ δ α ψ δ α ψ δ α ψ δ α ψ S ρ ερ ερ ερ ερ ε c i ααααα l I s s u εεεεε

I S S U E N O . 3 0 9 • O C T O B E R 2 0 0 9 • 351

2%. The proportionality between Ip and concentration

of Ga in 1 μM to 4 μM range was verified. Ip was

observed to increase linearly with Ga concentration,

as shown in Fig. 5 and a correlation coefficient of

0.998 was obtained. A few determinations of Ga at

0.2mg level were carried out by standard addition

approach and the results obtained are encouraging.

Further work on the determination of gallium at μM

concentration of gallium and interference of zinc in

gallium determination are being pursued.

Conclusion

SWASV studies, carried out employing Bi-film

electrode will be useful for gallium determination at

sub microgram level.

References

1. J.V. Kamat, N. Gopinath and S.K. Aggarwal,

Nuclear and Radiochemistry Symposium,

Amritsar, India (2005) 507.

Fig. 4: Ip as a function of SW amplitude (ÄE) under the

experimental conditions shown in Fig.3Fig. 5: I

p as a function of Ga concentration in 1μM -

4 μM range in acetate buffer, also shown (inset) SWASVfor increasing concentration of Ga . Other conditions,as in Fig.3

2. T.K. Bhardwaj, H. S. Sharma and S.K. Aggarwal,

J. Nucl. Materials 360 (2007) 215.

3. J. Wang, J. M. Lu, S.B. Hocevar, P.A.M. Farias,

B.Ogorevc, Anal. Chem. 72 (2000) 3218.

4. E.A.Hutton, S.B.Hocevar, B. Ogorevc, Anal.

Chem. Acta 537 (2005) 285.

5. M.A. Baldo, S.Daniele, C.Bragato, J. Phys. IV

107 (2003) 103.

6. J. Wang, J.M.Lu, S.B.Hocevar, B.Ogorevc,

Electroanalysis 13 (2001) 13.

7. S.A.A. Elsuccary, I. Svancara, R. Metelka,

L. Baldrianova, M.E.M. Hassouna, K.Vytras,

Sci. Pap. Univ. Pardubice, Ser. A-9 (2003) 5.

8. S.B. Hocevar, B.Ogorevc, J.Wang, B.Pihlar,

Electroanalysis 14 (2002) 1707.

352 • I S S U E N O . 3 0 9 • O C T O B E R 2 0 0 9

α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξα β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξφ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εψ ζ α β χ δ ε φ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ ε φ γ η ι ϕ κ λ μ ν ο π θ ρ σ τ υ ϖ ω ξ ψ ζ α β χ δ εD R . H O M I B H A B H A C E N T E N A R Y Y E A R

Dr. S.K. Aggarwal is Head, Fuel Chemistry Division, BARC since July 2005 and is also a

Professor of Chemistry at the Homi Bhabha National Institute (HBNI). He joined the 16th

Batch of BARC Training School in 1972 and received the Homi Bhabha Award. He did his

Ph.D. from Mumbai University and his post-doctoral training at University of Virginia, USA.

Dr. Aggarwal was honoured with the Eminent Mass Spectrometrist Award by the Indian

Society for Mass Spectrometry (ISMAS) in 1996 and was recently conferred with the DAE

Special Contributions award 2006. He is a specialist in the field of atomic mass spectrometry

and alpha spectrometry and is interested in various mass spectrometric techniques. His

other areas of interest include laser-based analytical techniques, Electrochemistry, X-ray spectroscopy and Separation

techniques like HPLC, solvent extraction etc. He has more than 100 publications in reputed International Journals

and is a recognized Ph.D. Guide of the Mumbai University and of HBNI.

A B O U T T H E A U T H O R S

Dr. J. V. Kamat obtained her M. Sc. Degree from Mumbai University. She joined BARC in

1982. After joining, she obtained her Ph. D. (Chemistry) from Mumbai University. Her

main field of research is electroanalytical chemistry of actinides. She is involved in developing

and employing various Electroanalytical Techniques for different applications in the nuclear

fuel cycle. She is the Treasurer of the Indian Society for ElectroAnalytical Chemistry (ISEAC).

Mr. N. Gopinath received M.Sc. degree from Sri Venkateswara University, Tirupati in

1973. He joined Radiochemistry Division, BARC in 1977. Presently he is working in Fuel

Chemistry Division, BARC. Since he joined BARC, he has been actively involved in the field

of quality assurance of nuclear fuel materials and has developed new electroanalytical

methodologies for determination of nuclear fuel materials. He has authored a good number

of research papers in the field of electroanalytical chemistry of nuclear materials. Presently

he is involved in the studies on exploitation of the significant electro catalytic properties of

nanomaterials for analytical purposes. He is the Secretary of the Indian Society for

ElectroAnalytical Chemistry (ISEAC).

Dr. H.S. Sharma joined Radiochemistry Division, BARC in 1978, after completing D.Phil.

from University of Allahabad and is presently Head, Electrochemistry Section, Fuel Chemistry

Division, BARC. His major fields of interest include development of analytical methodologies

for precise and accurate determination of actinides in nuclear fuel materials and

electrochemical synthesis of conducting-polymers and nano-scale materials and their

characterization employing spectroscopic and microscopic techniques. He has contributed

significantly to the development of coulometric method for precise and accurate

determination of U and Pu in nuclear fuel materials. He has introduced voltammetric and Electrochemical

Quartz Crystal Microbalance techniques in electrochemical research. Dr. Sharma was recently awarded Prof. S.

S. Sandhu Award (2007- 2008) by the Indian Chemical Society, for his outstanding contribution in Electrical

Research.