Journal of Hazardous Materials 169 (2009) 593–598
Contents lists available at ScienceDirect
Journal of Hazardous Materials
journal homepage: www.elsevier.com/locate/jhazmat
Synthesis of a novel chelating resin and its use for selective separation
and preconcentration of some trace metals in water samples
S ¸ erife Tokalıo˘ glu
a,∗
, Vedat Yılmaz
b
,S ¸ enol Kartal
a
, Ali Delibas ¸
c
, Cengiz Soykan
c
a
Erciyes University, Faculty of Arts and Sciences, Chemistry Department, 38039 Kayseri, Turkey
b
Erciyes University, Pharmacy Faculty, Analytical Chemistry Department, 38039 Kayseri, Turkey
c
Bozok University, Faculty of Arts and Sciences, Chemistry Department, 66200 Yozgat, Turkey
article info
Article history:
Received 31 October 2008
Received in revised form 27 March 2009
Accepted 31 March 2009
Available online 7 April 2009
Keywords:
Synthesis
Chelating resin
Solid phase extraction
FAAS
abstract
A new chelating resin, poly[N-(4-bromophenyl)-2-methacrylamide-co-2-acrylamido-2-methyl-1-
propanesulfonic acid-co-divinylbenzene], was synthesized and characterized. The resin was used for
selective separation, preconcentration and determination of Cu(II), Ni(II), Co(II), Cd(II), Pb(II), Mn(II)
and Fe(III) ions in water samples by flame atomic absorption spectrometry. Effects of pH, concentration
and volume of elution solution, sample flow rate, sample volume and interfering ions (Na
+
,K
+
, Ca
2+
,
Mg
2+
, Fe
3+
, Mn
2+
, Al
3+
, Zn
2+
, Pb
2+
, Cu
2+
, Ni
2+
, Cd
2+
, Cl
-
and SO
4
2-
) on the recovery of the analytes were
investigated. The sorption capacity of the resin was 25.6, 19.8, 32.1, 41.3, 38.9, 13.9 and 18.3mgg
-1
for
Cu(II), Ni(II), Co(II), Cd(II), Pb(II), Mn(II) and Fe(III), respectively. A high preconcentration factor, 100, and
low relative standard deviation, ≤2.5% (n = 7) values were obtained. The detection limits (gL
-1
) were
0.57 for Cu(II), 0.37 for Ni(II), 0.24 for Co(II), 0.09 for Cd(II), 1.6 for Pb(II), 0.19 for Mn(II) and 0.72 for
Fe(III). The method was validated by analysing fortified lake water (TMDA-54.4, a trace element fortified
calibration standard) and spiked water samples. The method was applied to the determination of the
analytes in tap and lake water samples.
© 2009 Elsevier B.V. All rights reserved.
1. Introduction
As the number of ecological and health problems associated
with environmental contamination continues to rise, the determi-
nation of heavy metal ion at trace level in environmental samples is
becoming great importance [1]. Cr(III) is considered to be an essen-
tial trace element for the maintenance of effective glucose, lipid
and protein metabolism in mammals. On the other hand, Cd(II)
and Pb(II) even at very low concentrations, are well-known toxic
elements. Both metals cause adverse health effects in humans and
their widespread presence in the human environment comes from
anthropogenic activities [2,3]. Copper is both micro-nutrient as well
as toxic element for living beings, depending upon the concentra-
tion level. Its deficiency causes the ischemic heart disease, anemia,
abnormal wool growth and bone disorders. Severe oral intoxica-
tions affect mainly blood and kidneys. Excess of copper enters
through into the body as a pollutant present in water, food con-
tamination and some other plant foods rich in copper. Nickel is a
moderately toxic element. The most common harmful health effect
of nickel in humans is an allergic reaction [4,5].
∗
Corresponding author. Tel.: +90 352 437 49 37; fax: +90 352 437 49 33.
E-mail address: serifet@erciyes.edu.tr (S ¸ . Tokalıo˘ glu).
The toxicity of cobalt is low and its considered as an essential
element, which is required in the normal human diet in the form of
vitamin B
12
(cyanocobalamin). For this reason, Co has been used in
the treatment of anemia. Iron is an essential element for all forms
of life, i.e. it is a cofactor in many enzymes and essential for oxy-
gen transport and electron transfer. It is potentially toxic in excess
concentration because of its pro-oxidant activity. Manganese is a
necessity for the proper function of several enzymes and an essen-
tial micro-nutrient for the function of the brain, nervous system and
normal bone growth. It optimizes enzyme and membrane transport
functions [6–8].
The direct determination of trace metals in various samples
may not be possible with sufficient sensitivity by also using
expensive analytical methods, such as inductively coupled plasma
atomic emission spectrometry or electrothermal atomic absorp-
tion spectrometry because of low concentrations and/or matrix
interferences. The most effective way to avoid these problems is to
perform appropriate sample pretreatment prior to analysis aimed
at lowering the limits of detection, by both removal of interferences
and increasing the concentration of the species of interest. There-
fore, a separation/preconcentration technique is necessary, prior to
determination of trace metals by an instrumental technique [9,10].
The widely used techniques for the separation and preconcentra-
tion of trace metals include coprecipitation [3,11], liquid–liquid
0304-3894/$ – see front matter © 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.jhazmat.2009.03.146