Third Day Poster Session, 17 June 2010 - NanoTR-VI

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P HNOR3R.
Poster Session, Thursday, June 17
Theme F686 - N1123
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Separation/Preconcentration of the Trace Amounts of Nickel in Tea, Spinach and Water Samples
Using Modified Magnetic Nanoparticles and its Determination by FAAS
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UMohammad Ali KarimiUP P* Manijeh KafiP
PDepartment of Chemistry &T
NanoscienceT and TNanotechnology Research LaboratoryT (NNRL), Payame Noor University (PNU), Sirjan 78185-
347, Iran
Abstract-A new, simple, fast and reliable solid-phase extraction (SPE) method has been developed to separation/preconcentration of trace
amounts of nickel ion from environmental water samples using dimethylglyoxim (DMG) /sodium dodecyl sulfate (SDS)-immobilized aluminacoated
magnetic nanoparticles (DSIACMNPs) and its determination by flame atomic absorption spectrometry (FAAS). The coating of alumina
on FeR3ROR4R NPs not only avoids the dissolving of FeR3ROR4R NPs in acidic solution, but also extends their application without sacrificing their unique
magnetization characteristics. This method avoided the time-consuming column-passing process of loading large volume samples in traditional
SPE through the rapid isolation of DSIACMNPs with an adscititious magnet. The preconcentration factor of the adsorbent at optimum
conditions including time, pH value, sample volume, eluent concentration, amount of SDS and DMG found as 95 %. The relative standard
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deviation and the detection limit for measurement of Ni(II) in our experiments were less than 4.0 % (n =6, 0.1 μg mlP P) and 1.0 ng mLP P,
respectively. The practical applicability of the developed sorbent was examined using tea, spinach, water and wastewater samples.
Solid phase extraction (SPE) is a preconcentration
technique of quickly growing significance in trace metal
determinations with atomic absorption spectrometry [1].
SPE has several interesting attribute compared with the
customary removal techniques. It is well enough simple,
cheap, can be used in the field, needs comparatively little toxic
solvents, and can be easily mechanized [2]. Flame atomic
absorption spectrometric analysis of heavy metal ions in real
samples is clearly hard, because of complex formation and
consequential matrices [3-6]. Separation/preconcentration step
make better the analytical detection limit, raise the sensitivity
by several order of size, enhances the preciseness of the results
and make easy the calibration [7]. Using magnetic micro and
nanoparticles for separation and preconcentration in analytical
chemistry is opening a new method that is rapid, simpler and
more exact than old ones. The greatest promote of this method
is that longed for materials are separated from solution by a
simple and dense process while less secondary wastes are
produced.
In this work, magnetic nanoparticles (MNPs) were
synthesised and then coated with alumina (ACMNPs) and
modified with DMG with aid of SDS (abbreviated as
DSACMNPs), based on the ion pair formation and simple
physical. This structure is suitable for preconcentration and
determination of nickel ion. Nickel ions are adsorbed on
DSACMNPs were isolated by an adscititious magnet and the
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adsorbed analyte was eluted with 1.0 mol LP
Optimum experimental conditions including SDS and DMG
concentrations, pH, sample volume, eluent conditions and coexisting
ions have been studied and established.
To enable useful application of ACMNPs, it is most
important that the sorbents should hold superparamagnetic
properties. Magnetic properties were characterized VSM and
result show both of the magnetic nanoparticles (MNPs and
ACMNPs) exhibited typical superparamagnetic behavior due
to not exhibiting hysteresis, remanence and coercively. The
modified ACMNPs were also confirmed by FT-IR, SEM,
TEM and XRD analysis. The result shows that the the
particles are hemi-spherical and diameters of MNPs and
ACMNPs are is in the range of 4-8 and 15-20 nm, respectively
and revealed that the resultant nanoparticles were pure FeR3ROR4R
with a spinel structure and the immobilized process did not change
its crystal phase and confirm binding mechanism too.
In summary we showed that DMG immobilized on
modified ACMNPs were capable and successfully for
separation and preconcentration of nickel ions from large
volume of the equeous solution and real samples using atomic
absorption spectroscopy. This method is simple, rapid and
sensitive and very suitable for adsorption nickel ions. Easy
regeneration is another property of ACMNPs, and the
experiments have proved that these ACMNPs can be reused at
least 3 times on average without the obvious decrease of
recovery after wash/calcine procedures.
Figure 1. SEM images of FeR3ROR4 Rnanoparticles (a) and alumina
coated FeR3ROR4 Rnanoparticles (b).
a
The authors are grateful for the financial support of the
Nanoscience and Nanotechnology Research Laboratory
(NNRL) of Sirjan Payam Noor University for this work.
*Corresponding author: ma_karimi43@yahoo.com
[1] A.M. Naghmush, K. pyrzynska, M. Trojanowicz, Talanta 42,85
(1995).
[2] R .Lima, K.C. Leandro, R.E. Santelli, Talanta 43,977 (1996).
[3] A. Tumuklu, M.G. Yalcin, M. Sonmez, Pol. J. Environ. Stud. 16,
651 (2007).
[4] Q.M. Li, R.Z. Ouyang, G.F. Zhu, G.G. Liu, Chem. Res. Chin.
Univ. 21, 622 (2005).
[5] M. Saqib, M. Jaffar, M.H. Shah, J. Chem. Soc. Pak. 29, 125
(2007).
[6] M. Soylak, L. Elci, M. Dogan, J. Trace Microprobe Tech. 19,
329 (2001).
[7] L.H.J. Lajunen, A. Kubin, Talanta 33, 265 (199
b
6th Nanoscience and Nanotechnology Conference, zmir, 2010 807