Environ Monit Assess (2007) 132:331338
DOI 10.1007/s10661-006-9537-6
Solid phase extraction of gold(III) on Amberlite XAD-2000
prior to its flame atomic absorption
spectrometric determination
Latif Elci & Derya Sahan & Aydan Basaran &
Mustafa Soylak
Received: 25 July 2006 / Accepted: 26 September 2006 / Published online: 16 December 2006
# Springer Science + Business Media B.V. 2006
Abstract A solid phase extraction method for the
determination of gold(III) at trace levels by flame
atomic absorption spectrometer (FAAS) was devel-
oped. The method was based on retention of gold as
chloro complexes through the Amberlite XAD-2000.
The effect of some analytical parameters including
hydrochloric acid concentration, sample volume,
sample and eluent flow rates, eluent volume, eluent
concentration and interfering ions on the recovery of
gold(III) was investigated. The retention of gold(III)
from 1.5 mol l1 HCl solution and the recovery of
gold with 0.07 mol l1 NH3 solution were quantitative
(95%). The relative standard deviation (RSD) was
calculated as 3.2% (n=10). The detection limit for
gold was 2 g l1. The accuracy was checked with the
determination of gold spiked an artificial seawater and
a pure copper samples.
L. Elci (*) : D. Sahan
Chemistry Department, Faculty of Arts and Sciences,
Pamukkale University,
20020 Denizli, Turkey
e-mail: elci@pamukkale.edu.tr
A. Basaran
Chemistry Department, Science Faculty,
Eagean University,
35000 Izmir, Turkey
M. Soylak
Department of Chemistry, Faculty of Arts and Sciences,
Erciyes University,
38039 Kayseri, Turkey
Keywords Gold . Amberlite XAD-2000 .
Preconcentration . Flame atomic absorption
spectrometer
1 Introduction
The determination of gold at trace level is a
requirement for the investigation of their properties
in metallurgical, geological and environmental sam-
ples. Recently, many kinds of conventional tech-
niques such as AAS, ICP-AES and voltametry have
been used for determination of gold at traces levels.
Of these analytical techniques, flame atomic absorp-
tion spectrometry is one of the most popular tech-
niques today for determination of gold in various
samples, because of its precise and simplicity to use.
However, concentrations of noble metals in metallur-
gical, geological and environmental materials are
usually too low (even below the detection limit of
the instrument) to be determined directly by conven-
tional techniques owning to insufficient sensitivity
and matrix interference.(Abegaz, 2005; Babu et al.,
2006; Mizuike, 1981; Soylak, Elci, & Dogan, 2001).
An effective separation and preconcentration procedure
is usually necessary prior to determination. Various
preconcentration and separation procedures including
coprecipitation (Novgorodova, Generelov, Trubkin, &
Ziborova, 1994; Sato & Ueda, 2000), cloud point
extraction (Akita, Rovira, Satre, & Takeuchi, 1998;
332
Wongwailikhit, Tasakorn, Prasassarakich, & Aratono,
2003), solvent extraction (Begerow, Turfeld, &
Dunemann, 1997; Chowdhury & Kamata, 1997;
Zhao, Wu, & Chen, 1999), ion-exchange (Lai et al.,
2002) and electroanalytical methods (Komarek &
Houserova, 2003) are widely used prior to flame
atomic absorption spectrometric determination of gold.
Solid phase extraction (SPE) based on adsorption
mechanism has been widely used for preconcentration
of trace elements from various matrices, mostly in
presence of suitable chelating agents (Komendova-
Vlasankova & Sommer, 2002; Koshima, 1986;
Vlasankova & Sommer, 1999). Chelex 100 (Koshima,
1986), modified silicas (Pu, Liu, Sun, & Sun, 2003;
Pu, Su, Hu, Chang, & Yang, 1998), chitin (Terada &
Kawamura, 1991), activated carbon (Chakrapani,
Mahanta, Murty, & Gomathy, 2001; Soylak, Elci, &
Dogan, 2000), microbeads (Kavakli, Ozvatan, Tuncel,
& Salih, 2002), thiol cotton fiber (Yu et al., 2002),
chelating fibers (Chang, Wang, & Zhao, 2003), c18
(Zhao et al., 2006), etc. have been successfully used
as solid phase extraction materials for the preconcen-
tration of gold. However, instead of the use of
chelating agent, especially, in case of noble metals,
SPE has been applied by using halogeno complexes
(Elci, 1993; Elci, Isildar, & Dogan, 1993; Tunceli &
Turker, 1997).
Because of good adsorption properties such as
large surface areas, their hydrophobic nature etc.,
Amberlite XAD resins are generally preferred for the
preconcentration of traces metal ions. Also, The XAD
resins were used for the preconcentration of gold ions
from the natural samples (Elci, 1993; Elci et al., 1993;
Tunceli & Turker, 1997). Amberlite XAD-2000, a
polystyrene divinylbenzene copolymer, is a relatively
new member in the Amberlite XAD resin series. The
usage of this resin on preconcentration of trace metal
ions is limited (Duran, 2000; Duran, Senturk, Elci, &
Tufekci, 1999; Narin, Soylak, Elci, & Dogan, 2001).
According to our best knowledge, there is no any
work with Amberlite XAD-2000 for preconcentration
of gold.
The aim of this work was to develop a rapid and
efficient method for the selective solid phase extrac-
tion, concentration of micrograms per liter levels of
gold(III) in aqueous solution, using a column filled
Amberlite XAD-2000. The influence of flow rate and
volume of sample solution, concentration of HCl for
quantitative retention of gold through the column,
Environ Monit Assess (2007) 132:331338
volume and concentration of ammonia solution for
elution of Au from the column was investigated.
2 Experimental
2.1 Reagents and samples
Analytical reagent-grade chemicals were employed for
the preparation of all solutions. Freshly prepared bi-
distilled water was used in all experiments. 1,010 mg l1
of the stock solution of gold was purchased from
Sigma. Working solutions were prepared by appropri-
ate dilution of the stock solution with water. The
calibration standards were not submitted to the
preconcentration procedure. Amberlite XAD-2000
resin (Sigma, St Louis) was purchased as 60 mesh.
Artificial sea water sample (250 ml) was prepared
by dissolving 0.3675 g of CaCl22H2O, 3.275 g of
MgSO47H2O and 6.975 g of NaCl in deionized water
(Reimer & Miyazaki, 1992). A pure copper sample
was taken from a copper electrolysis factory in
Kayseri, Turkey.
2.2 Apparatus
A Perkin Elmer AAnalyst 700 atomic absorption
spectrometer with deuterium background corrector
was used in this study. All measurements were carried
out in an air/acetylene flame. The operating parameters
were set as recommended by the manufacturer. The
wavelength, slit and lamp current for determination of
gold were 242.8 nm, 0.7 nm and 10 mA, respectively.
2.3 Column
The glass column, having a stopcock and a porous
disk, was 10 cm long and 1.0 cm in diameter. A small
amount of glass wool was placed on the disc to prevent
loss of the resin beads during sample loading. Then,
500 mg of Amberlite XAD-2000 resin was slurried in
water, and then poured into the column. The bed height
of resin in the column was approximately 20 mm. In
order to remove organic and inorganic contaminants,
the resin was washed successively with methanol,
water, 1 mol l1 HNO3, water, 1 mol l1 NaOH and
water. The column was preconditioned with 510 ml
of 1.5 mol l1 HCl prior to percolation of the sample
solution. After elution, Amberlite XAD-2000 was