Microchim Acta

DOI 10.1007/s00604-008-0011-8

ORIGINAL PAPER

Selective solid phase extraction and preconcentration of trace

mercury(II) with poly-allylthiourea packed columns
Wenshan Qu & Yunhui Zhai & Shuangming Meng &
Yueqin Fan & Qiang Zhao

Received: 9 November 2007 / Accepted: 5 February 2008

# Springer-Verlag 2008

Abstract A new method for selective solid-phase extraction and preconcentration of trace mercury(II) from aqueous solution was developed by using poly-allylthiourea as a
new extractant. The procedure is based on the retention of
analyte in the form of thiourea complex on a mini column
of polymer resin. The effects of pH, eluent type, eluent
concentration, sample volume, sample flow rate, and
foreign ions on the recovery of the analyte were investigated using model solutions. At optimal pH value, the
extraction capacity of the new sorbent was 1.13 mmol g1.
The adsorption behavior of mercury(II) on the sorbent can
be described by a Langmuir adsorption isotherm equation.
The method was validated by analyzing a certified
reference material with the results being in agreement with
those quoted by manufacturers. The method was applied to
the determination of trace inorganic mercury(II) in natural
water samples and vegetables with satisfactory results.
Keywords Mercury determination . Mercury(II) .
Poly-allylthiourea . Preconcentration . Solid phase extraction

Electronic supplementary material The online version of this article

(doi:10.1007/s00604-008-0011-8) contains supplementary material,
which is available to authorized users.
W. Qu (*) : S. Meng : Y. Fan : Q. Zhao
School of Chemistry and Chemical Engineering,
Shanxi Datong University,
Datong 037009, Peoples Republic of China
e-mail: wenshanqu@yahoo.com.cn
Y. Zhai
Department of Chemistry, Lanzhou University,
Lanzhou 730000, Peoples Republic of China

As the number of ecological and health problems associated

with environmental contamination continues to rise, the
determination of heavy metal ion at trace level in environment samples is becoming great importance [1].
Mercury(II) and its organometallic species are considered
to be highly toxic to the environment, especially the aquatic
system [2]. The formation of organometallic species in
water system is mainly initiated by the presence of free
mercury(II) ion as well as some bacteria producing methane
and methylcobalamin leading to the generation of highly
toxic organomercury species [3]. Atomic absorption spectrometry (AAS) is the most widely used technique for such
determinations because of simplicity and low initial and
running cost. However, this technique suffers from lack of
sensitivity for the ultra-trace metal concentrations usually
encountered in environmental samples. Therefore, sample
preconcentration is becoming an essential treatment step
before atomic absorption determination.
For this purpose, a lot of techniques have been proposed
for the separation and preconcentration of trace mercury(II)
in water and environmental samples. Among the various
methods, solid-phase extraction (SPE) is one of the most
effective trace element preconcentration methods because
of its simplicity, rapidity and ability to attain a high
concentration factor [4].
SPE is based on the distribution of analyte between an
aqueous solution and sorbent by mechanisms, such as
adsorption, co-precipitation, complex formation and other
chemical reactions on or in the sorbents [5]. An efficient
solid-phase extractant should consist of a stable and
insoluble porous matrix having suitable active groups
(typically organic groups) that interact with heavy metal
ions [6]. The selectivity, adsorption capacity and adsorption
rate are three key factors determining the success of a
sorbent separation process. So far, most of sorbents for

Microchim Acta

metal ions are prepared by immobilizing reagents onto the

surface of a matrix, such as silica gel, chelating fibers and
chelating resins etc. [7]. Using such solid-phase extraction
materials, preconcentration of mercury has been described
in off or on-line procedures with immobilizing reagents
such as dithiocarbamate derivatives [810], cysteine [11],
4-(2-Pyridylazo)-Resorcinol [12], dithioacetal derivatives
[13, 14], aliphatic amines 2-thiophenecarboxaldehyde
Schiffs bases [15], YPA4 chelating resin [16] or gold wire
[17] etc. Most of these methods have better sensitivity.
However, the main problem associated with SPE columns
packed with these materials is the low selectivity and small
extraction capacity [18]. Exploring new functional materials are still necessary because of complexities and diversities of real samples [19].
So in the present work, poly-allylthiourea was used as a
new solid-phase extractant for separation and preconcentration of trace mercury(II) from aqueous solution. As wellknown, thiourea group could easily form coordination
linkage with the mercury(II), which increased the selectivity of the sorbent. Moreover, the extraction capacity of the
sorbent was larger because abundant thiourea groups were
trapped in the sorbent matrix through in situ polymerization
method. The developed method shows potential application
for preconcentration and determination of trace mercury(II)
from sample solutions.

Experimental
Instruments and apparatus
Mercury was determined by cold vapor atomic absorption
spectrometry (CVAAS) with a Perkin-Elmer AA-6800
atomic absorption spectrometer. A Perkin-Elmer mercury
electrodeless discharge lamp operated at 180 mA was used
as the light source. The absorbances of other ions were also
measured using the absorption spectrometer equipped with
Perkin-Elmer single element hollow cathode lamps and an
airacetylene burner. The instrumental parameters were
those recommended by the manufacturer. The wavelengths
selected for Hg was 253.6 nm.
A model pH-10C digital pH meter (Xiaoshan Instrument
Factory, China) was used for the pH adjustments. Fourier
Transform Infrared (FT-IR) spectra (4,000400 cm1) in
KBr were recorded using Nicolet Nexus 670 FT-IR
spectrometer (Nicolet, USA). The adsorption column was
a glass tube (50.5 cm i.d.; 0.15 cm i.d. at the lower end).
The flow rate of solution through the columns was
controlled using a model YL-110 peristaltic pump (General
Research Institute for Nonferrous Metals, China). Elemental analysis was carried out on a Vario EL elemental
analyzer (Elementar, Germany).

Chemicals and reagents

Unless otherwise stated, all water are 18 M cm pure water
purified with a Milli-Q system (Millipore, USA) and all
reagents used were of analytical grade and all solutions
were prepared with pure water. Standard labware and
glassware were used throughout and repeatedly cleaned
with HNO3 and rinsed with pure water, according to a
published procedure [20].
Stock solutions (1.0 mg ml1) of the elements were
prepared by dissolving appropriate amounts of nitrate salts
in 1.0% HNO3 and further diluted daily prior to use.
Allylthiourea was procured from Shanghai Reagent Factory
(Shanghai, China, http://www.reagent.com.cn/). Azobisisobutyronitrile (AIBN) and thyleneglycoldimethacrylate
(EGDMA) were obtained from Fluka (Switzerland, http://
www.sigmaaldrich.com/Brands/Fluka_Riedel_Home/). The
certified water reference material (GBW 08603) was
provided by National Research Center for Certified Reference Materials (Beijing, China, http://www.nrccrm.org.cn/
eng/index_en.asp).
Preparation of poly-allylthiourea sorbent
Allylthiourea (5 mmol), EGDMA (20 mmol) and AIBN
(0.25 mmol) were dissolved in 10 ml of methanol and then
was sealed. The reaction temperature was kept constant at
60 C for 12 h. The resulting products were dried, ground,
treated with 1:1 (v/v) methanol/water for 12 h, cleaned by a
waterethanol mixture and finally dried in a vacuum oven
at 60 C for 6 h.
The IR spectra of allylthiourea and the synthesized
copolymers were showed in Fig. 1. The characteristic band
of C=C at 3,229, 3,176 and 927 cm1 which appeared in the
spectra of allylthiourea were disappeared after polymerization.

Fig. 1 FT-IR spectra of allylthiourea (a) and copolymers (b)

Microchim Acta

General procedure for SPE and determination of Hg(II)

Batch procedure
A portion of standard or sample solution containing Hg(II)
or other ions was transferred into a beaker. The pH was
adjusted to the desired value with aqueous ammonia and
diluted HNO3. Then the poly-allylthiourea was added. The
mixture was shaken for 30 min to facilitate adsorption of
the metal ions onto the sorbents. After filtration, the metal
ions in filtrate were determined by atomic absorption
spectrometer (AAS).
Column procedure
A total of 200 mg of poly-allylthiourea was slurred in
water, and then poured into the adsorption column. A small
amount of cottonwool was placed at both ends to prevent
loss of the polymers during sample loading. The column
high (adsorption bed) was about 2.5 cm. The column was
preconditioned by passing a blank solution, and then a
solution containing Hg(II) was passed through at a flow rate
of 4 ml min1 (controlled by a peristaltic pump) after
adjusting pH 2. The column was washed with 5 ml pure
water and then eluted with 5 ml of 0.25 M HCl and 2%
thiourea mixture.
Sample preparation
Tap water samples were taken from our research laboratory
without pretreatment. The surface river water samples were
collected from Yellow River, Lanzhou, China. To oxidize
organic matter such as humic acid, the samples were
digested by an oxidizing UV photolysis in the presence of
1% H2O2 using a low pressure Hg-lamp which was
integrated into a closed quartz vessel [21, 22]. Then the
samples were immediately filtered through a Millipore
cellulose membrane (pore size 0.45 m), acidified to pH
1.0 with hydrochloric acid and stored in pre-cleaned
polyethylene bottles. Analyses were performed with the
least possible delay.
Vegetable samples were purchased from Huayu supermarket (Datong, China). The digested method was according to the previous procedure [23]. After digestion, each
sample solution was determined by column procedure.

Results and discussion

Influence of initial pH
The effect of varying pH values on Hg(II) uptake was tested
using the batch procedure by equilibrating 50 mg of polyallylthiourea with 10 ml of aqueous solutions containing
0.4 g ml1 of Hg(II) under different pH condition. The
obtained results were presented in Fig. 2. As can be seen,
quantitative extraction (>95%) was found in the pH range of
26. The adsorption of other metal ions such as Co(II), Ni
(II), Cu(II), Zn(II), Cd(II) and Pb(II) were also studied at
these pH values. The results showed that Co(II), Ni(II), Cu
(II) and Zn(II) were not adsorbed at pH 2, and Cd(II) and Pb
(II) were only 2.8% and 3.4%. Moreover, these ions were not
quantitatively adsorbed on the poly-allylthiourea until pH 6.
The new sorbent exhibited excellent selectivity for target Hg
(II) ion. This result should contribute to the reason that
thiourea groups can easily form coordination linkage with
the mercury(II) even at lower pH value. So pH 2 was
selected as the optimal acidity for subsequent experiments.
The optimum pH range was found same for the column pack
with poly-allylthiourea. The adsorption of Co(II), Ni(II), Cu
(II), Zn(II), Cd(II) and Pb(II) on the column were not found
at optimum pH condition.
Effect of contact time
Figure 3 illustrated the time required for Hg(II) extraction
with present sorbent. The extraction rate of Hg(II) was very
rapid during the initial stage of the extraction process. After a
very rapid extraction, the percentage of extracted Hg(II)
reached equilibrium at about 10 min. And only about 2 min
was required for 50% adsorption (t1/2). It was clear that the
solid-phase extraction process was fast using present sorbent.
The thiourea group was hydrophilic. A lot of thiourea groups
existed in the polymers increased the sorbents hydrophilicity, so the target ions could easily reach the adsorption
sites and then were trapped by the sorbent.
100
Adsorption (%)

In the spectra of the poly-allylthiourea, C=N or C=S band

appeared at 1,636 and 1,046 cm1, C=O band at 1,728 cm1
and OC=O band at 1,262 and 1,158 cm1. The results of
elemental analysis of the dried power polymers indicated the
contents of C, N and S were 60.4%, 3.6% and 4.0%,
respectively. The content of 4.0% sulfur means that each 1 g
of copolymer contains 1.4 mmol of sulfur.

95
90
85
80
75
1

4
5
6
pH
Fig. 2 Influence of initial pH on Hg(II) extraction (batch method=50 mg
of sorbent; Hg(II) concentration=0.4 g ml1; temperature=20 C)

Microchim Acta

Hg(II) extraction (%)

100

90

80

70
0

10

20

30

40

50

60

Time (min)
Fig. 3 Effect of time on Hg(II) extraction (batch method: Hg(II)
concentration=10 mg l1; extractant dose=1 g l1; pH 2; temperature=
20 C)

Influence of initial Hg(II) concentration

Fifty milligrams of poly-allylthiourea was equilibrated with
50 ml of various concentrations of Hg(II) solutions at pH 2
for 1 h. As shown in Fig. 4, when the Hg(II) concentration
was increased from 10 to 600 mg l1, the percentage of Hg
(II) extracted on sorbent sharply decreased from 99.8% to
36.6%.
With the data in Fig. 4, the Langmuir equation was
employed to study the adsorption isotherm of Hg(II). The
linear Langmuir equation was shown as follows [24]:
Ce =Q Ce =Qm 1=bQm
where Ce (mg l1) is the concentration of the Hg(II)
solution at equilibrium, Q (mol g1) is the amount of Hg
(II) extracted at equilibrium, Qm is the maximum extraction
capacity and represents a practical limiting extraction
capacity when the sorbent surface is fully covered with
monolayer sorbate molecules and b is Langmuir constant.
The Qm value can be obtained form the slope (1/Qm) of
linear plot of Ce/Q versus Ce.
The experimental result indicated that the adsorption
isotherm of Hg(II) followed the Langmuir model (Ce/Q

Hg(II) extracted (%)

100

0.8935Ce +0.0753, R2 =0.9883). The maximum extraction

capacity (Qm) of poly-allylthiourea was 1.13 mmol g1.
It was clear that this extraction capacity was larger than
most of the traditional sorbents prepared by immobilizing
reagents onto the surface of matrix. In present work, the
sorbent was prepared through in situ polymerization
method. Comparing with the surface immobilization
reagent method, the functional groups of the synthesized
sorbent distribute at all the copolymers matrix, which
greatly increases the adsorption sites of the sorbent, so
more target ions can be adsorbed.
Effect of flow rate
The flow rate of solution through the packed bed column is
a very important parameter for controlling the time of
adsorption and analysis. Using the column procedure, the
effect of flow rate on adsorption of Hg(II) was investigated
at pH 2 by passing 50 ml of sample solution through the
column. The studies show that the flow rate influences the
adsorption and desorption of target ions. For adsorption, a
flow rate <2.0 ml min1 was not studied to avoid a long
time of analysis. The results showed that Hg(II) was
adsorbed quantitatively by the poly-allylthiourea at a flow
rate of 2.04.0 ml min1. However, at a flow rate greater
than 4.0 ml min1, there was a decrease in percentage
adsorption, as Hg(II) could not equilibrate properly with the
sorbent beds.
Elution characteristic and enrichment factor
Elution of Hg(II) from the poly-allylthiourea column was
investigated by using various concentrations of HCl as
eluent following the general procedure. The results showed
that the retained Hg(II) could not be desorbed even using
6 mol l1 HCl as eluent. So the elution procedure was carried
out by adding different concentrations thiourea into the HCl
solution. The obtained results were listed in the Table 1.
Although 0.5% thiourea and 0.25 mol l1 HCl mixture
could also elute the adsorbed mercury, a biggish elution
volume was needed. In order to obtain higher enrichment

80

Table 1 Elution recovery (%) for Hg(II) ions adsorbed on the polyallylthiourea

60
40

Recovery (%)

20

0.25
M

0.5
M

1.0
M

2.0
M

4.0
M

6.0
M

0
98.6

0
98.8

3.8
102.4

10.4
97.0

23.5
91.1

45.1
71.6

0
0

100 200 300 400 500

Hg(II) concentration (mg L-1)

600

Fig. 4 Influence of initial Hg(II) concentration (batch method:

extractant dose=1 g l1; pH 2; V=50 ml; contact=1 h; temperature=
20 C)

HCl
HCl+2%
thiourea

Eluent volume=5 ml

Microchim Acta

factor, 5 ml of 2% thiourea and 0.25 mol l1 HCl mixture

and a flow rate of 0.5 ml min1 were adopted as elution
conditions. After elution, the column was washed to neutral
with pure water for its reuse.
The enrichment factor was also investigated by recommended column procedure using increasing volume of Hg
(II) solution and keeping the total amount of loaded Hg(II)
constant to 2 g. The maximum sample volume can be up
to 800 ml with the 95% recovery, and so the enrichment
factor was 160 since the final elution volume was 5 ml.
Effect of foreign ions
The effects of common foreign ions on the adsorption of
Hg(II) were investigated. The results showed that thousandfold excesses of common foreign ions had no effect on the
preconcentration and determination of the analyte, indicating that the present poly-allylthiourea can be suitably used
as sorbents for Hg(II) in high electrolytes.
Effect of column reuse
To test the stability and potential recyclability of the
column, several loading and elution operations cycles were
carried out. The operating capacity was calculated from the
loading and elution tests. The column was relatively stable
up to at least ten extractionelution cycles without
obviously decrease in the Hg(II) recoveries. The sorbent
was conserved for more 6 months and the physical and
chemical characteristics had no evident change.
Analytical accuracy and precision
Under the selected conditions, 11 portions of 10 g l1 Hg
(II) standard solutions (100 ml) were treated and analyzed
simultaneously following the column procedure. The

relative standard deviations (RSD) of the method was

1.9%, indicating that the method had good precision for the
analysis of trace Hg(II) in solution samples. The detection
limit (3), defined as by IUPAC, was found to be 0.08 ng
ml1 for 200 ml sample.
In order to further check the selectivity of the method,
solutions containing Hg(II) and other metal ions such as Cu
(II), Zn(II) or Cd(II), were prepared and analyzed by the
proposed column procedure. Studies with 2.0 g l1 of Hg
(II) showed that 50 g l1 of Cu(II), Zn(II) or Cd(II) did not
interfere with Hg(II) determination by CVAAS after the
SPE and column procedure.
Hg(II) determination in real samples
The developed method was validated by analysis of a
standard reference material containing 10.0 g l1 Hg(II)
(GBW 08603, water) by recommended column procedure.
The analytical results for the standard material were in good
agreement with the reference values. Moreover, the prepared
poly-allylthiourea was applied for preconcentration and
determination of trace Hg(II) in two natural water samples
and vegetable samples by the recovery test method. The
recoveries of Hg(II) were in range of 96105%, and further
implied the suitability of present poly-allylthiourea for
selective solid-phase extraction and determination of trace
Hg(II) from real samples.
Comparison with other methods
Comparative information from some studies on preconcentration of Hg(II) by various methods for the figure of merits is
given in Table 2. As seen from the data, the proposed method
using poly-allylthiourea had a relatively high acidity and
adsorption capacity compared to other methods reported in
Table 2. The LOD and preconcentration factor of this

Table 2 Figures of merit of comparable methods for determination of Hg(II) by solid-phase extraction
Methods/reagent(s) used

pH

Capacity (mmol g1)

Silica gel-loaded/dithizone
Silica gel/dithiocarbamate derivatives
Nanometer SiO2/PAR
XAD/bis(o-aminophenylthio)ethane
XAD-2/2-aminoacetylthiophenol
PS-DVB/imidazolyl azo groups
Amberlite IRC-50/histidine
Polyaniline
Hg(II)-imprinted copolymer
Hg(II)-imprinted hybrid sorbent
YPA4 chelating resin
Poly-allylthiourea

56
1 M NaOAC
4
5
3.57
46
5.5
5
8
6.5
6
2

0.120.2
0.60.92
0.276
0.38
0.24
0.62
1.5
0.50
0.205
0.197
0.189
1.13

LOD limit of detection, PF preconcentration factor

LOD (ng ml1)

0.43
0.09
0.23

0.05
0.05
0.06
0.2
0.08

PF

Ref.

200

[13]
[8]
[12]
[25]
[26]
[27]
[28]
[29]
[18]
[30]
[16]
This work

50
300
50
120
200
100
160

Microchim Acta

method are also comparable The common foreign ions had

no evident interference for the preconcentration of Hg(II)
even at higher concentrations because these ions were not
adsorbed by the present sorbent at a relatively high acidity.
The simple and rapid preparation of the poly-allylthiourea is
another obvious advantage compared with other methods.
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