Microchemical Journal 86 (2007) 37 41

www.elsevier.com/locate/microc

Determination of trace levels of mercury in aqueous solutions by

inductively coupled plasma atomic emission spectrometry:
Elimination of the memory effect
Xiaoping Zhu, Spiro D. Alexandratos
Department of Chemistry, Hunter College of the City University of New York, 695 Park Avenue, New York, NY 10021, USA
Received 12 September 2006; received in revised form 26 September 2006; accepted 26 September 2006
Available online 1 November 2006

Abstract
The measurement of mercury in aqueous solutions by ICP-AES is adversely affected by the memory effect wherein mercury accumulates
within the sample introduction system and is slowly released over time to give increasing response signals at the same initial mercury
concentration. The memory effect is obviated by the addition of Hg(II) complexants: thiourea and gold(III) chloride are both effective in
preventing mercury sorption and vapor buildup with the latter being preferred because the memory effect vanishes more rapidly. Conditions are
described wherein it is possible to quantify low levels of mercury(II) in aqueous solutions by ICP-AES under routine operating conditions that can
be applied to other metal ions by adding 1 mg of gold(III) chloride per 3 mg of mercury(II) to those solutions.
2006 Elsevier B.V. All rights reserved.
Keywords: ICP-AES; Mercury; Memory effect

1. Introduction
The toxicity of mercury at very low levels has led to its
stringent control with a maximum contaminant level of 2 g/L
being set by the US Environmental Protection Agency [1]. This
has led to the development of techniques for accurate monitoring
of mercury levels [2] via cold vapor atomic absorption
spectrometry [3,4], plasma atomic emission spectrometry [5],
atomic fluorescence spectrometry [6,7], inductively coupled
plasma (ICP) optical emission spectrometry [8] and ICP-mass
spectrometry [911].
Despite methods with good sensitivity and selectivity, few
can directly measure Hg(II) in aqueous solutions under routine
operating conditions as can be done with other ions [12].
Mercury accumulates in instruments irrespective of its initial
concentration in solutions, leading to a memory effect whereby
there is a gradual increase of the mercury signal strength with
time, a non-linear calibration, and a long wash-out time [13].
Mercury contamination of the instruments may be attributed to
Corresponding author. Tel.: +1 212 650 3914; fax: +1 212 772 5332.
E-mail address: alexsd@hunter.cuny.edu (S.D. Alexandratos).
0026-265X/$ - see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.microc.2006.09.004

its adsorption on the transfer tubing, spray chamber and

nebulizer [14].
Mercury in solution exists as an equilibrium of Hg(0), Hg(I),
and Hg(II). Since only Hg(0) is volatile, one method of
eliminating the memory effect entails complete reduction of
the mercury to Hg(0) with the reducing agents stannous chloride
and sodium borohydride [15]. The mercury vapor is then purged
from solution into an absorption cell. This cold vapor technique
[16] is frequently used for mercury determination in solution
when coupled with atomic absorption or atomic fluorescence
spectrometry. The standard EPA mercury determination method
is based on this technique [17]. The generation of mercury vapor
does, however, require additional equipment for its generation
and measurement. An alternative technique involves the
stabilization of mercury in solution as Hg(II). Gold(III) chloride
and potassium dichromate are typical stabilizing agents that give
complete conversion to Hg(II) thus obviating volatilization [18].
The technique has been applied to the measurement of mercury
via ICP-mass spectrometry (MS) [19]. The addition of chelants
that bind Hg(II) also stabilizes it within aqueous solutions and
limits loss through volatilization. Thus the addition of Triton X100, ammonia and EDTA allows for the accurate measurement

38

X. Zhu, S.D. Alexandratos / Microchemical Journal 86 (2007) 3741

Table 1
ICP-AES operating conditions
Plasma power (w)
Coolant flow (L/min)
Auxiliary flow (L/min)
Nebulizer flow (L/min)
Fast preflush time (s)
Total preflush time (s)
Sample aspiration flow (mL/min)
Wash time between samples (min)

2.3. Analytical procedure

1200
15.0
0.5
1.0
12
20
2.0
12

of mercury in aqueous solutions by ICP-MS [20]. The use of 2mercaptoethanol reduces the memory effect to the point that
ICP-MS gives a detection limit for mercury of 5.1 g/L [21].
Techniques have been developed to allow the use of cold
vapor coupled atomic absorption spectrometry (CV AAS) [22]
and ICP-MS for mercury determination. The detection limits are
10 g/L for the former and 3 g/L for the latter [23]. While ICP
is thus an excellent technique for mercury determination, its
extension to the more commonly available ICP-atomic emission
spectroscopy (AES) remains problematic due to the memory
effect [24]. It is reasonable to expect that mercury-stabilizing
agents added to solutions would eliminate the memory effect in
ICP-AES as they have with ICP-MS. The use of a 2% L-cysteine
solution containing Hg(II), but only at a very low level (1 g/L),
obviates the memory effect in ICP-AES [25]. We now report a
rapid and accurate method for the determination of total
mercury in aqueous solutions at the mg/L level using ICP-AES
through a comparative study of gold(III) chloride, triethylamine, ethylenediaminetetraacetic acid (EDTA), disodium ethylenediaminetetraacetate (Na2EDTA) and thiourea.
2. Experimental section
2.1. Reagents
Mercury solutions are prepared by diluting a 1000 mg/L
mercury(II) nitrate reference solution containing 1.8% nitric
acid. Au(III) solutions are prepared from a 1000 mg/L gold
atomic absorption standard solution in 0.5 M HCl. Triethylamine, ethylenediamine tetraacetic acid (EDTA), disodium
EDTA (Na2EDTA), and thiourea (analytical grade) were
purchased from Acros and used directly without purification.
Nanopure water with resistivity N 18 M was used from a
Barnstead ultrapure water system.

Mercury(II) solutions with 2.0 mg Hg(II)/L were prepared in

50 mL volumetric flasks also containing one of the following:
Au(III) at 1.0 mg/L, 0.1% triethylamine, EDTA (saturated
solution), 0.1% Na2EDTA, or 0.1% thiourea (following reports
in the literature with ICP-MS, 0.1% Triton X-100 was added to
the amine and thiourea solutions as a wetting agent). One set of
solutions was allowed to stand for 1 h before analysis and a
second set was allowed to stand for 17 h. Au(III) solution at
1.0 mg/L was made by successive dilutions of a 1000 mg/L
standard reference solution. Triethylamine, Na2EDTA and
thiourea solutions were prepared by dilution of their 1% stock
solutions. Due to its low solubility (0.5 g/L), the EDTA solution
was prepared by adding 0.05 g directly to the Hg(II) solution in a
50 mL volumetric flask and then using only the supernatant for
the ICP measurement. Mercury standard solutions at levels up to
10.0 mg/L containing up to 10.0 mg Au(III)/L were prepared by
successive dilution of 1000 mg/L Hg(II) and Au(III) reference
solutions.
After the plasma was ignited, nanopure water acidified with
1% nitric acid was used to wash the sample introduction system
and the instrument allowed to stabilize for 1520 min. The
optics were then reprofiled, the sample solution aspirated into
the ICP-AES, and measurement initiated immediately after a
20 s preflush. Three measurements were taken as the solution
was continuously aspirated and averaged. Nitric acid solutions
(1 M) containing 1.0 mg Au(III)/L were used to rinse the sample
introduction system between samples for 12 min.
3. Results
The memory effect increases the mercury count and leads to
erroneous results for the concentration of mercury in successive
samples. Fig. 1 shows the changes in mercury signal intensity
measured at different times when Hg(II) standard solution at
0.2 mg/L is aspirated into the ICP-AES. The same result is seen

2.2. Instrumentation
A Spectroflame M120E (Spectroanalytical Instruments)
inductively coupled atomic emission spectrometer (ICP-AES)
controlled by Spectro Smart Analyzer Vision software was used
for analysis of the mercury in solution. Sample solutions were
introduced by peristaltic pump. Ultra-pure argon from Airgas
was used. The wavelength of analysis was set at 184.956 nm.
The operating conditions (also appropriate for the analysis of
other transition metal ions) are detailed in Table 1. Measurement
was initiated immediately after the preflush.

Fig. 1. Changes in continuous signal intensity measurements of Hg(II) (0.2 mg/L)

in aqueous solution (the lowest (black solid) line is the first measurement followed
by the second, third and fourth measurements).

X. Zhu, S.D. Alexandratos / Microchemical Journal 86 (2007) 3741

39

Table 3
Effect of Au(III) addition at varying levels on mercury signal intensity a
Au(III), mg/L
1.0
2.0
4.0
6.0
10.0
Hg(II) signal intensity (cps) 608,653 611,705 617,420 605,005 605,970
Variation (%) from average 0.80
1.24
0.53
0.52
0.44
a

Fig. 2. Attempt to wash out mercury remaining in the ICP-AES with distilled
water after measurement of 2.0 mg/L Hg(II) in aqueous solution.

with a Hg(II) solution at 0.005 mg/L, the lowest level in this

study. Continuously introducing the same mercury solution
results in a gradual increase of signal response, with equilibrium
not being achieved. The intensity of the mercury signal in Fig. 1
at the fourth measurement has increased about twice compared
to that of the first measurement. The mercury signal does not
correlate with the sample concentration and those concentrations are not reproducible. Mercury in the sample solution must
thus be adsorbed on the walls of the transfer tubing, spray
chamber and/or nebulizer during its transport before atomization and released over time. No maximum mercury sorption
within the sample introduction system is observed. Furthermore, signal response only slowly returns to the baseline level
after aspiration is changed from the mercury solution to distilled
water. Washing the system with water for 10 min does not
remove all of the adsorbed mercury: when 2.0 mg/L Hg(II)
solution is used, a mercury signal with intensity of 166410 cps
is still observed (Fig. 2). This significant memory effect
obviates the routine analysis of Hg(II) by ICP-AES without the
addition of mercury-stabilizing agents.
TEA, EDTA, Na2EDTA, thiourea and gold(III) chloride are
compared to determine which can most effectively stabilize Hg
(II) thus eliminating the memory effect in the ICP-AES. Since
the mercury standard concentrations are low (2.0 mg/L) and high
background concentrations can affect plasma temperature and
nebulization, the matrix composition is kept as dilute as possible.
The concentrations of TEA, Na2EDTA and thiourea in the
mercury sample solutions were thus set at 0.1% and the Au(III)
set at 1.0 mg/L; the saturated EDTA solution had the same Au
(III) level.

Intensities are the average of three measurements.

Table 2 shows the change in mercury signal intensities over

three measurements when TEA, EDTA, Na2EDTA, thiourea, or
gold(III) chloride is added to the mercury solutions and the
solutions allowed to stand for 1 h before measurement. Within
each set of three measurements, the second and third measurements were taken immediately after the one that preceded it. A
significant memory effect remains with all but the goldstabilized solution. With TEA, the third measurement gives a
mercury signal that is 2.5 times greater than the first
measurement while, with EDTA and Na2EDTA, it is nearly
twice as great. Thiourea shows a variation of less than 20% in the
maximum mercury signal intensity though the initial mercury
response is still much greater than that of the Au(III)-stabilized
solution. The latter shows no memory effect.
While complexants with nitrogen-and sulfur-based ligands
are known to form stable Hg complexes (e.g., immobilized
tertiary amines display a high affinity for Hg(II) from dilute
solutions after a contact time of less than 30 min [26] and soluble
thiourea can complex Hg2+ and CH3Hg+ from aqueous solutions
[27]), it is possible that attaining equilibrium requires a time
longer than 1 h. The respective solutions were thus allowed to
stand for 17 h after which point the measurements were made
(Table 2). Though the situation improves compared to the results
with a 1 h contact time, the increase in mercury signal response
remains evident with TEA, EDTA, and Na2EDTA. (The memory
effect is evident with Na2EDTA even after a 5-day contact time.)
The lengthy contact time, however, clearly diminishes, and may
eliminate, the memory effect when thiourea is used as the
complexant.
Table 3 shows the effect of adding varying amounts of Au
(III) to solutions of mercury at 2.0 mg/L. The addition of a level
as low as 1.0 mg/L eliminates the memory effect: reproducible
signal intensities are observed over three measurements after a
1 h contact time. A change in Au(III) level from 1.0 to 10.0 mg/L
does not affect the signal intensity at a Hg(II) level of 2.0 mg/L.
Each signal intensity varies from the average by b 1.5%. Au(III)
at the low level of 1.0 mg/L is sufficient to keep Hg(II) at low
concentrations stable in aqueous solutions. Given that the

Table 2
Mercury signal intensities upon addition of 0.1% Hg(II) complexants or 1.0 mg/L of Au(III) chloride
Complexant

Measurement after 1 h contact (cps)

Measurement after 17 h contact (cps)

1st

2nd

3rd

1st

2nd

3rd

TEA
EDTA
Na2EDTA
Thiourea
Gold(III)

1,083,810
1,699,610
1,042,820
922,500
615,360

1,850,390
2,402,990
1,448,300
998,900
603,270

2,713,280
3,265,870
1,945,750
1,074,940
609,880

945,090
758,660
672,780
679,780
604,990

1,218,090
818,230
726,450
685,530
611,090

1,453,340
849,620
788,340
682,570
597,860

40

X. Zhu, S.D. Alexandratos / Microchemical Journal 86 (2007) 3741

Table 4
Effect of Au(III) level on Hg signal intensity a
Hg(II), mg/L
Au(III) mg/L
1st Hg signal intensity (cps)
2nd Hg signal intensity (cps)
3rd Hg signal intensity (cps)
a

10.0
0.5
6,814,640
5,386,820
4,931,110

10.0
1.0
2,787,140
2,820,450
2,712,030

10.0
3.0
2,599,520
2,624,530
2,575,230

10.0
6.0
2,585,240
2,619,540
2,608,820

10.0
10.0
2,588,920
2,638,630
2,624,020

Between samples, the system was washed with 1.0 M nitric acid containing 1.0 mg Au/L.

contact time required to achieve this reproducibility is less than

that required by thiourea, gold(III) chloride is the agent of choice
for stabilizing the mercury signal.
A linear calibration curve was obtained (brN = 0.9991.000)
with solutions of 1.0 mg Au(III)/L and increasing levels of Hg
(II) (0.1, 0.2, 0.4, 0.6, 1.0, and 2.0 mg/L). No matrix effect was
found upon the addition of 0.04 N sodium nitrate, chloride, or
sulfate. Mercury at the g/L level can be measured with the gold
technique. For example, contacting a solution containing 10 mg
Hg(II) /L with crosslinked polystyrene beads bearing immobilized dimethylamine ligands for 17 h gave ICP-AES spectra that
were nearly identical to the baseline of a blank solution,
indicating a Hg(II) level of less than 10 g/L.
In order to determine the lower limit of the Au:Hg ratio, six
solutions of 10 mg Hg(II)/L were prepared with 0.5, 1.0, 2.0, 3.0,
6.0, and 10.0 mg Au(III)/L (Table 4). Three measurements were
recorded for each solution; 1 M HNO3 containing 1.0 mg Au
(III)/L was used to wash the sample introduction system between
Hg(II)-containing solutions. The solution with 10 mg of gold
was read first in the ICP, followed by the solutions with lower
gold levels, as given in Table 4. The steady Hg signals from the
last three solutions were as expected from the earlier runs.
However, the first solution with 0.5 mg Au showed a decrease in
signal intensity as each measurement was taken whereas an
increase in intensity would have been expected due to the
memory effect when the level of Au got too low. The solutions
with 1.0 and 2.0 mg Au also suggested a decrease but one much
less pronounced than the first solution. The first four solutions
(i.e., 10.0 mg Hg/L with 0.5, 1.0, 2.0, and 3.0 mg Au/L) were
then prepared again for re-investigation and to study the effect of
Au(III) in the wash solution by changing that solution to 2 M
HCl since the chloride ion is known to bind both mercury and
gold ions. The order of reading in the ICP was as given in Table 5,
from left to right; the solutions with 0.5, 1.0, and 2.0 mg Au
show a decrease in the Hg signal over the four measurements
taken (though the decrease is not pronounced with the 2.0 mg
solution) and a steady Hg(II) signal is obtained with the 3.0 mg
Au solution. These results suggest that there is an effect on the
Table 5
Optimization of the Au:Hg ratio a
Hg(II), mg/L
Au(III) mg/L
1st Hg signal intensity (cps)
2nd Hg signal intensity (cps)
3rd Hg signal intensity (cps)
4th Hg signal intensity (cps)
a

10.0
2.0
2,682,880
2,666,880
2,633,250

10.0
0.5
8,789,890
6,949,630
5,829,250
5,785,650

10.0
1.0
6,604,950
4,668,360
4,141,570
4,132,590

10.0
2.0
2,671,200
2,653,310
2,648,900
2,639,980

Between samples, the system was washed with 2.0 M HCl.

10.0
3.0
2,586,120
2,601,950
2,610,810
2,618,120

Hg(II) signal if the intensities are read in a sequence from more

concentrated to less concentrated Au solutions (Table 4) or less
concentrated to more concentrated solutions (Table 5); this is
discussed in the following section.
4. Discussion
The results clearly indicate that the addition of a low level of
gold(III) chloride to mercury-containing solutions yields a
reproducibly stable signal. The mercury may be stabilized by
binding to gold(III), though the nature of that binding is unclear.
In optimizing the gold level, it became evident from the lowest
Au level in Table 4 that there is another effect operative since
the Hg signal intensity decreases with time (rather than increases from the Hg memory effect). It was also noted that the
0.5 mg Au solution was measured last in the sequence shown in
Table 4 and that the sample introduction system had been
washed with a solution of 1 M HNO3 containing 1 mg Au/L
after measurement of the preceding 1 mg Au solution. The
decrease in mercury signal intensity may thus be due to the fact
that Au(III) has its own memory effect:[25] since Au(III) is
retained in the sample introduction system, its release into
subsequent Hg-containing solutions causes the decrease in Hg
signal strength as the Au memory effect diminishes the Hg
memory effect. The influence of Au(III) in the wash solution
was removed by changing the wash solution to 2 M HCl (since
the chloride ion complexes both Hg(II) and Au(III) to form
HgCl42 and AuCl42). Table 5 shows the signal from the 0.5 and
1.0 mg Au solutions decreases over time because of the memory
effect from the Au in solution; at 2 mg Au, the Au in the solution
is almost sufficient to overcome the Hg memory effect from the
outset; at 3 mg Au, it is now completely sufficient to overcome
the Hg memory effect and is thus the recommended ratio in
routine studies. Use of 1 M HNO3 with 1 mg AuCl3 /L as the
wash solution is recommended for more rapid removal of the
mercury. Therefore the addition of gold(III) chloride or thiourea
to Hg-containing solutions can obviate the memory effect
through their ability to complex Hg(II). However, Au(III) has an
additional advantage in having faster kinetics of complexation
than thiourea thus allowing for greater analytical throughput.
Acknowledgments
We gratefully acknowledge support from the US Department
of Energy, Office of Basic Energy Sciences, Separations and
Analysis Program, through Grant DE-FG02-02ER15287. XZ
is pleased to acknowledge helpful discussions with Dr.
Fengxiang Han of Mississippi State University. Discussions

X. Zhu, S.D. Alexandratos / Microchemical Journal 86 (2007) 3741

with Professor William Grossman (Hunter College) are also

gratefully acknowledged.
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