A new chemiluminescence method for the determination of nickel ion

Article abstract of DOI:10.1016/j.saa.2005.07.035

A new chemiluminescence (CL) phenomenon described as the second-chemiluminescence (SCL) was observed and a strong CL signal was detected, when Ni(II) ion was injected into the mixture after the end of the reaction of potassium permanganate with alkaline luminol. The possible CL mechanism is proposed based on the kinetic curve of the CL reaction, CL spectra, UV-vis spectra and some other experiments. A flow-injection analysis for the determination of nickle(II) ion has been developed, based on the catalysis of nickel(II) ion on the CL reaction between potassium manganate produced on-line and luminol under alkaline condition. Under the optimum conditions, the SCL intensity is linear with the concentration of nickel(II) ion in the range of 8.0-200.0 μg l^-1 and 0.2-2.0 mg l^-1. The R.S.D. was 4.5% for 11 determinations of 250 μg l^-1 nickel(II) ion and the detection limit (3σ) for nickel(II) ion was 0.33 μg l^-1. The method was applied to determine nickel(II) ion in synthetic samples with satisfactory results.

Full text of DOI:10.1016/j.saa.2005.07.035

Spectrochimica Acta Part A 64 (2006) 391–396
A new chemiluminescence method for the determination of nickel ion
Li Na Li, Nian Bing Li, Hong Qun Luo∗
School of Chemistry and Chemical Engineering, Southwest China Normal University, Beibei, Chongqing 400715, China
Received 27 January 2005; accepted 14 July 2005
Abstract
A new chemiluminescence (CL) phenomenon described as the second-chemiluminescence (SCL) was observed and a strong CL signal was
detected, when Ni(II) ion was injected into the mixture after the end of the reaction of potassium permanganate with alkaline luminol. The
possible CL mechanism is proposed based on the kinetic curve of the CL reaction, CL spectra, UV–vis spectra and some other experiments. A
flow-injection analysis for the determination of nickle(II) ion has been developed, based on the catalysis of nickel(II) ion on the CL reaction
between potassium manganate produced on-line and luminol under alkaline condition. Under the optimum conditions, the SCL intensity is
linear with the concentration of nickel(II) ion in the range of 8.0–200.0 ␮g l−1 and 0.2–2.0 mg l−1. The R.S.D. was 4.5% for 11 determinations
of 250 ␮g l−1 nickel(II) ion and the detection limit (3σ) for nickel(II) ion was 0.33 ␮g l−1. The method was applied to determine nickel(II) ion
in synthetic samples with satisfactory results.
© 2005 Elsevier B.V. All rights reserved.
Keywords: Nickel(II) ion; Second-chemiluminescence reaction; Flow-injection analysis
1. Introduction
of the determination of nickel in environmental samples can
hardly be overemphasized because they have undoubtedly a
serious potential hazard to the human organism. The main
sources of nickel in aquatic systems are from dissolution of
rocks and soils, biological cycles, atmospheric fallout, and
especially industrial processes and water disposal [4]. The
developmentofreliable, yetaffordable, analyticalapproaches
for the determination of Ni(II) ion in low concentration levels
seems worthwhile.
At present, the determination of nickel could be carried
out directly by X-ray fluorescence in electroplating solution
[5], flame atomic adsorption spectrometry (FAAS) in water
samples [6] and gasoline [7], graphite furnace atomic absorp-
tion spectrometry (GFAAS) in fingernails and forearm skin
[8], gasoline [9] and residual fuel oil [10], electrothermal
atomic absorption spectrometry (ETAAS) in aluminium-base
alloys [11] and marine sediments [12], inductively-coupled
plasma atomic emission spectrometry (ICP-AES) in plant
samples [13], square-wave adsorptive stripping voltamme-
try (SWASV) in duraluminium, iron ore and a reference
river water sample [14] and flow-injection solid-phase spec-
trophotometry (FI-SPS) in copper-based alloys [15]. Each
of these proposed methods often offer their own set of
Nickel is one of the essential elements in the organism
and can strengthen the secretion of the insulin, lower the
blood sugar level, stimulate the hemutopoiesis function, pro-
mote the regeneration of the red corpuscles, and treat the
anaemia and cirrhosis. Nickel still has buffer action to lung
worry, asthma and heart–lungs function in disfigurement [1].
Though nickel has such important function on people, the
amount of nickel needed is very little in human metabolism.
However, the source of nickel is very extensive in the sur-
rounding environment, and the phenomenon of lacking nickel
is very seldom. On the contrary, excessive nickel can cause
nose cancer, lung cancer and leukaemia in the rich nickel
environment [2,3]. In addition, it can also produce the dis-
eases such as heart attack, apoplexy, chronic hepatitis, uremia
and gall stone, etc. Therefore, people pay more and more
attention to their own health with the improvement of the liv-
ing standard, and the question about the pollution of nickel
has been paid close attention to. Therefore, the importance
∗
Corresponding author. Tel.: +86 23 68252360; fax: +86 23 68254000.
E-mail address: linb@swnu.edu.cn (H.Q. Luo).
1386-1425/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.saa.2005.07.035

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L.N. Li et al. / Spectrochimica Acta Part A 64 (2006) 391–396
advantages and disadvantages. However, some disadvan-
tages, such as several time-consuming manipulation steps,
sophisticated instruments and special training, or low sen-
sitivity, made these methods not simple, rapid and sensi-
tive for the determination of nickel. The chemiluminescence
(CL) analysis is attractive because very low detection limits
and wide linear response ranges can be achieved for cer-
tain species by using simple instrumentation. When coupled
with flow-injection analysis (FIA), CL-based FIA methods
provide a rapid, cheap, simple and reproducible means of
detection.
Over the last few decades, the CL analysis has become one
of most powerful technique for the determination of trace
metal ions, such as Co(II), Cu(II), Fe(II), Fe(III), Cr(VI),
Cr(III) and alkaline earth metal ions [16–20]. However, up to
now, there is no report about the use of this method to deter-
mine nickel. Recently, we surprisingly observed that when
nickel ion was injected into a reaction mixture of luminol and
potassium permanganate, whichhas just finishedthe CL reac-
tion, a new CL phenomenon was observed and a strong CL
signal was detected. We describe this new CL phenomenon
as second-chemiluminescence (SCL) reaction. Our experi-
ment discovered that the SCL intensity was a linear function
of the concentration of nickel. Based on this phenomenon, a
new method for the determination of nickel by SCL has been
established.
Fig. 1. Schematic diagram of the flow-injection SCL system: (a) luminol
solution, (b) potassium permanganate solution, (c) nickel ion solution, (P1)
auxiliary pump, (P2) main pump, (MT) mixing tube, (L) cell-valve distance,
(V) injection valve, (CE) CL reaction cell, (W) waste, (HV) high voltage
source, (PMT) photomultiplier tube, (AMP) amplifier, (R) recorder.
ing and treating the CL data. A series of interference filters
(Biophysics Institute of China, Beijing, China) were used for
obtaining the CL spectra. A UV–vis 8500 spectrophotometer
(Tianmei Co., Shanghai, China) was used for recording the
absorption spectra.
2.3. General procedure
The FIA system used for the detection of nickel ion is
shown in Fig. 1. Channels a and b was used for carrying
luminol and permanganate solutions and channel c was used
for carrying the nickel(II) solution. The permanganate stream
was initially merged with the luminol stream using a Y-piece
to make the two solutions mix thoroughly and interact with
each other until the CL signal became very weak and a stable
baseline was given. Subsequently, 50 ␮l of working solution
of nickel(II) ion was injected into the merged steam of per-
manganate and luminol solutions through a six-way injection
valve. The change of SCL intensity, ꢀI (ꢀI = In − Io, where
In and Io were the SCL signals in the presence and absence
of Ni(II) ion, respectively), was measured. The relative SCL
intensities, ꢀI, versus the concentrations of nickel(II) were
used for the calibration.
2. Experimental
2.1. Reagents
Nickel(II) ion stock solution (10.0 g l−1) was prepared by
dissolving appropriate amounts of nickel sulfate in water.
The working solution was freshly prepared by appropriate
dilution of the stock solution with water. Luminol stock-
ing solution (1.0 × 10−2 mol l−1) was prepared by dissolving
0.1771 g luminol (Sigma) with 0.1 mol l−1 sodium hydrox-
ide and diluting with 0.1 mol l−1 sodium hydroxide to 1 l.
The luminol working solution was prepared in a suitable
concentration of sodium hydroxide. Potassium permanganate
stock solution (4.0 × 10−2 mol l−1) was prepared by dissolv-
ing 1.5790 g of potassium permanganate in water and diluting
to 250 ml with water. More diluting solution of potassium
permanganatewaspreparedfreshlybydilutingthestocksolu-
tion of potassium permanganate with water. All of the other
reagents were of analytical-reagent grade and doubly distilled
water was used throughout.
3. Results and discussion
3.1. CL kinetic characteristics of the reactions
The CL kinetic characteristics of the reactions were stud-
ied in detail using the static injection method. The CL kinetic
curves are shown in Fig. 2. Curve 1 is the CL kinetic curve
obtained when 1.0 ml of 2.0 × 10−6 mol l−1 permanganate
solution was injected into 1.0 ml of 2.0 × 10−5 mol l−1 lumi-
nol solution. About 18 s later, the CL reaction terminated
and the CL signal declined to baseline. When the CL signal
returned to zero, 1.0 ml of 2.5 × 10−4 g l−1 nickel solution
was then injected into the reaction mixture solution, and a
new CL kinetic curve (curve 2) was appeared, which was
the SCL signal. The rate of the SCL reaction in solution was
2.2. Apparatus
An IFFL-D multifunction CL analyser (Xi’an Remax
Electronic Science-Tech Co. Ltd., China) was used for mea-
suring the CL signals. A personal computer employing an
IFFL-D multifunction data processing system (Xi’an Remax
ElectronicScience-TechCo. Ltd., China)wasusedforacquir-

L.N. Li et al. / Spectrochimica Acta Part A 64 (2006) 391–396
393
cluded that potassium manganate is produced during the
reaction of potassium permanganate with luminol in alkaline
solution.
Keeping permanganate concentration at 2.0 × 10−6
mol l−1, a series of the mixtures of permanganate and lumi-
nol with different molar ratios were prepared. They were
classified into two groups: in group A, the concentrations
of luminol are higher than that of potassium permanganate,
and in group B, the concentrations of luminol are lower than
that of potassium permanganate. According to the procedure
described above, when 2.5 × 10−4 mol l−1 nickel ion solu-
tion was injected into the reaction mixture of groups A and
B, respectively, it was founded that a strong CL signal was
obtained for the mixtures in group A; however, no CL sig-
nal was detected for the mixed solution in group B. These
results indicate that the CL signal was obtained only when the
concentration of luminol exceeded that of potassium perman-
ganate in the luminol–potassium permanganate CL system.
That is, the SCL phenomenon originates from the reaction of
luminol with potassium manganate. The study of the effect
of length of mixing tube on the SCL intensity illuminated
that potassium manganate, one of the SCL reagents, came
from the resultant of the reaction of luminol with potassium
permanganate on-line (see Section 3.3.1).
After setting the mixtures of groups A and B aside for
some time, the green color of the mixtures in group A was
observed to turn gradually to yellow and finally to produce
the granule brown-grey manganese dioxide precipitate. How-
ever, the color of the mixtures in group B was bottle green.
Whennickelionwasaddedintothefreshlypreparedsolutions
of group A, the color of solutions faded to colorless sharply
and small powder manganese dioxide precipitate generated
instantly. These experimental results indicate that potassium
manganate can react with luminol in alkaline condition. How-
ever, the rate of this reaction is too small to produce a
detectable CL signal. When nickel ion was added into the
above reaction system, the rate of reaction between luminol
and potassium manganate was accelerated and a strong CL
signal was produced. That is, nickel ion acts as a catalyst in
the reaction of luminol with potassium manganate. The dif-
ference in the reaction rate is also reflected by the difference
in shape and color of precipitate.
Fig. 2. Kinetic curves of chemiluminescence: curve 1: the CL signal of
luminol and potassium permanganate, curve 2: the CL signal of Ni(II) and
the mixture of luminol and potassium permanganate.
shown to be very fast. The SCL signal took approximately
0.8 s to reach the maximum value and then less than about
12 s to decline to baseline again.
3.2. Possible reaction mechanism
The absorption spectra of potassium permanganate solu-
tion and the mixed solution of luminol and potassium per-
manganate with different molar ratios were obtained and are
shown in Fig. 3. Examination of this figure shows that the
characteristic absorption peaks of potassium permanganate
at 504, 525 and 544 nm disappeared and a new absorption
peak at 605 nm emerged on the absorption spectra of the
mixtures of luminol and potassium permanganate with dif-
ferent molar ratios. The new absorption peak matches well
with that obtained for potassium manganate solution pre-
pared by reduction of potassium permanganate with sodium
sulfite. From the above experimental facts, it can be con-
It is well known that 3-aminophthalate is the luminophor
of the system of luminol–potassium permanganate, and the
maximum emission of the CL reaction is at 425 nm [21].
The emission spectrum of the luminol–potassium manganate
SCL reaction system in the presence of nickel ion is shown
in Fig. 4. The maximum emission also appeared at 425 nm.
It is easily seen that the luminophor for the SCL reac-
tion of luminol–potassium manganate–nickel ion is still 3-
aminophthalate.
According to the above discussion, the possible CL mech-
anism of the SCL reaction is suggested as follows: potas-
sium permanganate is firstly reduced by luminol to potas-
sium manganate in alkaline medium, while luminol was oxi-
dized to the excited species, 3-aminophtalate* ion. When the
Fig. 3. Absorption spectra of the different solutions: (1) 1.0 × 10−4 mol l−1
luminol, (2) 5.0 × 10−4 mol l−1 KMnO4, (3) mixed solution of
5.0 × 10−4 mol l−1 KMnO4 and 1.0 × 10−3 mol l−1 luminol, (4) mixed
solution of 5.0 × 10−4 mol l−1 KMnO4 and 5.0 × 10−4 mol l−1 luminol,
(5) mixed solution of 5.0 × 10−4 mol l−1 KMnO4 and 1.0 × 10−4 mol l−1
luminol.

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L.N. Li et al. / Spectrochimica Acta Part A 64 (2006) 391–396
Fig. 4. CL spectra of different reactions. Luminol, 1.0 × 10−4 mol l−1
;
Fig. 5. Effect of the length of mixing tube on the CL intensity.
KMnO4, 5.0 × 10−5 mol l−1; Ni(II), 5.0 × 10−3 g l−1
.
3.3. Optimization of reaction conditions
3.3.1. Effect of the length of mixing tube
excited species returned to ground state and loss its energy
by the emission of electromagnetic radiation, the CL signal
occurred. This is the common CL phenomenon observed (We
call this phenomenon as the first CL process, FCL.). The fur-
ther reaction of potassium manganate with excessive luminol
is too slow to observe the CL signal. However, at this time,
when nickel ion was added to the system, the reaction that
potassium manganate was reduced to MnO2 and that lumi-
nol was oxidized to 3-aminophtalate* ion was accelerated
because of the catalysis of nickel ion, resulting in the strong
CL signal appear (This is the SCL phenomenon we call.). The
processes described above can be expressed by the following
reactions:
The effect of the length of mixing tube on the SCL inten-
sity was very important, since nickel ion should be injected
to the mixture at that time when the CL reaction of per-
manganate with luminol has been completed sufficiently,
whereas the reaction of manganate with excessive luminol
did not obviously occur. Therefore, in order to obtain the
maximum SCL intensity, the effect of the length of mixing
tube on the CL intensity of the FCL process was tested and
the result is shown in Fig. 5, when the flow rate of pump 2 was
fixed at 1.0 ml min−1. It can be seen that the FCL intensity
The FCL process:
The SCL process:

L.N. Li et al. / Spectrochimica Acta Part A 64 (2006) 391–396
395
3.3.3. Effect of the voltage of PMT
The voltage of PMT influenced not only on the accuracy of
the experiment, but also on the sensitivity. The CL intensity
of the reaction rose with increasing the voltage of PMT, at the
same time, the noise increased, and the accuracy reduced. We
have investigated the influence of the voltage of PMT on the
SCL intensity in the voltage range from 500 to 850 V and the
experimental results showed that the reaction has maximum
signal noise ratio at 600 V.
3.3.4. Effect of the NaOH concentration
Both the FCL reaction (potassium permanganate–luminol
system) and the SCL reaction (potassium manganate–
luminol–Ni(II) system) occurred in alkaline solution. In
the experiments, the alkalinity of the reaction medium was
adjusted by preparing luminol with a suitable concentration
of sodium hydroxide. The effect of sodium hydroxide con-
centration in the range of 0.01–0.18 mol l−1 was examined.
When 0.1 mol l−1 sodium hydroxide was used, the SCL reac-
tion has the maximum CL intensity.
Fig. 6. Effect of the cell-valve distance. Luminol, 2.0 × 10−5 mol l−1
;
KMnO4, 2.0 × 10−6 mol l−1
.
decreased with increasing the length of mixing tube. When
the length of mixing tube exceeded 120 cm, the FCL intensity
decreased to the minimum value, and almost did not change
with increasing the length of mixing tube. In addition, the
effect of the length of mixing tube on the CL intensity of
the SCL process was examined as the length of mixing tube
exceeded 120 cm at the same flow rate of each channel. The
plot of the change of SCL intensity, ꢀI, versus the length
of mixing tube is also shown in Fig. 5. It can be seen that
the SCL intensity decreased with the length of mixing tube
increase. The degree of decrease in the SCL intensity was
small in the length of mixing tube range from 125 to 175 cm.
However, when the length of mixing tube exceeded 175 cm,
the SCL intensity decreased obviously at the flow rate of
pump 2 of 1.0 ml min min−1. From our experimental results
described above, it was known that when the length of mixing
tube was too short, potassium permanganate could not effec-
tively react with luminol, and the first CL signal would affect
the measure of SCL signal. However, when the length of
mixing tube was too long, excessive luminol would reacted
gradually with potassium manganate, which was just pro-
duced, resulting in the SCL signal decrease. Therefore, in
order to obtain the maximum SCL signal, it was important to
choose the optimum length of mixing tube. According to the
experimental results, the mixing tube of 150 cm was selected
for further studies when the flow rate was 1.0 ml min−1 for
pump 2.
3.3.5. Effect of Ni(II) solution acidity
Considering that the concentration of NaOH solution has
influence on the CL intensity, the acidity of nickel ion has
been investigated. The acidity of nickel ion solution was
adjusted with sulfuric acid and the effect of pH of the Ni(II)
solution on the SCL intensity was studied at different pH
values. The results showed that the optimum pH value was
5.10.
3.3.6. Effects of the concentrations of luminol and
permanganate
Under the experimental conditions described above, the
concentrations of luminol and potassium permanganate can
be changed in small concentration range. The effects of
luminol and potassium permanganate concentrations on the
SCL intensities were investigated and the results showed that
the SCL intensity reached to the maximum value when the
concentrations of luminol and potassium permanganate are
2.0 × 10−5 and 2.0 × 10−6 mol l−1, respectively.
3.4. Analytical parameters
Under the optimum conditions given above and using
the flow-injection system described in Fig. 1, the calibra-
tion curve was obtained for the nickel ion determination
by plotting the graph of ꢀI versus the nickel ion con-
centration, which gave linear ranges with different slopes
3.3.2. Effect of the cell-valve distance
Thecell-valvedistanceisanimportantparameterintheCL
flow-injection system because it determines the time inter-
val from the final mixing point of the reagents to the point
detected by the photomultiplier tube. The cell-valve distance
(L) was adjusted to yield the maximum light emission in the
cell. Fig. 6 demonstrates the effect of L on the SCL intensity.
It can be seen that the SCL signal almost did not change in
the range of 4.5 to 7.5 cm, then it decreased rapidly when
from 8.0 to 200.0 ␮g l−1 and from 200.0 to 2000.0 ␮g l−1
.
The linear regression equations for these two ranges were
ꢀI = 0.4082 C (␮g l−1) + 4.940 (r = 0.9988) and ꢀI = 3.118 C
(␮g l−1) − 662.3 (r = 0.9957), respectively. The detection
limit (3σ) for nickel ion was 0.33 ␮g l−1 and the R.S.D.
were 4.5% for 250 ␮g l−1 nickel ion in 11 replicated mea-
surements. A typical recording output of the proposed SCL
L exceeded 7.5 cm at a constant flow rate of 1.0 ml min−1
Therefore, L of 6.5 cm was selected.
.

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L.N. Li et al. / Spectrochimica Acta Part A 64 (2006) 391–396
4. Conclusion
Nickel(II) ion can catalyze the CL reaction between potas-
sium manganate produced on-line and luminol under alkaline
condition, which brings the SCL phenomenon. Based on
this, a flow-injection SCL method for the determination of
nickel(II) ion has been developed. The results demonstrate
that the proposed method offers the advantages of simplic-
ity, rapidity, wide linear range as well as high sensitivity for
the determination of nickel(II) ion. Further research work
on this subject is in progress along with new application,
suchascombiningwithionchromatographyorcapillaryelec-
trophoresis.
Fig. 7. Typical recorder outputs for a series of nickel(II) ion standard solu-
tions under the proposed conditions by the flow-injection SCL system. (A):
Nickel(II) ion concentrations from (a) to (g) are 10.0, 20.0, 40.0, 60.0, 80.0,
100.0 and 200.0 ␮g l−1, respectively. (B): Nickel(II) ion concentrations from
(1)to(7)are0.2, 0.25, 0.4, 0.5, 0.6, 1.0and2.0 mg l−1, respectively. Luminol,
Acknowledgements
This project is supported by the Municipal Science Foun-
dation of Chongqing City (No. CSTC-2004BB8646) and the
Doctor Foundation of Southwest China Normal University
(2003-10 and 2003-11).
2.0 × 10−5 mol l−1; KMnO4, 2.0 × 10−6 mol l−1; flow rate, 1.0 ml min−1
;
high voltage, −600 V.
system for the determination of different concentrations of
nickel ion is shown in Fig. 7.
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+
2.0 × 10−2 g l−1 Cl−, 2.5 × 10−3 g l−1 SiO32−, 0.125 g l−1
SO42− and nickel ions of different concentrations. The deter-
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108.0%.
Table 1
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Samples
Ni(II) added
(g l−1
Ni(II) found
(g l−1
Recovery
R.S.D.%
(n = 6)
)
)
1
2
3
4
5
6
1.25 × 10−4
2.50 × 10−4
6.25 × 10−4
8.25 × 10−4
1.00 × 10−3
2.00 × 10−3
1.35 × 10−4
2.66 × 10−4
6.01 × 10−4
8.43 × 10−4
9.60 × 10−4
2.08 × 10−3
108.0
106.4
96.16
102.2
96.0
3.47
1.53
4.25
3.21
2.75
0.98
104.0