Anal. Method Environ. Chem. J. 5 (1) (2022) 49-60
Research Article, Issue 1
Analytical Methods in Environmental Chemistry Journal
Journal home page: www.amecj.com/ir
AMECJ
Measurement of heavy metals in soil, plants and water
samples based on multi-walled carbon nanotube modied
with Bis(triethoxysilylpropyl)tetrasulde by ame atomic
absorption spectrophotometry
Mohammad Reza Rezaei Kahkhaa, Ahmad Salarifarb,*, Batool Rezaei Kahkhaa
a Department of Health Engineering, Zabol University of Medical Sciences, Zabol, Iran.
b Environmental Engineering Department, Faculty of Natural Resources, Islamic Azad University, Bandar Abbas Branch, Iran
ABSTRACT
Heavy metals (HMs) are considered as the major environmental
pollutants that accumulated in soil and plant. Consumption of such
contaminated plants by humans and animals would ultimately harm
the health of communities. This study aims to evaluate the amount
of copper(Co), cadmium(Cd), and lead(Pb) in soil and cultivated
plants that are irrigated by the city of Zabol’s wastewater. Also,
the heavy metals determined in 20 mL of Zabol’s water based on
Bis(triethoxysilylpropyl)tetrasulde (S4[C3H6Si(OEt)3]2, TEOSiP-
TS) modied on MWCNTs as an adsorbent by the uniform dispersive
-micro-solid phase extraction (UD-µ-SPE) at optimized pH. In this
study, 52 samples including wheat, corn grain, and wild spinach, as
well as agricultural soil were selected randomly from three village
stations. The concentrations of heavy metals in plants, soils, and water
samples were measured using a ame atomic absorption spectrometer
(F-AAS). The one-way ANOVA test was applied to compare the mean
value of heavy metals at the three mentioned stations. The results
indicate that the amount of lead at all three stations and in all types
of plants exceeds the permissible range. The amount of copper in
plant species and water is lower than the permitted range, while it is
higher in agricultural soil. By optimizing parameters, the linear range
(LR) and the detection limit (LOD) of Cu, Cd, and Pb were obtained
1.5-1000 μg L-1, 1-200 μg L-1, 5-1500 μg L-1 and 0.5 μg L-1, 0.25 μg
L-1, 1.5 μg L-1, respectively in water samples (RSD%<2). This study
indicates that irrigation of agricultural elds using wastewater causes
the accumulation of heavy metals in soil and plants.
Keywords:
Heavy Metals,
Environment sample,
Bis(triethoxysilylpropyl)tetrasulde,
Uniform dispersive -micro-solid phase
extraction,
Flame atomic absorption spectrophotometer
ARTICLE INFO:
Received 17 Nov 2021
Revised form 23 Jan 2022
Accepted 12 Feb 2022
Available online 28 Mar 2022
*Corresponding Author: Ahmad Salarifar
Email: salarifar562@gmail.com
https://doi.org/10.24200/amecj.v5.i01.167
------------------------
1. Introduction
Heavy metals(HMs) as hazardous elements,
caused by human activities in different sections
of industry, agriculture, and business. It has been
discharged for years into the ecosystem and has
polluted water, soil, and agricultural farms. Also,
heavy metals have endangered the health of
humans and other creatures [1]. Heavy metals enter
the environment on a large scale through natural
and human-made resources. The releasing amount
of heavy metals to the environment is considerable
[2]. The rst inuencing element of metal pollution
in an ecosystem is the existence of heavy metals
in the biomass of polluted areas which endangers
human health. One of the most fundamental issues,
50 Anal. Methods Environ. Chem. J. 5 (1) (2022) 49-60
in terms of heavy metals, is that body does not
metabolize them [3]. This would cause several
diseases and complications in the body. In general,
neurological disorders (Parkinson’s, Alzheimers,
depression, schizophrenia), various cancers,
nutrient deciency, and hormones imbalance are
the results of heavy metals amass in the human
body [4]. Some analytical techniques were used for
the measurement of HMs in environmental samples
such as atomic absorption spectrophotometry [5,6],
laser-induced breakdown spectroscopy [7], X-ray
uorescence spectroscopy [8], and electrochemical
methods [9]. Among these techniques, atomic
absorption spectrophotometry has a very advantages
such as simplicity, effectiveness, reliability, and low
detection limit[10]. Zabol’s urban wastewater is
used in some villages to irrigate agricultural farms
at the time of drought. In this study, to evaluate the
amount of heavy metals lead, copper, and cadmium
in agricultural soil and cultivated plants, such as
wheat, corn, and a species of wild spinach, which
are irrigated with wastewater, three stations were
selected in which the irrigation of agricultural
elds with wastewater is common. After wheat
sampling and given that most of the planted wheat
used to feed livestock in late winter or early spring
is immature, the root of the plant was separated
and all methods of sample preparation were
applied to analyze the plant, without considering
other parts of it. A similar approach was applied
to grain corn. Wild spinach is a volunteer plant in
wheat elds, and as it is used widely in the Sistan
region for the purpose of cooking a type of local
food during fall and winter, it was sampled from
mentioned stations in order to evaluate the heavy
metals accumulation. Recently, many adsorbents
such as graphene/graphene oxide [11], CNT [12],
activated carbon [13 ], and silica pours [14] were
used for extraction HMs in water samples. Also
functionalized nanocarbon structures were also
reported for extraction heavy metals in water, plant
and soil samples [15]. In addition, the different
technology such as, liquid-liquid extraction [16],
dispersive ionic liquid –liquid extraction [17],
dispersive micro solid-phase extraction [18], and
magnetic solid phase extraction were presented for
water samples. In this study, the plants and soil
samples were analyzed with F-AAS after sample
digestion procedure and water samples determined
after sample preparation method based on TEOSiP-
TS@MWCNTs adsorbent by the UD-µ-SPE
procedure.
2. Materials and Methods
2.1. Sampling and reagents
This research is conducted to evaluate the number
of heavy metals such as lead, copper, and cadmium
in three different types of plants, i.e. wheat, corn,
and spinach, as well as in agricultural soil of
selected elds. Given that use of wastewater in
irrigation is performed in only three stations of
Zabol in the east of Iran, and taking the extent
of farmland areas, in total 52 samples were
selected from all stations. Samples were randomly
collected in June 2020 and February 2021. The
water sample was prepared from Zabol by a
clean glassy tube (100 mL) which was acidied
with HNO3 (2%) and ltered by Whatman lter
Sigma, Germany (200 nm) by ASTM method for
sampling of waters. The calibration of copper(Co),
cadmium(Cd), and lead(Pb) in soil, cultivated
plants, and water solution was prepared daily
by appropriate Co(II), Cd(II), and Pb(II) stock
solution (1000 mg L-1) in Deionized water (DW,
Millipore, USA) which was purchased from
Sigma, Germany. The acid solutions such as HCl,
H2SO4, and HNO3 were purchased from Sigma,
Germany. The bis(triethoxysilylpropyl)tetrasulde
(S4[C3H6Si(OEt)3]2, TEOSiP-TS, CAS N:40372-
72-3) was purchased from Merck, Germany.
2.2. Synthesis of Adsorbent
The modication of the Bis(triethoxysilylpropyl)
tetrasulde (S4[C3H6Si(OEt)3]2, TEOSiP-TS) on
the surface of MWCNTs nanostructure has shown
in Figure 1. By the acid treatment methods (HNO3
& H2SO4), the carboxylic acid-functionalized
MWCNTs (MWCNTs-COOH) were synthesized
based on previously reported papers [19]. By
reducing the COOH to the OH groups, MWCNTs@
51
Measurement of heavy metals by Nanotechnology Mohammad Reza Rezaei Kahkha et al
OH created. By stirring, 5 g of MWCNTs-COOH
mixed with 0.5 g of NaBH4 and CH3OH in a
100 mL ask condenser. Then, the mixture was
reuxed for 3 h and then it was cooled in room
temperature after 2 h. Finally, the MWCNTs-OH
nanomaterials were ltered with a Whatman lter
and washed many times with the methanol/DW.
For the synthesis of the EOSiP-TS@MWCNTs
adsorbent, 2 g of MWCNTs-OH were added to a
solution of Bis(triethoxysilylpropyl)tetrasulde
(TEOSiP-TS) in presence of toluene in a 100
ml round-bottom ask equipped with magnetic
stirring, and then the mixture was heated at 80 °C
for 3.5 h by Ar gas. Finally, the TEOSiP-TS @
MWCNTs product was ltered with a Whatman
lter.
2.3. Sample preparation
Soil samples were collected from the depth of
2 cm. Polyethylene sampling containers were
initially washed with detergent powder and then
kept in a container containing 5% nitric acid for a
certain period (acid washing). Then, it was rinsed
with ionized water. Plant samples were collected
inside polyethylene bags, then transferred to the
laboratory, and after that completely washed with
three-time distilled water to eliminate potential
pollutions.
Afterward, the samples were dried up at room
temperature. Dried samples were milled and
completely crushed and then passed through a
sieve with a pore diameter of approximately 0.5
mm. The milled plant samples were placed inside
clean glass containers and were dried again at 65°C
for 24 hours. For digestion of plant sample, 2g of
milled dried samples were placed inside a round-
bottom ask, and then concentrated perchloric
acid (4ml), concentrated sulphuric acid (2ml),
and concentrated nitric acid (20ml) were added,
respectively. The above solution was heated to
boil carefully under a hood and over a heater to
reduce its volume. In the next step, 20ml water
was added to dissolve the sediments, and heated
up again to reduce their volume. Afterward, the
solution was ltered and its volume was reduced
to 250ml. Soil samples were completely oven-
dried for 24 hours in the laboratory at 70°C. In
the next stage, they were sieved and milled to
obtain a completely smooth powder. 0.5 g of the
above sample was prepared to be injected into the
device, using the complete digestion method [20-
22]. After digestion, all samples were analyzed
with F-AAS.
2.4. Analytical measurement
Flame atomic absorption spectroscopy (F-AAS,
Agilent 55B-AA) was used to measure all elements
in the sample. To obtain the required sensitivity in
measurements, air/acetylene ame was applied. In
order to ensure the accuracy of evaluation, each
measurement was performed three times on each
sample, and standard deviation and mean of data
were obtained. One-way analysis of variance
was used to compare the average heavy metals
content in various types of selected plants at those
three stations. The instrumental conditions for the
determination of Cu, Pb, and Cd by F-AAS have
explained in Table 1.
Fig. 1. Synthesis of EOSiP-TS@MWCNTs adsorbent by the Bis(triethoxysilylpropyl)tetrasulde
52
2.5. General Procedure
The plant and soil samples were digested with acid
solutions and after dilution with DW, the Cu, Pb,
and Cd ions were determined with F-AAS. On the
other hand, by the UD-µ-SPE method, 20 mL of
water samples were used for the separation and
extraction of the Cu, Pb, and Cd ions at pH 6-6.5.
In this procedure, 20 mg of EOSiP-TS@MWCNTs
adsorbent dispersed to a mixture of ionic liquid
([HMIM][PF6], 50 mg) and acetone (250μL). The
mixture was rapidly injected into 20 mL of water
and standard solution (5-200 μg L−1) at pH≈6. After
ultrasonic for 5.0 min, the Cu, Pb, and Cd ions
were chemically adsorbed by four sulfur groups of
EOSiP-TS@MWCNTs ([Cu, Cd, Pb]+2→[: S-S─
EOSiP]). By procedure, the Cu+2, Cd2+, Pb+2 ions
were extracted by coordination of dative bond
of sulfur at pH= 6.5. At high pH of more than
7.5, Cu+2, Cd2+, Pb+2 ions converted to Cu(OH)2,
Pb(OH)2, Cd(OH)2 and precipitated (Recovery of
extraction: 65%, 57%, 36%). Finally, the Cu+2,
Cd2+, Pb+2 ions were extracted from waters by a
dative bond of S-S and trapped on the IL phase.
Then, the IL/ EOSiP-TS@MWCNTs phase was
collected by centrifuging for 5 min at 3500 rpm
and settled down in the bottom of the conical tube.
After back extraction of Cu+2, Cd2+, Pb+2 ions, the
resulting solution was determined by FAAS after
dilution up to 1 mL with DW (Fig. 2).
Table1. The instrument conditions for determination Cu, Pb, and Cd ions by F-AAS
Metal Lamp current Fuel Wavelength
(nm)
Slit Width
(nm)
Working
Range (μg/mL)
Copper 4.0 Air- acetylene 324.7 0.5 0.03-10
327.4 0.2 0.1-24
217.9 0.2 0.2-60
Lead 5.0 Air- acetylene 217.0 1.0 0.1–30
283.3 0.5 0.5–50
261.4 0.5 5–800
Cadmium 4.0 Air- acetylene 228.8 0.5 0.02–3
326.1 0.5 20-1000
Fig. 2. General procedure for determination Ions in the plant, soil, and, water sample
Anal. Methods Environ. Chem. J. 5 (1) (2022) 49-60
53
3. Results and Discussion
3.1. Evaluation of Lead in plant and soil
Figure 3 represents that the amount of lead
in wild spinach in three stations is above the
permissible level for human consumption (2
mg kg-1 ). While; it is within the normal range
for plants (0.1-10 mg kg-1). In addition, the
concentration of this metal in agricultural soil
of all areas is above its permissible range (10
mg kg-1). The statistical analysis was done using
SPSS 19 and ANOVA. The findings showed that
there is a significant difference between lead
concentration in selected areas (P 7.13>4.1),
where the confidence level is 95% and the
significance level is less than 0.05.
3.2. Evaluation of Cadmium in plant and soil
Figure 4 indicates that the concentration of
cadmium in wild spinach at all three stations is
close to the borderline of the permissible range. By
increasing in irrigation of wastewater, the cadmium
concentration in the plant increased a little. The
level of cadmium in wheat and grain corn is lower
than the detection limit of the atomic absorption
spectrophotometer and therefore not mentioned
in Figure 4. The agricultural soil has high level of
cadmium. The ANOVA analysis of results indicated
that at a condence level of 95% and a signicance
level of lower than 0.05, (P 2.26>4.1), there is a
signicant difference between mean concentrations
of cadmium in the selected regions.
Fig. 3. The concentration of lead in plants and soil in selected stations.
Fig. 4. The amount of cadmium in plant and soil in selected stations
Measurement of heavy metals by Nanotechnology Mohammad Reza Rezaei Kahkha et al
54
3.3. Evaluation of copper in plant and soil
Figure 5 showed that the amount of copper in plant
samples is lower than its permissible level (20
mg Kg-1) but, in soil samples at all three stations
is higher than its permissible range. The ndings
of ANOVA, at condence level of 95% and
signicance level of lower than 0.05 (P 12.43>4.1),
indicate that the difference of means in copper
measured at mentioned stations is signicant.
3.4. Optimization process
3.4.1. Digestion reagent and time
1.0 g of plants and soil samples put on the beaker
and digested with 10 mL of HNO3/H2SO4 solutions
and 2 mL of H2O2. The mixture is placed on a
heater magnet for 60 min under the hood condition,
then 12 mL of extra reagents HNO3/H2SO4/H2O2
solutions are added to samples and heated for 60
min at 90oc. The results showed us the favorite
time for digestion process is 2 h. The solutions of
digested samples (plants and soil) were determined
by F-AAS after dilution with DW.
3.4.2. The effect of the amount of adsorbent
The favorite extraction of Cu, Cd, and Pb ions
based on the EOSiP-TS@MWCNTs adsorbent
was obtained in water samples. By the UD-µ-
SPE procedure, the amount of the EOSiP-TS@
MWCNTs was studied for 1.5-1000 μg L-1, 1-200
μg L-1, 5-1500 μg L-1 concentrations of Cu, Cd, and
Pb ions, respectively. Therefore, the amount of the
EOSiP-TS@MWCNTs adsorbent between 5-50
mg was evaluated for the Cu, Cd, and Pb extraction
in 20 mL of water samples before being determined
by the F-AAS. The high extraction for the Cu, Cd,
and Pb ions was achieved at 20 mg, 18 mg and
15 mg of the EOSiP-TS@MWCNTs adsorbent in
standard and water samples. Therefore, 20 mg of
the EOSiP-TS@MWCNTs adsorbent was used at
pH 6-6.5 (Fig. 6).
3.4.3.The effect of pH
For extraction of Cu, Cd, and Pb ions in water
samples, the pH samples were studied from 2 to 11 for
20 mg of adsorbent. So, the different pH sample was
evaluated for ions extraction in water and standard
samples. The results showed, the high recovery based
on the EOSiP-TS@MWCNTs adsorbent for the Cu,
Cd, and Pb ions was obtained at pH of 5.5-6.5, 6-7,
and 6-6.5, respectively. So, pH 6 was selected for the
Cu, Cd, and Pb extraction in water samples (Fig. 7).
Also, the recoveries were decreased at less than pH
5.5 and more than pH 7. So, the pH of 6.0 was used
as optimum pH for the Cu, Cd, and Pb extraction in
water samples (Fig.7). The mechanism for the Cu,
Cd, and Pb extraction based on the EOSiP-TS@
MWCNTs adsorbent was obtained by the dative
bond of sulfur groups (MWCNTs-S:-S:) at pH 6.0.
Also, the Cu, Cd, and Pb ions participated at a pH of
more than 8 (M(OH)2).
Fig. 5. The amount of copper in plants and soil in selected stations
Anal. Methods Environ. Chem. J. 5 (1) (2022) 49-60
55
3.4.4. The effect of sample volume
Due to the Figure, the extraction of the Cu, Cd, and
Pb ions was studied for various volumes of water
samples. So, the different volumes between 5-50
mL were evaluated for a concentration of 1.5-1000
μg L-1, 1-200 μg L-1, 5-1500 μg L-1, respectively.
The efcient recovery was observed at less than 25
mL, 30 mL and 20 mL for extraction of the Cu,
Cd, and Pb ions in water samples, respectively at
pH 6.0. So, 20 mL of water samples were used as
optimum sample volume for extraction of the Cu,
Cd, and Pb ions in water samples by the EOSiP-
TS@MWCNTs adsorbent (Fig. 8).
3.4.5. Interference of ions and absorption
capacity
The effect of some ions such as Co2+, Ni2+, Zn2+,
V3+, Ag+, Mn2+, Na+, Li+, K+, Mg2+, Ca2+, S2 , CO3
2
, NO3
, F , Cl and I for extraction of the Cu, Cd,
and Pb ions in water samples were evaluated by the
UD-µ-SPE procedure. For evaluating, the different
interfering ions with various concentrations (2-10
Measurement of heavy metals by Nanotechnology Mohammad Reza Rezaei Kahkha et al
Fig.6. Effect of EOSiP-TS@MWCNTs adsorbent for extraction of Cu, Cd,
and Pb ions in water samples by the UD-µ-SPE procedure
Fig.7. Effect of pH on extraction of Cu, Cd, and Pb ions in water samples
by the UD-µ-SPE procedure
56
mg L-1) were examined for 20 mL of water samples.
The main concomitant ions in water samples were
used and the Cu, Cd, and Pb ions concentrations in
the liquid phase were determined by the F-AAS.
The results showed that the interference ions
cannot decrease the extraction recovery of the Cu,
Cd, and Pb ions in water samples by the EOSiP-
TS@MWCNTs adsorbent (Table 2).
The absorption capacities of the EOSiP-TS@
MWCNTs adsorbent are related to the size,
chemical adsorption, and surface area for the
Cu, Cd, and Pb ions extraction in water samples.
In a closed tube, 20 mg of the EOSiP-TS@
MWCNTs adsorbent were mixed to 100 mg
L-1 of the standard solution of the Cu, Cd, and
Pb ions in 100 mL of water sample at pH 6.0.
After 40 minutes, the Cu, Cd, and Pb ions were
chemically adsorbed by the sulfur group of the
Table 2. The effect of the interference of ions for extraction of the Cu, Cd, and Pb ions in water
and digested plant/soil samples by the UD-µ-SPE procedure
Interference of
Elements
Mean ratio
(CIE /CPb,Cd,Cu)Recovery Pb (%) Recovery Cd (%) Recovery Cu (%)
Zn2+ 600, 650,750 97.3 98.4 96.8
V3+ 600, 650, 800 97.2 97.9 98.5
Co2+ 400, 400, 600 98.3 97.5 98.6
Na+, K+, Li+, Mg2+, Ca2+ 800, 850,1000 98.7 99.2 98.1
F, Cl, I 900, 1000, 1200 98.2 98.6 97.9
Ni2+ 400, 500, 500 97.1 98.4 96.9
Mn2+ 500, 600,700 97.9 99.3 96.5
Ag+200, 200, 250 97.8 98.5 97.1
CO3
2  , NO3
, S2  700, 900, 900 98.0 97.5 97.8
Anal. Methods Environ. Chem. J. 5 (1) (2022) 49-60
Fig.8. Effect of sample volume on extraction of Cu, Cd, and Pb ions
in water samples by the UD-µ-SPE procedure
57
EOSiP-TS@MWCNTs adsorbent. Finally, the
final concentration of mercury in the liquid phase
was determined by F-AAS. Due to the results,
the mean of adsorption capacities (AC) of the
EOSiP-TS@MWCNTs adsorbent for the Cu, Cd,
and Pb ions was achieved at 135.6 mg g-1.
3.4.6. Validation in real samples
By the UD-µ-SPE procedure, the Cu, Cd, and Pb
ions were extracted based on the EOSiP-TS@
MWCNTs adsorbent in water samples at a pH of
6.0. The results were validated by spiking to the
water samples by the UD-µ-SPE procedure. So,
the different concentrations of the Cu, Cd, and
Pb ions were spiked by standard solutions (Table
3-5). Also, the Cu, Cd, and Pb ions in plant and
soil samples were simply measured by F-AAS
after acid digested samples and validated by a
microwave digestion system (Table 6).
Table 3. Determination of lead (Pb2+) in water samples based on the EOSiP-TS@MWCNTs adsorbent
by the UD-µ-SPE procedure
Sample Added (μg L-1)*Found (μg L-1) Recovery (%)
a Drinking water ------- ND -------
5.0 4.91 ± 0.15 98.2
b Well water ------- 15.75 ± 0.54 -------
15 29.94 ± 0.15 94.6
c Wastewater ------- 765.76 ± 28.4 -------
750 1496.32 ± 56.33 97.4
d River water ------- 9.54 ± 0.43 -------
10 19.85 ± 0.88 103.1
Mean of three determinations ± condence interval (P= 0.95, n=5)
ND: Not Detected
a drinking water prepared from Zabol city
b well water prepared from agricultural water of Zabol
c Wastewater prepared from an industrial chemical in Zabol city
d River water prepared from Helmand river of Zabol
Table 4. Determination of cadmium (Cd2+) in water samples based on the EOSiP-TS@MWCNTs adsorbent
by the UD-µ-SPE procedure
Sample Added (μg L-1)*Found (μg L-1)Recovery (%)
a Drinking water ------- ND -------
1.0 0.95 ± 0.15 95.0
b Well water ------- 6.34 ± 0.22 -------
5.0 11.46± 0.46 102.4
c Wastewater ------- 87.26 ± 3.72 -------
100 185.82 ± 8.34 98.6
d River water ------- 2.54 ± 0.11 -------
2.0 4.47 ± 0.88 96.5
Mean of three determinations ± condence interval (P= 0.95, n=5)
ND: Not Detected
a drinking water prepared from Zabol city
b well water prepared from agricultural water of Zabol
c Wastewater prepared from an industrial chemical in Zabol city
d River water prepared from Helmand river of Zabol
Measurement of heavy metals by Nanotechnology Mohammad Reza Rezaei Kahkha et al
58
4. Conclusions
Today, due to potential adverse ecological effects,
soil contamination with heavy metals has become
a critical concern for the environment. Results
obtained in this research showed that amount
of heavy metals is accumulated in soil and some
plants. Although, the mentioned plants in this
study are used to feed livestock and only in a few
cases the wheat is used to prepare our, but lack
of suitable grasslands and pastures in Sistan and
water shortage would stimulate ranchers to use
wastewater increasingly for farmlands. Also, the
Cd, Pb, and Cu were determined in digested plant
and soil samples by F-AAS. Moreover, the Cd,
Pb, and Cu ions in water and wastewater samples
based on EOSiP-TS@MWCNTs adsorbent
were determined by F-AAS after the UD-µ-SPE
procedure at pH 6-6.5. The RSD% of results was
obtained between 1.23-3.11. The mean absorption
capacity (AC) of EOSiP-TS@MWCNTs adsorbent
for Cd, Pb, and Cu ions was achieved at 144.8 mg
g-1, 127.4 mg g-1, and 134.6 mg g-1, respectively in
a static system.
5. Acknowledgments
The authors sincerely appreciate the efforts of the
chemistry laboratory of Zabol and the department
of health engineering, Zabol University of medical
sciences, Zabol, Iran.
6. References
[1] S. Qayyum, I. Khan, K. Meng, Y. Zhao, C.
Peng, A review on remediation technologies
for heavy metals contaminated soil, Cent.
Table 5. Determination of copper (Cu2+) in water samples based on the EOSiP-TS@MWCNTs adsorbent by the
UD-µ-SPE procedure
Sample Added (μg L-1)*Found (μg L-1) Recovery (%)
a Drinking water ------- 4.65 ± 0.23 -------
5.0 9.61 ± 0.39 99.2
b Well water ------- 44.94 ± 2.13 -------
50 93.96± 4.32 98.1
c Wastewater ------- 523.94 ± 20.73 -------
500 999.87 ± 43.62 95.2
d River water ------- 13.65 ± 0.47 -------
10 23.41 ± 1.08 97.6
Mean of three determinations ± condence interval (P= 0.95, n=5)
a drinking water prepared from Zabol city
b well water prepared from agricultural water of Zabol
c Wastewater prepared from an industrial chemical in Zabol city
d River water prepared from Helmand river of Zabol
Table 6. Validation of acid digested procedure for determination of the Cu, Cd, and Pb ions in plant
and soil samples by F-AAS and compared to microwave digestion system coupled to F-AAS
Sample *Microwave/F-AAS (mg L-1)*Acid digestion/F-AAS (mg L-1) A Recovery MW (%)
Plant 1.77 ± 0.11 1.82 ± 0.12 102.8
Soil 11.56 ± 0.42 10.96 ± 0.38 94.8
Plant 2.01 ± 0.09 1.93 ± 0.12 96.1
Soil 8.85 ± 0.28 8.66 ± 0.25 97.8
Mean of three determinations ± condence interval (P= 0.95, n=5, RSD< 2%)
A Recovery MW: Recovery Acid digestion/microwave digestion
Anal. Methods Environ. Chem. J. 5 (1) (2022) 49-60
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