Hindawi

Journal of Chemistry
Volume 2018, Article ID 5036581, 8 pages
https://doi.org/10.1155/2018/5036581

Research Article
Evaluation of Acid Leaching on the Removal of Heavy Metals and
Soil Fertility in Contaminated Soil

Chen-Yao Chu and Tzu-Hsing Ko

Anxi College of Tea Science, Fujian Agriculture and Forestry University, Fuzhou 350002, China

Correspondence should be addressed to Tzu-Hsing Ko; hsingko@gmail.com

Received 12 March 2018; Accepted 8 May 2018; Published 4 June 2018

Academic Editor: Amit Bhatnagar

Copyright © 2018 Chen-Yao Chu and Tzu-Hsing Ko. This is an open access article distributed under the Creative Commons
Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is
properly cited.
Heavy metal-contaminated soils were leached with various acid reagents, and a series of treatments was assessed to understand soil
fertility after acid leaching. Aqua regia digestion and a five-step sequential extraction procedure were applied to determine heavy
metal distribution. The average total concentrations of Zn, Cd, Cu, and Pb for contaminated soil were 1334, 25, 263, and
525 mg·kg−1 based on the ICP/AES quantitative analysis. Other than Pb extracted by H2SO4, over 50% removal efficiency of other
heavy metals was achieved. A five-step sequential extraction revealed that the bound-to-carbonate and bound-to-Fe-Mn oxides
were the major forms of the heavy metals in the soil. The addition of organic manure considerably promoted soil fertility and
increased soil pH after acid leaching. Seed germination experiments demonstrated that after acid leaching, the soil distinctly
inhibited plant growth and the addition of manure enhanced seed germination rate from 35% to 84%. Furthermore, the procedure
of soil turnover after acid leaching and manure addition greatly increased seed germination rate by 61% and shortened the initial
germination time. Seed germination in untreated soil was superior to that in acid-leached soil, illustrating that the phytotoxic
effect of acid leaching is more serious than that of heavy metals.

1. Introduction of heavy metals, polychlorinated biphenyls (PCBs), and

polychlorinated dibenzo-p dioxins and dibenzofurans
Soil pollution is a serious environmental issue worldwide (PCDD/DFs) into the water [7]. Due to lack of environ-
[1, 2]. Heavy metals are considered a serious soil pollutant mental consciousness during early agricultural cultivation,
because of their toxicity, persistence, and nondegradable the Er-Jen River was used as an irrigation source, which
characteristics in the environment [3–5]. In addition, the caused a detrimental heavy metal contamination to the
self-purification process of heavy metals present in con- paddy field. Therefore, remediation of the contaminated
taminated soil is slower than that in contaminated air and farmland near the Er-Jen River is of high priority.
water; thus, inadequate treatment of contaminated soil can To remediate heavy metal-contaminated soils, many
pose a great human health risk. In Taiwan, more than 50,000 effective techniques have been developed and employed,
hectares of farmland has been contaminated by heavy metals such as electrokinetics, phytoremediation, chemical ex-
to the fourth level classification, and more than 160 sites traction, vitrification, solidification, stabilization, and flo-
have been identified to be contaminated by heavy metals. tation [8–11]. However, soil washing is the most commonly
Surveys state that approximately 785 hectares of farmland is used treatment technology for remediation of metal-
contaminated by zinc to the fifth level classification [6]. contaminated soil. Several washing reagents, namely,
The Er-Jen River located in the south western Taiwan is water, acids, bases, chelating agents, alcohol, and other
one of the most seriously contaminated rivers, caused by the additives, have been investigated [12]. Increased attention
waste from metal reclamation, smelting, and disposal of has been recently focused on the use of citric acid or the
motors and electrical capacitors that released a large amount chelating agents such as ethylenediaminetetraacetic acid
2 Journal of Chemistry

(EDTA), nitrilotriacetic acid (NTA), and diethylene- 103.2% for Zn. The standard stock reagents (Merck, Germany)
triaminepentaacetic acid (DTPA) to remove heavy metals containing 1000 mg·kg−1 of metals were used. Calibration
from contaminated soils [13–15]. reagents containing between 0.5 and 5000 mg·kg−1 of Cd, Cu,
Although acid leaching is an effective treatment for Pb, and Zn in 3% HNO3 were daily prepared.
heavy metal removal from soil, it severely damages soil
fertility and its use for remediating farmland is time-
consuming. The rapid enrichment of soil fertility after 2.3. Acid Leaching Experiment. In this study, five acid re-
acid leaching is increasingly becoming a topic of concern for agents were taken into account for leaching heavy metals
farmers. Therefore, this study used acid leaching techniques from contaminated soil, including 0.05 M HNO3, HCl,
to remove heavy metals from contaminated farmland that H3PO4, and H2SO4. A liquid-to-soil ratio of 1:10 was
can be helpful in understanding the mobility and bio- adopted by adding 5 g of soil with 50 mL above acid reagents
availability of metals in contaminated soil and to investigate in a glass vessel, and they were continuously stirred at
the extraction efficiencies of heavy metals. In addition, the 100 rpm for 5 h. After leaching experiments, the suspension
assessment of soil fertility and seed germination tests after was centrifuged at 3500 rpm for 30 min and then was filtered
the acid leaching procedure were investigated to understand through a 0.2 μm membrane filter for metals analysis. The
the condition of remediation in the contaminated farmland. contents of metals were analyzed by ICP/AES. To reduce the
systematic errors, duplicate measurements were carried out
for each sample, and the average values were determined. A
2. Experimental five-step sequential extraction procedure used in this study
was developed by Tessier [20]. The five fractions of bound
2.1. Sampling Area. Soil samples were collected from the top heavy metals included the following: exchangeable form
layer (0–30 cm) of a paddy field near the Er-Jen River in Tainan (EXC) was extracted with 1 M NH4OAc at pH 7, carbonates
city, Taiwan province, China, which has been recognized as form (CAR) was extracted with 1 M NaOAc at pH 5, Fe–Mn
a previous history of irrigation with metals-rich wastewater. oxide form (MNO) was extracted with 0.04 M NH2OH·HCl
The paddy field contaminated with heavy metals has been in 25% HOAc, organic matter and metals associated with
strictly prohibited cultivating. Soil samples were collected by easily oxidizable solids or compounds (OM) were extracted
mixing ten subsamples from each site within a 50 × 50 meter with H2O2 (30%) at pH 2 and 0.02 M HNO3, and residual
area and were recorded for the central point position by using form (RES) was extracted with a 5 : 1 mixture of HF-HClO4.
GPS equipment. The soil samples were air-dried at room All extracted reagents were centrifuged for 30 min at
temperature and then were ground with an agate mortar to 10000 rpm and filtered with a 0.2 μm Teflon filter. The
pass through a 2 mm sieve. After sieving, the soil samples were suspensions were analyzed by ICP/AES. Soil particle size is
experimentally pretreated by a vortex mixer with 100 rpm for an important factor to affect removal efficiency of heavy
24 h to ensure the complete mixing of the samples. metals. However, it is difficult to screen soil particle size
when the in situ remediation is throughout used to a real
2.2. Chemical Analysis. Soil properties, including soil pH, heavy metal-contaminated site. Therefore, the effect of soil
organic matters, soil texture, and cation exchange capacity, particle size is not mentioned in this study.
were determined. Particle size distribution was obtained by
the pipette method after removal of carbonate, organic 2.4. Seed Germination Experiment. For the germination tests,
matters, and MnO2. Carbonate was removed by 1 M NaOAc seeds of cabbage (Brassica chinensis L.) were used because this
with a pH 5 at 60°C, and organic matters and MnO2 were species is a general vegetable and can be popularly seen for
digested by 30% H2O2 [16]. The soil pH value was measured a whole year. Twenty-five seeds of cabbage were sowed in
on a mixture of 1 : 1 soil/deionized water by a glass electrode a sterilized individual tray (15 × 20 × 3 cm3) containing
[17]. Organic matter content was determined by the 1200 cm [3] of modified leached soils. Duplicate of the seed
Walkley–Black wet oxidation method [18]. Cation exchange germination experiment was simultaneously conducted. The
capacity was determined by the ammonium acetate method trays were placed in a greenhouse at 25–28°C and 70% hu-
at pH � 7 [19]. Total content of heavy metals in soils was midity. The experiment was examined daily for 30 days, and
extracted by aqua regia digestion with a volume ratio of 1 : 3 seeds were recognized to have germinated when the cot-
HNO3/HCl at 120°C for 8 h. The suspension was filtered yledon was observed. After cotyledon appearance, the root
through a 0.2 μm filter paper after the digestion process and lengths in each tray were measured and recorded every
was placed into precleaned 100 ml volumetric flasks with 12 h. The untreated soil sample was also conducted under
0.5 M HNO3 for analysis. The contents of heavy metals were the identical condition for comparison. To assess the seed
analyzed by inductively coupled plasma atomic absorption germination criteria, the percentage of relative seed ger-
spectrometry (ICP/AES). To preclude unexpected contam- mination was chosen to understand the seed germination
inations in the analysis procedure, all equipment used were condition [21].
washed with a phosphate-free soap and cleaned with
deionized H2O. The detection limits for metals were as 3. Results and Discussion
follows: Cd (0.05 mg·kg−1), Zn (0.02 mg·kg−1), Pb
(0.06 mg·kg−1), and Cu (0.05 mg·kg−1). The percentages of The physical and chemical properties of the soil samples
recoveries for each metal were ranged from 96.7% for Cd to along with their total heavy metal concentrations are listed
Journal of Chemistry 3

Table 1: The brief description of contaminated soil used in this 100

study.
90
Property Original soil
Texture Sandy clay loam 80
pH 7.6 ± 0.11
Organic matter (%) 1.91 ± 0.18 70
CEC (cmol·kg−1) 4.58 ± 0.21

Removal efficiency (%)

Total N (%) 0.13 ± 0.01 60
Total P (%) 2.82 ± 0.10
Total K (%) 1.74 ± 0.04 50
Available N (mg·kg−1) 22.4 ± 1.17
Available P (mg·kg−1) 187 ± 8.60 40
Available K (mg·kg−1) 764 ± 40.54
Total metal concentrations 30
(average content, mg·kg−1)
Zn 1334 ± 83 20
Cd 25 ± 3
Cu 263 ± 18 10
Pb 525 ± 31
0
HNO3 HCl H3PO4 H2SO4
Cd Pb
in Table 1. The average total concentrations of Zn, Cd, Cu,
Zn Cu
and Pb were 1334, 25, 263, and 525 mg·kg−1, respectively,
and their maximum concentrations of Zn, Cd, Cu, and Pb Figure 1: Removal efficiency of heavy metals by using various acid
were 4852, 46, 1470, and 1430 mg·kg−1, respectively. The reagents.
total heavy metal concentrations were not only higher than
the tolerable limits recommended by the World Health
600
Organization (WHO) and European Union (EU), but also
exceeded the Chinese standard for agricultural soil [22]. This 550
contaminated site needs to be appropriately treated to avoid 500
heavy metals moving into deeper layers and causing phreatic
450
zone pollution. As shown in Table 1, the organic matter
Concentration (mg·kg–1)

content is much lower than the normal content. This is 400

because that the Er-Jen River is contaminated by metal 350
reclamation, smelting, and electrical capacitors and results
300
in a high content of heavy metal accompanying a low pH
value. Due to long-term irrigation from Er-Jen River, it is 250
believed that the organic content of soil in this site is much 200
lower than that of the uncontaminated site. The removal 150
efficiency of heavy metals by various acid reagents is shown
in Figure 1. The leaching experiments indicated that Zn and 100
Cu had the highest removal efficiency and more than 70% 50
removal efficiency was achieved for all acid reagents. For the 0
Cd species, regardless of the acid reagents used, the removal EXC CAR MNO OM RES
efficiency ranged from 55% to 66%, indicating a high
Cd Pb
chemical affinity between the Cd and the soil, yielding lower Zn Cu
removal efficiency for all acid reagents. A sequential ex-
traction method was used to determine the Cd distribution Figure 2: The sequential fractionations of heavy metals in con-
in the surface sediment and found the major binding taminated soil.
structure between Cd and soil was attributed to a residual
form [23]. Among the four acid reagents, HNO3 had the
lowest Cd, Zn, and Cu removal efficiency, whereas H2SO4 showed that Cd was distributed predominantly in the re-
had the highest Cd, Zn, and Cu removal efficiency; this result sidual form with a value of 45% in the contaminated soil
was not observed for Pb. To further understand the speci- [24]. Thus, the Cd retained in the crystal lattices of minerals
ation distribution of heavy metal in soil, the chemical se- has a strong bond and consequently is not easily released
quential extraction was used and is shown in Figure 2. The into the environment. The overall percentage of Cd in the
highest Cd concentration was associated with the RES fractions was in the order: RES > OM > CAR > MNO > EXC.
fraction, whereas the EXC had the lowest concentration. The Unlike Cd, the largest portion of Zn was observed in the
presence of Cd in the RES fraction was consistent with the CAR fraction (39%) and followed in the descending order of
result obtained by Mendoza et al. in which their report EXC > MNO > OM > RES. This fraction could be easily
4 Journal of Chemistry

2.5 0.30

0.25
2.0

0.20
Organic matter (%)

1.5

Total N (%)
0.15

1.0
0.10

0.5
0.05

0.0 0.00
Original soil HNO3 HCl H3PO4 H2SO4 Original soil HNO3 HCl H3PO4 H2SO4

(a) (b)
2.5 6000

5000
2.0

4000
Total P (mg·kg–1)

1.5
Total K (%)

3000

1.0
2000

0.5
1000

0.0 0
Original soil HNO3 HCl H3PO4 H2SO4 Original soil HNO3 HCl H3PO4 H2SO4

(c) (d)

Figure 3: The changes in content of (a) organic matter, (b) total N, (c) total K, and (d) total P after leaching by various acid reagents.

made exchangeable under conditions such as pH change soil and repeat the cycle [26]. These forms of metals are
[25]. Pb and Cu demonstrated an identical trend in that CAR potentially dangerous for plants because they can transform
and MNO appeared to be the major fraction. The proportion into being bioavailable under environmental changes [27].
of heavy metals bounds to Fe-Mn oxides was highly variable Organic matter (OM), nitrogen (N), potassium (K), and
and depended on the depth of the water and redox reactions phosphor (P) are important substances for vegetable and
with the soils. The redox cycle is important in controlling Fe plant growth in soil. To understand the changes in these
and Mn in most aquatic and soil systems. However, it varies substances after acid reagents leaching, OM, total N, total K,
seasonally in summer, when the oxygen between the water and total P contents were determined and are depicted in
and soil interface often decreases. This causes the reduction Figure 3. The content of OM in the soil decreases by 18.5%
of Fe3+ and Mn4+ into soluble Fe2+ and Mn2+, which is and 8.74% when H3PO4 and H2SO4 were used for pickling,
transported upward in the water column and oxygenated, respectively. No significant change in the OM content for
resulting in the reoxidation of insoluble metals to settle the HNO3 and HCl was observed. The total N content increased
Journal of Chemistry 5

8.0 power. Figure 5 shows the changes in the OM, total N, total P,
and total K contents as a function of the duration after HCl
leaching and fertilization treatment. The identical feature
could be observed after the addition of organic manure, which
7.5 increased the OM, total N, total P, and total K content within
30 days. Over the first 15 days, the OM and total N contents
became more than twice of this manure addition, and a steady
7.0
state was gradually achieved. However, the total K content
pH

rapidly increased with the duration with the highest content

value of 2.5% within 5 days. On the basis of these findings, the
organic manure additive improves soil fertility within a short
6.5 period. To assess the suitability of farmland for cultivation,
a seed germination experiment was performed to evaluate
suitability for planting after various treatments. Seeds were
cultivated in an incubator and observed daily for germi-
6.0 nation with the seed germination rate as a function of time
0 10 20 30 40 50 60 70 80 90 100 110
at various treatments presented in Figure 6. The lowest
Duration period (day)
germination rate was observed when soil was treated
Figure 4: The change in soil pH as a function of the duration period through acid leaching because after acid leaching the soil
after HCl leaching and fertilized by adding organic manure. fertility decreased and affected plant growth. On the other
hand, initial seed germination occurred earlier than the
other treatments. Although heavy metals were moderately
removed after acid leaching, the nutrient loss was a major
by 57.07%, 22.86%, and 21.47% after leaching with HNO3, barrier to seed germination. After the addition of organic
H3PO4, and H2SO4, respectively. The N content decreased by manure, the seed germination rate considerably increased
10.65% after leaching with HCl. Higher N content after by more than 80% and the initial seed germination time was
HNO3 treatment may be attributed to the presence of NO3− four days, earlier than that of the experiments assessed after
released from HNO3 during the leaching process. Figure 3(d) acid leaching. Notably, the seed germination rate in un-
shows the phosphorus content in the soil after acid treated soil was superior to that in acid-leached soil. This
leaching. All reagents, except H3PO4, reduced the total P demonstrates that the inhibition effect of acid leaching to
content after acid leaching. No significant difference was the plant is more serious than that of heavy metals, and the
noted between the original soil and the other three acid addition of organic manure could be a suitable approach to
reagents. The P content increased by 83.17% after leaching by improve soil fertility and plant cultivation. To obtain
H3PO4, presumably because of the presence of PO43− released a higher seed germination rate, the procedure of soil
from the H3PO4 during leaching process. The result of turnover was applied simultaneously. As shown in Figure 6,
changes in total K is also depicted in Figure 3(c). The soil K the procedure of adding manure to soil turnover rapidly
concentration changed because of acid liquid precipitation. increased the seed germination rate and initial seed ger-
HNO3 reduced the total K content by 26.2%, followed by mination time, and a seed germination rate of approxi-
others in a descending order HCl > H3PO4 > H2SO4. Com- mately 85% was achieved. The procedure of soil turnover
mercial organic manure was used after the leaching treatment diluted heavy metals and acidic species and thus resulted in
to fertilize the soil. Commercial organic manure contains 21% the redistribution of these species.
OM, 4.2% total N, 4.1% total P, and 3.5% total K. Most Although seed germination rate is a suitable indicator to
manure containing considerable amounts of soluble salts evaluate soil fertility, heavy metal concentration in test
increases soil’s electrical conductivity (EC), resulting in plants should be considered to ensure food safety. Therefore,
damage to plants. The result of the experiments showed that cabbage roots and leaves were collected and analyzed to
the EC increased after manure treatment and reached stability understand heavy metal distribution. The experimental re-
after 30 days. Over 30 days, the EC ranged from 0.86 to sult is presented in Table 2. The major uptake was found in
0.41 mS·cm−1, an acceptable range for plant growth. Figure 4 the root of cabbage, and the fraction of Cd, Zn, Pb, and Cu
shows the changes in soil pH as a function of duration after uptake by the root was 46.8%, 51.3%, 17%, and 25.4%, re-
HCl leaching and fertilization by organic manure. The initial spectively. This finding is in agreement with the observation
pH for original and leached soils was 7.6 and 6.3, respectively. of Shi et al., who reported that heavy metal concentration is
The acid leaching treatment reduced the soil pH conse- much higher in the root than in the shoot and leaf [28]. The
quentially caused an unfavorable effect to crops cultivation. root is the first mode of entry for heavy metal pollutants
The pH increased with the duration and reached a maximum from the soil into the plant. Nevertheless, it excretes organic
of 7.02 at 30 days; it then gradually decreased and eventually acids, amino acids, sugars, and growth substances into the
stabilized to approximately 6.3. The addition of organic rhizosphere, affecting metal adsorption. By changing the
manure significantly improved soil pH over a short period; physiochemical properties of the rhizosphere, the heavy
however, in the long-term, the soil pH returned to a meta-acid metals will be detained in the roots through chelation,
state, which was probably associated with the soil buffering complexation, and disposition with root exudates. Notably,
6 Journal of Chemistry

6 0.5

5
0.4
Organic matter (%)

Total N (%)
0.3

0.2
2

1 0.1
0 10 20 30 40 50 60 70 80 90 100 0 10 20 30 40 50 60 70 80 90 100
Duration period (day) Duration period (day)
(a) (b)

6000 3.0

5000
2.5
Total P (mg·kg–1)

4000
Total K (%)

2.0

3000

1.5
2000

1000 1.0
0 10 20 30 40 50 60 70 80 90 100 0 10 20 30 40 50 60 70 80 90 100
Duration period (day) Duration period (day)
(c) (d)

Figure 5: The changes in contents of (a) organic matter, (b) total N, (c) total P, and (d) total K as a function of the duration period after HCl
leaching and fertilized by organic manure.

in this case, the Pb uptake by the root was the lowest, when used to cultivate plants. The procedure of soil turnover
whereas a much higher fraction was noted for Zn; the leaf may be a suitable approach to overcome this obstacle.
demonstrated the same result. Pb and Zn are essential ele-
ments for plants growth, but their excessive amounts in soil 4. Conclusions
lead to the inhibition and poisoning of plants. The normal Pb,
Cu, and Zn contents in plants are 0.5–10 mg·kg−1, A series of acid leaching tests and soil fertility assessment for
3–30 mg·kg−1, and 10–150 mg·kg−1, respectively, whereas contaminated soil containing Cd, Pb, Zn, and Cu were
their toxic concentrations to plants are 100–400 mg·kg−1, performed to investigate leaching behavior. Most heavy
70–400 mg·kg−1, and 60–125 mg·kg−1, respectively [29]. Here, metals could be removed through acid leaching with a nearly
the Pb, Zn, and Cu concentrations in bulk cabbage were 60% removal efficiency achieved. The major species for Cd,
120.23 mg·kg−1, 283.52 mg·kg−1, and 37.14 mg·kg−1, re- Zn, and Cu were distributed in residual, bound-to-
spectively. Except Cu, Pb and Zn concentrations were slightly carbonate, and bound-to-Fe-Mn oxides forms, respectively.
higher than the aforementioned range, indicating the soils The addition of organic manure distinctly increased soil
after acid leaching and organic manure addition remain a risk nutrient content as well as soil pH within a short period. Seed
Journal of Chemistry 7

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