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Ecotoxicology and Environmental Safety 164 (2018) 270–276
Contents lists available at ScienceDirect
Ecotoxicology and Environmental Safety
journal homepage: www.elsevier.com/locate/ecoenv
Passivating effect of dehydrated sludge and sepiolite on arsenic
contaminated soil
T
⁎
Chuxiong Denga,b,1, Jiajun Wena,b,1, Zhongwu Lia,b, , Ninglin Luob,c, Mei Huangb,c, Ren Yangb,c
a
College of Resources and Environmental Sciences, Hunan Normal University, Changsha 410081, Hunan, PR China
College of Environmental Science and Engineering, Hunan University, Changsha 410082, PR China
c
Key Laboratory of Environmental Biology and Pollution Control (Hunan University), Ministry of Education, Changsha 410082, PR China
b
A R T I C LE I N FO
A B S T R A C T
Keywords:
Sepiolite
Dehydrated sludge
Arsenic
Passivator
Exploring an efficient and economical method to remove arsenic from soil is of great practical significance but
there were few studies on the combined use of sepiolite and dehydrated sludge as a repair agent to passivate
heavy metals. Through soil passivation experiments, arsenic sequential extractions, and analysis of basic physicochemical properties of contaminated soils and repair agents, this study was to explore the applicability of
dehydrated sludge–sepiolite compound repair agents and dehydrated sludge individual repair agents to passivate
soil arsenic and its passivating effect. After passivation experiment, the best remediation period was 1–10 days.
The best cultivated time was 10 day using DS2 repair agent. With a comparison of passivation effect of different
repair agents, it was found that the best treatment group in individual repair agents was DS2 (10 days), and the
best treatment group in compound repair agents was S1 (1 day). The passivation effect of individual repair
agents was better than compound repair agents in 10–days cultivation. In the short term, the repair effect was
increasing and then decreasing, thus this experiment was only suitable for use as a short-term repair method. The
application of dehydrated sludge combined with sepiolite as repair agents provided a new way for both making
full use of dehydrated sludge and controlling metal mobility.
1. Introduction
Nowadays, heavy metal pollution in the soil has become an environmental problem that could not be ignored (Huang et al., 2015a,
2015b; Weil et al., 2016). Among them, arsenic in the soil will cause
great harm to the environment, and it will enter the human body
through the food chain, causing harm to the human body (Fresno et al.,
2016; Huang et al., 2014). The acceptable level (second grade, for
agriculture) in paddy soil was 30 mg/kg in the south of China
(Lingamdinne et al., 2016). The research and development of arseniccontaminated site remediation technology is a research hotspot, and
many technologies such as physical, chemical and biological remediation have been formed (Hu et al., 2007; Zhang et al., 2013). However,
there are problems such as poor control effect, serious soil destruction,
short-term and secondary pollution. Therefore, exploring an efficient
and economical method to remove arsenic from soil is of great practical
significance.
Sludge, as a by-product of urban sewage treatment process, has
become a heavy burden of sewage treatment plants due to high yield,
high treatment cost and high treatment difficulty (Iqbal et al., 2012).
Therefore, the use of sludge as a modifying agent for the rehabilitation
of arsenic-contaminated sites can not only utilize sludge bio-energy, but
also improve the heavy metal pollution of contaminated soil (Wang
et al., 2018). At present, the commonly used passivation repair agents
contained phosphate, alkaline matter, clay minerals and organic materials (Huang et al., 2018, 2016). As one of the key components of the
soil, clay minerals are one of the most environmentally friendly passivation agents (Nie et al., 2018). Sepiolite is a fibrous magnesium silicate
hydrate with strong surface adsorption and ion exchange capacity
(Shen et al., 2016). China is one of the few countries in the world that
are rich in producing sepiolite (Zhang and He, 2016). In recent years,
some scholars at home and abroad have applied sepiolite to the in-situ
passivation repair of heavy metal contaminated soil and have achieved
good results (Keller et al., 2005; Yang et al., 2013). However, there
were few studies on the combined use of sepiolite and dehydrated
sludge as a repair agent to passivate heavy metals.
In this study, dehydrated sludge was used to compound sepiolite as
compound repair agent to passivate soil arsenic, and dehydrated sludge
⁎
Corresponding author at: College of Resources and Environmental Sciences, Hunan Normal University, Changsha 410081, Hunan, PR China.
E-mail address: lizw@hnu.edu.cn (Z. Li).
1
These authors contribute equally to this article.
https://doi.org/10.1016/j.ecoenv.2018.08.019
Received 16 July 2018; Received in revised form 2 August 2018; Accepted 5 August 2018
0147-6513/ © 2018 Elsevier Inc. All rights reserved.
Ecotoxicology and Environmental Safety 164 (2018) 270–276
C. Deng et al.
Zhang et al., 2013). The sample to extractant ratio was modified to 1/
25 (1 g soil + 25 ml extractant in 50 ml centrifugation tubes) to ensure
that each extractant did not become exhausted. After each step, the
mixtures were centrifuged at 4000 g for 30 min and the supernatant was
filtered to 10 ml centrifugation tube. All extractions were conducted for
triplicate. All of the supernatant samples were tested with inductively
coupled plasma–optical emission spectrometry (ICP–OES) (Optima
5300 DV) to measure arsenic concentrations.
was applied alone as an individual repair agent to adsorb arsenic in the
contaminated soil. Through soil passivation experiments, arsenic sequential extractions, and analysis of basic physicochemical properties
of contaminated soils and repair agents, this study was to explore the
applicability of dehydrated sludge–sepiolite compound repair agents
and dehydrated sludge individual repair agents to passivate soil arsenic
and its passivating effect. The passivation effect of arsenic was used to
select the optimum ratio and repair time of the compound and individual repair agents. The best repair time was then obtained from the
experiment.
There were few studies on the combined use of sepiolite and dehydrated sludge as a repair agent to passivate heavy metals. This paper,
by using dehydrated sludge–sepiolite compound repair agents and dehydrated sludge individual repair agents to passivate soil arsenic to
improve soil, heavy metal migration behavior and biological effectiveness, to promote the recovery of vegetation and microbial activity,
realize the resource utilization of sludge dewatering, forming the low
cost of energy conservation and environmental protection repair application mode.
2.4. Analytical methods
Basic properties of soils including pH, soil organic matter, CEC
(cation exchange capacity) and free soil iron oxide were determined
according to Soil Agro-chemical Analysis (Gardi, 2001). The total metal
contents were obtained through inductively coupled plasma–optical
emission spectrometry (ICP–OES) (Optima 5300 DV; Perkin Elmer,
USA) after fully digested (Zhang et al., 2017). The pH values of repair
agents were set at 1:4 solid: liquid suspensions and were measured after
equilibration for 0.5 h. The scanning electron microscope (SEM,
TM–3000; Shimadzu, Japan), X–Ray Diffraction (XRD, D8–Advance;
Bruker, Germany) and Fourier transform infrared (FTIR, THS–108;
Nicolet, America) analysis of both repair agents and cultivated soil
samples were conducted (Yang et al., 2018). X–Ray Diffraction (XRD)
analysis was carried out using a copper target (Cu Kα), a crystal graphite monochromator, and a LynxEye array detector with step-scanning
from 3° to 80° 2θ at increments of 0.02° 2θ. Data processing of SEM,
XRD and FTIR analysis was carried out with Origin 9.0 software.
2. Material and methods
2.1. Experiment materials
Arsenic contaminated soil samples derived from high-contaminated
rice paddy field near the zhuzhou smelter in qingshuitang, Hunan
province, China (28° 09′ 35″ N, 112° 52′ 37.5″ E) (Zhang et al., 2017).
The soil samples were diverted to laboratory and then drought naturally
in the laboratory. Then the soil was ground to pass a 2-mm nylon
screen. Dehydrated sludge was collected from Yanghu Reclaimed Water
Plant in Changsha, Hunan province, China. About 500 g of dehydrated
sludge were completely drought with 100 °C in the oven before ground
to pass a 0.149 mm nylon screen. About 500 g sepiolite powder with the
particle size 0.149 mm was bought from Xinlei Mineral Powder Plant.
These materials were prepared for passivation experiment next.
3. Results and discussion
3.1. Properties of soil and passivators
The physical and chemical properties of soil directly influence the
presence of arsenic in soil, among which pH and organic matter (OM)
are the major influencing factors (Park et al., 2011). The pH of soil was
5.71 and was consistent with the values of acid soils in the south of
China (Table 1) (Zhang et al., 2017). The acid soils have a tendency to
increase the immobilization of arsenic. Content of soil organic matter
was greatly higher than general soils because of paddy field usually
accumulating large amounts of humus (Zeng et al., 2011). OM contains
many functional groups which have strong complexation and enrichment of arsenic. Content of CEC and free soil Fe2O3 in soil was about the
same as general soils (Table 1), thus they have little influence on
morphology and content of arsenic in soil in this study.
Fig. 1 showed the SEM results of sepiolite (a), dehydrated sludge (b)
and dehydrated sludge–sepiolite compound repair agents (c). Sepiolite
(a) was densely arranged in rows of acicular fibers and stacked layer
upon layer. The dehydrated sludge (b) was granular and had many
particles on the surface, which was very dense and the pore structure on
the surface was not developed. However, compared to the dehydrated
sludge, the surface of dehydrated sludge–sepiolite compound repair
agents (c) had more obvious medium pores and a large number of fine
pores, and the pore structure was more than that of dehydrated sludge.
These features would be more beneficial to the immobilization of arsenic (Zhang and He, 2016).
2.2. Passivation experiment
The three concentration levels of dry sludge–sepiolite compound
repair agents were made up through adding 2, 4, 6 g sepiolite powder to
40 g dry sludge respectively, making them mixed well. Then added
these three compound repair agents to a basin containing 400 g soil
samples and mixed them well (sepiolite powder accounting for 5, 10,
15 g/kg of soil samples) (expressed by S1, S2, S3). Furthermore, 20, 40,
60 g dry sludge serving as individual repair agents were added to 400 g
soil samples respectively (dry sludge accounting for 5%, 10%, 20% of
soil samples), and mixed them well (expressed by DS1, DS2, DS3). The
basin containing 400 g soil samples for control group (expressed by CK)
were prepared without any addition of repair agents. Hence 7 basins
were prepared and placed in a constant temperature humidity chamber
at 25 ± 1 °C. Deionized water was replenished by daily weighing
during cultivation to maintain the moisture content of soil up to 70%
(Huang et al., 2015b). Each culture pot was taken out on 1 day, 5 days,
10 days, 20 days and 40 days respectively and each time 80 g was taken
out for frozen drought in a freeze drier for 48 h. Then mixing the materials in the pot well and placed in the chamber again. The frozen
drought samples were then ground to pass a 0.149-mm nylon screen for
the following experiment and analysis.
2.3. Sequential extractions of arsenic
Table 1
General properties of soil samples.
Sequential extraction procedure (SEP) could provide important information about the defined phase associations and potential mobility
of arsenic (As) in paddy soil (Zhang et al., 2013). Based on the dissolution strength, five reagents were chosen in the method to extract
five As fractions as shown in previous studies (Wenzel et al., 2001;
Soil
pH
Soil organic matter
CEC
Free soil Fe2O3
5.71
64.35 g/kg
9.125 mol/kg
36.53 g/kg
The values were the means for each group (n = 3).
271
Ecotoxicology and Environmental Safety 164 (2018) 270–276
C. Deng et al.
a
b
c
Fig. 1. Scanning electron microscope (SEM) of passivators.
3.2. FTIR analysis of cultivated soil
3.3. XRD analysis of cultivated soil
FTIR analysis was conducted to insight into the different characteristics of functional groups between cultivated soils added with
different doses of passivators (Wen et al., 2018b). The FTIR spectroscopy of sepiolite was quite different from the other two kinds of passivators (Fig. 2a). At the band ~3450 cm−1, the lowest transmittance
was the sepiolite, meaning the highest content of ‒O–H functional
groups in sepiolites. At the band ~2925 cm−1, the lowest transmittance
was the dehydrated sludge. It showed that dehydrated sludge contained
abundant –CH2- groups compared to sepiolite. The sepiolite was shown
to have more C˭C stretching vibration of mononuclear aromatic hydrocarbons (1627 cm−1), and C‒O‒C or P‒O‒C symmetric stretching
vibration (1031 cm−1). Furthermore, dehydrated sludge–sepiolite
compound repair agents expressed similar characteristics with dehydrated sludge (Fig. 2a). One explanation was that compound repair
agents only accounted for 10% of sepiolite.
For different cultivated soils, the characteristic peaks of absorption
band were changing with different cultivated days (Fig. 2). The S3
treatment groups showed lowest transmittance in only 1 day (b) and 10
days (d) cultivated time. In the first 10 days, the soil cultivated with
compound repair agents (S3 and S1) showed the highest absorption
band of ‒O‒H, ‒CH2‒, -C˭C stretching mononuclear aromatic hydrocarbons. However, in the last 30 days, the soil cultivated with individual repair agents (DS2 and DS1) showed the highest absorption
band (Fig. 2). One reason could be that the sepiolite contained large
amounts of ‒O‒H and -C˭C stretching mononuclear aromatic hydrocarbons, increasing the contents of functional groups in compound repair agents. However, with the increasing cultivated time, the porosity
and specific surface area of sepiolite could be decreased due to the
constantly high water content and its mixture with dehydrated sludge.
Hence the effects of sepiolite on amounts of functional groups of
compound repair agents decreased and the individual repair agents
showed slightly more amounts of functional groups (Fig. 2). The other
reason could be that the functional groups of compound repair agents
reacted with metals and depleted functional groups (Gupta and
Karthikeyan, 2016). These functional groups (‒O‒H, ‒C˭C mononuclear
aromatic hydrocarbons) had been find out to have complexation and
adsorption with metals (Gorny et al., 2016; Wen et al., 2018b). Compared to passivators, the cultivated groups tended to have stronger peak
intensity and significant upward frequency shift in the absorption band
of C˭C stretching vibration of mononuclear aromatic hydrocarbons
(1627 cm−1) (Fig. 2). The more electron-withdrawing groups or hydrogen bond could account for the upward frequency shift (Wen et al.,
2018a).
XRD analysis was conducted to insight into the different characteristics of phase in various cultivated soils. At 9.6°, the characteristic
diffraction peak of sepiolite was different from the other two kinds of
passivators (Fig. 3a). The XRD spectrum of sepiolite was concentrated
on 26–31°, which was the characteristic diffraction peak of quartz
(Zhang and He, 2016). The content of quartz in dehydrated sludge was
less than dehydrated sludge–sepiolite compound repair agents (26.7°).
From Fig. 3 it can be shown that dehydrated sludge nearly belong to
amorphous substance with nearly no recognizable characteristic diffraction peak (Chen et al., 2008).
For different cultivated soils, the recognizable characteristic diffraction peaks were only 26.7° and 20.9°, meaning that the samples
belong to amorphous substance or they contained nearly no mineral
substances. However, at 20.9° the characteristic diffraction peak was
weakening with the increasing amounts of repair agent addition
(Fig. 3), especially for the DS3 and S3 treatments. The explanation
could be that the functional groups of repair agent may have complexation and adsorption with quartz and decrease the content of quartz
in soil (Dong and Wan, 2014).
3.4. Arsenic morphological grading analysis
Arsenic morphological grading analysis was conducted to insight
into the remediation effects of different repair agents on soil samples
(Table 2). Fraction of F1–F5 represented non-specifically sorbed As,
specifically sorbed As, As associated with amorphous hydrous oxides of
Fe and Al, As associated with crystalline hydrous oxides of Fe and Al,
and residual As, respectively (Wenzel et al., 2001). The forms of F4 and
F5 have a stronger stability than the other three mobile forms (Zhang
et al., 2013). It can be found out that soil samples cultivated with repair
agents greatly increased the concentrations of F4 and F5 of arsenic
forms in the first 10 days cultivation (Table 2). Among these cultivation
times, the 10 day cultivated samples (DS2) showed highest passivation
effect. It was shown that the passivation effect of dehydrated sludge–sepiolite compound repair agents played a more important role in
shorter cultivated times (S1 within 5 days), while in longer cultivated
times (10 days) the dehydrated sludge lonely took effect more (DS2)
(Table 2). The reason might be that the addition of sepiolite contained
large amounts of porosity and great specific surface area which could
bind or adsorb arsenic (Fig. 2) (Ruirui et al., 2017). However, with the
increasing cultivated time, the porosity and specific surface area of
sepiolite were decreased due to the constantly high water content and
its mixture with dehydrated sludge (Che et al., 2011). Hence the effects
of sepiolite on adsorption of arsenic decreased.
With cultivated time increasing after 10 days, the passivation effect
of repair agents decreased greatly (Table 2). One explanation of this
272
Ecotoxicology and Environmental Safety 164 (2018) 270–276
C. Deng et al.
Fig. 2. FTIR Spectroscopy of passivators and cultivated soils in 1 day (b), 5 days (c), 10 days (d), 20 days (e), 40 days (f) with 70% water content in 25 ± 1 °C
condition.
continuous high humidity and the addition of alkaline passivation
agents, the soil and passivation agents were fully mixed, resulting in the
increase of pH value of cultivated soil. Furthermore, the pH value of
cultivated soils added with compound repair agents were greatly higher
than that added with individual repair agents, and becoming the
highest in 40–days cultivation (Table 3). It was resulted from the high
alkaline characteristics of sepiolite, which consists mainly of hydrated
magnesia silicate clay mineral (Ruirui et al., 2017). In addition, it was a
reason for increasing arsenic mobility in compound repair agent treated
groups after 10 days cultivation (Table 2).
phenomenon could be that the addition of repair agents was alkaline
substances which increased soil pH greatly after 10 days cultivation
(Table 3) (Hinsinger et al., 2003; Sorokin et al., 2011). However, in the
first 10 days, the ascending range of soil pH was not significant, making
passivation of repair agents took effect. It was also shown that total As
concentrations decreased with cultivated time increasing (Table 2). The
volatilization of arsenic could make an explanation for this phenomenon (Park et al., 2011).
With cultivated time increasing, the soil pH was increasing constantly (Table 3). The soil pH value (mean value) after 40 days of
culture of each treatment (including the original soil) was higher
~18–20% than that after 1 day of culture. In the case of high humidity,
the loss of oxygen content in the original soil tends to increase the pH
value of the soil (Das et al., 2016; Hu et al., 2015). However, under the
4. Conclusion
The application of dehydrated sludge combined with sepiolite as
273
Ecotoxicology and Environmental Safety 164 (2018) 270–276
C. Deng et al.
Fig. 3. XRD Spectrum of passivators and cultivated soils in 1 day (b), 5 days (c), 10 days (d), 20 days (e), 40 days (f) with 70% water content in 25 ± 1 °C condition.
repair agents in 10–days cultivation. The best cultivated time was
10 day using DS2 repair agent. However, if 1 day cultivated time was
used, the compound repair agents (S1) treatment was advised. In the
short term, the repair effect was increasing and then decreasing, thus
this experiment was only suitable for use as a short-term repair method.
The pH value of all tested soils increased, and the mobility and bioavailability of arsenic increased, which also confirmed the previous view
repair agents provided a new way for both making full use of dehydrated sludge and controlling metal mobility. After passivation experiment, the best remediation period was 1–10 days. With a comparison of passivation effect of different repair agents, it was found that the
best treatment group in individual repair agents was DS2 (10 days), and
the best treatment group in compound repair agents was S1 (1 day). The
passivation effect of individual repair agents was better than compound
274
Ecotoxicology and Environmental Safety 164 (2018) 270–276
C. Deng et al.
Table 2
The concentrations of five arsenic forms in different treatment groups.
Fraction
CK
DS1
DS2
DS3
S1
S2
S3
1D (mg/kg)
F1
0.025
F2
3.125
F3
1.650
F4
26.925
F5
0.000
0.475
3.325
1.475
26.975
0.000
1.400
3.600
1.525
27.150
0.000
0.000
3.425
1.650
27.475
0.000
1.200
3.625
1.700
30.100
1.800
0.650
3.500
1.375
25.775
0.000
0.600
3.900
1.225
28.050
0.000
5D (mg/kg)
F1
0.000
F2
4.900
F3
2.450
F4
30.600
F5
0.000
0.400
3.500
1.675
29.350
0.000
0.700
3.875
1.675
28.150
0.000
1.500
4.075
1.700
30.250
0.700
0.975
3.825
1.250
28.550
0.000
1.000
4.075
1.700
30.025
1.450
1.05
4.025
1.225
26.350
2.050
10D (mg/kg)
F1
0.350
F2
3.925
F3
10.075
F4
9.125
F5
0.25
0.800
4.075
10.150
8.500
1.900
1.250
4.200
8.700
8.800
2.500
2.500
4.950
6.400
8.850
1.150
1.000
4.525
8.600
8.375
0.900
1.075
4.850
7.750
8.150
0.600
0.825
4.850
8.500
9.350
0.000
20D (mg/kg)
F1
0.250
F2
5.750
F3
10.850
F4
11.625
F5
0.100
0.825
6.600
8.600
9.775
0.800
1.375
7.200
8.200
9.300
0.550
2.675
7.650
6.250
7.675
0.150
1.325
7.775
8.100
8.800
1.650
1.025
7.550
7.975
7.350
0.450
1.025
7.350
8.050
6.950
0.000
40D (mg/kg)
F1
0.000
F2
2.800
F3
4.975
F4
10.150
F5
0.000
0.000
4.750
3.275
7.475
0.000
0.000
4.875
1.675
6.025
0.000
0.000
4.250
0.600
4.850
0.000
0.000
4.950
1.575
6.325
0.000
0.000
5.675
1.925
6.100
0.000
0.000
4.600
1.650
4.475
0.000
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The values were adopted from ICP–OES at arsenic wavelength = 188.979 nm.
Table 3
pH values of cultivated soils in different treatment groups.
CK
DS1
DS2
DS3
S1
S2
S3
1D
5D
10D
20D
40D
5.47
5.50
5.56
5.78
5.98
6.35
6.38
5.14
5.62
6.14
6.02
6.29
6.21
6.86
6.05
6.27
6.08
6.12
6.30
6.41
5.90
6.69
6.92
6.29
6.65
6.35
6.95
7.38
6.69
7.05
7.09
7.03
6.84
7.37
7.35
The values were the means for each group (n = 3).
on the effect of pH value on arsenic.
There are also some areas needing improvement in this study. For
example, there was only one concentration of arsenic-contaminated soil
in the experiment, and the comprehensive performances of the remediation agents could be better seen only when other soil pollution
degree is set. Hence more studies need researching in future.
Acknowledgements
The authors gratitude to the anonymous reviewers for providing
suggests and advices. This work was funded by Key R&D Program of
Science and Technology of Hunan Province in China (No. 2017SK2351)
and National Natural Science Foundation of China (No. 51521006).
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