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In: Management of Hazardous Residues ...

ISBN 978-1-61209-526-4
Editor: M.J. Balart Murria, pp.
2011 Nova Science Publishers, Inc.

Chapter 3

INORGANIC AND ORGANIC SOIL


AMENDMENTS USED FOR
THE IMMOBILIZATION OF
CADMIUM IN CONTAMINATED SOILS
Silvana Irene Torri*
School of Agronomy, University of Buenos Aires
Av San Martn 4453, Buenos Aires, C1417 DSE, Argentina

ABSTRACT
Chemical stabilization is an in situ remediation method that uses
inexpensive amendments to reduce contaminants availability in polluted
soil. Amendments may adsorb, bind or co-precipitate the contaminating
elements. Cadmium (Cd) is known as more mobile and soluble than
many other potentially trace element in soils. Furthermore, it has been
identified as a major toxic element reaching the food chain, directly
through crop uptake or indirectly through animal transfer. Recently there
has been increasing interest in the immobilization of Cd using a range of
inorganic compounds, such as lime and phosphate compounds, or organic
compounds, such as biosolids compost. In this chapter, the feasibility of

E-mail: torri@agro.uba.ar

Silvana Irene Torri


using these amendments to immobilize Cd in Cd-contaminated soils is
discussed.

1. INTRODUCTION
Soil contamination with potentially toxic elements (PTE) is a worldwide
problem. Excessive accumulation of PTE in agricultural soils may not only
result in environmental contamination, but also lead to elevated PTE uptake by
crops, which may affect food quality and safety (McLaughlin and Singh 1999;
Zhu et al, 2008). Among PTE, cadmium (Cd) and lead (Pb) have been
recognized as priority pollutants by the United States Environmental
Protection Agency (USEPA) and other organizations. Cadmium may easily
reach the food chain through common agricultural practices such as
fertilization, irrigation or pesticide application (Mees et al., 2002). Other
anthropogenic activities primarily associated with industrial processes,
atmospheric fallouts, manufacturing and the disposal of domestic and
industrial waste materials may also result in a significant input of soil Cd.
The Pampas Region, Argentina, is one of the largest temperate field
cropland areas of the Southern Hemisphere. At present, the concentrations and
dispersion values of PTE in agricultural or grazed soils in this region are
similar to other non-contaminated soils of the world (Lavado et al., 2004).
However, these soils recently started to receive an increased amount of
phosphate fertilizers. Depending on its provenance, Cd in the phosphate rock
can be present in relatively large amounts, from 0 to 150 mg Cd kg1 (Lpez
Camelo et al, 1997). Hence, there is an increasing local concern for protecting
the environmental quality of croplands of the Pampas Region.
In contrast to agricultural soils, some urban areas of Argentina and its
surroundings are starting to show signs of anthropogenic accumulation of Cd
and other PTE (Wannaz et al, 2006; Lavado, 2006). Anthropogenic sources of
cadmium for urban and peri-urban areas include traffic emission (vehicle
exhaust particles, tire wear particles, brake lining wear particles), industrial
emission (power plants, coal combustion, metallurgical industry, chemical
plants, etc.), domestic emission, weathering of building and pavement surface,
atmospheric deposition and so on (Sindern et al, 2007; Christoforidis, Stamatis
2009; Lu et al, 2009; Morton-Bermea et al, 2009; Wei, Yang 2010). Some
alluvial soils of the Riachuelo River in Buenos Aires province were also
reported to accumulate between 1-5 mg Cd kg-1 due to anthropogenic activity
(Ratto et al, 2004). High concentration of Cd in sediments may lead to Cd

Inorganic and Organic Soil Amendments ...

release to water and pose risk to aqueous organisms and human health. Lavado
et al. (1998) reported that concentrations of Cd and other PTE in some urban
and peri-urban soils of Buenos Aires province, were much higher than
thresholds proposed by several international standards and by the Argentine
Hazardous Wastes Law (law 24051). Like most other metals, Cd does not
undergo microbial or chemical degradation and therefore persists in soils for a
long time after its introduction. Cadmium has been identified as a major toxic
trace element reaching the food chain, directly through crop uptake or
indirectly through animal transfer (Adriano 2001). Furthermore, Cd is the only
metal that might pose human or animal health risks at plant tissue
concentrations that are not generally phytotoxic (Peijnenburg et al. 2000).
Once ingested or absorbed by humans, it has a long biological half-life and
causes numerous health concerns (Goyer, 1997).
Due to the growing size of the population of Buenos Aires City,
horticulture in urban areas and its surroundings is a means of employment of
migrants from agricultural areas or inmigrants from neighboring countries
(Schnitzler et al., 1999). According to the United Nations (2001), nearly all of
the expected growth in population in the next two decades (20102030) will
take place in urban areas, with almost no growth in the rural population. As a
result, peri urban environments are conducive to intensive production of
perishable foods (fruits, vegetables, meat and dairy products) to be consumed
by urban inhabitants. Many studies have shown that Cd is readily taken up by
roots crops and translocated to aerial organs where it accumulates to high
levels (Jiang et al, 2010; Perilli et al, 2010). In particular, vegetables are
capable of accumulating relatively high levels of Cd in the edible portion at
concentrations that may exceed food safety limits (McLaughlin et al., 2006,
Peralta-Videa et al., 2009; Yang et al, 2009).

2. CADMIUM AVAILABILITY IN CONTAMINATED SOILS


Soils normally contain 0.11.0 mg Cd kg1 (Kabata-Pendias, 2004). Total
Cd concentration over 10 mg kg1 may be toxic for plants, inhibiting root and
shoot growth (Palgyi et al., 2006), decreasing soil microbial activity and soil
fertility (Belimov et al, 2005). Nevertheless, total soil concentration of PTE
gives some indication of the level of contamination, but provides no insight
into element bioavailability or mobility. Traditionally, bioavailability refers to
the biologically available fraction that may be taken up by organisms and may
react with its metabolic machinery (Campbell, 1995), or it refers to the fraction

Silvana Irene Torri

that can interact with a biological target. The chemodynamics of Cd in the soil
environment is controlled by its interactions with both solid and aqueous
phases. Processes such as adsorption/desorption, ion exchange,
precipitation/dissolution, soil and solution phase composition regulate the
toxicity and mobility of Cd through soil profiles (Alloway, 1990; Helmke and
Naidu, 1996). Single extraction and/or sequential extraction procedures are
used to estimate the distribution of PTE associated with particular phases in
soils and sediments. A large number of sequential extraction schemes have
been proposed for soils, generally attempting to identify PTE held in any of
the following fractions: soluble, exchangeable, sulfide/carbonate-bound,
organically bound, oxides-bound, and residual or lattice mineral bound
(Tessier et al, 1979; Sposito et al, 1982; Shuman 1985; Rauret et al, 1999).
Assessment of metal mobility and bioavailability in soils and sediments using
sequential extraction proceduress assumes that mobility and bioavailability
decrease in the order of extraction. Thus, metals in the exchangeable fractions
are most mobile and bioavailable, whereas metals in residual fraction are
tightly bound and least mobile under natural environmental conditions.
Technologies to minimize the chances of Cd reaching the food chain aim to
reduce the concentration of bioavailable forms by increasing adsorption,
precipitation or entrapment of Cd in crystal lattices (Hamon et al, 2002).

3. REMEDIATION TECHNIQUES
Different remediation techniques have been developed in order to reduce
PTE and, in particular, Cd bioavailability in soils (Chen, Lee 1997; Gray et al.,
2006). Several physicalchemical treatments based on excavation, landfilling,
thermal treatment, acid leaching and electro-reclamation have been proposed.
Unfortunately, these methods are not suitable for practical application, because
of their high cost and low efficiency, limiting its use on vast contaminated
areas (Khan et al, 2005). Moreover, they are often environmentally invasive
and do not permit a natural reshaping of the environment (Lombi et al., 2002).
In contrast, bioremediation is cost-effective and environmentally friendly. Two
bioremediation technologies, phytoremediation and stabilization, have been
widely investigated for the remediation of Cd polluted sites (Dushenkov et al,
1997; Carrillo-Gonzlez et al, 2006).
Phytoremediation of Cd-contaminated soils is a fast-expanding
technology, which uses specific plants species which have an innate ability to
tolerate and accumulate Cd (Blaylock and Huang, 2000; Ghosh, Singh 2005;

Inorganic and Organic Soil Amendments ...

2004). This technology is increasingly being considered as an alternative to the


conventional engineering-based remediation methods and has the advantage of
being cost effective, environmental friendly, and less disruptive to the soil and
therefore the associated site ecosystem (Marques et al, 2009). However, the
ability to accumulate Cd varies significantly between species and between
cultivars within a species (DalCorso et al, 2008). Further, this technique may
require extremely long times, e.g. centuries, to achieve the complete
remediation of soil. The requisite time with no agricultural activity during the
remediation process and the necessary biomass treatment after remediation are
the major drawbacks that limits its use (Marques et al, 2009).
Considering the limitations described above, in situ immobilization is
gaining considerable interest over the last decade (van der Lelie et al., 2001).
The aim of immobilization techniques is to use a soil amendment to alter the
soil chemistry and sequester or absorb PTE into the amendments matrix. In
this way, the bioavailable fraction is reduced, and the detrimental effects of
PTE on environmental receptors, such as microorganisms, plants, animals,
water bodies, and humans are minimized (Castaldi et al, 2005). A range of
inorganic compounds, such as lime and phosphate fertilizers (Bolan et al.
2003a, b; Hong et al, 2010 a) or organic amendments (Mohamed et al, 2010;
Basta et al., 2001) have been used to immobilize Cd in contaminated soils.
Various mechanisms have been attributed to the effect of these amendments,
including enhanced Cd adsorption (Adriano, 2001); precipitation of metals as
phosphates, hydroxides or carbonates (Basta et al., 2001); and formation of
insoluble Cdorganic complexes in the presence of organic amendments
(Shuman 1999; Farrell, Jones 2010). This Chapter discusses the potential
values of phosphate compounds and biosolids compost, relative to their ability
to immobilize Cd in Cd-contaminated soils.

3.1. Phosphate Compounds


Although phosphate amendments have been initially applied to remediate
Pb-contaminated soil, they also proved to immobilize Cd and Zn in
contaminated soils (Lambert et al., 1997; Hettiarachichi et al., 1998).
Moreover, addition of phosphorus to soil is the basis of a patented process to
reduce bioavailability of PTE (Pierzynski and Hettiarachchi, 2002). Sources of
phosphate may include either water-insoluble minerals, such as natural or
synthetic apatites and hydroxyapatites, or water-soluble salts, such as
diammonium phosphate and phosphoric acid. Depending on the source, soil

Silvana Irene Torri

application of phosphate may cause the precipitation of Cd or phosphateinduced Cd2+ adsorption.

Water-insoluble Phosphate Compounds


Many apatite [Ap, Ca10(PO4)6(OH,F,Cl)2] based materials, such as natural
mineral phosphate and synthetic apatite, bind Cd and other PTE ions from
aqueous solutions and soils (Mandjiny et al., 1995; Chen et al., 2007a; Chen et
al., 2007b; Peld et al, 2004; Knox et al, 2003). Calcium-hydroxyapatite (HAp,
Ca10(PO4)6(OH)2) has also attracted considerable interests because of its high
adsorption capacity, biological compatibility, low solubility in basic and
neutral media, excellent buffer property, high stability and low cost. Both
synthetic and natural HAp reduced bioavailability of soil Cd, limiting its
uptake by crops (Chlopecka, Adriano 1997; Keller et al, 2005). In general,
HAp has demonstrated the best removal efficiency due to its moderate
solubilitybetween highly insoluble and highly soluble phosphate bearing
materials such as phosphate rock and phosphate fertilizers, respectively
(Hodson et al, 2000).
Several mechanisms were proposed to explain the sorption process of Cd
on apatites, including superficial sorption, ion exchange, and precipitation.
The sorption process was studied in detail by Jeanjean et al (1995) and
Fedoroff et al. (1999). A detailed description of the structure of calciumhydroxyapatite was provided by Beevers and McIntyre (1945) and later by
Kay and Young (1964) and Hughes et al. (1989). Calcium-hydroxyapatite
crystallizes in the hexagonal system, where Ca2+ occupies two different
crystallographic sites, Ca(1) and Ca(2). Calcium(1) is found on ternary axes at
x=1/3, y =2/3 whereas Ca(2) is found at sites with symmetry m at z=1/4,
z=3/4; HO- ions are found in channels along the hexagonal screw-axes, at
z=0,198. Sorbed Cd ions substitute for Ca, which is released into the soil
solution (Takeuchi, Arai 1990; Mandjiny et al, 1998). The ion exchange
reaction mechanism can be expressed as (Equation 1):
Ca10(PO4)6(OH)2 + x Cd2+ (Cdx,Ca10x)(PO4)6(OH)2 + x Ca2+
(Equation 1)
For low sorbed quantities, Cd is located in Ca(2) sites, while for larger
quantities, it is located in both Ca(1) and Ca(2) sites (Fedoroff et al., 1999).
Scanning electron microscope observations showed that there is no
modification of the crystallite morphology after Cd fixation. This process is
only partly reversible and takes place in a large pH range. In addition, Cd may

Inorganic and Organic Soil Amendments ...

diffuse into the bulk of apatite crystals. Nuclear microprobe measurements


showed that Cd penetrated into the whole thickness of the crystals (Toulhoat et
al., 1996). Fedoroff et al. (1999) concluded that Ca(2) sites, which are adjacent
to the channels centred on the hexagonal screw-axes, are first substituted by
sorbed Cd, suggesting that these channels are the main pathways for diffusion
into the solid. Nonetheless, diffusion seems to slow down as the concentration
of Cd increases in apatite crystals.
Chen et al (1997b) reported that the sorption of aqueous Cd onto apatite
increased abruptly when pH increased above 6,2. X-ray diffraction (XRD)
patterns of the reaction products also indicated the formation of otavite (Chen
et al, 1997a; Chen et al, 1997 b) and cadmium hydroxide, as expressed by
Equations 2 and 3 respectively (Chen et al, 1997 b). No crystalline cadmium
phosphates were detected.
Cd2+ + HCO3- CdCO3(c) + H+

(Equation 2)

Cd2+ + 2H2O Cd(OH)2(c) + 2H+

(Equation 3)

Therefore, the main mechanisms of Cd retention by apatite seem to be


diffusion and ion exchange, leading to the formation of a (Cd-Ca) solid
solution; while Cd surface complexation or precipitation are minor
contributing processes. The fact that Cd is incorporated into the bulk of the
apatite with only partial reversibility is important in the context of the safe
storage of used sorbent material.

Water-soluble Phosphate Compounds


Soluble phosphate compounds include fertilizers such as single
superphosphate, triple superphosphate, monoammonium phosphate and
diammonium phosphate. Several studies reported that application of high
levels of water-soluble P compounds decreased the bioavailability and
mobility of Cd in contaminated soils, which has been attributed to a decrease
in Cd solubility (Pearson et al., 2000; McGowen et al., 2001; Chen et al. 2007
a; Thawornchaisit, Polprasert 2009).
Two reasons have been attributed to phosphate-induced immobilization of
Cd in soils: phosphate-induced Cd2+ adsorption; or Cd precipitation as
Cd(OH)2 and/or Cd3(PO4)2.
Phosphate-induced Cd2+ adsorption may be the result of an increase in pH
(Levi-Minzi, Petruzzelli 1984), increase in surface charge (Naidu et al., 1997)
or the formation of surface complexes of Cd on the phosphate compound

Silvana Irene Torri

(Helyar et al. 1976). Different phosphate sources may impact the effectiveness
of Cd stabilization. Thawornchaisit and Polprasert (2009) evaluated the
efficiency of three commercial phosphate fertilizers: triple superphosphate,
diammonium phosphate, and phosphate rock as stabilizing agents in Cd-highly
contaminated soils. Addition of all tested phosphate fertilizers induced a shift
of Cd mobile forms towards more stable fractions; however, the shifting
degree occurred at different rates depending on the phosphate fertilizer used,
and followed the sequence: triple superphosphate > diammonium phosphate >
phosphate rock. Consequently, stabilization efficiency appeared to be
correlated with dissolution of phosphate sources.
Other studies have shown that many PTE-phosphates are
thermodynamically stable and relatively insoluble in natural environments
(Santillan-Medrano, Jurinak, 1975; Nriagu, 1984; Vieillard and Tardy, 1984;
Ruby et al., 1994). The possibility of forming cadmium phosphate [Cd3(PO4)2]
upon the addition of soluble phosphate compounds in Cd contaminated soils
has been proposed, without direct evidence (Ma et al., 1993; Cotter-Howells,
Caporn, 1996). In effect, Bolan et al. (2003 a) found no evidence of Cd3(PO4)2
formation in soil samples even at the highest level of KH2PO4 and Cd addition.
Moreover, the solubility of Cd3(PO4)2 has been shown to be too high to control
the concentration of Cd in soil suspensions involving iron and aluminium
hydrous oxides (Kuo, 1986; Soon, 1981). Thus, although the precipitation as
Pb or Zn phosphates has been proved to be one of the main mechanisms for
the immobilization of Pb and Zn in contaminated soils (Hettiarachchi et al.
2000; McGowen et al., 2001) no conclusive evidence was provided up to this
time on the existence of new solid phases of Cd-phosphate compounds upon
addition of phosphates on Cd-contaminated soils.

Problems Associated with the Use of Phosphate as an Immobilizing


Agent
Numerous studies have demonstrated that phosphates should be applied at
very high rates to decrease Cd availability in field contaminated soils
(McGowen et al., 2001; Hong et al, 2009; Hong et al. 2008), resulting in new
environmental problems. Surface runoff from croplands with high levels of
soil phosphorus may originate phosphorus enrichment of streams, lakes and
estuaries (Sharpley et al., 1996). Accumulation of phosphorus in water bodies
can result in rapid algae growth, oxygen depletion when algae decompose, and
accelerated eutrophication in saline and fresh waters (Sims et al., 1998; Lin et
al., 2009).

Inorganic and Organic Soil Amendments ...

Although phosphate fertilizers provide effective immobilization of Cd in


highly contaminated soil (Wang et al, 2008), their application may also result
in soil acidification (Chen et al., 2007c; Thawornchaisit, Polprasert 2009). The
effect of phosphate addition on soil pH depends on the buffering capacity of
the soil, the nature of phosphate compounds and the extent of phosphate
adsorption (Havlin et al., 1999). Dissolution of phosphate fertilizers,
particularly triple superphosphate and diammonium phosphate, yield the
release of phosphoric acid (Chrysochoou et al, 2007; Spuller et al, 2007),
decreasing soil pH. Thus, phosphate-induced variation in soil pH may
influence the solubility of Cd in soils, as reported by Levi-Minzi and
Petruzzelli (1984). It has often been observed that the phytoavailability of Cd
increased with decreasing pH (Naidu et al., 1994). Hence, if immobilization of
Cd is followed by soil acidification, the contaminated soil will continue to
pose a potential ecological risk and the remediation treatment may not be
sustainable without continued management inputs. Consequently, coapplication of liming materials with phosphate fertilizer would be necessary to
offset soil acidification, especially in non-alkaline soils.

3.2 Organic (Biosolids) Amendments


Organic matter has been of particular interest in studies of PTE retention
by soils, because of its significant impact on cation exchange capacity (CEC),
and more importantly, the tendency of transition metal cations to form stable
complexes with organic ligands (Elliott et al., 1986; Chen, 1996). Organic
materials provide a large number of non-specific and specific sorption sites for
metals from which they may be difficult to displace (Shuman, 1999). Thus, in
situ application of organic amendments is becoming increasingly widespread
for its low cost and beneficial effect on soil fertility (Tapia et al, 2010).
Organic matter has quite a different effect on Cd availability depending
upon whether it is in soluble or insoluble forms. Soil addition of insoluble
(humified) organic amendments encourage the formation of stable organocadmium complexes, which diminishes Cd solubility (Udom et al. 2004;
Mohamed et al, 2010). The ability of humic substances to bind Cd was
attributed to their high content of oxygen-containing functional groups,
including carboxyl, phenol, hydroxyl, enol, and carbonyl structures of various
types (Rocha et al. 2009). Some studies reported different interactions between
humic acids and Cd, depending on the nature and properties of functional

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Silvana Irene Torri

groups, especially regarding their content of phenolic groups (Datta et al.,


2001).
Dissolved or soluble organic carbon consists of several types of low
molecular weight organic compounds, such as polyphenols, simple aliphatic
acids, amino acids and sugar acids (Fox, Comerfield 1990). Soluble organic
carbon can facilitate the transport of Cd through the formation of soluble
complexes (Antoniadis and Alloway, 2002; Kaschl et al, 2002; Pan, Zhou
2007). Although these compounds may reduce Cd adsorption onto soil
surfaces (Guisquiani et al., 1998), they have been shown to be less readily
available for plant uptake (Hamon et al., 1995; Han et al., 2001).
Throughout the world, there have been increasing interests in the
utilization of waste materials such as biosolids or biosolids compost as lowcost adsorbents rather than disposal in a landfill. Traditionally, biosolids have
been viewed as one of the major sources of PTE accumulation in soils, and a
large volume of work has been carried out to examine the mobilization and
bioavailability of biosolid-borne metals in soil (Merrington, Madden 2000; Li
et al, 2001; Li et al, 2006; Torri, Lavado 2008 a, Torri, Lavado 2008 b).
Biosolids contain a high proportion of humified organic matter. Torri et al
(2003) reported that between 29-45% of biosolids-borne carbon was
recalcitrant in three representative soils of the Pampas Region, Argentina.
During composting, organic compounds are transformed through successive
activities of different microbes into stabilized humic substances (Garca et al.,
1993; Par et al., 1998).
Although biosolids and biosolids compost may contain Cd themselves,
further studies have shown that biosolid addition to soil enhanced the ability of
soil in adsorbing heavy metals, thereby limiting its bioavailability (Merrington
and Smernik, 2004, Tapia et al, 2010). Actually, soil application of this
organic waste has improved Cd immobilization in extremely contaminated
soils (Li et al., 2001; Bolan et al., 2003 c; Brown et al., 2003; Hettiarachchi et
al, 2003; Tapia et al, 2010, among others), aiding the re-establishment of
vegetation (Castaldi et al., 2005; Gadepalle et al, 2009). The presence of
phosphates, aluminum compounds and other inorganic minerals in biosolids is
also responsible for the retention of Cd, preventing the increased metal
availability suggested in the time bomb hypothesis (Li et al, 2001;
Hettiarachchi et al., 2003; Torri, Lavado 2009). Such observations imply that
the sequestration capacity of biosolids of sludge origin might be indefinite due
to the residual effects of the mentioned constituents. This observation
complements those of Mahler et al (1987) and Brown et al. (1998) which
indicated that either inorganic phases in biosolids or recalcitrant organic

Inorganic and Organic Soil Amendments ...

11

carbon are responsible for maintaining low plant availability in biosolidsamended soils. Currently, there is intense debate whether the organic or the
inorganic fraction is responsible for Cd and other PTE immobilization (Li et
al., 2001; Stacey et al., 2001, Bolan et al., 2003 c, Hettiarachchi et al., 2003,
Merrington et al., 2003; Kumpiene et al., 2008).
Liming of contaminated soils is the most widely used remediation
treatment to reduce the bioavailability of Cd (Bolan et al. 2003 b; Tlusto et
al., 2006; Hong et al, 2009). Alkaline amendments increase soil pH (McBride
et al., 1997 and Filius et al., 1998) and facilitate the formation of oxides,
metal-carbonate precipitates and complexes that decrease metal solubility
(Mench et al., 1994). Biosolids compost can therefore be combined with
alkaline materials to complement Cd sequestering ability on compost
components (Mench et al., 1994 and Chlopecka and Adriano, 1996). Recent
studies have shown that alkaline-stabilized biosolid compost that are low in
total and/or bioavailable metal content can be used as an effective sink for
reducing the bioavailability of Cd in contaminated soils (Brown et al., 2000; Li
et al., 2000; Basta et al., 2001; Clemente et al., 2005). Numerous
investigations have been carried out for biosolids compost as potential
contamination sources of heavy metals. Conversely, limited work has been
done regarding the capacity of biosolids compost obtained at different stages
of the composting process, lime and a mixture of mature compost and lime to
immobilize Cd on an artificially Cd contaminated soil of the Pampas Region,
Argentina. These aspects are further discussed.

3.2.1. Immobilization Studies on a Typical Soil of the Pampas Region,


Argentina Soil
The study selected a typic Argiudoll (U.S. Soil Taxonomy) of the Pampas
Region, Argentina. Pristine topsoil samples (<20 cm depth) were collected
from San Antonio de Areco town (34 15' S - 59 29' W). The samples were
homogenized, air-dried, and ground to pass through a 2-mm plastic sieve. The
main physico-chemical characteristics of the soils are presented in Table 1.
The soil was enriched with Cd applied as nitrate. The artificially polluted soil
was moistened to field capacity and allowed to dry in cycles of approximately
15 days within a 3-month period in order to reach equilibrium with soil
colloids (Martnez, Motto, 2000). At the end of the stabilization period, total
Cd concentration was determined by atomic absorption spectrometry after
digestion of the samples with aqua regia according to ISO 11466 (1995).
Blanks were measured in parallel.

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Silvana Irene Torri

Table 1. Selected properties of the soil and the organic amendments used
in the study
pH

EC
(dS
m-1)
0.7

%C

Conta5.72
2.02
minated soil
Compost 1
7.5
2.10 13.42
Compost 2
7.6
2.08 11.08
Compost 3
7.6
2.62 4.05
1
EC: Electrical Conductivity.
2
CEC: Cation Exchange Capacity.

Soluble
C
%C
0.24
0.06
0.031

CEC2

Texture (%)
Clay
(%)
30.3

Silt
(%)
53.6

Sand
(%)
16.1

(cmol
kg-1)
24.5

Total
Cd
(mg kg
MS-1)
10.94

24
18.13
14.3

<4
<4
<4

Biosolids
Biosolids from Buenos Aires City was provided by the local water
operator Agua y Saneamientos Argentinos S.A. (AySA). The aerobically
stabilized biosolids used in these experiments was previously dried in holding
pools in the biosolids treatment plant. Biosolids was thoroughly mixed with
pine sawdust (1:1, V:V) and composted in piles. Composite samples were
taken at three different stages of the composting process: i) a day after
composting started (compost 1); ii) at the end of the thermophilic stage, 10
days after the process started (compost 2); iii) mature compost, after 90 days
composting started (compost 3).
Incubation Experiments
Artificially soil contaminated samples were amended at proportions
equivalent to a field application rate of i) 50 Mg ha-1 of compost 1 (C1); ii) 50
Mg ha-1 of compost 2 (C2); iii) 50 Mg ha-1 of compost 3 (C3); iv) 50 Mg ha-1
of compost 3 + 20 Mg ha-1 lime (LC3); v) 20 Mg ha-1 lime (L). A control
(artificially contaminated soil CS) with no amendment was also included.
Deionized water was regularly added to keep amended and control soils to
moisture contents of 60% to ensure minimum denitrification (Rowell, 1994).
Soils were incubated in glass flasks (360 ml) in darkness in a temperaturecontrolled incubator at 24 C to achieve stable soil conditions. Sampling was
managed by removing three pots per treatment at 0, 14, 28 and 42 days.
The sequential extraction procedure of McGrath and Cegarra (1992) was
used to investigate the mechanism of action of the amendments. Briefly, soil
was sequentially extracted with 0.1 M CaCl2 for 16 h (exchangeable fraction,

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Inorganic and Organic Soil Amendments ...

EXCH-Cd); 0.5 M NaOH for 16 h (organic matter bound fraction, OM-Cd );


0.05 M Na2EDTA for 1 h (inorganic precipitate fraction, INOR-Cd) at a soil:
solution ratio of 1:10. The concentration of Cd in each fraction was
determined by Flame Atomic Absorption Spectroscopy (FAAS).
The statistical analysis was done with the Statistics 7.0 (2000) package,
processing the data for Analysis of Variance (ANOVA) for a completely
randomized design. One-way ANOVA was carried out to compare the means
of different treatments; where significant F values were obtained, differences
between individual means were tested using Tukeys test. Statistical
significance was defined as p < 0.05.

Treatment Effect on Cd Soil Fractions


The percent of total Cd associated with different fractions in the control
sample was in the following order: exchangeable fraction (55%) > organic
matter bound fraction (31%) > inorganic precipitate fraction (13%). These
results indicate that a substantial quantity of Cd in the contaminated soil may
be available for plant uptake (Basta and McGowen, 2004), in good agreement
with results reported by Chen et al, (2007). The concentrations of Cd in the
different soil fractions following treatments in each sampling date are shown
in Figures 1, 2 and 3.
7
CS

EXCH-Cd (mg kg-1)

C1
C2

C3

C3+L

3
L

14

28

1
0
0

42

days

Figure 1. Water-soluble and exchangeable fraction of Cd (EXCH-Cd) in the


contaminated soils as a result of the addition of amendments: SC: control, Ci: soil
amended with compost i; L: soil amended with lime. For each date, different letters
indicate significant differences according to Tuckey's test at 5% probability level (n =
3).

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Changes in Cd Water-Soluble and Exchangeable Fraction (EXCH-Cd)


The addition of C1, C2 or C3 did not significantly modify EXCH-Cd over
the incubation period compared to control (Figure 1), which ranged from 47 to
55% of Cd total content. These results are at variance with some other
published papers where the application of compost significantly reduced the
concentration of EXCH-Cd in contaminated soils (Castaldi et al, 2005; Lin,
Zhou 2009; Tapia et al, 2010). Conversely, the application of L or C3+L
significantly reduced the concentrations of EXCH-Cd compared to control,
revealing that there was a net movement of Cd towards other soil fractions
following the addition of this amendment. These results are similar to
observations made by others for EXCH-Cd in the presence of lime (Brallier et
al. 1996; Fernandes et al. 1999; Hong et al. 2007, 2009).
Among soil factors controlling the adsorption of Cd, pH is probably the
most important (Christensenn, 1984). It has often been observed that the
adsorption of Cd2+ increased with increasing pH, resulting in low Cd
phytoavailability (Naidu et al., 1994; Bolan et al., 1999; Hong et al. 2007).
The effect of pH is related to its great influence on the charge and structure of
the adsorbing surfaces and on the ionic composition of the soil solution
(Garcia-Miragaya and Page, 1978; Abd-Elfattah and Wada, 1981). An increase
in pH increases soil net negative charge, which is attributed to the dissociation
of H+ from weakly acidic functional groups of organic matter or from some
clay minerals (Curtin et al. 1996).
Table 2. pH in the contaminated soils as a result of the addition of
amendments: SC: control, Ci: soil amended with compost i; L: soil
amended with lime. For each date, different letters indicate significant
differences according to Tuckey's test at 5% probability level (n = 3)
day 14
treatment
CS
C1
C2
C3
C3+L
L

pH
5,72
5,66
5,83
6,00
7,75
7,93

0,05
0,07
0,05
0,04
0,03
0,01

day 28
a
a
a
a
b
b

5,54
5,55
5,66
5,62
7,72
7,98

0,01
0,10
0,06
0,13
0,13
0,09

day 42
a
a
a
a
b
b

5,54
5,47
5,48
5,54
7,74
7,95

0,13
0,14
0,10
0,01
0,12
0,31

a
a
a
a
b
b

Inorganic and Organic Soil Amendments ...

15

Application of liming materials significantly increased soil pH compared


to the other treatments (Table 2). The increase in pH by lime can be explained
by the release of hydroxyl ion after hydrolysis of calcium carbonate. This
increase in pH resulted in enhanced Cd adsorption, as reported by other
authors (Szkov et al, 2007; Ghafoor et al., 2008; Hong et al, 2010b).
Conversely, no significant differences in soil pH values were observed
between control and soils treated with C1, C2 and C3 in each sampling date.
Interestingly, in most of the studies reported in the literature, biosolids
compost addition increased soil pH across all treatments in comparison to
control samples (Castaldi et al, 2005; Gadepalle et al, 2009; Tapia et al, 2010).
The lack of significant differences in soil pH values between control, C1, C2
and C3 in this study suggests that pH may be regarded as the key factor
controlling the concentration of exchangeable Cd in Cd contaminated soils. A
negative and significant correlation could be established between EXCH-Cd
and soil pH [EXCH-Cd (mg kg-1) = -1,4818 pH + 13,66, R2 = 0.98, p<0.01]
among all sampling dates.

Changes in Cd Organic Fraction (OM-Cd)


At the end of the studied period, the fraction of Cd associated with organic
matter increased in all amended soil samples and control (Figure 2). Only
C3+L significantly increased OM-Cd compared to control at day 14, 28 and
42. No significant differences between the other treatments and control were
observed.
The formation of stable complexes between Cd and organic matter in
composted biosolids has been reported by other authors (Bolan et al., 2003c;
Lin, Zhou 2009; Chen et al, 2010; Mohamed et al, 2010 and Tapia et al, 2010).
However, these studies also reported an increase in soil pH due to the
amendments incorporation. Depending on soil pH, soil organic matter
generally carries more surface charge than do inorganic soil components, as
discussed before. However, in this study, increases in soil pH were only
observed in lime treated soils. Therefore, increase in surface charge of
composts organic matter was not the cause for the increase in OM-Cd in nonlime amended soils. Kaschl et al (2002) studied the relative importance of
different types of organic ligands (dissolved organic matter, humic and fulvic
acids) for the binding of Cd at pH=7. The highest complexing capacity for Cd
was found for the most humified and less soluble organic materials, and could
not be directly related to total acid-titratable or carboxylic groups, indicating
the importance of sterical issues and other functional groups. The high content
of humified organic matter in biosolids (Torri et al, 2003) may have hindered

16

Silvana Irene Torri

slight increases in humic substances originated in the compost process,


explaining the lack of significant differences in OM-Cd between C1, C2 or C3.
Moreover, there was no difference in the concentration of OM-Cd between
control and C1, C2 and C3, which may be attributed to the high level of
organic matter in the control, together with the fact that Cd is one of the more
weakly bonded ions by soil organic matter (Harter, Naidu 2001).
Nonetheless, an increase in OM-Cd was observed in control and
composts, lime or lime + compost amended soils during the incubation period,
and accounted between 30-50% of the total soil Cd.

Changes in Cd Precipitated Fraction (INOR-Cd)


The amounts of INOR-Cd in control and amended soils are shown in
Figure 3. No significant differences in INOR-Cd were observed with the
addition of C1, C2 or C3 compared to control in all sampling dates. On the
contrary, lime application resulted in a significant increase of INOR-Cd
compared to control. These results are in agreement with some other published
papers which indicate that application of lime can significantly increase the
precipitated fraction of Cd in contaminated soil (Knox et al. 2001; Hong et al,
2010 b), possibly as Cd-carbonate (Knox et al. 2001; Basta et al., 2001) at the
expense of the EXCH-Cd fraction. A positive and significant correlation could
be established between INOR-Cd and soil pH [INOR-Cd (mg kg-1) = 0,6443
pH - 2,267 (R2 = 0,96, p<0.01)] among all sampling dates.
The decrease in the phytoavailability of Cd in the presence of biosolids or
biosolids compost has often been attributed to increased complexation by the
organic constituents (Adriano, 2001). However, inorganic compounds present
in biosolids are responsible for inducing the plateau effect in Cd uptake by
crops (Brown et al., 1998). Biosolids contain from 30 to 60% of inorganic
mineral forms, like Fe, Mn, and Al oxides, silicates, phosphates and
carbonates (Sommers et al., 1976; Torri 2009) that are highly reactive with
PTE. Many authors have documented the role of these inorganic components
in the formation of heterogeneous precipitates as well as their ability to adsorb
Cd (Corey et al., 1987; Essington and Mattigod, 1991; Kuo, 1986).
Furthermore, several authors have reported the predominant role of Fe and Mn
oxides in the almost irreversible adsorption of Cd in biosolid amended soils
(Li et al., 2001; Hettiarachchi et al., 2003 and Merrington and Smernik, 2004).
In this study, fixation was more pronounced in C3+LL. These results may be
due to the presence of elevated concentrations of iron oxyhydroxides in the
compost, in agreement with Buekers et al. (2007) and Torri (2009). Cadmium
specifically adsorbed by these inorganic phases would be expected to have a

17

Inorganic and Organic Soil Amendments ...

low phytoavailability, and could become no phytoavailable as surfaces become


occluded.
7
a

OM-Cd (mg kg-1)

CS

C1

ab

ab

C2

ab

C3

C3+L

3
L

b
2
1
0
0

14

28

42

days

Figure 2. Organic fraction of Cd (OM-Cd) in the contaminated soils as a result of the


addition of amendments: SC: control, Ci: soil amended with compost i; L: soil
amended with lime. For each date, different letters indicate significant differences
according to Tuckey's test at 5% probability level (n = 3).
7

INOR-Cd (mg kg-1)

CS

C1

C2

C3

4
a

C3+L

2
1
b

28

42

0
0

14

days

Figure 3. Inorganic precipitates of Cd (INOR-Cd) in the contaminated soils as a result


of the addition of amendments: SC: control, Ci: soil amended with compost i; L: soil
amended with lime. For each date, different letters indicate significant differences
according to Tuckey's test at 5% probability level (n = 3).

18

Silvana Irene Torri

Considerations on Compost Application


Biosolids and biosolid composts are likely to increase in many countries,
so there is an urgent need for sustainable ways for their disposal. In this shortterm study, EXCH-Cd and INOR-Cd were closely related to soil pH.
Application of biosolids compost alone did not substantially modify the
availability of Cd in Cd contaminated soils, possibly because soil pH was not
modified. The application of mature compost plus lime significantly reduced
Cd soluble/exchangeable fractions, with a proportional increase in the organic
and, to a lesser extent, inorganic-bound fractions. However, some uncertainty
may raise about Cd becoming more bioavailable with time through
mineralization or soil acidification. The long-term efficacy of this amendment
requires careful examination.

4. CONCLUSION
Remediation of Cd-contaminates soils can be achieved by adding
phosphate compounds or biosolids compost. Both amendments can enhance
Cd immobilization by redistribution of Cd to less available fractions.Phosphate
addition was found to decrease Cd availability, although the mechanisms of
Cd fixation is not fully known. Alternatively, the addition of alkaline biosolid
compost decreased the concentration of the soluble and exchangeable Cd
fraction, and increased the concentration of organic and, to a lesser extent,
inorganic-bound Cd fractions.
The environmental factor more likely to have the largest effect on Cd
availability is soil acidification. Consequently, if in situ remediation materials
exert their effect through changes in soil pH, then reacidification of soil would
return Cd to the original toxic level. Therefore, there may be a need to manage
soil pH in perpetuity if toxicity is to be avoided. Nevertheless, one of the
major inherent problems associated with these immobilization techniques is
that, although Cd becomes less bioavailable, total Cd concentration in soils
remains unchanged. In the long-term the immobilized element may become
more mobile and bioavailable through natural weathering processes.

Inorganic and Organic Soil Amendments ...

19

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