Environ Monit Assess (2010) 166:331–346

DOI 10.1007/s10661-009-1005-7

Distribution and partitioning of iron, zinc, and arsenic

in surface sediments in the Grande River mouth
to Cuitzeo Lake, Mexico
Benjamín Villalobos-Castañeda ·
Ruth Alfaro-Cuevas · Raúl Cortés-Martínez ·
Verónica Martínez-Miranda ·
Liliana Márquez-Benavides

Received: 27 August 2008 / Accepted: 17 May 2009 / Published online: 3 June 2009
© Springer Science + Business Media B.V. 2009

Abstract Cuitzeo Lake is one of the largest and
most important lakes in Mexico. It receives differ-
ent types of pollutants through its main tributary,
the Grande River of Morelia. The aim of this work
was to determine if high concentrations of iron,
zinc, and arsenic are present in sediments in an
area near the river mouth to the lake, as well as
to estimate the partitioning of these metals using a
sequential extraction procedure in order to obtain
B. Villalobos-Castañeda · R. Alfaro-Cuevas
Instituto de Investigaciones Químico Biológicas,
Universidad Michoacana de San Nicolás de Hidalgo,
Francisco J. Mújica s/n, Ciudad Universitaria,
Edif. B1, Morelia, Michoacán, México
R. Alfaro-Cuevas · V. Martínez-Miranda
Centro Interamericano de Recursos del Agua,
Facultad de Ingeniería, Universidad Autónoma
del Estado de México, Km. 14.5, Carretera
Toluca–Ixtlahuaca, Toluca, Edoméx, México
R. Cortés-Martínez (B)
Facultad de Químico Farmacobiología,
Universidad Michoacana de San Nicolás de Hidalgo,
Tzintzuntzan 173 Col. Matamoros,
Morelia, Michoacán, México
e-mail: raulcortesmtz@gmail.com
L. Márquez-Benavides
Instituto de Investigaciones Agropecuarias y
Forestales, Universidad Michoacana de San Nicolás
de Hidalgo, Av. San Juanito Itzícuaro, Col. San
Juanito Itzícuaro, Morelia, Michoacán, México
information of their potential bioavailability. Sed-
iment samples were collected from three different
sites in Cuitzeo Lake and two sites in Grande
River in both dry and wet seasons. A sequential
extraction procedure was carried out to determine
the concentrations of these elements in different
geochemical phases of the sediments. Total metal
concentrations were evaluated by using the en-
richment factor and the geoaccumulation index.
A comparison with sediment quality guidelines
and shale values has also been made. The results
indicate that sediments are considered unpolluted
by iron and moderately polluted by zinc and ar-
senic. However, fractionation studies showed that
significant amounts of Zn and As could be re-
leased to the lake ecosystem depending on the
environmental conditions, representing a medium
risk potential of bioavailability to the biota.
Keywords Cuitzeo lake · Sediments · Zinc ·
Bioavailability · Sequential extraction · Arsenic
Introduction
Environmental pollutants that enter water bod-
ies from municipal, agricultural, and industrial
sources may remain suspended in the water col-
umn, be taken up by aquatic biota, or settle on
the bottom and become incorporated into the sed-
iments (Beg et al. 2001). Among these pollutants,
332
heavy metals have been of great concern due to
their toxicity, abundance, persistence, and sub-
sequent accumulation in aquatic habitats. There-
fore, heavy metal assessment in surface sediments
is important in order to estimate the extent of
pollution or identify pollution sources (Green-
Ruiz and Páez-Osuna 2003; Barlas et al. 2005).
Recently, it has been recognized that the to-
tal concentration of an element in an ecosys-
tem does not necessarily represent its biological
availability or potential toxicity. This concept is
known as “bioavailability” and is a function of
the abundance and chemical form of the toxin
in solution (i.e., oxidation state) and the nature
of its binding to sediment grains (Newman and
Jagoe 1994; Price and Pichler 2005). Therefore, it
is not sufficient to measure only the total metal
concentrations for these purposes, it is also impor-
tant to establish the proportions of heavy metals
present in various easily and sparingly soluble
sediment fractions, since the mobility of metals,
their bioavailability, and their toxicity to biota
depend strongly on their specific chemical forms
or ways of binding. However, the determination
of specific chemical species or binding forms is
difficult and often hardly possible. Thus, deter-
minations of broader forms of metals in surface
sediments, using sequential extraction procedures,
can be a good compromise to give information
on environmental contamination risk (Pueyo et al.
2001; Svete et al. 2001). Furthermore, it has gener-
ally been accepted that sequential extractions are
the most appropriate methods to evaluate solid
speciation and are widely used to asses the long-
term emission potential of pollutants and to study
their distribution among the different geochemi-
cal phases of sediments (Ianni et al. 2001).
Cuitzeo Lake is one of the largest and most
important lakes in Mexico. The basin is part of the
upper Lerma River, whose watershed is one of the
most polluted in Mexico. Cuitzeo Lake presents
serious problems of contamination, drying up, and
refilling by sediments, as well as weathering of ash
fall deposits into hardened volcanic soils, which
causes Fe enrichment (Servenay and Prat 2003;
Ostrooumov et al. 2005). The origin of potential
pollution at Cuitzeo Lake comes from the increase
in industrial, urban, and agricultural activities dur-
ing the last decades in the region. Domestic and
Environ Monit Assess (2010) 166:331–346
industrial wastewaters have been diverted directly
to the lake and to the rivers arriving to it. At
present, the basin has an evident environmental
deterioration due to an increase in the pollution
coming from the main affluent: the Grande River
of Morelia.
The objectives of this work were to deter-
mine the total concentrations of iron, arsenic, and
zinc in surface sediments from Cuitzeo Lake and
Grande River, as well as to estimate the partition-
ing of these metals using a sequential extraction
procedure in order to obtain information of their
potential bioavailability.
Materials and methods
Site description
Cuitzeo Lake is located in the northeast part of
Michoacan State, Mexico, between 20◦ 05 13 and
19◦ 52 48 N and 100◦ 50 08 and 101◦ 19 40 W,
at 1,820 m altitude. The region belongs to the
middle part of the Mexican Volcanic Belt (Israde-
Alcántara and Garduño-Monroy 1999). The basin
is part of the upper Lerma River and is one of the
largest lakes of the zone having an extension of
3,977 km2 . The weather is moderate with summer
rains (May–October), giving an average annual
precipitation of 906 mm and a temperature range
from 10◦ C to 28◦ C. The Grande and Querén-
daro rivers are the main tributaries of the lake
that empty on its south shore (Fig. 1). Grande
River receives municipal and industrial wastewa-
ters from Morelia City, as well as agricultural
runoffs. Moreover, there are many geothermal
boreholes around the lake that could be increasing
the As concentration. Some studies (Alfaro et al.
2002; Paez-Sánchez et al. 2008) have reported As
concentrations between 0.001 and 3.8 mg/L in
springs and wells around Cuitzeo Lake, specially
at the eastern limit of the lake. However, such
concentrations are originated by a thermal spring
located on a magmatic chamber, contributing to
As dissolution (Israde-Alcántara and Garduño-
Monroy 1999). This could be related to the As
concentrations found by Israde-Alcántara et al.
(2002), ranging between 0.38 and 0.95 mg/L in
water samples from the lake.
Environ Monit Assess (2010) 166:331–346 333

Fig. 1 Studied area

located about 35 km
north of Morelia City,
northern Michoacán State

Sediment sampling and preparation Sakan et al. 2007). Sediment samples were ho-
mogenized and then transferred to acid-washed
Sediment samples were collected from three dif- polyethylene bags and kept frozen until analyzed.
ferent sites in Cuitzeo Lake and two sites in Each time, two subsamples were collected from
Grande River (Table 1, Fig. 2) on three sampling each site and were analyzed separately. Sediment
campaigns from January to November 2006. Sed- samples were allowed to defrost and then dried for
iment sampling, management, and storage were 6 h in a circulating oven at 60◦ C. Dried samples
carried out according to recommended and widely were ground with a mortar and pestle and sieved
used procedures (Allen Burton 1992; Mudroch mechanically using a 2-mm sieve.
and Azcue 1995; EPA 2001a, b). The samples
were collected to a depth of 5 cm from the surface Grain size distribution
using a PVC coring tube, this depth was chosen in
order to obtain metal concentrations due to recent Grain size analysis was carried out according to
deposition of material in surface sediments that the pipette method (Rowell 1994). This method
could be related to actual contamination sources is based on the difference in sedimentation speed
(Lau and Chu 2000; Mudroch and Azcue 1995; between small and large particles. The pipetted
suspension is condensed and dried and weighing
Table 1 Geographical coordinates of sampling points determines the mass ratio of the pipetted fraction
Sampling point Geographical coordinates
(Çevik et al. 2009).
Río Grande 1 (RG1) 19◦ 56 099 N, 100◦ 57 551 W
Río Grande 2 (RG2) 19◦ 56 253 N, 100◦ 58 650 W Sequential extraction
La Hacienda (HDA) 19◦ 56 829 N, 100◦ 57 085 W
Río Grande 3 (RG3) 19◦ 51 893 N, 101◦ 00 448 W The metal sequential extraction was carried out
Río Grande 4 (RG4) 19◦ 54 576 N, 101◦ 00 207 W to samples from all sites, based on the Tessier’s
334
Fig. 2 Location
of sampling points
in the studied area
sequential chemical extraction method (Tessier
et al. 1979), modified by using 1 M NaOAc,
pH 8.2, for the first extraction (Lima et al. 2001).
The selective extractions were carried out in cen-
trifuge tubes in a water bath with reciprocal shak-
ing. At the end of each extraction, the samples
were centrifuged at 3,000 rpm for 30 min. The
supernatant was separated with the aid of a mi-
cropipette and it was analyzed for Fe, Zn, and As.
The sediment was washed with 5 mL of deionized
water, centrifuged, and decanted again for its use
in the next extraction step. The following metal
fractions were determined:
F1 Exchangeable fraction: the sediment was ex-
tracted at room temperature for 1 h with
8 mL of 1 M NaOAc (pH 8.2) with contin-
uous agitation.
F2 Bound to carbonates: the residue from F1
was leached at room temperature with 8 mL
of 1 M NaOAc/HOAc (pH 5) for 5 h with
continuous agitation.
F3 Associated with Fe–Mn oxides: the residue
from F2 was extracted with 15.0 mL of 0.04 M
NH2 OH·HCl in 25% acetic acid at 96 ± 2◦ C
for 6 h with occasional agitation.
Environ Monit Assess (2010) 166:331–346
F4 Associated with organic matter and sulfides: to
the residue of F3, 2.3 mL of 0.02 M HNO3
and 3.8 mL of 30% H2 O2 (pH 2 with HNO3 )
were added and the mixture was heated to
85 ± 2◦ C for 2 h with occasional agitation.
Another 2.3 mL aliquot of 30% H2 O2 (pH 2)
was then added and the sample was stirred
and heated again to 85 ± 2◦ C for 3 h. After
cooling, 3.8 mL of a 3.2-M NH4 OAc in 20%
HNO3 (v/v) solution was added and the sam-
ple was diluted to 20.0 mL and stirred contin-
uously for 30 min.
F5 Residual fraction: an acid digestion was car-
ried out to different sediment subsamples in
order to determine total As, Fe, and Zn con-
centrations. One gram of dry sediment was
added to a digestion vessel and 10 mL of
a deionized water and ultrapure nitric acid
solution (1:1 v/v) was added to the vessel. The
mixture was put in reflux and several 5 mL
aliquots of the nitric acid solution were added
until no brown fumes were detected. Then,
the mixture was heated for 2 h, cooled down,
and put in reflux by adding several aliquots
of H2 O2 . Later, 10 mL of ultrapure HCl was
added to the sample and heated for about
Environ Monit Assess (2010) 166:331–346
15 min. The sample was cooled, filtered, and
taken to 100 mL in a volumetric flask.
The metal concentrations in the supernatants col-
lected from each extraction and from the acid
digestions were measured by flame atomic ab-
sorption spectroscopy using an atomic absorption
spectrometer (Perkin-Elmer AAnalyst 200) for Fe
and Zn, using air–acetylene flame and using a
hydride generation system for As.
Results and discussion
Grain size distribution
Grain size distributions of the study area are
shown in Fig. 3. It can be noticed that the sedi-
ments consist of three sediment types (sand, silt,
and clay). However, fractions of silt (2–63 μm)
and clay (>2 μm) are the dominant fractions in
all sites, while almost all sediment samples contain
low amounts of sand fraction (<2%) except at site
RG3 where it may account for around 8% of the
sediment. In sites RG2 and HDA, sediments were
typified as clayey; and sediments of sites RG1,
RG3, and RG4 were typified as clayey silt. It has
been demonstrated that grain size is an important
factor controlling heavy metals concentrations in
surface sediments (Axtmann and Luoma 1991; Li
et al. 2007).
Fig. 3 Grain size distribution of sediments of Cuitzeo Lake
and Grande River
335
Total metal concentrations
Iron (Fe)
Iron is the most abundant metal in all sediments
because it is one of the most common elements
in the earth’s crust (Jain et al. 2007). Figure 4
shows the total metal concentrations in surface
sediments from the studied area. In general, to-
tal iron concentrations, calculated as the sum of
metal concentration released in all five fractions
(Fig. 4), are higher in sites located in Grande
River (RG3 and RG4) or at its vicinity (RG1
and RG2) and lower total iron concentrations are
present in sediments inside the lake located far
from the outfall of the river, particularly in site
HDA (Fig. 4), suggesting that iron concentrations
in sediments could be attributed to the iron-rich
soil of Cuitzeo area, due to Fe enrichment and ox-
idation of hardened subsurface layers in the zone
(Ostrooumov et al. 2005), and they are influenced
also by anthropogenic inputs. The Grande River
has been reported to contain a high concentration
of iron on the water column which could be in-
troducing significant quantities of this metal to the
lake. It is also important to mention that total iron
concentrations in these sediments do not present a
significant seasonal variation as observed in Fig. 4,
but tends to decrease for the samples collected
in November (wet season), except for site HDA.
This behavior could be attributed to sediment
resuspension where surface sediments could be
easily disturbed because of the shallow nature of
the lake in conditions of high flow in the river,
as well as the effect caused by wind flows, which
is also important, because of their velocity and
provenance, the winds can change environmental
conditions and flows regime in the lake. In the case
of Cuitzeo Lake, winds from southwest facilitate a
constant resuspension of sediments during the wet
season.
It can be observed that iron concentrations in
sediments are not higher than the average shale
value for iron of 34,000 mg/kg (Li 2000), except
for slight increments in sites RG1, RG3, and RG4
at dry season (January) and site HDA at wet sea-
son (May–November). Comparison with a “shale
standard” is a quick and practical mean of assess-
ing metal enrichments or depletions in sediments
336 Environ Monit Assess (2010) 166:331–346

Fig. 4 Total 45000

- - - Average shale
concentrations of a iron, (a)
40000
b zinc, and c arsenic in
sediments from Cuitzeo 35000
Lake and Grande River
30000

Fe (mg/kg)
25000

20000

15000

10000

5000

Jan-06.

May-06.

Nov-06.

Jan-06.

May-06.

Nov-06.

Jan-06.

May-06.

Nov-06.

Jan-06.

May-06.

Nov-06.

May-06.

Nov-06.
RG1 RG2 HDA RG3 RG4
Site
400

350
(b)
300

250 - - - Average shale

Zn (mg/kg)

200

150

100

50

0
Jan-06.

May-06.

Nov-06.

Jan-06.

May-06.

Nov-06.

Jan-06.

May-06.

Nov-06.

Jan-06.

May-06.

Nov-06.

May-06.

Nov-06.
RG1 RG2 HDA RG3 RG4
Site
200

180

160
(c)
140
As (mg/kg)

120

100

80 - - - Average shale

60

40

20

0
Jan-06.

May-06.

Nov-06.

Jan-06.

May-06.

Nov-06.

Jan-06.

May-06.

Nov-06.

Jan-06.

May-06.

Nov-06.

May-06.

Nov-06.

RG1 RG2 HDA RG3 RG4

Site
Environ Monit Assess (2010) 166:331–346 337

and it is a well-known method to verify if a par-
ticular element could be considered as “naturally
occurring.” Soils and sediments are usually com-
pared with standard shales (Korfali and Davies
2005; Ribeiro et al. 2005). From this comparison,
it can be concluded that iron in sediments of
Cuitzeo Lake and Grande River is mostly geo-
logically (naturally) derived. However, there are
some industrial activities, especially metal manu-
facturing and tanneries, located near the Grande
River mouth that could increase the levels of Fe
to the aquatic system, as well as other metallic
contaminants like, Zn, Cr, Cu, etc., by discharging
their wastes directly to the stream.
Zinc (Zn)
Total concentrations of this metal (Fig. 4) in sites
inside Cuitzeo Lake are lower than the average
shale value of 95 mg/kg for zinc (Turekian and
Wedepohl 1961), indicating that they are not Zn-
contaminated, but in sites RG3 and RG4 located
in Grande River, Zn levels vary from 79.5 to
374 mg/kg, suggesting a Zn enrichment probably
due to anthropogenic discharges to the river. It
could be also observed that zinc concentrations
decrease from dry to wet season in all sites; but
in this case, a significant decrement is observed in
Grande River sites, suggesting that some of the
zinc in sediments from RG3 and RG4 could have
been mobilized to the water column. Sediments
can be classified by the Sediment Quality Criteria
(SQC) for the protection of aquatic life (CCME
1999). Total concentrations of Zn and As obtained
in this study, which are considered as priority
pollutants, are presented in Table 2 and compared
with literature values, like SQC, background con-
centrations of elements (Turekian and Wedepohl
1961), and concentration ranges reported from
different parts of the world. It can be noticed
from these data that the levels of Zn in sites
inside the river are higher than the SQC threshold
effect level and even higher values (RG3 site) for
the probable effect level (315 mg/kg) that rep-
resents the level above which usually, or always,
adverse biological effects are observed. However,
Espinosa and Armienta (2007) reported a sig-
nificantly higher range for contaminated river
sediments classified as very strongly polluted.
However, some studies have shown that fishes are
susceptible to low concentrations of Zn in water
(Fatoki et al. 2002; Awofolu et al. 2005). Based
on these facts, sediments of Grande River could

Table 2 Total Location Sampling Total concentration (mg/kg)

concentrations of Zn and
As in surface sediments Zn As
from Cuitzeo Lake and RG1 Jan 2006 72.3 30.5
Grande River May 2006 54.5 145.6
Nov 2006 47.3 72.2
RG2 Jan 2006 104.5 109.9
May 2006 70 17.2
Nov 2006 39.2 176.1
HAD Jan 2006 63.1 37.3
May 2006 43.1 159.3
Nov 2006 51.1 29.8
RG3 Jan 2006 366 2.1
May 2006 374 0.3
Nov 2006 79.5 22.6
− below detection limit RG4 May 2006 211.1 20.7
a Espinosa and Armienta Nov 2006 92.7 4.8
(2007) Xochula River sediments (range)a − 5,200−34,088 −
b Pandey et al. (2004) Surface sediments, India (range)b − − 8−209
c Belucci et al. (2002) Venice lagoon (range)c − − 5−132
d Turekian and Wedepohl Average shaled − 95 13
(1961) SQCe Threshold effect level 123 5.9
e CCME (1999) Probable effect level 315 17
338
be considered as a contamination risk for the lake
ecosystem.
Arsenic (As)
Arsenic concentrations range between 0.71 and
176.12 mg/kg for all sites in the study area. Com-
paring with the SQC values, arsenic concentra-
tions in all sites located inside the lake exceeded
the probable effect value, as well as the average
shale value, except for RG1 in the May sampling.
For the sites inside the river (RG3 and RG4),
only in some samplings the As concentrations
were higher than the shale and SQC threshold
effect values, which indicates that arsenic levels in
sediments are significantly higher in sites located
inside Cuitzeo Lake than the sites inside Grande
River, as can be clearly observed in Fig. 4. The
increase in As concentrations in sites RG1 and
HDA in May could be attributed to environmen-
tal conditions during the dry season when resus-
pension of surface sediments is not significant.
However, the decrease shown by RG2 in As total
concentration, in the same sampling campaign,
could be attributed to the more anoxic condi-
tions specifically at this site and to the values of
Eh and pH at that time, which could lead to a
release of As concentration from the sediments.
Moreover, the fact that arsenic concentrations in
sites inside Grande River are relatively low sug-
gests that there is not an anthropogenic source of
this element, indicating also that a natural source
could be responsible for the high As concentra-
tions in sediments inside the lake, especially from
geothermal springs located at the eastern side of
the lake, as mentioned before (Alfaro et al. 2002;
Paez-Sánchez et al. 2008; Israde-Alcántara et al.
2002).
Arsenic levels in lake sediments could repre-
sent a toxicological risk for aquatic life and the
ecosystem. It has been demonstrated that high
concentration of As are bioaccumulated in fish
like tilapia (Oreochromis mossambicus) because
this species disturbs the surface sediment layer,
increasing such accumulation (Wang et al. 2007).
It is important to mention that this species is one
of the most commercially exploited at the studied
Environ Monit Assess (2010) 166:331–346
area and it could represent a health risk. Besides,
metal bioaccumulation has been related with a
decrement in reproduction and survival of fish,
which could represent an ecological risk to the
species (Liao et al. 2003).
Similar concentrations range (8–209 mg/kg) has
been reported in sediments from surface water
bodies in India (Pandey et al. 2004) where such
As levels have been classified as a high degree
of contamination and have been attributed to
natural sources. Based on the above-mentioned,
the sediments of sites inside Cuitzeo Lake could
be considered as highly contaminated for arsenic
because the As levels found in this study are about
eight to ten times higher than the SQC probable
effect level. Besides, a similar range for As levels
has also been reported (Table 2) in an industrial
contaminated site (Belucci et al. 2002).
Metal enrichment
As mentioned before, comparison with shale can
be used to assess metal enrichment in sediments.
Many authors prefer to express the metal ratio
with respect to average shale in order to represent
the degree of quantification of pollution (Singh
et al. 1997; Korfali and Davies 2005; Çevik et al.
2009). Metal ratios with respect to average shale
for the Cuitzeo Lake and Grande River sedi-
ments are presented in Table 3. For the case of
iron, the metal ratios are less than 1 in almost
all sediment samples, confirming the natural or
geological origin of this metal in sediments. For
Zn, enrichment factors are significant only in RG3
and RG4 sites in dry season samplings, showing
metal ratios ranging from 2.2 to 3.94, indicating
a pollution source entering the river system. Ar-
senic shows a maximum value of 13.55 in site RG2
and, generally, ratios above 2 are presented in
sites inside Cuitzeo Lake. This enrichment by As
of Cuitzeo sediments may be due to the transport
of colloidal particles brought by runoffs in the
watershed, which could be the major source of
arsenic to the lake.
The geoaccumulation index proposed by
Müller (1979) for the quantification of metal
accumulation in sediments was also calculated for
Environ Monit Assess (2010) 166:331–346 339

Table 3 Metal ratios Location Sampling Fe Zn As

with respect to average
shale values in Cuitzeo RG1 Jan 2006 1.08 0.76 2.35
Lake and Grande River May 2006 0.99 0.57 11.20
sediments Nov 2006 0.87 0.50 5.56
RG2 Jan 2006 1.00 1.10 8.46
May 2006 0.97 0.74 0.74
Nov 2006 0.93 0.41 13.55
HDA Jan 2006 0.89 0.66 2.87
May 2006 0.74 0.45 12.25
Nov 2006 1.08 0.54 2.29
RG3 Jan 2006 1.10 3.85 0.07
May 2006 0.91 3.94 0.00
Nov 2006 0.79 0.84 1.74
RG4 May 2006 1.12 2.22 1.59
Nov 2006 0.85 0.98 0.05

the Cuitzeo Lake and Grande River sediments in
all sampling campaigns. This index is expressed
as:

Igeo = Log2 Cn 1.5Bn (1)
where Cn is the measured concentration of el-
ement n, Bn is the background concentration
value (average shale) of the element n, and 1.5
is the background matrix correction factor that is
included to correct possible background value
variations due to lithogenic effects. The geoaccu-
mulation index consists of seven grades (Table 4)
with the highest corresponding to 98-fold enrich-
ment over the background values (Singh et al.
1997; Espinosa and Armienta 2007).
Table 5 shows the geoaccumulation indexes for
Fe, Zn, and As in sediment samples of the studied
area. The Igeo for Fe remains in 0 class, while the
Igeo for Zn and As could be considered in class
1, especially for As where the calculated indexes
were slightly higher in sites located inside Cuitzeo
Lake. Therefore, according to the classification
in Table 4, sediments can be considered unpol-
luted with respect to Fe and Zn and moderately
polluted with respect to As.
Partitioning of Fe, Zn, and As
The total metal concentrations in surface sedi-
ments can be used as a parameter to identify
metal pollution in a water body. However, in or-
der to asses better the heavy metal environmental
impact and to ascertain their bioavailability and
probable toxicity, it is important to know the
metal partitioning obtained through sequential
extraction procedures.
Iron (Fe)
Iron concentrations in different geochemical frac-
tions of sediments are shown in Fig. 5. According
to this figure, the partitioning of this metal in

Table 4 Geoaccumulation Class Igeo Sediment quality Contamination intensitya

index and pollution
extent
a Times above
background values
0 0 Unpolluted 0
1 0–1 Unpolluted to moderately polluted 3
2 1–2 Moderately polluted 6
3 2–3 Moderately to strongly polluted 12
4 3–4 Strongly polluted 24
5 4–5 Strongly to very strongly polluted 48
6 >5 Very strongly polluted 98
340 Environ Monit Assess (2010) 166:331–346

Table 5 Geoaccumulation index for Cuitzeo Lake and

Grande River sediments evident that the highest concentrations of iron
were extracted in the F5 phase (more than 84%),
Location Sampling Fe Zn As
characterizing stable compounds in sediments
RG1 Jan 2006 0 0.03 0.18
May 2006 0 0.03 0.26
and reflecting a predominance of iron from a
Nov 2006 0 0.03 0.22 lithogenic source. The metal associated with this
RG2 Jan 2006 0 0.03 0.24 fraction cannot be remobilized under normal con-
May 2006 0 0.03 0.12 ditions encountered in nature. This distribution
Nov 2006 0 0.03 0.27 suggests the existence of crystalline and partially
HDA Jan 2006 0 0.03 0.19 crystalline Fe oxides (Soltan et al. 2005; Sakan
May 2006 0 0.03 0.26 et al. 2007) that could act as collectors for heavy
Nov 2006 0 0.03 0.17
metals in the sediments from Cuitzeo Lake and
RG3 Jan 2006 0 0.04 0
May 2006 0 0.04 0 Grande River. Besides, since the collected sam-
Nov 2006 0 0.03 0.16 ples represent the oxidized surface sediments and
RG4 May 2006 0 0.04 0.16 since the pH range of Cuitzeo Lake and Grande
Nov 2006 0 0.03 0 river waters was alkaline, this would be consistent
with the Fe occurrence as oxides and oxyhydrox-
ides (Korfali and Davies 2000). Iron is associ-
ated to a significant level (about 2–14%) to F3
sediments was in the following order: residual (84– in almost all sediments samples and to a lesser
99%)>Fe–Mn oxides (0.88–14%)>organic mat- extent to F4 (about 0.2–4.3%). The concentrations
ter and sulfides (0.11–4.3%)>bound to carbonates of iron in these two fractions vary according to
fraction (0.007–0.061%)>exchangeable (0.001– all sites and sampling campaigns and may be at-
0.017%). This partitioning is similar to the frac- tributed to iron organic complexes and hydrous
tionation reported in Xochula River (Espinosa iron oxide forms (Jain et al. 2007). Only small
and Armienta 2007) and the Nahr-Ibrahim River concentrations of iron were found in F2 and F1
in Lebanon (Korfali and Davies 2000). It was and could be considered negligible.

Fig. 5 Partitioning of iron 100%

in surface sediments from
Cuitzeo Lake and Grande 90%
River (F1 exchangeable,
F2 bound to carbonates, 80%
F3 associated with
70%
Fe–Mn oxides, F4
associated with organic
60%
matter and sulfides,
F5 residual fraction) 50% F5
F4
40%
F3
30%

20%

10%

0%
May-06.

May-06.

May-06.

May-06.

May-06.
Nov-06.

Nov-06.

Nov-06.

Nov-06.

Nov-06.
Jan-06.

Jan-06.

Jan-06.

Jan-06.

RG1 RG2 HDA RG3 RG4

SITE
Environ Monit Assess (2010) 166:331–346
Zinc (Zn)
The partitioning of Zn in sediments from Cuitzeo
Lake and Grande River are presented in Fig. 6.
It can be noticed that the fractionation profile for
sites inside the lake follow the order: F5>F3>
F4>F2>F1. For the sites located in the river,
the fractionation was: F5>F3>F2>F4>F1. Sim-
ilar Zn partitioning has been reported in sed-
iments of Damodar River, India (Singh et al.
1999). Although F5 shows the highest percentage
of Zn, an important amount of Zn is bounded to
F3 (Fig. 6), particularly in sediments of Grande
River, suggesting that these sediments are playing
an important role as scavengers for Zn from the
aqueous phase. Singh and Subramanian (1984)
explained that colloidal particles of Fe and Mn
oxides act as efficient scavengers of heavy metals
due to adsorption processes occurring between
these particles and metals in the aqueous phase.
Furthermore, adsorption processes are affected
directly by particle size, being enhanced by fine
grain particles which are the main type in Cuitzeo
Lake and Grande River sediments. The dominant
role of Fe and Mn oxides on metal distribution
in sediments has also been reported in different
studies (Singh et al. 1999; Jain et al. 2007). Zn
also shows significant associations with the organic
Fig. 6 Partitioning of zinc
in surface sediments from
Cuitzeo Lake and Grande
River (F1 exchangeable,
F2 bound to carbonates,
F3 associated with
Fe–Mn oxides, F4
associated with organic
matter and sulfides,
F5 residual fraction)
341
matter and sulfides fraction (F4), especially in
Grande River sediments, increasing its proportion
on dry season sampling (January). The organic
phase has also been found as significant scav-
enger for heavy metals, especially for Cu and Zn
(Singh et al. 1999), and the dominant conditions
in the dry season could promote the distribution
of Zn to this fraction. Moreover, partitioning of
Zn reveals that the carbonates fraction (F2) rep-
resent a relevant phase for this metal in Grande
River sediments, ranging from 5.3% to 17% of
the total metal concentration. The association of
Zn with the carbonate fraction is also reported
by many workers (Singh et al. 1999; Korfali and
Davies 2005). This may lead to an easy mobility
and bioavailability of this metal in the Grande
River system (Boughriet et al. 2007). According
to Soltan et al. (2005), particulate or dissolved
organic matter in the water column acts as a metal
scavenger, once the heavy metals are trapped by
this matter they precipitate and incorporate to
sediments. Under this context, Navas and Machín
(2002) found positive correlations between Fe and
Zn concentrations and organic carbon content,
which could also explain the Fe bounded to the
organic phase in sediments (Fig. 5). Such capacity
of organic matter to adsorb metals leads to an in-
crement in total metal concentration in sediments
342
(Green-Ruiz and Páez-Osuna 2003), particularly
in the nonbioavailable phases in Cuitzeo Lake and
Grande River sediments.
It is well known that redox potential (Eh) is
a property strongly related to pH; therefore, by
inspecting Eh–pH diagrams (GSJ 2005) for the
redox-sensitive Fe ion, it may be assumed that
the most abundant form of Fe in most of the
sampling sites would be as Fe2 O3 , considering that
the pH values of sampled sediments were close
to 8 and physicochemical conditions in sediments
were close to neutral redox potential. However,
iron in amorphous iron oxides is usually in the
form of Fe(III), as in FeOOH (Sakan et al. 2007).
Although, in some sites like RG2 and RG3, where
pH values were closer to 7, Fe2+ and Fe(OH)+
would appear as significant species present in sed-
iments. These facts are in agreement with Fe par-
titioning where most of the Fe content is present
in the residual fraction (Fig. 6), except in sites like
RG2 and RG3. According to the Eh–pH diagram
for Zn, the most important species present could
be Zn2+ ion; however, in sites like RG1 and HAD
where higher pH values were detected, hydroxide
species of zinc could be present in surface sedi-
ments, which is also in agreement with higher con-
centrations in residual fractions of the samples.
Practically, measured pH that was mildly alkaline
Fig. 7 Partitioning
of arsenic in surface
sediments from Cuitzeo
Lake and Grande River
(F1 exchangeable,
F2 bound to carbonates,
F3 associated with
Fe–Mn oxides, F4
associated with organic
matter and sulfides,
F5 residual fraction)
Environ Monit Assess (2010) 166:331–346
and redox potential around zero kept the investi-
gated heavy metals in very susceptible equilibrium
between the solid and aquatic phases where the
solid phase should have ion-exchangeable char-
acteristics (Sakan et al. 2007). The pH values of
the water samples of all sites were between 7.3
and 9.1
Arsenic (As)
The fractionation profile of arsenic in surface sed-
iments from all sites is presented in Fig. 7. The
partitioning order was: F5>F4>F3>F2>F1. It is
important to mention that, in sites where total
arsenic levels are not significantly high (like RG3
and RG4, and RG2 in May samplings), this frac-
tionation is not observed. Despite the high con-
centrations of total arsenic found in all sediment
samples, this fractionation profile indicates that
most of the As found in sediments of Cuitzeo
Lake have low mobility because it is mainly
bounded to nonlabile fractions (F5 and F4). How-
ever, in sites like RG1 and HAD, the extent of
As associated with more labile fractions (F3, F2,
and F1) is notable, especially in HDA where the
exchangeable As showed the highest level for
this fraction in all samples, considering the total
Environ Monit Assess (2010) 166:331–346 343

Table 6 Values of RAC

RAC Criteria (%)
No risk <1
Low risk 1–10
Medium risk 11–30
High risk 31–50
Very high risk > 50
As concentrations. Changes in the abundance
of As in fractions associated with Fe and Mn
oxides could be explained by possible adsorption
processes where it is well established that As(V)
sorbs onto sediments and coprecipitation with
iron and manganese oxyhydroxides is known to
happen (Pandey et al. 2004).
Geochemically, exchangeable arsenic present
in Cuitzeo Lake sediments could be released if
there is any change in the ionic strength of the
system, like an increase in pH, water salinity, or
redox potential caused by human activities. Simi-
larly, any increment in concentration of ions (like
phosphates and nitrates) competing for adsorp-
tion sites on different phases of sediments may
induce release of arsenic bounded to Fe and Mn
oxides (F3) or clays (Pandey et al. 2004). Such
ions are usually present in agricultural runoffs and
its ionic strength increases with the use of fertil-
izers. Therefore, the fact that significant concen-
trations of As were found in sediments of Cuitzeo
Lake in labile fractions could represent a poten-
tial risk and should be considered for monitoring
geochemical and pollution conditions that could
lead to the release of this element to the water
column.
The sediment fractions representative of con-
tamination by anthropogenic sources are the ex-
changeable and carbonate bounded phases, which
are considered to be weakly bounded, and thus,
metals associated to these phases could migrate
easily to the water column becoming more bio-
available and potentially toxic. In solution, the
free metal ion is by far the most biologically
toxic, although easily exchangeable forms in sed-
iments can also be harmful (Newman and Jagoe
1994); therefore, the bioavailability of even a
small amount of the total metal in sediment can be
important. Conversely, metals in residual and or-
ganic matter fractions are not considered to have
high bioavailability since they are difficult to re-
lease and equilibrate with the aqueous phase.
The Risk Assessment Code (RAC), as given in
Table 6, indicates that sediment, which can release
less than 1% of the total metal in exchangeable
and carbonate fractions, could be considered safe
for the environment. On the contrary, sediment
releasing in the same fractions more than 50% of
the total metal has to be considered highly dan-
gerous and can easily enter the food chain (Perin
et al. 1985; Jain et al. 2007).
The RAC was applied for the case of zinc
in geochemical fractions of Cuitzeo Lake and
Grande River sediments, revealing that zinc in
sediments comes under the low risk category in

Table 7 RAC values for Sampling site Date RACa value (%) RACb value (%)
Zn and As at different
Zn As Zn As
sampling sites
RG1 Jan 2006 2.7 4.1 5.3 15.4
May 2006 8.2 0.9 11.4 4.1
Nov 2006 1.5 3.1 5.1 8.6
RG2 Jan 2006 2.8 1.7 6.6 6.9
May 2006 4.8 6.9 10 47.2
a Percentage calculated Nov 2006 4.9 0.9 25 6.0
with F1 and F2 HAD Jan 2006 3.0 18.0 7.4 30.1
concentrations of each May 2006 1.4 1.4 3.0 3.8
element Nov 2006 2.1 2.3 11.3 6.3
b Percentage calculated
RG3 Jan 2006 6.2 85c 24.8 100c
with F1, F2, and F3 May 2006 18 55.9c 25.6 100c
concentrations of each
Nov 2006 10.5 0.0 47.7 0.0
element
c Low arsenic total RG4 May 2006 13.1 4.3 36.4 5.9c
concentration Nov 2006 6.2 22.6c 20.5 23.4c
344
sites inside the lake (RG1, RG2, and HDA)
according to the values of Table 7, but in sites
of Grande River, zinc exists in F1 and F2 mostly
from 10% to 18% (Table 7), which indicates a
medium risk according to the RAC criteria. For
As, only the sites inside Cuitzeo Lake have signif-
icant concentrations of this element and the more
labile fractions contain from 1% to 7%, except
in HDA in dry season where the sum of these
fractions was 18% of the total concentration of
As (Table 7). Therefore, the sediments in Cuitzeo
Lake could be considered as low risk according to
this code. However, it is important to notice that
the sum of Zn and As concentrations in the first
three fractions (F1: exchangeable, F2: bounded
to carbonates, and F3: associated with Fe–Mn
oxides) is also significant, around 15% to 47%
(Table 7) in some sites inside the lake for As and
from 11% to 47% of zinc in sites of Grande River
(Table 7). This consideration is important since
changes in environmental conditions may easily
release significant amounts of these elements, as
mentioned before.
Conclusions
The study of total concentrations of iron, arsenic,
and zinc in sediments of Cuitzeo Lake and Grande
River showed that they can be considered as un-
polluted for Fe and Zn and moderately polluted
for As according to the geoaccumulation index.
However, with respect to zinc, the relatively high
concentrations in sediments of Grande River in-
dicate the existence of an anthropogenic source
of pollution, whereas for arsenic, the high levels
found on lake sediments are thought to be of
natural origin. The partitioning of these elements
in the different geochemical phases presented in
this paper demonstrated that some iron in all sed-
iment samples largely existed in the sedimentary
matrix and it should be considered as of litho-
genic origin, and the significant levels of this metal
as Fe oxides, as well as their fine particle size,
give the sediments of this area the possibility to
act as metal scavengers. Although the relatively
high concentrations of Zn and As in sediments of
Grande River and Cuitzeo Lake and their com-
Environ Monit Assess (2010) 166:331–346
paratively low bioavailability represents only a
low to medium risk according to the RAC criteria.
However, the risk may increase in the future if no
measures are taken to assess the anthropogenic
contamination of the lake.
Acknowledgements The authors acknowledge the finan-
cial support from Consejo Nacional de Ciencia y Tec-
nología (Project 12445 Fomix-Gobierno del Estado de
Michoacán).
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