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Engineering Geology 60 (2001) 6168

www.elsevier.nl/locate/enggeo

pH inuence on sorption characteristics of heavy metal in the


vadose zone
M. Elzahabi a,*, R.N. Yong b
a
Department of Civil Engineering and Applied Mechanics, University of McGill, Canada
b
Geoenvironmental Engineering Research Centre, University of Wales, Queen's Buildings, P.O. Box 917, Newport Road, Cardiff CF2 1XH, UK
Accepted for publication 25 April 2000

Abstract
Sorption is an important process in the modelling and prediction of the movement of heavy metals in unsaturated clay
barriers. This experimental study investigates the effect of pH changes in the acidic range on the sorption characteristics of
heavy metals such as: lead, copper and zinc in an unsaturated soil. A series of one-dimensional coupled solute and moisture
leaching column tests, using different heavy metal solutions, were conducted on an unsaturated illitic soil at varying pH values.
Variations of volumetric water content (VWC) with distance were measured for different time durations, and concentrations of
heavy metals in the liquid and solid phases were analysed. Partitioning coefcient proles of contaminants along the soil
column were determined for each individual layer in the soil.
Results from column leaching tests showed that the sorption characteristics of heavy metals are controlled by many factors
which should be taken into consideration, i.e. the VWC, time of wetting, soil pH, and the inuent heavy metal concentrations.
Simplication of Kd as a constant and of the VWC as a linear function cannot be considered a good assumption and may lead to
an improper evaluation of the sorption phenomena and also to serious errors in predicting contaminant transport through
unsaturated soils. q 2001 Elsevier Science B.V. All rights reserved.
Keywords: Leaching column; One-dimensional ow; Unsaturated; Heavy metals; Sorption

1. Introduction and nickel (Ni). The concentration of these heavy


metals varies from 0 to 100 ppm in municipal solid
Heavy metals migration through the vadose zone is waste leachate to 10010,000 ppm in sewage sludge,
one of the most serious environmental problems and is mining wastes and various industrial wastes (Yong
a major topic of investigation and research worldwide. and Diperno, 1991). Their solubility is highly pH
The heavy metals largely originate with the combus- dependent and increases with the decrease in the
tion of fossil fuels or from spills or uncontrolled soil pH. Heavy metal sorption mechanisms in soils
dumping of solvents and wastes. The most common are different at different soil pH values and the soil's
heavy metals found in leachate solution are lead (Pb), ability to retain them depends on its resistance to any
copper (Cu), zinc (Zn), cadmium (Cd), chromium (Cr) change in soil pH. The sorption of heavy metals
increases with increasing pH and decreases with
* Corresponding author. 3225 Leduc, Vile ST Hubert, Quebec,
decreasing pH (Farrah and Pickering, 1977; Yong et
Canada J3Y 5B5. Tel.: 11-450-926-9058; fax: 11-514-484-2752. al., 1993).
E-mail address: malakelz@civil.lan.mcgill.ca (M. Elzahabi). Movement of chemicals in the ground water is
0013-7952/01/$ - see front matter q 2001 Elsevier Science B.V. All rights reserved.
PII: S 0013-795 2(00)00089-2
62 M. Elzahabi, R.N. Yong / Engineering Geology 60 (2001) 6168

primarily a liquid phase process involving the move- (Darban, 1997). Sorption characteristics obtained
ment of water and dissolved solutes. Chemicals that from leaching column tests provide a better means
are not sorbed will exist primarily in the dissolved of evaluating soil sorption performance and also
phase and their movement in the ground water will account for the effects of partial soil saturation. For
be controlled by the relative amount of water, and by these reasons leaching tests are more valuable than
soil processes that govern the fate of the contami- batch tests of soils.
nants. Soil is an excellent adsorbent for both organic This paper experimentally investigates heavy metal
and inorganic chemical compounds. The major sorption through the vadose zone at varying pH. The
adsorbing surfaces in soil are clay particles and heavy metals investigated are lead, copper and zinc.
organic matter. The interactions between contami- The soil sorption characteristics of these metals are
nants and soil fractions can be expected to inuence measured in terms of metal retention and migration.
the physical and physico-chemical behaviour of the
material.
2. Methodology
Sorption data are needed to determine the transport
properties of the soil with respect to the contaminants
In order to determine the sorption characteristics of
under consideration. Test data permits one to calcu-
the soils, a series of one-dimensional coupled solute
late the partition coefcient Kd required in the
and moisture ow tests, were conducted on an unsa-
contaminant transport equations. Most transport
turated illitic soil at varying pH values. Samples were
models use Kd obtained from `linear' adsorption
tested in horizontal leaching columns designed to
isotherms, i.e. as a constant parameter (Freeze and
simulate slow ow of leachate through unsaturated
Cherry, 1979; Rowe, 1988). Simplication of (Kd)
clay (Elzahabi and Yong, 1997). The soil was rst
as a constant and linear function may lead to an
statically compacted into the leaching column cell to
improper evaluation of the adsorption/desorption
its maximum dry density (1.88 Mg/m 3) and optimum
phenomena. `Although it is well recognized that the
moisture content (14.16%). The cell was then leached
partitioning coefcient can play a crucial role in
with a continuously supplied nitrate permeant solution
controlling the rate mass transfer through saturated
of lead, copper or zinc. Two concentrations of each
soils and has been extensively investigated, there is
solution were used: 2500 and 5000 mg/l. All trials
an unfortunate dearth of information on the effect of
were conducted at constant atmospheric pressure,
partial saturation on the partitioning coefcient,'
under a negligible hydraulic gradient and at room
(Fityus et al., 1999). Davidson et al. (1976) concluded
temperature. Samples were tested after time durations
that at high concentrations, the assumption of a linear
of 52 h and 17.8 days. For each time duration, the test
isotherm can lead to serious errors in predicting
sample was removed and sectioned into disc shapes
contaminant migration. `Although the convenience
for chemical analysis. Variations of volumetric water
of the approach is beyond dispute, its validity as a
content (VWC) with distance were measured for
means of developing reliable predictions of the beha-
different time durations, and metal partitioning analy-
viour of inorganic contaminants in actual ground
sis of heavy metals in the pore uid (soluble ions) and
water systems is questionable in many situations,'
the solid phases (extractable ions) were analysed. The
(Cherry et al., 1984).
partitioning coefcient (Kd) proles were determined
It is known that batch equilibrium tests usually used
for each individual layer in the soil and are investi-
to determine adsorption isotherms utilize small
gated in the following sections.
portions of soil and representative contaminants.
The problem with this method is that the small quan- 2.1. Metal partitioning analysis
tity of soil may not adequately simulate the actual soil
conditions. Also, the batch method may not reect the The metal partitioning analyses were conducted
actual leachatesoil-interaction. The ratio of solution according to the Environmental Protection Agency
to soil and the time required to attain equilibrium does (EPA) procedures and ASTM standards. Two differ-
not always give a good estimate of the migration and ent soil suspension methods were used to determine
adsorption of heavy metals through a clay barrier the concentration of heavy metals in the soil: (a) the
M. Elzahabi, R.N. Yong / Engineering Geology 60 (2001) 6168 63

pore uid removal or the batch shaker test was used to metal bonds and to prepare soil samples for analysis
determine the soluble cations concentration in the by AAS in order to determine the background level of
liquid phase; and (b) the acid digestion method was the trace metals in soil. Hot diluted nitric acid (HNO3)
used to measure the metals concentration in the solid was used to dissolve the inorganicmetal bonds and
phase. For both methods, analysis of the uid for to ensure complete oxidation. Hydrogen peroxide
heavy metal ions (Zn 21, Pb 21, Cu 21) associated with (H2O2) was added to the soil, and was warmed until
the sample solution was performed using the Perkin the effervescence was minimal or the general sample
Elmer Model 3110 atomic absorption spectro- appearance was unchanged to ensure complete
photometer (AAS). The cation concentrations were destruction of the organicmetal bonds. After cool-
expressed in mg/100 g. ing, the sample was diluted up to 100 ml and then
allowed to settle overnight. The sample was then
2.1.1. Soluble phase centrifuged at 5000 rpm for 10 min to clear the super-
Soluble cations were determined using the pore natant of any particulates that may clog the nebuliser.
uid removal method or the batch shaker test. Dupli- The concentration of a particular species adsorbed by
cate suspensions with a ratio of 1:10 soil weight to the clay and found in the supernatant for each slice
solution volume of distilled water were prepared as was obtained using the following formula:
recommended by the United States Environmental DF Csmg=l Vml 100g
Protection Agency (USEPA) (USEPA, 1987) to esti- Ctmg=100 g 2
1000ml WDSg
mate the attenuation of chemicals from batch tests.
For each batch test, 30 ml of distilled water was where Ct is the total concentration of metals by the
added to 3 g of soil and mechanically shaken in the clay which was found in the supernatant and is
end-over-end shaker for 24 h. After agitation, the expressed in mg per 100 g of the soil, DF the dilution
sample was then centrifuged in plastic Nalgene centri- factor, Cs (ppm) or (mg/l) is a particular species
fuge tubes at 10,000 rpm for 20 min and the clear concentration in the supernatant and is obtained
supernatant was collected for heavy metals (Zn 21, from AAS readings, V the volume of distilled water
Pb 21, Cu 21) analysis by means of AAS. The concen- used during the test (100 ml was used), 1000 ml is
tration of a particular species found in the supernatant used to convert from 1 l to 1 ml and WDS is the
(i.e. in the pores of each slice) was calculated using weight of dry soil expressed in grams (where 1 g or
the following formula: 2 g was used). Thus,
DF Csmg=l Vml 100g S Ct 2 C 3
Cmg=100 g 1
1000ml WDSg
where (S) is the total concentration of metals in the
where C is the soluble species concentration found in solid phase which can be obtained by subtracting the
the supernatant and is expressed in mg per 100 g of soluble species concentration C from the total concen-
the soil, DF the dilution factor, Cs (ppm) or (mg/l) is a tration (Ct) of metals by the clay. The units of S, Ct
particular species concentration in the pore uid and C are expressed in mg of constituent per 100 g of
which is obtained from AAS readings, V the volume dry soil.
of distilled water used during the test (where 30 ml
was used, 1000 ml is to convert from 1 l to 1 ml) and 2.2. Partitioning coefcient (Kd)
WDS the weight of dry soil in grams (where 3 g was
used). The partition coefcient (Kd) is used to describe
contaminant partitioning between the liquid and solids
2.1.2. Solid phase only if the reactions that cause the partitioning are fast
Heavy metals in the solid phase were measured and reversible, and only if the isotherm is linear,
using the acid digestion method (3050) of the (Yong et al., 1992).
USEPA (USEPA, 1986). This method is an acid S
digestion method used to dissolve all the sample Kd 4
C0
64 M. Elzahabi, R.N. Yong / Engineering Geology 60 (2001) 6168

Table 1
Summary of volumetric water content and heavy metal partitioning coefcient Kd results for illitic soil C at pH 4.0, (5000 mg/l input
concentration)

Input time 5000 mg/l 52 h 5000 mg/l 17.8 days

Heavy metals (HM) Pb Cu Zn Pb Cu Zn

Before leaching
VWC (%) 26.69 27.26 26.32 26.69 27.26 26.32
After leaching above: 40 mm
VWC (%) 35.8131.06 37.1531.45 35.8731.43 38.3033.58 37.7933.29 37.9733.28
Kd 12.68-innite 5.58-innite 5.16-innite 41.64-innite 18.46-innite 4.7724.16
Below 40 mm
VWC (%) 31.0628.09 31.4528.93 31.4329.84 33.5831.77 33.2931.11 33.2831.32
Kd Innite Innite Innite Innite Innite Innite

where S represents the ratio between the mass of the where r w is the water density and r d the bulk density
contaminant adsorbed onto the solid phase divided by or the dry density, and is dened as the weight of the
the mass of the soil to obtain a measure of the relative soil divided by the total volume of the soil, (Yong and
mass of the constituent adsorbed on the solid phase. The Warkentin, 1975).
units of the numerator are expressed in mg of adsorbed
Ws
constituent/100 g of soil. The denominator C 0 represents gd 8
the concentration of the contaminant in solution and its Vs 1 V V
unit is expressed in mass of constituent/volume of
moisture or g/ml. The partitioning coefcient (Kd) unit
is expressed in ml/g. According to Yong et al. (1992) 3. Results and discussion
and Mohsen (1993), the mass of constituent in moisture/
volume can be computed from: 3.1. Moisture distribution
C C r
C0 C d 5 The soil moisture distribution is the central to sorp-
nSV uV u tion characteristics because heavy metals are trans-
where C is the concentration of the contaminant in the ported in solution. Heavy metals in illite are mostly
solution and is expressed in (mass/mass) or (mg/100 g), retained as carbonates or hydroxides at soil pH values
r d the bulk density of the soil (g/ml), u the VWC (frac- above 4. Below pH 4, retention of heavy metals is
tion), n the porosity (fraction), S (fraction) the water mostly by ionic exchange, (Yong et al., 1992). In
saturation and V (ml) is the total volume of soil. order to study the movement of heavy metals in acidic
The VWC (u ) is dened as volume of water per soil, the buffering capacity of the illitic soil was
volume of moist soil: reduced by using nitric acid. Lowering the pH value
of the soil increases the solubility of heavy metals in
Vw V the soil water by redissolving the heavy metals preci-
u w 6
Vs 1 Vv V pitates (e.g. with carbonates and hydroxides) in the
where Vs is the solid volume and Vv is the void soil water. The greater availability of ions will
volume. enhance mobilization and the rate of their loss by
The relation between the water content (w) and the leaching (Yong and Phadungchewit, 1993; Yong
VWC (u ) is: et al., 1992). The retention of heavy metals increased
when the pH of the soil solution exceeded the value
w 1 required for precipitation, (Farrah and Pickering,
u r 7
100 d rw 1976, 1977, 1979). Since the focus of this study is
M. Elzahabi, R.N. Yong / Engineering Geology 60 (2001) 6168 65

Table 2
Summary of volumetric water content and heavy metal partitioning coefcient Kd results for illitic soil D at pH 3.5, (5000 mg/l input
concentration)

Input time 5000 mg/l 52 h 5000 mg/l 17.8 days

HM Pb Cu Zn Pb Cu Zn

Before leaching
VWC (%) 26.69 26.32 26.32 26.69 26.32 26.32
After leaching: above 40 mm
VWC (%) 41.7532.28 38.3131.02 38.6732.09 38.8632.67 38.9033.11 39.2433.09
Kd 1.20-innite 6.74-innite 5.50-innite 15.07-innite 4.9959.30 2.5811.79
Below 40 mm
VWC (%) 32.2828.67 31.0228.18 32.0929.22 32.6730.40 33.1132.37 33.0931.15
Kd Innite Innite Innite Innite Innite 34.34-innite

on the retention of heavy metals by ionic exchange concentration are summarized in Tables 14, respec-
mechanisms, and since sorption of lead onto illite soil tively. The test results show moisture and solute
at high pH values is by precipitation mechanisms distribution along the soil column from the source
(Macdonald and Yong, 1997; Yong et al., 1993), the point due to the internal suction gradients as
soil pH in this study was reduced to values below pH 4 expected. For soil C, it was observed that at initial
to avoid heavy metals precipitation. The carbonate time of wetting (52 h) and for high input concentra-
contents for soil C and D decreased with decreasing tion of nitrate solution (5000 mg/l), the steepest gradi-
soil pH and ranged between 5.22 and 4.60%, respec- ents of the VWC occurred near the source point,
tively. Also, the dissolution of carbonates and the where the soil is considered to be fully saturated for
acidication of the soil cause a decrease in the CEC all trials, (Tables 1 and 3). Also for lead the higher
values obtained, ranging from 34.20 meq/100 g (illite concentration solution resulted in a higher VWC. This
at pH 9.5) to 7.94 meq/100 g (soil B, pH 6.9), to difference was most pronounced in the 52 h samples.
6.81 meq/100 g (soil C, pH 4) and to 5.34 meq/ For copper or zinc there was no apparent correlation
100 g (soil D, pH 3.5). between concentration and VWC. The same conclu-
Results before and after leaching for illitic soils C sions may be drawn from soil D, (Tables 2 and 4). The
and D due to 5000 and 2500 mg/l of heavy metal input high average of the VWC when leached with Cu is

Table 3
Summary of volumetric water content and heavy metal partitioning coefcient Kd results for illitic soil C at pH 4.0, (2500 mg/l input
concentration)

Input time 2500 mg/l 52 h 2500 mg/l 17.8 days

HM Pb Cu Zn Pb Cu Zn

Before leaching
VWC (%) 26.69 27.26 26.32 28.20 27.26 26.32

After leaching: above 40 mm


VWC (%) 32.0428.61 37.0432.07 38.6531.73 36.8533.71 36.5133.45 38.0732.88
Kd 41.03-innite Inniteinnite 16.54-innite 3.23-innite 48.35-innite 10.3339.79
Below 40 mm
VWC (%) 28.6127.60 32.0730.47 31.7329.46 33.7131.94 33.4530.47 32.8831.68
Kd Innite Innite Innite Innite Innite Innite
66 M. Elzahabi, R.N. Yong / Engineering Geology 60 (2001) 6168

Table 4
Summary of volumetric water content and heavy metal partitioning coefcient Kd results for illitic soil D at pH 3.5, (2500 mg/l input
concentration)

Input time 2500 mg/l 52 h 2500 mg/l 17.8 days

HM Pb Cu Zn Pb Cu Zn

Before leaching
VWC (%) 26.32 26.32 26.32 26.69 27.26 26.32
After leaching: above 40 mm
VWC (%) 33.0129.08 36.9431.87 36.9231.45 37.6032.92 38.8433.05 38.7134.27
Kd 1.36-innite 117.7-innite 55.92-innite 35.50-innite Innite-Inni. 16.7153.48
Below 40 mm
VWC (%) 29.0831.15 31.8728.71 31.4529.20 32.9231.98 33.0531.96 34.2731.98
Kd Innite Innite Innite Innite Innite Innite

due to the high initial value of the VWC before leach- sections, as given in Section 2. The Kd results for illitic
ing (Table 1). soils C and D are shown in Tables 14.
Generally, VWC is higher in the longer time inter- The partitioning coefcient Kd is seen to increase
val samples of soils C and D. The only exception is the with soil pH and distance from leachate source. It
soil D, high concentration of lead, in the rst 40 mm decreases with an increase in time of wetting, inuent
Sample. This may be explained by the longer diffu- heavy metal concentrations and in degree of satura-
sion time for more leachate solution and by the tion or VWC. Results showed a maximum sorption
leachate lowering the soil pH. It seems natural to and retention of heavy metals near the source point.
conclude that the presence of lead increases the Sorption decreases in absolute terms, along the soil
VWC in a way that is somewhat proportional to column. For soil D, it was observed that for a high
the concentration of lead. This conclusion explains input concentration of (5000 mg/l) and at initial time
the higher water content with concentration and the of wetting (52 h), Pb is more retained than Cu and Zn.
one noted exception to longer time intervals having These results are similar to those of soil C using a
higher water content (soil D, 5000 mg/l, 52 h, rst 5000 mg/l permeant solution with the following
40 mm). It should be noted that for low input concen- exceptions. The total weight of sorbed heavy metal
tration, the high average value of the VWC in soil C is signicantly higher at this lower pH for Pb and
when leached with Pb and Cu is due to the high initial Cu at 52 h and for Cu at 17.8 days. Nevertheless,
value of the VWC before leaching, (Table 3). the distribution of the sorbed metal is approximately
Interpretation of volumeric water content results the same except that more Pb is found in the soluble
should be made with the knowledge that the pH of state in the saturated zone at 52 h, and a greater
the samples changed along the soil column length. percentage of Cu is found in the 040 mm saturated
The pH in the unsaturated zone (.40 mm) increased zone. The low value of Kd obtained when leached with
over time with leaching. high Pb concentration can be attributed to the high
amount of lead released to the soluble phase as a result
3.2. Partitioning coefcient results of the acidic water entrapped in the rst section of the
soil D, resulting in an increase in the VWC from 26.69
A partition coefcient Kd is calculated for each to 41.75%.
section of the leaching soil column and the results In comparison with soil D and at high input concen-
are summarized as a function of soil depth and time tration, soil C (pH 4.0) showed an increase in Kd
of wetting for soil pH values of 3.5 (soil D) and 4.0 due to the increase of heavy metal attenuation. The
(soil C) and for lead, copper and zinc nitrate solution. selectivity order of Kd values fall in the order
Solid and liquid phases were determined from the soil of 12.68innite ml/g (Pb) . 5.58innite ml/g
M. Elzahabi, R.N. Yong / Engineering Geology 60 (2001) 6168 67

(Cu) . 5.16innite ml/g (Zn) were associated with enough to resist the acidic leachate input, and sorption
high concentration (5000 mg/l), (Table 1). While processes will prevail in the carbonate phase. There-
values of inniteinnite (Cu) . 41.03innite ml/ fore, heavy metals were accumulated in the rst
g (Pb) . 16.54innite ml/g (Zn) were associated section of soil with pH 6.9 resulting in a calculated
with low concentration (2500 mg/l), (Table 3). partition coefcient value of innity. As the soil pH
However, at shallow depths (above 40 mm) and as decreases, the dissolution of carbonates increases and
the time of wetting increased (17.8 days), the parti- ionic exchange becomes the more dominant process
tioning coefcient Kd decreased with an increase in in heavy metal retention. In acidic soil, CEC of the
the degree of saturation. soil decreases slightly with a lowering the soil pH.
The overall test results revealed that as the distance This however does not detract from the ability of
and time of wetting from heavy metals source the soil to retain heavy metals under unsaturated
increased, and within the unsaturated phase (below conditions. At shallow depths and as the time of
40 mm depth), the amount of heavy metals released wetting increased, the partitioning coefcient
to the soluble phase decreased sharply. This indicates decreased with an increasing degree of saturation.
that heavy metals migrates only a very short distance However, as the distance and time of wetting from
from the input source during the specied migration heavy metals source increased, and within the unsa-
time, and this causes innite Kd values. The reason for turated phase, the amount of heavy metals released to
the soluble phase decrease might be related to the the soluble phase decreased sharply, indicating that
decrease in the degree of saturation along the soil heavy metals migrates only a very short distance
column and may also be explained by the cation from the input source during the specied migration
exchange capacity (CEC) of the soil. The CEC was time, resulting in innite Kd values. This might be
still able to almost completely retain the introduced related to the decrease in the VWC or the degree of
heavy metals under unsaturated conditions. saturation along the soil column and may be also
Furthermore, the presence of carbonates in the illite explained by the CEC of the soil, which was still
soil increases the retention of heavy metals at high pH able to almost completely retain the introduced
and also enhances the buffering capacity of the soil. heavy metals under unsaturated conditions.
The higher the carbonate content of the soil, the Results showed that the partitioning coefcient of
greater the retention of heavy metals by the carbonate heavy metals are controlled by many factors which
phase (Yanful et al., 1988). Therefore, because of its should be taken into consideration, i.e. the degree of
high carbonate content (11.73%) and high CEC saturation or VWC, soil pH, time of wetting and the
(7.94 meq./100 g), heavy metals were accumulated inuent heavy metals concentrations. Therefore,
in the rst section of soil with pH 6.9 resulting in a simplication of (Kd) as a constant and of the degree
calculated partition coefcient value of innity. of saturation as a linear function cannot be considered
a good assumption and may lead to an improper
evaluation of the sorption phenomena in the vadose
4. Concluding remarks zone and also to serious errors in predicting contami-
nant migration through unsaturated soils.
This research study provides the experimental
information necessary for numerical analyses on the
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