The Environmentalist, 21, 187195, 2001

2001 Kluwer Academic Publishers. Manufactured in The Netherlands.

Lead removal from contaminated water using

mineral adsorbents

M. N. RASHED
Faculty of Science, 81528 Aswan, Egypt

Summary. This study records experiments undertaken to determine the suitable conditions for the use
of naturally occurring minerals (talc, chalcopyrite and barite) as an adsorbent for the removal of lead ions
from liquid wastes. The adsorption of lead ions from solutions containing different initial lead concentra-
tions (50, 100, 200, 400, 600, 800 and 1000 mg l1 Pb as lead nitrate) using different size fractions (<63

m, 63150
m) of talc, chalcopyrite and barite at different pH (3, 5, 7 and 9) and different adsorp-
tion times (24, 48, 72 and 96 hr) was examined. The results revealed that of the studied minerals, the
chalcopyrite fraction at 63150
m showed the highest adsorption capacity. The adsorption data of Pb
ions was also analyzed with the help of the Langmuir and Freundlich models to evaluate the mecha-
nistic parameters associated with the adsorption process. The adsorption isotherms obtained from the
Langmuir and Freundlich equations were generally linear and the adsorption of Pb by the studied miner-
als was correlated with the adsorption maximum and binding energy constant of the Langmuir equation
and equilibrium partition constant and binding partition coefcient of the Freundlich equation. It was con-
cluded that the equilibrium time of adsorption was 72 hr at an optimum pH from 7 to 9. This technique
might be successfully used for the removal of lead ions from liquid industrial wastes and wastewater.

Keywords: lead, absorption, models, Langmuir-Freundlich isotherm, heavy metals, pollution

Introduction occurring minerals. Pyrolusite has been used for

The discharge of contaminated industrial wastes
into rivers and lakes frequently causes the pollu-
tion of their water with heavy metals. Lead is one
of these heavy metals, and can be introduced to
liquid wastes from the manufacturing processes of
storage batteries, smelting and rening of lead and
from the processes of mining. In water, lead tends
to accumulate in aquatic organisms through the
food chain and by direct uptake (Smith, 1992).
Lead is believed to cause hypertension, repro-
ductive disorders and neurological and metabolic
problems in humans (Smith, 1992).
Adsorption of the heavy metal ions from solu-
tion has been studied by others using naturally
adsorption of Pb, Zn and Mg ions from aque-
ous solution (Ajmal et al., 1995) and zeolites
have been used for the removal of heavy metals
from wastewater (Yuan et al., 1999). Sigworth and
Smith (1972), Dabrowshi and Tertykh (1992) and
Muscas (1995) have also used adsorption tech-
niques for the removal of heavy metals from solu-
tions. Lin and Puls (2000) studied the arsenic
attenuation capacities of different clay minerals
and the aging process affecting the transforma-
tion of arsenic. The adsorption of Zn to col-
loidal quartz, hydrargillite and goethite (50,300
and 70 mg l1 , respectively) has been stud-
ied with variations of pH (310) (Duker et al.,
1995). Other adsorbents which have been used for

the removal of lead from solution include soils

Dr M. N. Rashed is a Lecturer (assistant professor) of Envi-
ronmental Analytical Chemistry in the Chemistry Department,
Faculty of Science, South Valley University, Aswan, Egypt. Fax:
02097480449; e-mail: mnrashed@hotmail.com.
(Campbell and Davies, 1995) and carbonaceous
material developed from fertilizer waste slurry
(Srivestava et al., 1989). Adsorption of lead ions
188 Rashed
from polluted water using activated carbons pro-
duced from burning date pits or stones (Girgis and
Hendawy, 1997), and by ferrite and chealating
resin (Tokunaga and Uthium, 1997) have also
been studied. Other workers such as Sigworth and
Smith (1972) and Koshima and Onishi ( 1986)
reported detailed investigations on the adsorption
of metal ions (including Pb) by commercial acti-
vated carbons. Kaolinite and alumina were used
for the removal of lead from incinerated lubricat-
ing oil by Hall (1998), kaolinite was found to bind
chemically to airborne lead emissions because of
the strong chemical bond between the lead and
the kaolinite surface. Lead sorption onto an oxide
mineral surface was observed in powder sorption
solution at equilibrium, x/m is the amount of
adsorbate adsorbed per unit mass of adsorbent.
The Langmuir isotherm is constructed by plot-
ting 1/x/m against 1/c; if the data lie on a
straight line then the Langmuir model can be con-
sidered to be appropriate. Using least square lin-
ear regression, the term b (reciprocal of the slope)
and k1/b may be found.
The other model for adsorption is the
Freundlich isotherm, which is expressed as:
x/m = kc 1/n
where x/m is the amount adsorbed per unit mass
of adsorbent, c is the solution concentration at
experiments and modeled using a surface com-
plexation approach by Davis and Kent (1990). Cal-
cite, is an important mineral that is common in
soils and sediments, and was successfully applied
for the Pb adsorption from dilute aqueous solu-
tions by Strurchio et al. (1997). Mn, Co, Ni, Zn
and Pb were strongly adsorbed by the calcite sur-
face in experiments by Reeder (1996). Jain and
Ram (1997) studied the effect of initial Pb ion
concentrations, pH, contact time, adsorption dose
and particle sizes on the adsorption of Pb by
stream sediment. Pb(II) adsorption onto goethite
and alumina was studied in aqueous 0.1 M NaCl
solution as a function of pH (57), sorption den-
sity (1.25
moles m2  and Pb concentrations
(0.244.53 mM) (Bargar et al., 1998). Coffee has
been used for the removal of Pb, Cu, Hg, Cd and
Zn from drinking water at a rate of 7890 percent
of the dissolved heavy metals (Strong, 2000).
Adsorption is a term commonly used for sev-
eral different processes involving physical as well
as chemical interactions between the solid sur-
face of a substance and a dissolved metal species.
Thus, adsorption in general can be inuenced by
changes in hydrochemical parameters, such as pH
and Eh.
The Langmuir equation was used as the model
for adsorption by Bohn et al. (1985), the adjusted
Langmuir equation in its linear form being
1/x/m = 1/cb + 1/a
where a is Langmuir binding energy coefcient,
b (mg kg1  is the adsorption maximum, c (mg
dm1  is the concentration of adsorbate left in
equilibrium, k n are constants relating to adsorp-
tion capacity and intensity.
The Freundlich model is constructed by plot-
ting log x/m against log c and the intercept
of the line, log k, is roughly an indication of
the adsorption capacity, while the slope, 1/n,
is an indication of adsorption intensity (Weber,
1972). The Freundlich adsorption isotherm is gen-
erally regarded as being less sensitive than the
Langmuir isotherm in describing adsorption phe-
nomena because more information is required in
the Langmuir model (Campbell and Davies, 1995;
Tokunaga and Uthium, 1997). From these adsorp-
tion models, the adsorption maximum, the binding
energy from the Langmuir model, and the adsorp-
tion capacity and intensity from the Freundlich
model can be calculated, and so the efciency of
the adsorbent for the removal of heavy metals can
be obtained.
The aim of this study was to nd out the effec-
tiveness of new material (minerals) with large sur-
face areas which could be used as adsorbents for
the removal of lead ions from wastewater and
industrial liquid wastes. The minerals used were
talc, barite and chalcopyrite.
Experimental work
Mineral sample collection and preparations
Talc, barite and chalcopyrite samples (5 kg of
each) were collected from the Eastern Desert of
Nasser Lake at Aswan in the south of Egypt.
The minerals were crushed using a mechanical

crusher and ball mill and then ground by using
an electric agate mortar. The powdered ores were
sieved in sieve series of <63, 63150, 150250 and
250500
m.
Standard solutions
Certied atomic absorption spectroscopic stan-
dard solution as lead nitrate (1000 ppm). Work-
ing standard solutions 800, 600, 400, 200, 100 and
50 ppm were prepared by dilution with distilled
water.
Analysis
An atomic absorption spectrophotometer
equipped with air-acetylene burner was used
in the lead analysis. A lead hollow cathode lamp
at the recommended current and conditions was
used.
Adsorption studies
To determine the best size to obtain a high adsorp-
tion capacity, a one gram sample of each grain size
of each mineral was washed with 50 ml bidistilled
water three times,then treated with 50 ml of solu-
tion containing 1000 ppm Pb in a conical ask.
Constant stirring of the solution was maintained
for 24 hr. After attainment of equilibrium, the
content of the ask was ltered through a 0.45
m
cellulose nitrate membrane lter and subsequently
analysed for residual concentration of Pb ion using
the atomic absorption spectrophotometer (AAS).
The concentration of adsorbed Pb ion was calcu-
lated from the known total amount of adsorbate
added and the amount measured in the ltrate
after equilibration.
Effect of concentration
To evaluate the effect of initial Pb ion concentra-
tion on adsorption behaviour for each of the min-
erals used, studies were conducted with initial Pb
ion concentration of 1000, 600, 400, 200, 100 and
50 ppm with a xed adsorbent dose of one gram
and particle sizes of <63 and 63150
m.
Lead removal from contaminated water 189
In order to choose the mineral size that had
maximum adsorption capacity, the mineral sizes
of talc, barite and chalcopyrite (<63, 63150
m)
were treated with 50 ml lead standards (1000, 600,
400, 200, 100, 50 ppm) in a conical ask for 24 hr.
After attainment of equilibrium, the content of
the ask was ltered through a 0.45
m cellulose
nitrate membrane lter and the Pb ion concentra-
tion was analysed using atomic absorption spec-
trophotometer. The nal concentration of lead at
equilibrium was determined and the adsorption
capacity was calculated.
Effect of time on adsorption
To determine the adsorption time required for
equilibrium of Pb solution with adsorbate, one
gram of the study mineral (two sizes <63, 63
150
m for each mineral) was treated with 50 ml
of 1000 ppm Pb standard solution, shaken sev-
eral times and the nal concentration of Pb was
determined at different times i.e. 24, 48, 72 and
96 hr. The adsorption capacity was calculated in
each case.
Effect of pH on adsorption
One gram of each mineral sample was treated with
50 ml of 1000 ppm lead solution; then the pH of
the adsorption mixture was adjusted to various pH
values (3, 5, 7 and 9) by using 0.5 M NaOH or
0.5 M HCl. The nal concentration of lead was
determined after 24 hr and the adsorption capac-
ity was calculated in each case.
Effect of mineral dosage
0.25, 0.5, 1 and 2 g of each mineral size was treated
with 50 ml of 1000 ppm lead standard solution.
The nal concentration of lead after 24 hr, was
determined using AAS,and the adsorption capac-
ity was calculated for each case.
Removal of lead ion from synthetic wastewater
Synthetic wastewater samples containing different
metal ions were prepared by diluting stock solu-
tion containing various metal ions in 1:1 distilled
190 Rashed
water. 50 ml of this wastewater was treated with
2 g of chalcopyrite size 63150
m in a conical
ask; pH was adjusted to pH 9. After 96 hr the
amount of lead was then determined by atomic
absorption spectrophotometery.
Results and discussion
Particle size
The experimental data for the adsorption of Pb
ions for different sizes of talc, barite and chal-
copyrite (<63, 63150, 150250 and 250500
m)
and at a xed adsorbent dose (one gram) and ini-
tial Pb concentration of 1000 ppm are shown in
Table 1. In the tables percent refers to the mass
of Pb removed from treated waste divided by the
mass of Pb in the initial untreated waste, times one
hundred. From the table the maximum adsorption
of Pb on talc (15.7 percent) is at the size <63

m. This adsorption decreases with increase in
both talc and barite sizes. Maximum adsorption
for chalcopyrite was over the size range 63150

m. Consequently, these optimum sizes were used
in the other experiments. These small particle
sizes (<63
m and 63150
m) have large surface
area per unit weight and so provide more adsorp-
tion capacity than the larger particle size of the
mineral (Langmuir; 1918). Others (Ajmal, 1995)
have shown similar results, pyrolusite size 100125
mesh has been used for the removal of lead ions
from polluted water (maximum adsorption 96.2
percent). Srivastava et al. (1989) used 200500
m
carbonaceous materials developed from a fertil-
izer waste slurry for the removal of heavy metals
which included Pb. The experimental data of Jain
and Ram (1997) for the adsorption of Pb ions for
different sizes of sediment (75150, 150210, 210
250, 250300 and 300425
m) showed that the
Table 1. adsorption percentage of lead (1000 ppm) for
different minerals of different sizes.
% Pb adsorption
Mineral sizes (
m) Talc Barite Chalcopyrite
<63 15.7 13.9 16.9
63150 2.9 5 17.7
150250 11.5 3 16.4
250500 10.7 5.3 11.2
percent of Pb ions adsorbed decreased linearly
from 30 to 20 percent with increasing geometric
mean of adsorbent size. They again attributed this
to adsorption being a surface phenomenon; the
smaller sizes offered a comparatively larger sur-
face area.
Effect of lead concentration on adsorption
The adsorption data (Table 2) of lead adsorbed
on talc, barite and chalcopyrite sizes <63 and
63150
m following use of different initial Pb
concentrations (50, 100, 200, 400, 600, 800 and
1000 ppm) indicates that the maximum adsorp-
tion occurred with the lowest initial lead concen-
tration (50 ppm) and the adsorption decreased
with increasing initial Pb concentration. Mineral
sizes showed variable adsorption with initial Pb
concentrations. Talc size <63
m showed max-
imum Pb adsorption (24 percent) using initial
Pb concentration of 50 ppm; then the adsorption
values decreased as the initial concentration was
increased up to 1000 ppm. Size 63150
m showed
a different trend in which the maximum adsorp-
tion observed (22 percent) using initial Pb con-
centration of 100 ppm.
Chalcopyrite exhibited a higher adsorption
maximum than either talc or barite. Srivastava
et al. (1989) found that the maximum adsorption
(100 percent) occurred at a low concentration
of Pb ions when using carbonaceous material
developed from the waste of a fertilizer plant,
and at higher solute concentration, the maximum
removal of lead was 75 percent.
Effect of pH on adsorption
Experiments with solution pH as a variable were
also conducted to determine the optimum pH
range for maxmium Pb adsorption by talc, barite
and chalcopyrite. Graphical representation of the
adsorption data for Pb ions on talc, barite and
chalcopyrite over the studied pH range are shown
in Fig. 1.
The results reveal that adsorption increases
with the increase in pH from pH 3 to 7 and
the maximum adsorption is at pH 7 for talc (78
percent) and barite (90 percent). At pH 9 there
 Lead removal from contaminated water 191

Table 2. Effect of concentration of lead adsorption for different adsorbent minerals

% Pb adsorption

Talc Barite Chalcopyrite

Initial Pb
Conc. (ppm) <63 63150 <63 63150 <63 63150

50 24 18 30 16 50 44
100 16 22 14 14 41 11
200 8 16 19 5 2 5 45 25
400 2 5 5 8 7 2 1 5 17 5 13
600 3 1 4 1 2 5 0 8 9 1 1 1
1000 15 7 2 9 13 9 5 16 9 17 2

was no adsorption, while chalcopyrite revealed
maximum adsorption at pH 9 (100 percent).
Other studies (Hunng et al., 1977; Srivestava et al.,
1989) have shown an abrupt increase in the
adsorption of Pb in the pH range 56. Lead
adsorption on chalcopyrite seems to be correlated
to surface pH, where greater adsorption occurs
at the highly basic surface, pH(OH)2 is formed
and raises Pb uptake (Girgis and Hendawy, 1997).
The strong pH dependency of adsorption reects
solution hydrolysis or protonition at the adsorb-
ing ions, and the surface charging propriety of the
adsorption (Jenne and Zachara, 1982).
Another study revealed that the maximum
adsorption of Pb on pyrolusite occurred at pH
7 (Ajmal, 1995). Girgis and Hendawy (1997)
reported that activated carbon from date pits or
stones removed considerable amounts of lead ions
(62200 mg g1 ) from lead-polluted wastewater;
lead uptake seemed to be correlated to surface
pH, where at high basic surface it raised the
uptake. Gadde and Laitinen (1974) concluded that
maximum adsorption of Pb (100 percent) with
hydrous manganese oxide (HMO) occurred at pH
67. The adsorption characteristics of a variety
of divalent and trivalent metal-EDTA complexes
onto goethite (a-FeOOH) showed high adsorption
at a low pH (Nowack and Sigg, 1996).
Effect of time on adsorption
From Fig. 2 it can be seen that for talc and barite
of size <63
m, the Pb adsorption increased with
time to reach its maximum adsorption at almost
72 hr and 96 hr respectively. Chalcopyrite sizes
<63
m and 63150
m attain equilibrium after
96 hr. Ajmal et al. (1995) reported 100 percent
lead adsorption from pyrolusite after 30 minutes.
Koshima and Onishi (1986) reported an optimum
time of contact of 4 hr for the adsorption of heavy
metals on commercial activated carbon. Jain and

120
Talc
100
Barite
% Pb adsorbed

80 Chalcopyrite

60

40

20

0
3 5 7 9
pH

Figure 1. Effect of pH on Pb adsorption.

192 Rashed

80
Talc
70
Barite
60
% Pb adsorbed
Chalcopyrite
50
40
30
20
10
0
24 48 Time (hours) 72 96

Figure 2. Effect of different times on lead adsorption for different minerals (<63
m).

Ram (1997) studied the effect of contact time of
the Pb adsorption on sediments size 210250
m
and found the most effective to be 45 hr.
Effect of adsorbent mineral dose on adsorption
After obtaining the suitable mineral sizes, opti-
mum pH, initial Pb concentration and equilibrium
time for Pb adsorption, it was decided to obtain
the suitable dose of the adsorbent that provided
a maximum adsorption capacity. The results are
shown in Fig. 3 where the adsorption of Pb indi-
cates change with the amount of the adsorbent
mineral. The adsorption increased as the amount
of mineral used increased, and it reached a maxi-
mum adsorption at 2 gm adsorbent.
Removal of Pb ions from
the synthetic wastewater
Chalcopyrite size 63150
m exhibited the high-
est value of lead adsorption (99100 percent) and
it was used as an adsorbent for removing lead
ions from synthetic wastewater. It was conrmed
that 100 percent removal of Pb was possible from
wastewater containing 50 ppm Pb ion under exper-
imental conditions of pH 9 and 96 hr treatment
time, whereas only 80 percent removal of lead was
possible when the concentration of Pb was higher
(at 300 ppm in the wastewater).
Adsorption isotherms
Langmuir isotherms. The Pb adsorption data were
plotted according to linear Langmuir isotherms

40
35
30
% Pb adsorbed

25
20
15 Talc
10 Barite
5 Chalcopyrite
0
0.25 0.5 1 2
Mineral weight (gm)

Figure 3. Effect of the amount of the adsorbent minerals (<63
m) on lead.
 Lead removal from contaminated water 193

0.1 Table 3. Langmuir isotherms: linear regression data and lead

0.08 adsorption parameters for talc barite and chalcopyrite
minerals of different sizes
1/(x/)

0.06
0.04 y = 2.3393x + 0.0281 a b
R2 = 0.7491
0.02 Adsorption Binding r 2 for
0 Sizes maximum energy Langmuir
0 0.005 0.01 0.015 0.02 0.025 0.03 Adsorbents (
m) (mg kg1 ) (mg 11 ) equation
1/c
Talc <63 36 0.427 0.749
(a)
63150 44 0.312 0.821
0.08
Barite <63 32 0.766 0.871
0.06 63150 31 0.248 0.869
1/(x/m)

Chalcopyrite <63 99 1.35 0.906

0.04 63150 71 1.08 0.937
y = 1.3047x + 0.0309
0.02 R2 = 0.8718

0
0 0.005 0.01 0.015 0.02 0.025 0.03
The chalcopyrite fraction (<63
m) has a higher
1/c
capacity (99 percent) to adsorb Pb ions than the
(b)
fraction 63150
m (71 percent). The order of
0.045
0.04 lead adsorption capacity for fractions <63
m and
0.035 63150
m is:
0.03
1/(x/m)

0.025
0.02
0.015
0.01
0.005
0
0 0.01 0.02
1/c
(c)
Figure 4. Langmuir adsorption isotherms for minerals of size
<63
m. a) talc, b) barite, c) chalcopyrite.
(Figs. 4a-c) Regression data and adsorption
parameters obtained from them are indicated in
Table 3. Adsorption data obtained with the dif-
ferent adsorbents of different sizes <63
m and
63150
m correlated well with the Langmuir
adsorption model. The Langmuir parameters (a
and b) are calculated from the slope and inter-
cept of the graphs and are given in Table 3. One
advantage of the Langmuir equation in its linear
form is that the adsorption maximum can be cal-
culated from the regression. This parameter and
the equilibrium lead concentrations are useful in
describing the adsorbent capacity (Tokunaga and
Uthium, 1997).
Examination of the linear regression data and
the lead adsorption parameters (Table 3) suggests
9 for
that chalcopyrite size <63
m has a higher Pb
adsorption (99 percent) than either barite or talc
of sizes <63
m and 63150
m (3144 percent)
Chalcopyrite > talc > barite
y = 0.7366x + 0.0101
R2 = 0.9062 The Langmuir binding energy coefcient
(Table 3) indicates that the binding of Pb ion to
0.03 0.04 0.05
chalcopyrite is higher (1.35 for size <63
m and
1.08 for size 63150
m) than that for either talc
or barite. Other studies of bioadsorption of Pb
by biomass of Alfalfa revealed a binding capac-
ity of 43 mg Pb bound per gram of the biomass
(Gardea-Torresdey et al., 1996). Srivastava et al.
(1989) stated that Pb adsorption data obtained
with the adsorbent which they used (commercial
activated carbon) correlated well the Freundlich
and Langmuir adsorption models.
Freundlich isotherms. Figs. 5a-c and Table 4 rep-
resent Freundlich models and parameters for
chalcopyrite, talc and barite adsorption which
indicate highly signicant relationships. Table 4
shows the Freundlich linear regression data and
Pb adsorption parameters for talc, barite and chal-
copyrite adsorbents of different sizes. The high
values for correlation coefcients (r 2 ) indicate
a strong linearity of the two models (Langmuir
and Freundlich) for describing the adsorption data
obtained in the present study. All positive correla-
tion coefcients (r 2 ) of Langmuir and Freundlich
models are highly signicant at r 2  > 0
chalcopyrite, while barite and talc have low pos-
itive correlation coefcients for Freundlich and
Langmuir isotherms.
194 Rashed

2 lead ions from wastewater and industrial liquid

1.5
wastes at recommended pH 79. The increase of
the amount of adsorbent increased Pb adsorption,
Log x/m

1 while the equilibrium time was up to 72 hr. Adsor-

0.5
y = 0.5013x + 0.221
R2 = 0.8874
bent minerals that were tested for Pb adsorption
were conrmed by either the Langmuir or the
0
Freundlich models.
0 0.5 1 1.5 2 2.5 3 3.5
Log C
(a)
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