Chapter 12

Effect of the Solid:Liquid

Ratio on the Sorption of
Sr^"^ and Cs"^ on Bentonite

Dennis W. Oscarson and Harold B. Hume

AECL, Whitehall Laboratories, Pinawa, Manitoba, Canada

Several factors can affect the magnitude of the distribution coeffi-

cient, K^, for contaminants with earthen materials, but one of the
most puzzling is the commonly observed decrease in K^ with an in-
crease in the solid: liquid ratio or particle concentration, C —the so-
called particle concentration effect. The main explanations advanced
for the phenomenon are the presence of nonsettling particles in so-
lution and the effects of particle-particle interactions. Here we ex-
amine the effect of C on K^ for Sr^"^ and Cs"^ with unconfined and
compacted Avonlea bentonite. The solution phase was either a syn-
thetic groundwater (a Na-Ca-Cl-dominated solution with an effec-
tive ionic strength of 0.22 mol-L~^) (Cs experiments) or 0.1 mol-L~^
NaCl (Sr experiments). The particle concentration ranged from 5.2 to
41.6 g-L-i for Sr and from 2.4 to 18.6 g-L"! for Cs. For both sorbates,
K^ decreased with increasing C . Moreover, the effect was more pro-
nounced for the compacted clay system. The difference observed be-
tween the unconfined and the compacted clay systems is likely due
to the presence of more occluded pores or very small pores in com-
pacted clay that the sorbates cannot enter; thus they carmot access as
many of the sorption sites on the clay surface. The results indicate
that the particle concentration effect is largely due to particle-parti-
cle interactions, or the blocking of some sorption sites, and not to the
presence of nonsettling particles.

Adsorption of Metals by Geomedia

Copyright © 1998 by Academic Press. All rights of reproduction in any form reserved. 277
278 Oscarson and Hume

I. INTRODUCTION
The distribution or partition coefficient, K^, measured at equilibrium, is a use-
ful concept that expresses the relative affinity for a sorbate in solution to sorb to a
particular solid. The parameter has been used extensively in models to predict the
behavior of contaminants in the environment. The batch method is often used to
determine this coefficient in the laboratory and the results extrapolated to field sit-
uations.
The K^ is defined as
_ (mass sorbed/mass of solid) .
^ (mass in solution/volume of solution)
or, alternatively.
(mass sorbed) ^
^ ~ (mass in solution)C '
where C is the particle concentration in mass per unit volume.
The magnitude of K^ is a function of the properties of the solid phase, such as
mineralogical composition, particle size, and organic carbon content, and of the
solution phase, like pH, ionic strength or salinity, and concentration of complex-
ing ligands. The influence of these factors can generally be rationalized within
the frameworks of solution and surface chemistry. However, another, more puz-
zling, factor that can affect K^ values is the solidiliquid ratio or C . In theory, at
trace sorbate concentrations, K^ should not depend on C . Commonly, though,
measured K^ values decrease with increasing C (Honeyman and Santschi, 1988;
Meier et al, 1987; Di Toro et al, 1986; Gschwend and Wu, 1985; Voice et al,
1983; O'Connor and Connolly, 1980)—the so-called particle concentration ef-
fect.
Two schools of thought have evolved over the interpretation of the particle con-
centration effect: (1) it is essentially an experimental artifact caused by colloids
that are operationally defined as part of the dissolved fraction but are nonetheless
sorbing solutes (an implicit assumption is that the concentration of the sorbing col-
loids in solution is proportional to C ), and (2) the phenomenon is the consequence
of physical-chemical processes such as particle-particle interactions that affect the
equilibrium distribution of solutes.
Clearly, if K^ values determined by the batch method are to be used in models
to predict the fate of contaminants in natural environments, the particle concen-
tration effect must be clarified. Here we examine the effect of particle concentra-
tion on K^ for Sr and Cs with Avonlea bentonite in both an unconfined and a com-
pacted state.
We are interested in bentonite and the K^ parameter because compacted ben-
tonite has been proposed for use as a barrier material in the disposal of nuclear fuel
Sr^'^ and Cs"^ Sorption on Bentonite 279

waste in many countries, and the K^ is a common component of mass transport

models used to predict the migration of trace levels of radionuclides in these com-
pacted bentonitic barriers (Johnson et ah, 1994).

11. MATERIALS AND METHODS

A. CLAY

Avonlea bentonite from the Bearpaw Formation of Upper Cretaceous age in

southern Saskatchewan, Canada, was used. It contains about 80 wt % dioctahedral
smectite, 10 wt % illite, 5 wt % quartz, and minor amounts of gypsum, feldspar,
and carbonate (Oscarson and Dixon, 1989). The clay has a cation exchange ca-
pacity of 60 cmol-kg"^ and a specific surface area of 480-10^ m^-kg~\ and Na"^
is the main exchangeable cation.
The Avonlea bentonite contains about 0.2 g-kg"^ of Sr (Oscarson and Dixon,
1989). If soluble, this could lead to an increase in Sr concentration in the experi-
mental systems to a level where precipitation as well as sorption reactions occur.
[The likely solid Sr phase to form in these systems is strontianite, SrC03 (Benson
and Teague, 1980).] Because of this native Sr, for the Sr experiments the clay was
washed several times with a 1 mol-L~^ solution of NaCl. Afterward the clay was
dialyzed against deionized water for several days to remove excess salt, and then
freeze-dried. Subsequent analysis showed that this treatment removed about half
of the Sr in the clay. After this treatment, the clay's exchange complex is, of course,
also saturated with Na"^.

B. SOLUTIONS

A synthetic groundwater (SGW) solution was used in the Cs/bentonite experi-

ments; it has an effective ionic strength of 0.22 mol-L~^, and the following com-
position (in mmol-L-i): Na, 83; K, 0.36; Mg, 2.5; Ca, 53; CI, 170; and SO4, 12.
It was chosen to represent groundwater found deep in granitic rock in the Canadi-
an Shield where a nuclear fuel waste disposal vault could be sited (Johnson et ah,
1994).
The SGW solution contains some Sr, derived from impurities in some of the
salts used in its preparation; this source of Sr could also affect the K^ measurement
as already discussed. Consequently, a 0.1 mol-L~^ solution of high-purity NaCl
was substituted for the SGW solution in the Sr/Na-bentonite experiments.
The salinity of the solution phase in both the Sr and the Cs experiments was
such that the ionic strength and pH—9.0 for the Sr and 7.8 for the Cs experi-
ments—were effectively constant throughout the reaction period. Thus, during the
280 Oscarson and Hume

course of the experiments, the sorption reactions were not influenced by changes
in the solution phase.

C. SORPTION EXPERIMENTS

1. Unconfined Clay
Bentonite was suspended in 0.1 L of a 0.1 mol-L~^ NaCl solution containing
^^Sr, or 0.5 L of the SGW solution containing ^^'^Cs. The initial ^^Sr concentration
was about 0.1 nmol-L"\ and that of ^^^Cs, 1 nmol-L~^; the total initial Sr con-
centration was, however, about 2.1 |xmol-L~^ because of the soluble native Sr
present in the clay and the NaCl solution. The clay or particle concentration ranged
from 5.2 to 41.6 g-L~^ for Sr and from 2.4 to 18.6 g-L~^ for Cs. All experiments
were conducted in triplicate in polyethylene containers. The suspensions were
gently shaken periodically. Every few days, a 1-ml aliquot of solution was care-
fully withdrawn without disturbing the sedimented clay and analyzed for ^^Sr or
^^^Cs by liquid scintillation counting. Sorption equilibrium was assumed when the
sorbate solution activity was constant with time; this occurred in less than a week
for both sorbates.

2. Compacted Clay
For comparison with unconfined clays, sorption experiments were conducted
with ^^'^Cs and compacted bentonite using specially designed cells (Fig. 1). A hy-
draulic press was used to statically compact the clay in the stainless-steel rings of
the sorption cells to target dry densities, p, ranging from 0.5 to 1.5 Mg-m~^; in the
sorption experiments these densities gave particle concentrations that cover the
same range as those used in the Cs/unconfined clay system. The rings containing
the compacted clays were placed in the sorption cells and the cells immersed in
0.5 L of SGW solution in polycarbonate containers. When the cells are immersed,
Cs diffuses through the porous disks of the cell and into the pores of the clay, where
some of it is sorbed; hence its concentration in the contacting solution decreases.
The activity of ^^^Cs in solution was monitored periodically by liquid scintillation
counting. The experiment was continued until the activity of ^^'^Cs in solution be-
came constant with time, indicating that sorption equilibrium had been established.
The reaction period depended on the clay density—the greater the density, the
longer the reaction period—but was generally about 600 days. The uniform dis-
tribution of ^^^Cs within the clay plugs after the reaction periods also indicated
that equilibrium was achieved in these systems (Oscarson et al, 1994).
For both the compacted and the unconfined clay systems, control experiments,
conducted identically but without clay, showed that no detectable amounts of Sr
or Cs sorbed on the walls of the polyethylene or polycarbonate containers, nor on
Sr^'^ and Cs'^ Sorption on Bentonite 281

Porous Disk
Stainless Steel Cylinder
Clay Plug
Porous Disk
Polysulfone Cell

5cm
_l
Figure 1 Diagram of the sorption cell.

any of the components of the sorption cell. All experiments were conducted at
22 ± 2 T .

D. D I S T R I B U T I O N COEFFICIENTS

Distribution coefficients were calculated from

A,V, - A V
Ka = [3]
AVC
where A. is the net (total activity minus background activity) initial activity and
A is the net equilibrium activity of ^^Sr or ^^'^Cs in solution [the activities were
corrected for the radioactive decay of ^^Sr (1^^ = 64 days) and ^^'^Cs (t^^ = 30
yr) that occurred during the experiments], V. is the initial volume of solution, V^
is the solution volume when sorption equilibrium was established, and Cp is the
particle concentration at sorption equilibrium.
282 Oscarson and Hume

E. PORE PARAMETERS OF COMPACTED BENTONITE

Pore parameters of compacted bentonite (p = 1.3 Mg-m"^) were measured to

provide supporting evidence that colloidal material does not move in these com-
pacted clays, and hence there should be little or no colloidal material in the solu-
tion phase in the experiments with compacted clay. Therefore, if the particle con-
centration effect was observed in these systems, it could not be attributed to
suspended colloids.
The pore parameters were obtained as follows. A clay plug was sandwiched be-
tween porous disks and constrained in a specially designed stainless-steel holder.
The plug was saturated by immersing it in the SGW solution for 4 weeks; it was
then slowly dried—to minimize disruption of the pore structure—in chambers
having progressively drier atmospheres. The relative humidities (over H^SG^ so-
lutions) in the chambers were 81, 58, and 3.2%. The plug was kept at a given hu-
midity for at least two weeks. The clay was then examined by Hg intrusion
porosimetry to 414 MPa. At the maximum intrusion pressure of 414 MPa, Hg can
theoretically enter pores with a diameter as small as 3.6 nm. Before the measure-
ment, the sample was outgassed at 6.5 Pa at room temperature.

III. RESULTS AND DISCUSSION

The K^ values for Sr and Cs obtained at various C are given in Table I. The
greater values for Cs than for Sr are attributed, at least in part, to minor amounts

Table I
Distribution Coefficients, K^, for Sr and Cs with Unconfined Avonlea Bentonite

Sr Cs

Cp K^ Cp K^
(kg-L-i-lO^) (L-kg-Q (kg-L-^-103) (L-kg-i)

5.2 83.7 ± 9.60« 2.4 1840 ± 56

8.1 73.7 ± 1.08 3.5 1700 ± 14
10.4 71.1 ±2.12 11.2 1390 ± 1 7
11.1 70.3 ±0.64 16.7 1290 ± 31
15.8 65.4 ± 2.52 18.6 1200 ± 15
19.6 64.8 ± 1.50
20.8 63.9 ± 1.40
21.9 63.1 ± 1.40
41.6 54.9 ± 1.93

'^Arithmetic mean ± one standard deviation of three replicates.

Sr^'^ and Cs'^ Sorption on Bentonite 283

of illitic material present in Avonlea bentonite—about 10 wt % (Oscarson and

Dixon, 1989): illite has a unique affinity for certain alkali metals, including Cs"^
(Sawhney, 1972). Also evident in Table I, consistent with the observations report-
ed by many others, is a decrease in K^ with increasing C—the particle concen-
tration effect. Figure 2 shows log K^-log C plots of the data. O'Connor and Con-
nolly (1980) noted that the particle concentration effect is generally more
pronounced for sorbates with higher K^ values. This is not the case for our data,
despite the fact that K^ is more than an order of magnitude greater for Cs; the slope
of the log-log plot for both Sr and Cs is -0.19.
As noted, the particle concentration effect has been largely attributed to either
nonsettling particles or to particle-particle interactions. The compacted clay ex-
periment was designed, in part, to test these hypotheses.
A log K^-log C plot for Cs with unconfined and compacted bentonite is
shown in Figure 3. About one-third less Cs is sorbed on compacted versus un-

3.3 k Cs / bentonite
SGW;l = 0.22mol»L"^
pH = 7.8

3.2 h

3.1
•

• 3.0

^ 2.0
Sr / Na-bentonite
0.1 mol*L"^ NaCI
o pH = 9.0
i.9r

1.8 -h

1 i 1 1
1.7
-2.8 -2.4 -2.0 -1.6 -1.2
1-1^
log Cp (kg.L^)
Figure 2 K, versus C for Sr and Cs with unconfined bentonite. I, effective ionic strength.
284 Oscarson and Hume

-
3.3 h
Cs
unconfined clay
pH 7.8
3.2

3.1 h Y
•

3.0 V- • (0.50)
s
Cs
^ 2.9 ^ (0.70) compacted clay
pH 11.1
o
2.8 r

k (0.90)
2.7 h Y
\(1.25)
\(1.50)
2.6 1 1 1 1
-2.8 -2.4 -2.0 -1.6 -1.2
log Cp (kg-L-^)
Figure 3 K^ versus C for Cs with unconfined and compacted bentonite. The values in parentheses
for the compacted clay are the clay dry densities in Mg-m~^.

confined bentonite, and the slope of the plot for Cs with compacted clay is sig-
nificantly greater than that obtained with unconfined clay. Hence, the particle con-
centration effect is more pronounced for the compacted clay system. These data
are confounded to some extent by the fact that the solution pH in the compacted
clay system (pH = 11.1) is greater than that of the unconfined clay (pH = 7.8).
The K^ for Cs with bentonite, however, increases with increasing pH (Fig. 4).
Therefore, the higher pH for the compacted clay system cannot explain the low-
er K^ measured in this system (Fig. 3). [We have determined that the relatively
high pH in the compacted clay system is due to the porous Ni disk used in the
sorption cell. Because of the effect of the porous disk on pH, we have not yet de-
termined the sorption of Sr on compacted clay: at this high pH, the concentration
of Sr in solution would exceed the solubility limit of SrC03(s) (Benson and
Teague, 1980). Before testing other sorbates with compacted clay, other porous
Sr^'^ and Cs'^ Sorption on Bentonite 285

materials that do not significantly alter the solution chemistry need to be identi-
fied for use in the sorption cell.]
It is likely that Cs cannot access as many of the sorption sites on the compact-
ed clay as it can on the unconfined clay. This exclusion may be due, at least in part,
to the presence of more extremely small pores, occluded pores, or "ink bottle"
pores in compacted clay that the Cs ions cannot enter—and the higher the densi-
ty, the greater the number of inaccessible pores.
The particle concentration effect observed for the compacted clay system (Fig.
3) is not due to nonsettling colloids. Based on the following arguments, there
should be few, if any, colloidal particles in the solution phase because such col-
loids cannot move from the compacted clay into the solution.
The migration of colloidal particles in compacted bentonite is extremely slow,
if they can move at all. To our knowledge, no reliable measurements of diffusion
coefficients for colloidal material in compacted bentonite have been obtained, al-
though attempts have been made. In a study of colloid and radionuclide transport
in compacted bentonite (p = 0.9 Mg-m~^), for example, Nowak (1984) reported
that colloidal gold (mean particle diameter = 16.4 nm) was completely excluded
from compacted bentonite. Moreover, Eriksen and Jacobsson (1982) found no dif-
fusion of large organic molecules (molecular weight ranged from 350 to 30,000
g-mol~^) in compacted bentonite, and concluded that diffusion coefficients for
these solutes must be <10~^^ m^-sec~^ (Because of size similarities, diffusion
measurements of large organic molecules in compacted bentonite are relevant to
colloid transport.) With a diffusion coefficient of <10~^^ m^-sec~\ a colloidal
particle could only migrate <0.2 nmi in compacted bentonite within the time of
the Cs sorption experiments with compacted clay, about 600 days; this distance is

3500 Cs/bentonite
SGW
Cp = 26 g«L-^

^ P 2500

s^ 1500

•
Kf\n _ 1 1 1 I I

8 9 10 11 12

Equilibrium pH
Figure 4 K^ versus equilibrium pH for Cs with unconfined bentonite.
286 Oscarson and Hume

<2% of the total plug length. Therefore, only colloidal material at the interface of
the clay and porous disk could possibly migrate into the solution phase. Technical
data obtained from the supplier of the Ni disks used in the sorption cells indicate
that their average pore diameter is 25 jxm. Thus colloidal transport through even
the porous disks would be very slow.
This immobility of colloids in compacted bentonite is supported by the mea-
surement of the pore size distribution of compacted bentonite (Fig. 5). The diam-
eter of nearly all pores is close to 0.01 jxm, and there are few, if any, larger pores.
The associated pore parameters obtained from Hg intrusion porosimetry are total
Hg intrusion volume, 141 cm^*kg~^ median pore diameter, 14.1 nm; and average
pore diameter, 11.6 nm. These values are close to those obtained for compacted
Na- and Ca-bentonite, and the pore size distribution shown in Figure 5 is essen-
tially the same as that of Na-bentonite compacted to a similar density (Choi and
Oscarson, 1996).
In the compacted clay system, therefore, there are likely few, if any, colloidal
particles in the solution phase. Even if some are present, they are almost certain-
ly at a much lower concentration than in the unconfined clay systems, yet the par-
ticle concentration effect is more pronounced for the compacted clay system. We
conclude, therefore, that the particle concentration effect observed in Fig. 3 is
largely due to particle interactions, through the blocking of some sorption sites,
rather than nonsettling colloids in the solution phase.
Di Toro et al. (1986) also concluded that particle interactions were the main rea-
son for the particle concentration effect they observed in a study of the sorption of
heavy metals on clay and quartz. Their experiments also virtually eliminated the
possibility of nonsettling colloids as being responsible for the effect. On the other
hand, Gschwend and Wu (1985) and Voice et al. (1983) present convincing evi-
dence that nonsettling (or nonfilterable) colloids were the cause of the particle con-

-I—I I I i i i i | 1 I I I iiiij 1—I I I i i i i | I—I I i m i | I—I I I i i i i |

• o f 20
S"
I t ^5
!s 9> 10
c •2c 5
O 3
E o 0
t t i f f i i i n l i i i n i i K i i 111 J •• ^t tiir^ilTitLafc

£9>o> 0.001 0.01 0.1 1 10 100

Pore diameter (|im)
Figure 5 Incremental intruded pore volume versus pore diameter for compacted Avonlea bentonite
( p = 1.3Mg-m-3).
Sr^'^ and Cs'^ Sorption on Bentonite 287

logCp(kg*L^)
Figure 6 K^ versus C for Ni and Co with montmorillonite and quartz at constant equilibrium met-
al concentration (40 |JLg-L~0 and pH 9 (data adapted from Di Toro et al, 1986).

centration effect in studies of the sorption of hydrophobic organic compounds on

sediments.
McKinley and Jenne (1991) reported that K^ for Cd with Fe oxide was inde-
pendent of the particle concentration. They concluded that the particle concentra-
tion effect is caused in some cases by inappropriate experimental design or errors
of data interpretation. They state, "If all three variables (meaning Cp, and the mass
sorbed and the mass in solution at equilibrium) are computationally unconstrained,
the value of K^ is, likewise, not constrained to a meaningful value. If C^ is to be
treated as a variable, then K^ has a vahd definition only at constant [M^+]
(p. 2086)." (In their notation, [M^"^] is the equilibrium sorbate concentration.) We
cannot test this assertion from our data as sorption isotherms at different C^ are
not available. Di Toro et al (1986), however, present sorption isotherms for Ni and
Co with montmorillonite and quartz at different Cp (Fig. 3 in their paper). From
these data, we calculated K^ values at a constant equilibrium sorbate concentra-
tion for the C values used by these authors; the log K^-log Cp plots are shown in
Figure 6. A similar plot can be constructed from the data on Kepone sorption on
sediments reported by O'Connor and Connolly (1980). Clearly, even at a constant
equilibrium sorbate concentration, the particle concentration effect is evident in
these systems. At our present level of understanding, it is not clear why the parti-
288 Oscarson and Hume

cle concentration effect should be observed in some systems, but apparently not
in others.

IV. SUMMARY AND CONCLUSIONS

A decrease in K^ with an increase in C—the particle concentration effect—is
conmionly observed for a variety of sorbate-sorbent systems, and our data for Sr
and Cs sorption on both unconfined and compacted bentonite also exhibit this phe-
nomenon. Although extensively studied, the reason for the particle concentration
effect remains obscure. Main explanations involve nonsettling colloids and parti-
cle-particle interactions. Our data for Sr and Cs sorption on both unconfined and
compacted bentonite suggest that particle-particle interactions play a predominant
role.
Despite the particle concentration effect, K^ can be a useful parameter in mod-
els used to predict contaminant behavior at trace levels (<|xM) in natural envi-
ronments. However, K^ values should be measured under conditions as close as
possible to those in the environment of interest; these conditions include particle
concentration, solution composition, and sorbate concentration.

ACKNOWLEDGMENTS
The Canadian Nuclear Fuel Waste Management Program is funded jointly by AECL and Ontario
Hydro under the auspices of the CANDU Owners Group.

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