Calculation on Ion Exchange Capacity for an Ion Exchanger

Using the Potentiometric Titration

WON-KEUN SON,1SANG HERN KIM,1 TAE IL KIM2

1
Department of Chemical Technology, Taejon National University of Technology, Taejon 300-717, Korea

2
Department of Chemical Engineering, Chungnam National University, Taejon 305-764, Korea

Received 24 May 2000; revised 19 July 2000; accepted 8 September 2000

ABSTRACT: We calculated the characteristics of a phosphoric cation exchanger and

studied an accurately computable method for ion exchange capacity for a type of
potentiometric titration curve. The ion exchanger was prepared by phosphorylation of
a styrene-divinylbenzene copolymer. The ion exchange capacity was 5.7 meq/g. The
experimental pK values versus ␹ in a phosphoric cation exchanger can explain a linear
equation. The ⌬pK values were obtained from the slope of a linear equation. The ⌬pK
values were the differences of pK values between the apparent equilibrium constant at
complete and zeroth neutralization of the ion exchanger. The experimental pK values
at ␹ ⫽ 0.5 (␹:degree of neutralization of ion exchanger) showed good agreement with the
theoretical data. When it was titrated with NaOH and Ba(OH)2 solutions, a good
agreement between experimental and theoretical pK values for various ␹ was found in
all potentiometric titration curves. The potentiometric titration curve near the inflec-
tion point in the case of divalent ions was changed more sharply than that for mono-
valent ions. The plot of ⭸pH/⭸g versus g (number of moles of alkali to 1 g of ion
exchanger) was fitted to the Lorenzian distribution, from which ion exchange capacity
was accurately evaluated. © 2000 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 38:
3181–3188, 2000
Keywords: ion exchanger; phosphoric ion exchanger; potentiometric titration; equi-
librium constant

INTRODUCTION tory removal rate to meet the pollution control

Recently, with a rapid development of industry,
removal of heavy metal ions and toxic gases in
environmental pollution has received much atten-
tion. Materials for treatment of wastewater and
toxic gas must be developed. Toxic heavy metal
can be separated easily from wastewater by ion
exchange resin.1–3
Traditional precipitation processes, such as ze-
olite and clay, do not always provide a satisfac-
Correspondence to: S.H. Kim
Journal of Polymer Science: Part B: Polymer Physics, Vol. 38, 3181–3188 (2000)
© 2000 John Wiley & Sons, Inc.
limit. However, ion exchange resin has various
functions, such as waste treatment, separation of
rare earth metals and heavy metals, separation of
amino acids, purification, sorption of toxic gases,
drying agents, and bleaching agents.4 Ion ex-
change resin can selectively separate toxic gases
from the industrial resources of air pollution with
simple equipment and little energy. There have
been many studies on ion exchange resin by many
researchers.5
The electrolytes are commonly divided into
nonpolymeric and polymeric. An ion exchanger is
a polymeric electrolyte. It is commonly recognized
that potentiometric titration is one of the most
3181
3182 SON, KIM, AND KIM
important methods for investigation and charac-
terization of ion exchangers. At the same time, a
great discrepancy between theory and practice of
this method in application to ion exchangers ex-
ists.6 Because the inflection points of the poten-
tiometric titration curve for strong acidic and ba-
sic ion exchangers are obvious, the capacity of the
ion exchanger can be accurately determined from
potentiometric titration curves. However, week
acidic and basic type ion exchangers have an equi-
librium constant, which is changed by the concen-
tration of supporting electrolytes, and the inflec-
tion points of the potentiometric titration curve in
this case appear ambiguous.7–12
In this work, we studied a method for compu-
tation of the main characteristics of a phosphoric
cation exchanger by considering the effects of po-
tentiometric titration curves in an ion exchanger/
solution system. The acidity parameters of ion
exchangers, such as thermodynamic constant
(pK0), apparent equilibrium constant, and correc-
tion for the apparent equilibrium constant (b),
were used for expressing the characteristics of a
carboxylic ion exchanger. For proving the theory,
the phosphoric cation exchanger type was used
for an experiment on potentiometric titration and
potentiometric titration curves at different con-
centrations of the supporting electrolyte. From
these results, characteristic equations related to
the acidity parameters of ion exchanger systems
were obtained. Also, the characteristic parame-
ters such as solution pH, supporting electrolyte
concentration (C), and degree of neutralization of
ion exchanger (␹) were calculated.
EXPERIMENTAL
Materials
Phosphoric ion exchanger (PI-4) was prepared by
phosphorylation to a granular type of styrene co-
polymer and 4% divinylbenzene and then purified
by washing with HNO3 aqueous solution before
use. The ion exchange capacity of PI-4 was 5.70
meq/g and the swollen volume in water was 0.59
H2O/g. HCl and NaOH aqueous solutions (0.1 N)
were used as a standard solutions. Ba(OH)2 was
purchased form Aldrich Co. and used without fur-
ther purification. NaCl, BaCl2, buffer solution,
and other chemical reagents were reagent grade
and used without further purification.
Potentiometric Titration
PI-4 was transformed into the H-form by slow
treatment with 0.5 N HNO3 aqueous solution.
Subsequently, it was washed to show neutral pH
with distilled water. PI-4 (1 g) was added in 100
ml of 1 M NaCl aqueous solution with various
NaOH concentrations, and was allowed to stand
for 3 days at 20 ⫾ 1 °C. From the supernatant
liquid in a flask, 10 ml of solution was titrated
with 0.1 N HCl standard solution. In order to
investigate the effects of supporting electrolytes
of NaCl and BaCl2, the concentration of electro-
lytes was varied in the range of 1.0 ⵒ 1.0⫺3 M of
NaCl and BaCl2.
Determination of Ion Exchange Capacity
An error in determination of the ion exchange
capacity from the titration could be unreasonably
large if the titration conditions were not chosen
properly. We evaluated the precision of the deter-
mination by analysis of the potentiometric titra-
tion curves near the equivalent point. The preci-
sion depends on the number of experimental
points in this region, and to imitate conditions for
the real experiments we have chosen 10ⵒ12
points around the inflection point. The curves
were differentiated and the differential was fitted
to the Lorenzian distribution curve, which ap-
peared to be the best fit. Then, the parameters of
the maximum peak in ⭸pH/⭸g were found. The g
value of the maximum peak was equal to the ion
exchange capacity.
Theoretical Discussion
Calculation of the Acidity Function
When a cation exchanger in H-form is placed in
the contact with a solution of alkali M(OH)z, the
ion exchange H⫹-Mz⫹, followed by the neutraliza-
tion reaction, occurs. This can be expressed as:
1 Z⫹ 1
RH ⫹ M º H ⫹ ⫹ R zM z⫹ (1)
z z
The relative equilibrium constant is given as:
a៮ M
1/z
䡠 aH
k⫽ (2)
a៮ H 䡠 a M1/z
where a is the activity of the species in the sub-
script, z is the charge of counter-ion, and a៮ is the
activity in the ion exchanger. However, it is prac-
tically impossible to determine a៮ M and a៮ H. There-
fore, apparent equilibrium constant (K) was intro-
 CALCULATION ON ION EXCHANGE CAPACITY 3183

duced to determine k. The K can be calculated

冘 共i ⫺i!j兲!j! 䡠 y共i ⫺ j, j兲 䡠 共1 ⫺ ␹兲
j⫽i
from experimental data on the equilibrium from log K ⫽ 共i⫺j兲
䡠 ␹j
eq 3: j⫽0
(7)
C 䡠 aH
1/z
M fH
K⫽ 1/z ⫽ k 1/z (3) where i, j and y(i⫺j,j) are the Soldatov’s model
CH 䡠 aM fM
constants. Their physical meaning is given as fol-
lows: i is the maximum number of neighboring
where C is concentration, and f is the activity exchange groups in the microenvironment of any
coefficient for the related forms of ion exchanger. selected exchange group in the ion exchanger.
It is convenient to express the apparent equilib- The nearest neighbors are those groups that af-
rium coefficient via relative equivalent fractions fect the energy of interaction of counterion (Mz⫹)
of the counter ions in the phase of the ion ex- with a selected exchange group. The constant j is
changer, ␹: the number of neighboring exchange groups occu-
pied with counterion (Mz⫹); y(i ⫺ j,j) are con-
zC M stants. In an actual case, i is not higher than
␹⫽ (4) three and y(i ⫺ j,j) are constants with the same
zC M ⫹ C H
order of magnitude as the log K.
The pH of equilibrium solution in the potentio-
where values CM and CH are concentrations of the
metric titration curve of an ion exchanger de-
metal and hydrogen form of the ion exchanger,
pends on the concentration of the acids or the
dependant on the degree of neutralization. The K
base. The potentiometric titration curve of an ion
obtained from equations 3 and 4 is calculated as
exchanger does not imply that there are simple
follows:
physico-chemical characteristics, because the
curve depends on the solution volume in the sys-
␹ 1/z 䡠 a H ⫺1/z tem undergoing potentiometric titration. It is im-
K⫽ 1/z 䡠 z 䡠 共zC M ⫹ C H兲 共1/z⫺1兲 (5)
共1 ⫺ ␹ 兲 䡠 a M portant to foresee how the conditions for the po-
tentiometric titration of the ion exchangers will
After rearranging the logarithm of eq 5 we obtain influence the shape of the potentiometric titration
the following equation: curve, and also what the best conditions for titra-
tion and the different factors in determining
curve shape and position will be. Therefore, the
␹ 1/z 1 1
log ⫺ pH ⫺ log a M ⫺ log z potentiometric titration curves can be computed
共1 ⫺ ␹ 兲 z z with knowledge of the solution pH and ␹ using the

⫹ 冉 冊
1
z
⫺ 1 log共zC M ⫹ C H兲 ⫹ pK共 ␹ , C M兲 ⫽ 0 (6)
material balance condition to find the number of
the alkali equivalent (g) added to 1 g of the ion
exchanger with capacity E in a volume V.12,13 The
relationship between g and pH in the potentio-
where pK (␹, CM ) ⫽ ⫺log K(␹, CM ) and CM is the
metric titration curve is as follows:
concentration of the supporting electrolyte. This
equation relates to the most important properties
1
of our system: pH of the solution, degree of neu- g⫽ 共E ␹ ⫹ VC OH ⫺ VC H兲 (8)
tralization of the ion exchanger (i.e. the counte- z
rion sorption value), and the concentration of a
background electrolyte. Therefore, we refer to it The equations 6,7, and 8 can be used to express
as the function of acidity of ion exchangers. The the potentiometric titration curve of the ion ex-
acidity parameters can be used to describe all changer.
ionic equilibria in the system “ion exchanger-so-
lution” containing H⫹ and counter ions Mz⫹.
RESULTS AND DISCUSSION

Calculation of Apparent Equilibrium Constant (K) Potentiometric Titration Curve

An equation for X dependency of log K has been Figure 1 shows the theoretical and experimental
derived, using Soldatov’s model: 9 –11 data of the ␹ dependency of log K in 1 M of NaCl
3184 SON, KIM, AND KIM
Figure 1. A plot of log K versus ␹ at CNaCl ⫽ 1.0
mol/l. The data points were experimental data and
were fitted by different interpolation curves.
supporting electrolyte. The ␹ dependency of log K
for experimental data showed the S curve [Fig.
1(a)] of a third-order equation. For sufficient ac-
curacy, log K from eq 7 needs four parameters as
follows:
log K ⫽ y共3,0兲共1 ⫺ ␹ 兲 3 ⫹ 3y共2,1兲共1 ⫺ ␹ 兲 2␹
⫹ 3y共1,2兲共1 ⫺ ␹ 兲 ␹ 2 ⫹ y共0,3兲 ␹ 3 (9)
where the constants of y(3,0), y(2,1), y(1,2), and
y(0,3) were ⫺0.97, ⫺3.56, ⫺1.88, and ⫺4.14, re-
spectively, and their mean error was 0.08. It can
be rewritten as follows:
log K ⫽ ⫺0.97 ⫺ 7.78␹ ⫹ 12.80␹2 ⫺ 8.21␹3 (10)
The straight line [Fig. 1(b)] was obtained by the
first-order equation to minimize the parameters.
In order to obtain the straight line from eq 7,
there needs to be at least two parameters. This
can be written as follows:
log K ⫽ y共1,0兲共1 ⫺ ␹ 兲 ⫹ y共0,1兲 ␹ (11)
where the constants of y(1,0) and y(0,1) were
⫺1.29 and ⫺3.95, respectively, and their mean
error was 0.17. It can be rewritten as follows:
log K ⫽ ⫺1.29 ⫺ 2.66 ␹ (12)
These data were used to calculate the apparent
equilibrium constant (K). The pK values for ␹ can
be calculated from equations 10 and 12. Because
the concentration of the supporting electrolyte
(NaCl) was 1.0 M and the ion charge (z) is 1, eq 6
can be rewritten as follows:
␹
log ⫺ pH ⫺ log a M ⫹ pK共 ␹ , C M ⫽ 1.0兲 ⫽ 0
1⫺␹
(13)
where, because aM is the activity of counterion,
the CM practically coincides with the concentra-
tion of the supporting electrolyte. Therefore, the
concentration CM can replace activity aM in eq 13.
Eq 13 can thus be rewritten as follows:
␹
log ⫺ pH ⫺ log C M ⫹ pK共 ␹ , C M ⫽ 1.0兲 ⫽ 0
1⫺␹
(14)
␹
log ⫺ pH ⫹ pK共 ␹ , C M ⫽ 1.0兲 ⫽ 0 (15)
1⫺␹
The pH for a certain ␹ can be calculated from eq
15. In order to figure out the calculated potentio-
metric titration curve, the g values can be ob-
tained by using eq 8. Because ion charge (z) is 1,
eq 8 can be rewritten as follows:
g ⫽ E ␹ ⫹ V共10 pH⫺14 ⫺ 10 ⫺pH兲 (16)
Therefore, the g values for a certain pH can be
calculated from eq 16.
The theoretical potentiometric titration curves
fitted by using lines and the third-order equation
in Figure 1 were presented in comparison with
the experimental potentiometric titration curve
in Figure 2. The (a) and (b) curves in Figure 2
were obtained by using the theoretical equation
for the (a) and (b) lines in Figure 1, respectively.
As Figure 2 shows, it was found that the poten-
tiometric titration curves obtained from the third-
order equation are more coincident with the po-
tentiometric titration curves obtained from exper-
imental data, than those from the linear
equation. Even though the fit resulting from the
third-order equation showed a better result, the
expression using one parameter was adopted be-
cause of its sufficient accuracy and simplicity.
Using the third-order equation can certainly im-
prove the accuracy in describing the characteris-
tic behavior of ion exchangers, but it leads to more
 CALCULATION ON ION EXCHANGE CAPACITY 3185

Figure 2. Potentiometric titration curves computed Figure 3. A plot of pK versus ␹ for various concen-
from different approximations and experimental data. trations of NaCl.

complicated calculations, and requires more pa-

rameters and initial information for their deter-
mination. It was found that the ␹ dependency of
logK could be expressed with sufficient accuracy
by approximation of a straight line.
The pK value for the degree of neutralization
(␹) in the titration of phosphoric ion exchanger
PI-4 at various concentrations of NaCl and BaCl2
is presented in Figures 3 and 4. The plot of exper-
imental pK values versus ␹ in phosphoric cation
exchanger PI-4 can be expressed as linear eq 17.11
value for all concentrations. The correlation be-
tween ⌬pK and the degree of neutralization (␹) for
an ion exchanger can be expressed by the follow-
ing equation obtained from an empirical equa-
tion:13,14
pK共 ␹ , C ⫽ const.兲 ⫽ pK 0 ⫹ ⌬pK共 ␹ ⫺ 1/2兲 (18)

pK ⫽ pK ␹⫽0 ⫹ ⌬pK 䡠 ␹ (17)

The ⌬pK values were obtained from the slope

of the straight lines in Figure 3 and 4. The slopes
for various concentrations of NaCl and BaCl2 ap-
peared to be the same values, but their slopes
were not the same. In Table I, the pK values
obtained from experimental data at ␹ ⫽ 0.5 are
presented in comparison with the pK values cal-
culated from eq 17. The ⌬pK values increased as
the concentration of NaCl electrolytes increased,
but in the case of BaCl2 electrolytes, there was no
particular trend in the ⌬pK values, which were
smaller than those of the NaCl electrolytes. Be-
cause the differences of the ⌬pK values at various
concentrations of supporting electrolytes were not
large, the ⌬pK value in the titration of NaOH and
Ba(OH)2 (which was 1.968 and 1.805, respec- Figure 4. A plot of pK versus ␹ for various concen-
tively) was replaced by an intermediate ⌬pK trations of BaCl2.
3186 SON, KIM, AND KIM

Table I. Constants of Eq 17 for Various pK ⫽ 2.740 ⫺ 0.05 log C Cl ⫹ 1.805共 ␹ ⫺ 21 兲 (24)

Concentrations

Electrolytes C (mol/l) ⌬pK pK ex pK in The experimental pK values for various ␹ were

presented in comparison with the potentiometric
NaCl 0.002 1.78 2.98 3.07 titration curves obtained from equations 23 and
0.025 1.73 2.91 3.93 24 in Figure 6 and 7, respectively. As shown in
0.1 2.25 2.81 2.93 Figures 6 and 7, there is good agreement between
1.0 2.11 2.72 2.72 the calculated curves and the potentiometric ti-
BaCl2 0.002 1.75 2.78 2.71 tration points. When the ion exchanger PI-4 was
0.025 1.82 2.81 2.66
titrated with NaOH and Ba(OH)2, the character-
0.1 1.90 2.71 2.63
istic parameters (pK0,⌬pK, and b) were pKNa 0
1.0 1.75 2.58 2.58
⫽ 2.72, ⌬pKNa ⫽ 1.97, and bNa ⫽ 0.13 in the case
pK ex : experimental pK value at ␹ ⫽ 0.5. of NaOH and pKBa 0
⫽ 2.58, ⌬pKBa ⫽ 1.81, and bBa
pK in : interpolation pK value of Eq 17 at ␹ ⫽ 0.5. ⫽ 0.047 in the case of Ba(OH)2.
Figure 8 shows the potentiometric titration
curves that resulted when the ion exchanger PI-4
where the pK0 is the thermodynamic equilibrium was titrated with NaOH and Ba(OH)2 in 0.002 M
constant in the ion exchange between a H⫹ ion of NaCl and BaCl2.When the ionic charge (z) in-
functional groups and a counterion Mz⫹. The pK creased from one to two, ⭸pH/⭸g increased more
can be expressed as follows: sharply near the inflection point.

pK 0 ⫽ 冕
0
1
pKdx (19)
Determination of Ion Exchange Capacity
The ion exchange capacity can be obtained only by
potentiometric titration as a position of the inflec-
This linear approximation is equal to the arith- tion point. The inflection point of the potentiomet-
metic average and can be rewritten as follows: ric titration curve for an ion exchanger is changed
by the concentration of supporting electrolytes,
1 the volume of equilibrium solution, and the
pK 0 ⫽ 2 共pK ␹⫽1 ⫹ pK ␹⫽0兲 ⫽ pK ␹⫽1/2 (20)
charge of titration ions. An error in determination
of the ion exchange capacity from the titration
The change of pK for the various concentrations of
NaCl and BaCl2 at specific ␹ is shown in Figure 5.
The CM dependency of pK can be expressed by the
following eq:

pK共 ␹ ⫽ const., C M兲 ⫽ pK 0 ⫺ b log C M (21)

The constant b in eq 21 is the correction value of

pK for various concentrations of NaCl and BaCl2,
and can be obtained from the slope of the linear
equation. The pK values, as a function of the
degree of neutralization (␹) and the concentration
of NaCl and BaCl2 (from equations 18 and 21) can
be rewritten as follows:

pK共 ␹ , C M兲 ⫽ pK 0 ⫹ ⌬pK共 ␹ ⫺ 12 兲 ⫺ b log C M (22)

Therefore, when the ion exchanger PI-4 is titrated

with NaOH and Ba(OH)2, the pK values for the
degree of neutralization (␹) can be given as fol-
lows:
Figure 5. A plot of pK versus log C for different
pK ⫽ 3.090 ⫺ 0.13 log C Cl ⫹ 1.968共 ␹ ⫺ 21 兲 (23) titration media.

Figure 6. Potentiometric titration curves for phos-
phoric acid ion exchanger PI-4 in various concentra-
tions of NaCl. The data points were experimental data.
can be unreasonably large if the titration condi-
tions are not chosen properly. In order to deter-
mine an accurate ion exchange capacity, the data
around the inflection point were fitted to the
Lorenz distribution curve. The error in determi-
nation of abscissa of the maximum in ⭸pH/⭸g is
equal to the error in determination of the ex-
Figure 7. Potentiometric titration curves for phos-
phoric acid ion exchanger PI-4 in various concentra-
tions of BaCl2. The data points were experimental data.
CALCULATION ON ION EXCHANGE CAPACITY 3187
Figure 8. Potentiometric titration curves for phos-
phoric acid ion exchanger PI-4 in 0.002 M solutions of
NaCl and BaCl2.
change capacity in absence of experimental er-
rors. As the ratio of the maximum height to its
width at half height was increased, the error in
determination of ion exchange capacity was de-
creased.
The data around the inflection point obtained
from the potentiometric titration curve in Figure 8
Figure 9. Curve fittings of a plot of ⭸pH/⭸g versus g
by Lorenzian distribution for NaCl and BaCl2 solutions
(0.002 M).
3188 SON, KIM, AND KIM
Table II. Parameters of Lorenzian Equation [⭸pH/
⭸g ⫽ f( g)]
Backgrounds g max ⌬g H E ⫺ g max H/⌬g
NaCl 5.690 0.28 17.67 0.01 63.11
BaCl2 5.696 0.14 51.57 0.004 369.64
pK: equilibrium constant, g max: g value of maximum peak.
⌬g: the width at half ⭸pH/⭸g value of peak.
H: ⭸pH/⭸g value of peak, E: true capacity (5.7 meq/g).
were presented by Lorenz distribution curves in
Figure 9. The g value for maximum ⭸pH/⭸g was
equal to the inflection point of the potentiometric
titration curve and the ion exchange capacity of ion
exchanger PI-4. The inflection point of the potentio-
metric titration curve is observed clearly with in-
creasing ⭸pH/⭸g. The parameters calculated from
the Lorenz distribution curve are shown in Table II.
The ratio of the maximum height of ⭸pH/⭸g to
the width at half height for BaCl2 is larger than
that of NaCl. The ion exchange capacity of NaCl
and BaCl2 can be evaluated accurately within
⫾ 0.01 and ⫾ 0.004 meq/g, respectively. From
these results, we know that the error range of
NaCl was larger than that of BaCl2, and the ion
exchange capacity is determined accurately in the
case of titration with a divalent counterion.
CONCLUSIONS
This experiment calculated the characteristics of
a phosphoric cation exchanger and studied an
accurately computable method for ion exchange
capacity for a type of potentiometric titration
curve. The conclusions obtained from these exper-
iments are as follows: The ⌬pK values were ob-
tained from the slope of a linear equation. The
experimental pK values at ␹ ⫽ 0.5 showed good
agreement with the theoretical data. Also, when
the supernatant liquid from cation-exchanged
solution was titrated with NaOH and Ba(OH)2
solutions, a good agreement between experimen-
tal and theoretical pK values for various ␹ was
found in all the potentiometric titration curves.
The data points of the potentiometric titration
curve in the case of divalent ions were changed
more sharply than those for monovalent ions. The
plot of ⭸pH/⭸g versus g was fitted to the Loren-
zian distribution curve, from which ion exchange
capacity was evaluated accurately.
This work was supported by the Korea Science and
Engineering Foundation through the Advanced Mate-
rials Research Center for Better Environment at Tae-
jeon National University of Technology.
NOMENCLATURE
a Activity
b Correction for the apparent constant shift
with changing supporting electrolyte
C Concentration of supporting electrolyte
(mol/l)
f Activity coefficient
i, j Constant
g Number of moles of alkali to 1 g of ion
exchanger
E Exchange capacity (meq/g)
k Equilibrium constant
K Apparent equilibrium constant
pK0 Thermodynamic constant of ion exchanger
⌬pK Difference of the apparent equilibrium
constant at complete and zero neutral-
ization of the ion exchanger
V Solution volume, ml/g of ion exchanger
␹ Equivalent fraction
z Ion charge
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