War. Res. Voi. 27, No. II, pp. 1663-1668,1993 0043-1354/93 $6.00+0.

00
Printed in Great Britain. All fightsreserved Copyright© 1993PergamonPress Ltd

BICARBONATE-TREATED PEANUT HULL CARBON

FOR MERCURY (II) REMOVAL FROM
AQUEOUS SOLUTION
C. NAMASIVAYAM* and K. PERIASAMY
Environmental Chemistry Division,Department of Environmental Sciences,BharathiarUniversity,
Coimbatore-641 046, Tamil Nadu, India

(First received May 1992; accepted in revised form March 1993)

AImtrKt--Activated carbon prepared from bicarbonate-treated peanut hulls (BPHC) has been used for
the adsorption of Hg(II) over a range of initial metal ion concentrations (10-20 mg dm-3), agitation time
(5-180 rain), adsorbent dosage (5-120rag 100mi-I) and pH (1.5-10.0). Adsorption of Hg(II) increased
with increase in its initial concentration from 10 to 20 mg dm-3 and the equilibrium time of adsorption
increased from 75 to 90 rain for a BPHC dose of 100mg 100m1-1. The process of uptake obeys both the
Frenndlich and Langmulr isotherms. The applicability of the Lagergren kinetic model has also been
investigated. Quantitative removalof 20 mg dm-3 Hg0I) in I00 ml by 70 mg adsorbent was observed over
a pH range of 3.5-10.0. A comparativestudy with a commercialgranular activated carbon (CAC) showed
that BPHC is 7 times more effective compared to CAC.

Key words--bicarbonate-treated peanut hull carbon, Hg(II) adsorption, adsorption isotherms, adsorption
kinetics, pH effect

~rrnoDucnoN capacity of the powdered activated carbon (PAC),

Filtrasorb-300, to remove 90% of inorganic mercury
Mercury is one of the most toxic pollutants (10mgdm -3) was nearly 10 times higher at pH 4.0
introduced into natural waters mainly from the dis-
than at pH 10.0. Considerable reduction in the
charges of the chlorine manufacturing industry, concentration of inorganic mercury was obtained
Paper and pulp, oil refining, plastic and battery when the conventional coagulation treatment was
manufacturing industries also contribute to mercury combined with activated carbon (Logsdon and
pollution. The tolerance limit for Hg(II) for discbarge Symons, 1973; Ebersole and O'Connor, 1978).
into inland surface waters is 10/tgdm -3 (ISI, 1981) Mercury(II) sorption by waste rubber in the pH
and for&inking water, 1/~gdm -2 (ISI, 1991). Mer- range 5.5-6.0 has been reported by Knocke and
cury causes damage of the central nervous system and Hemphill (1981). Ma et al. (1992) found that the
chromosomes, impairment of pulmonary function
uptake of Hg(II) (10~gdm -3) by a commercial
and kidney, chest pain and dyspnoea (Berglund and
GAC increased from 70 to >90% when 5 mgdm -3
Berlin, 1969; WHO, 1991). The harmful effects of
humic acid or 5 mg dm -3 nitrilotriacetic acid (NTA)
methylymercury include the contamination of fish in
were added.
Minamata Bay (WHO, 1990). Logsdon and Symons Many reports have appeared on the development
(1973) observed that 80% of inorganic and organic of activated carbon from cheaper and readily avail-
mercury could be removed using granular activated
able materials (Hassler, 1974). Activated carbon
carbon (GAC). Maruyama et al. (1975) conducted a
derived from rice husk (Srinivasan et al., 1988) and
pilot plant test for the removal of 0.5 mg dm -3 of
coconut shell (Arulanantham et al., 1989) has been
Hg(II) from wastewater using a high lime process successfully employed for the removal of heavy
that consists of flash mixing, flocculation and GAC
metals from aqueous solutions. We recently found
filtration and reported a removal efficiency of
that 240 mg of activated ground nut (peanut) shell
70%. Theim and O'Connor (1977) evaluated several
carbon removed 80% Cr(VI) from a 100 ml aqueous
varieties of activated carbon samples derived from
solution of 10 mg dm -3 at pH 2.0 (Periasamy et al.,
lignite for the removal of inorganic and organic 1991).Waiss et al. (1973) reported that 0.5 g peanut
Hg(II) at 0.01 mg dm -3 from simulated drinking hull removed 22% Hg(II) from a 50 ml solution of
water and showed that at a 100mgdm -3 dosage of 0.1M Hg(OAc)2 at an equilibrium time of 24h in
carbon nearly 50% of both inorganic and organic batch mode studies. Azab and Peterson (1989) used
mercury were removed in the pH range 7.0-9.0. 20g peanut hull for the removal of 100mgdm -3
Humenick and Schnoor (1974) reported that the Cd(II) at pH 5.2 from a 1-1itre solution in column
studies and showed a removal efficiency of 68 and
*Author to whom all correspondenceshould be addressed. 99% by untreated and alkaline-treated peanut hull,

1663
1664 C. NAMASlVAYAM and K.

respectively. A t present the peanut hull, a waste Table 1. Characteristics of the carbons
agricultural product, is utilized in India as fuel and Sl. No. Characteristics BPHC CAC
manure. The investigation reported here deals with 1 Bulk density (g ml-~) 0.63 0.60
a comparative study o f B P H C and a C A C for the 2 Moisture(%) 14.14 6.79
3 Ash (%) 2.11 3.84
removal o f Hg(II) from aqueous solutions. 4 Solubilityin water (%) 0.74 t.42
5 Solubilityin 0.25 M HCI (%) 2.25 1.56
6 pH 6.68 8.18
EXPERIMENTAL 7 Decolorizingpower (mg g- I) 36.00 77.00
8 Phenolnumber 68.00 20.00
Preparation of BPHC 9 Ion exchange capacity (m equiv g J) 0.49 NIL
BPHC was prepared by treating one part of peanut hulls 10 Surfacea r e a ( m 2 g - ] ) 208.1 354.6
with 1.8 parts by weight of concentrated sulphuric acid 11 Iron (%) 0.27 1.43
and keeping it in an air oven at 150 + 5 °C for 24 h. The BPHC= bicarbonate-treated peanut hull carbon.
carbonized material was washed with distilled water to CAC =commercial activated carbon.
remove the free acid and dried at 105-t-5 °C, The dried
material was ground and sieved to 0.575 mm size (20-50
mesh ASTM). The carbonized material was repeatedly decolorizing power and lower phenol number which
soaked in 1% sodium bicarbonate until effervescence ceased imply that it is more suitable for organic adsorption.
and finally soaked in 1% sodium bicarbonate solution Unlike C A C , B P H C has a moderate ion exchange
overnight to remove any residual acid. The material was capacity,
then washed with distilled water, dried at 105 + 5 °C and
again sieved to 0.575 mm size. Preliminary studies with the Effect of agitation time and initial concentration
peanut hull carbon before and after bicarbonate treatment
showed a removal efficiency of 88 and 100% H8(II), respect- Figure 1 shows the effect o f agitation time on the
ively. Hence subsequent experiments were carried out with removal o f Hg(II) by B P H C and CAC. The removal
the BPHC. The CAC, obtained from M/s-Burbidges corn- increases with time and attains equilibrium in 75, 90
pany, Bombay, India was ground and sieved to a 0.575 mm
size. The characteristics of BPHC and CAC are summarized and 90 min for B P H C and 120, 150 and 180 rain for
in Table 1. C A C for initial Hg(II) concentrations of 10, 15 and
20 mg dm -3, respectively. This indicates that B P H C
Batch mode studies would require less residence time for the complete
A stock solution of Hg(II) was prepared by dissolving removal of Hg(II) compared to CAC.
0.3385 g of HgCI2 in 100 ml distilled water containing 0.1 ml
concentrated hydrochloric acid and diluting to 250 ml. This Effect of carbon dose
solution was diluted as required to obtain standard sol-
utions containing 10-20 mg dm -3 Hg(II). One hundred ml Figure 2 shows the removal of Hg(II) as a function
of Hg0I) solution of a desired concentration adjusted to a o f carbon dosage by B P H C and C A C . It is evident
desired pH were taken in reagent bottles of 300 ml capacity, that for the quantitative removal of 20 mg dm-3
known amounts of BPHC or CAC were added and pH was
adjusted using dilute hydrochloric acid (0.01, 0.1 or 1.0 M) Hg(II) in 100 ml, a minimum carbon dosage o f 70 mg
or dilute sodium hydroxide (0.01, 0.1 or 1.0 M) solutions.
All the chemicals used were of Analar grade and were
obtained from Ranbaxy, BDH and Merck. The solutions 20 --
were agitated for a predetermined period at 30 + I °C in a ~-~
reciprocating shaker. The carbons were separated by 7 18
filtration and the filtrate was analysed by
a spectrophotometric procedure for Hg(II) content ~ 16
(Ramakrishna et al., 1976). Adsorption isotherm studies -a 14
were carried out with different initial concentrations of
Hg(lI) while maintaining the carbon dosage at constant o: 12
level. For pH effects, 20 mg dm -3 Hg(II) and a BPHC dose .a
of 100mg 100ml -I or a C A C d o s e o f 5 0 0 m g 100ml -I were ~ 10
used. In order to correct for any adsorption of Hg(II) due ~,
to the containers, control experiments were carried out ~ 8
without adsorbent. It was found that there was no adsorp-
tion by the container walls. In addition, all mixing vessels ~ 6
were kept sealed throughout the duration of each isotherm
test to minimize mercury loss to the atmosphere. ~ 4 -- o_o_o_a_o-o-o-o-o-o-o-o-o-o-o-o
e[~l--l--pl--m--1--i--n--g~,-~l--l--l--i--I--I
~ ..t;.=--
v r -
RESULTS AND DISCUSSION
0 I I l ] I I I I I
Examination o f carbon characteristics (Table 1) 0 20 40 60 80 ]00 120 ]40 ]60 180
shows that both the carbons possess similar bulk B P H C - Time (min)
densities. Moisture content o f B P H C is higher than I I I I I I I I I r
that o f C A C , which suggests that the acid treatment 0 60 120 180 240 300 360 420 480 540
has made the B P H C more porous; however, no C A C - Time (min)
attempts were m a d e in this study to determine the
Fig. 1. Effect of agitation time on the adsorption of
porosity o f B P H C and CAC. In comparison to Hg(II) on BPHC and CAC. BPHC: O, 20mgdm-3;
BPHC, C A C has a higher ash content which indi- [], 15mgdm-3; A, 10mgdm-3; CAC: O, 20mgdm-3;
cates less carbon content. Also, C A C shows higher II, 15 mgdm-3; A, 10 mgdm -3.
 Adsorption of mercury by carbon 1665

(A) BPHC o BPHC

2.0 -- ~ - - ~ Carbon dose : 85 mg 100 m1-1
pH : 4.0
1.6 Agitation time : 3.0 h
A CAC
1.2
Carbon dose : 700 mg 100 ml -!
0.8 mg dm -3 pH : 4.0
Agitation time : 3.0 h Agitation time : 7.0 h
0.4 0.25 - - 2.0
pH : 4.0
I I I I t I I I ~ 0.20 ~ - 1.6~,
0 20 40 60 80 100 120 140 160
o t~,~ 0.15 / - 1.2 "m
•~ CAC ,~ ,~
(B) ~ 0.10 - 0.8
~o 0.05 0.4
,,./ 2.0
1.6 ~ d
o --"1 I I I I I o
1.2 0 4 8 12 16 20 24
o C e ( m g d m -3)
0.8 m -3
< Agitation time : 7.0 h Fig. 3. Langmuir plot for the adsorption of Hg(II) on BPHC
0.4 pH : 4.0 and CAC.
I I I I I I I I
0 200 400 600 800 1000 1200 1400 1600 explain the observed phenomena. T h e F r e u n d l i c h
D o s a g e of carbon ( m g 100 ml - t ) isotherm is represented by the equation (McKay
Fig. 2. Effect of carbon dose on the adsorption of Hg(II). et al., 1982):
(A) BPHC; (B) CAC. log(x/m) = log K + (1/n) log Ce (2)

of BPHC or 500 mg of CAC is required. The data where Cc is the equilibrium concentration (rag dm-3)
clearly show that the BPHC is 7 times more effective and x/m is the m o u n t adsorbed per unit weight
than CAC for the removal of Hg(II). This may be due of BPHC or CAC (mg g - i). Plots of log (x/m) vs
to the higher porosity and the moderate ion exchange log C, are linear for both BPHC and CAC (Fig. 4).
capacity of BPHC compared to CAC. The constants K and n were found to be 42.17 and
3.50, respectively, for BPHC and 4.68 and 3.16,
Adsorption isotherms respectively, for CAC. Values of 1 < n < 10 show
The Langmuir equation was applied for adsorption favourable adsorption of Hg(II) on both BPHC and
equilibrium for both BPHC and CAC: CAC (McKay et al., 1982). Similar results have been
observed in the adsorption of Hg(II) on bicarbonate
Cdq~ = 1/(Qob)+ CdQo (1) treated rice husk carbon (Srinivasan, 1986), where
where C, is the equilibrium concentration (mg dm-3), the K and n values were found to be 15.84 and 2.00,
qc the amount adsorbed at equilibrium (mg g-i) and
Q0 and b the Langmuir constants related to adsorp- o BPHC
tion capacity and energy of adsorption, respectively. Carbon dose : 85 mg 100 ml -I
The linear plots of Cdq¢ vs C, show that the adsorp- pn : 4.o
tion obeys the Langmuir model for both BPHC Agitation time : 3.0 h
and CAC (Fig. 3). Q0 and b were determined from ~ CAC
the Langmuir plots and found to be 109.89 mg g-m Carbon dose : 700 mg 100 m1-1
and 0.364dm 3 mg -~, respectively, for BPHC; and pH :4.0
12.38 mg g-i and 0.505 dm 3 mg -t, respectively, for Agitation time : 7.0 h
CAC. The ratio of Q0 values of BPHC and CAC 2.2 ~ - - 1.2
works out to be 8.88. 2.1 - ~ - 1.0
The essential characteristics of the Langmuir
isotherm can be expressed in terms of a dimensionless ~[~ 2.0 7 / ' ~ f ~ 7 - 0.8 8[E
constant separation factor or equilibrium parameter, o~ 1.9 ~ I I - 0.6
RL, which is defined by R L ~- 1/(1 + bCo) where b is ,a ,~
the Langmuir constant and Co is the initial concen- Lg - 0.4
tration of Hg(II) (McKay et al., 1982). R L values 1.7 - 0.2
indicate favourable adsorption of Hg(II) on both
BPHC and CAC at the concentrations studied at 1.6 0
30--+ 1 °C. 0 0.2 0.4 0.6 0.8 1.0 1.2 1.4
The Freundlich model was also used because the Log C e
Langmuir model alone is unable to satisfactorily Fig. 4. Freundlich adsorption isotherm.
1666 C. NAMASlVAYAM and K. PEm~AMY

respectively. The correlation coefficients for the linear 10.0 I-

regression fits ofthe Langmuir plots were found to be ~ o 20 mg dm-3
0.9956 and 0.9949 for BPHC and CAC, respectively. A 15 mg dm -3
The corresponding values for the Freundlich plots Q lO mg dm-3
were 0.9940 and 0.9898. ~ 1.o ~ pH: 4.0

Adsorption kinetics
The kinetics of Hg(II) adsorption on both BPHC Y"
and CAC follow the first-order rate expression given ~ 0.1
by Lagergren (Singh et al., 1989).

log(qe - q) = log q= - K~dt/2.303 (3) 0.01 J I

where q is the amount of Hg(II) adsorbed (mg g-m)
at time t, q= is the amount adsorbed (rag g-~) at
equilibrium time and K~ is the rate constant of
adsorption. Linear plots of log ( q , - q) vs t show
the applicability of the above equation for both
BPHC and CAC (Figs 5 and 6). The K~d values from
the slopes of the plots for BPHC are 6.09 x 10 -2,
4.39x 10 -2 and 5.43 x 10-2min -I for the initial
Hg(II) concentrations of 20, 15 and 1 0 m g d m -3,
respectively; the corresponding values for CAC are
1.94 x 10-2, 1.92 x 10 -2 and 3.76 x 10-2min -I. The
rate constant for intraparticle transport, K~, was
calculated using the equation of Weber and Morris
(1963):
q effective within a narrow range of pH 3.5-4.5. It can
/~ -- t-~ (4)
where q is the amount of Hg(II) (rag g - l ) adsorbed
at time t. The Kd values calculated from the plots
of q vs t ~/2 (Fig. 7) were found to be 0.35, 0.76 and
0.50mg g-i min-i/, for BPHC and 0.08, 0.03 and
0.05 mg g-I rain-l/2 for CAC for the initial Hg(II)
concentration values of 20, 15 and 1 0 m g d m -3,
respectively. The linear plots do not pass through the
origin for either BPHC or CAC. It appears that pore
5o
10o 15o 200
Time (rain)
Fig. 6. Lagergren plots for the adsorption of Hg(II)
on CAC.
diffusion is not the only rate controlling step in the
removal of Hg(II) for both the carbons (Singh et al.,
1989).
Effects o f p H
Figure 8 presents the effects of initial pH on the
removal of Hg(II) by BPHC and CAC. It is clear that
BPHC is effective for the quantitative removal of
Hg(II) over the pH range 3.5-10.0. CAC, however, is
be shown by stability constant calculations that in the
presence of C I - , the predominant species at pH > 4.0
is Hg(OH)2 and at pH < 4.0 is HgCI2 (Knocke and
Hemphill, 1981). The formation of HgCI2 has been
found to decrease the Hg(II) sorption onto a com-
mercial FS-400 GAC (Ma et ai., 1992). Accordingly,
the Hg(II) adsorption decreased when the pH was
lowered from 4.0 to 2.0 with hydrochloric acid for
(A) BPHC

100 I o 20 mg dm-3 16
15 mg dm-3 12
[] 10 mg dm-3 8 mg dm-3
10 ~. pH: 4.0
4 A 15 mg dm-3
~. h : ~ . ~ o n 10 mg dm-3
7 ~ .'-" I ) I I I I I I I
i 0 2 4 6 8 10 12 14 16 18
"-" 1.0 ~ B) CAC

3
0.1 - o =

1 -- A 15 m g d m -3
n 10[ mg[dm-3
o.ot I I I I I I l ,I ) I I
0 20 40 60 80 100 0 2 4 6 8 10 12 14 16 18
Time (min) tl/2 ( m i n ) l / 2
Fig. 5. Lagergren plots for the adsorption of Hg(II) Fig. 7. Plots for intraparticle diffusion for the adsorption of
on BPHC. Hg(II). (A) BPHC; (B) CAC.
 Adsorption of morcury by carbon
A BPHC
Carbon d o s e : 100 mg 100 m1-1
[Hg (II)] 20 mg dm-3
Agitation time : 3.0 h
- o CAC
'~
Carbon dose : 500 mg 100 ml-I
.~ [Hg (1I)] 20 mg dm-3
.~ Agitation time : 7.0 b
O O
.~ 20 A.~.~-~-g~-fr-A -- 4.5
~, 12 3.5 ,%
~ T.V. (1989). Coconut shell carbon for treatment of
8 3.0 ~
"~ 4 -- 2.5 ~
o ~
<E [ [ [ [ [ 2.0 <
0 2 4 6 8 10
pH
Fig. 8. Effect of pH on adsorption of Hg(II).
both BPHC and CAC. In the case of CAC, an
increase in pH above 4.0 shows a decreasing trend in
adsorption probably because of the formation of
soluble hydroxy complexes of mercury, Hg(OH)2
(aq). This is in agreement with the studies by
Humenick and Schnoor (1974) and Ma et al. (1992)
on the effect of pH on mercury sorption by activated
carbons FS-300 and FS-400, respectively. On the
contrary, increase of pH above 4.0 shows no change
in the uptake of Hg(II) by BPHC. These results imply
that a third process may be involved, namely, reten-
tion of the Hg(OH)2 species in the micropores of the
BHPC particles. Chemisorption and/or precipitation
of a new phase may be the dominant process with
surface complex dissociation equilibria,
DESORPTION STUDIES
Desorption studies help elucidate the nature of
adsorption and help to recover the metals from
wastewaters and the adsorbent. Attempts were made
to desorb the Hg(II) from the carbon surface using
hydrochloric acid and potassium iodide of various
strengths. For BPHC, the optimum % recoveries of
Hg(II) were: 47 with 0.6 M hydrochloric acid and 87
with 1.0% potassium iodide. In the case of CAC, the
corresponding values were: 12.6 and 23.6. Higher
desorption of Hg(II) by I - is due to the formation
of relatively more stable iodide complexes compared
to the chloride complexes (Cotton and Wilkinson,
1972).
CONCLUSION
The preliminary studies presented here show
that peanut hull carbon is an effective adsorbent for
the removal and recovery of Hg(II) from aqueous
solutions. Its capacity is much superior to the com-
mercial activated carbon. It would be useful for the
1667
economic treatment of wastewater containing Hg(II)
as the carbon is easily prepared from this agricultural
waste product.
'~ Acknowledgements--One of the authors (K.F.) is grateful
~ to Dr M. Shanmugam, Principal, Institute of Road and
~,~ Transport Technology, Erode, Tamil Nadu, for providing
"~ facilities
and encouragement. The authors are grateful to the
.~ referees for their useful comments and suggestions.
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