Journal of Hazardous Materials 166 (2009) 13621366

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Journal of Hazardous Materials

journal homepage: www.elsevier.com/locate/jhazmat

Treatment of cyanide efuents by oxidation and adsorption in batch

and column studies
E.Y. Yazc, H. Deveci , I . Alp
Mineral Processing Division, Department of Mining Engineering, Karadeniz Technical University, 61080 Trabzon, Turkey

a r t i c l e

i n f o

Article history:
Received 23 September 2008
Received in revised form 5 November 2008
Accepted 9 December 2008
Available online 14 December 2008
Keywords:
Cyanide removal
Air oxidation
Adsorption
Activated carbon
Environment

a b s t r a c t
In this study the removal of free cyanide from aqueous solutions by air oxidation and adsorption was
investigated. Effects of air and pure oxygen, and catalyst on the rate and extent of the removal of cyanide
were studied. It was found that the oxidative removal of cyanide by air/oxygen was very limited although
it tended to improve in the presence of pure oxygen and catalyst such as activated carbon (AC) and copper
sulphate. In the presence of continuous aeration, the non-oxidative removal of cyanide was correlated
with a decrease in pH effected apparently by the transfer of carbon dioxide from air phase into the medium.
The removal of cyanide by adsorption on activated carbon, nut shell (NS) and rice husk (RH) was also examined. Adsorption capacity of activated carbon was shown to be signicantly enhanced via impregnation
of activated carbons with metals such as copper (ACCu) and silver (ACAg). In the column tests, the
breakthrough capacity of adsorbents was found to be in an increasing order of RH < AC < ACCu ACAg.
2008 Elsevier B.V. All rights reserved.

1. Introduction
Cyanide has been the most preferred solvent in the extraction
of gold and silver ores over a century due to its strong complexing
capability, ready availability, relatively low cost and its well-known
chemistry [1,2]. Cyanide is also most extensively used in metal nishing and production of plastics [35]. Wastewaters generated
in these operations often contain cyanide species i.e. free and
metalcyanides and cyanide related compounds at various levels [57]. Regarding the toxicity of cyanide species with the free
cyanide being the most toxic, treatment of cyanide containing efuents is prerequisite to lower cyanide content to admissible levels to
fulll environmental regulations.
Natural attenuation, chemical and biological oxidation, complexing/precipitation and recovery/recycling processes are currently exploited to remediate the efuents containing cyanide
[816]. Natural attenuation is a slow process and closely controlled by climate conditions [1,11,1719]. Oxidative treatment
methods e.g. ozonation, hydrogen peroxide and SO2 /air are effectively used for the removal of weak acid dissociable (WAD) cyanide
compounds (pK < 30) [11,20,21]. Advanced oxidation processes e.g.
photochemical oxidation, ultrasonic waves for the treatment of
cyanide efuents has been also studied by some researchers [22,23].
However, these are expensive and not effective for the treatment of
strong acid dissociable (SAD) cyanides (pK > 30). Activated carbon

Corresponding author. Tel.: +90 462 377 3681; fax: +90 462 325 7405.
E-mail address: hdeveci@ktu.edu.tr (H. Deveci).
0304-3894/$ see front matter 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.jhazmat.2008.12.050

and various agricultural products can be used as adsorbent for the

removal of cyanide [1,2427] from efuents. Although its adsorptive properties were exploited in most studies, activated carbon
can act as an oxidation catalyst in the presence of oxygen [28,29].
The aeration can signicantly improve the adsorptive properties of
activated carbon probably linked with the oxidation of chromeneand/or quinone-type functional groups and, thus, the generation
of positively charged active sites for further adsorption [2730].
However, the contribution of aeration to the adsorptive removal of
cyanide has not been considered in most studies.
In this study the removal of cyanide from aqueous solutions
by catalytic air oxidation and adsorption was investigated. Effect
of solution pH and catalyst such as copper and activated carbon
in the presence of air/oxygen on the rate and extent of cyanide
removal were examined. Removal of cyanide using plain and metalimpregnated activated carbons and agricultural by-products i.e. rice
husk and nut shell was also studied through batch and column tests.
The importance of aeration for the adsorptive removal of cyanide
by these adsorbents was demonstrated.

2. Experimental
2.1. Reagents and adsorbents
Reagent grade sodium cyanide (NaCN), copper chloride
(CuCl2 2H2 O), copper sulphate (CuSO4 5H2 O), silver nitrate
(AgNO3 ), sodium hydroxide (NaOH) and hydrogen peroxide (H2 O2 ,
35%, w/w) were used to prepare stock solutions in distilled water.

E.Y. Yazc et al. / Journal of Hazardous Materials 166 (2009) 13621366

1363

present in solution; albeit, the recovery of cyanide associated with

copper is not complete [1]. pH was controlled by the addition of 1 M
NaOH, if required.
3. Results and discussion
3.1. Removal of cyanide by air oxidation

Fig. 1. Experimental setup for air oxidation ([CN ]0 : 100 mg/l and [CuSO4 ]0 :
020 mg/l in OR).

2.2. Air oxidation studies

Air oxidation tests were performed in a closed system consisting
of two glass reactors i.e. oxidation and absorption reactors (Fig. 1).
The oxidation reactor (OR, 1 l) contained cyanide waste solution
(100 mg/l CN , 800 ml) and NaOH solution (400 ml) was used in the
absorption reactor (AR) to entrap HCN gas formed in the oxidation
reactor. Air was supplied using a sparger to oxidation reactor at a
ow rate of 0.27 l/min. Effect of pH control, the use of pure oxygen
and the catalytic effect of activated carbon (1020 g/l) and copper
sulphate (20 mg/l) on the oxidative removal of cyanide was also
determined.
A separate experiment was also designed to conrm the generation of H2 O2 by activated carbon in the presence of air. A known
amount of activated carbon (10%, w/vol.) was added into distilled
water and air (0.27 l/min) was blown into the solution. The concentration of hydrogen peroxide was determined using a lter
photometer at 520 nm.

No signicant change in cyanide concentration in oxidation

reactor was observed over an initial period of 22 h as shown in
Fig. 2. However, cyanide level in solution decreased to 76 mg/l
between 22 and 46 h apparently in coincidence with the corresponding decrease in pH (Fig. 3). Following this period, a further
substantial reduction in cyanide level (from 76 to 3 mg/l) was also
consistent with the further decrease in pH (Fig. 3) and with the accumulation of cyanide in absorption reactor over the same period. This
change in cyanide level depending on pH was strongly related with
volatilisation of cyanide as HCN (g) due to the acidifying effect of
atmospheric carbon dioxide in air:
H2 O + CO2 (g) H2 CO3 HCO3 + H+

(1)

H+ + CN HCN(g)

(2)

Fig. 4 represents the Eh pH diagram of the aqueous cyanide system (a) and the pH-dependent fractionation of HCN and CN (b)
[1]. Cyanide exists essentially in the form of HCN at pHs below
9.3 (pKa ) under non-oxidising conditions. The level of free cyanide
(CN ) in equilibrium with HCN decreases further with increasing
acidity. These theoretical calculations conrm the substantial loss

2.3. Adsorption studies

Coconut shell activated carbon (4 + 1 mm, BET: 546 m2 /g)
as plain (AC) and impregnated with copper (ACCu) and silver
(ACAg), hazel nut shell (4 + 1 mm) with/without heat treatment (for 15 min at 300 C) and rice husk (2 + 1 mm) were used
in adsorption tests. Copper and silver impregnation of activated
carbons were conducted in CuCl2 (1 g/l) and AgNO3 (110 g/l) solutions, respectively over a period of 72 h. Activated carbons with a
nal metal content of 5.07% Ag and 0.43% Cu by weight were used
in the experiments. Details of the preparation of these adsorbents
for experiments can be found elsewhere [30].
The adsorption tests were carried out in Pyrex beakers (600 ml)
with an initial cyanide concentration of 100 mg/l (300 ml) at an
adsorbent dosage of 1 g/l. Magnetic stirrers were used to agitate
the reactor contents. Column tests were performed in PTFE columns
with an inside diameter (I.D.) of 26 mm (145 mm in length) at an
adsorbent charge of 5 g. Fresh cyanide solution (100 mg/l CN ; pH
11) was fed from the top of the column at a ow rate of 1.5 ml/min.
Samples were taken from the efuent solution at certain intervals
to construct the breakthrough curve.
Concentration of cyanide in solution was determined by
silver nitrate titration in the presence of p-dimethylaminobenzylrhodanine (0.02%, w/w in acetone) as indicator [31]. Though
the titration method used is suitable for the determination of free
cyanide, some species of WAD cyanide e.g. Zn(CN)4 2 and copper
cyanide complexes (Cu(CN)n 1n ), can also be detected, if they are

Fig. 2. Effect of aeration (0.27 l/min) on the removal of cyanide ([CN ]0 : 100 mg/l in
oxidation reactor (OR)).

Fig. 3. Evolution of pH in oxidation (OR) and absorption reactors (AR).

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E.Y. Yazc et al. / Journal of Hazardous Materials 166 (2009) 13621366

Fig. 4. (a) Eh pH diagram for the free cyanidewater system at 25 C ([CN ] = 103 M) and (b) pH-dependent fractionation of HCN and CN at 25 C ([CN ] = 103 M).

dissolved oxygen were also monitored and found to be around 6 and

11 mg/l for the tests performed with air (Fig. 5) and pure oxygen
(Fig. 6), respectively. These also reveal the relationship between
higher cyanide removal and oxygen content in the medium.
3.2. Catalytic effect of activated carbon on cyanide removal

Fig. 5. Effect of copper as catalyst on the oxidative removal of cyanide in the presence
of aeration (0.27 l/min) ([CN ]0 : 100 mg/l and [CuSO4 ]0 : 20 mg/l in oxidation reactor
(OR)).

of cyanide in the form of HCN (g) observed with a decrease in pH

(Figs. 2 and 3).
In natural attenuation process, loss of cyanide by volatilisation
was proposed to be the most important contributing to 90% of
cyanide removal [4,32]. This can be related with the ready volatilisation of HCN (g) due to its high vapor pressure and low boiling
point compared with water [33,34]. Consistent with the literature,
current ndings (Figs. 2 and 3) apparently showed that volatilisation of cyanide as HCN is the most signicant mechanism on the
rate and extent of cyanide removal.
Fig. 5 illustrates the cyanide removal (19%) in the presence of
aeration and copper at pH 11 over 72 h. More extensive (by 3.4- to
4.3-fold over 45 h) removal of cyanide was observed in the presence
of pure oxygen with/without copper (Fig. 6). The concentration of

Fig. 6. Removal of cyanide in the presence of pure oxygen (0.27 l/min) ([CN ]0 :
100 mg/l and [CuSO4 ]0 : 20 mg/l, pH 11).

Fig. 7 illustrates that aeration exerted a signicant effect on the

catalytic removal of free cyanide in the presence of AC (10 g/l) i.e.
44% CN removal (with aeration) compared with 12% (no aeration).
The increase in AC dosage from 10 to 20 g/l led to an improvement
in cyanide removal (Fig. 7). Addition of copper sulphate (10 mg/l)
and hydrogen peroxide (10 mg/l) was found to produce a negligible
effect on the cyanide removal (Fig. 7).
Activated carbon is known to act as a catalyst in the presence
of air since it promotes chemical reactions such as oxidation of
cyanide (Eqs. (3)(5)) [29,35,36]. The generation of H2 O2 (0.17 mg/l
over 0.5 h at pH 10.511) in the presence of air was conrmed in
a separate experiment. This suggests that a portion of CN could
have been catalytically oxidized by activated carbon (Eqs. (4) and
(5)) in the current tests. It is mooted that cyanide is rst adsorbed
on the surface of activated carbon, and then catalytically oxidized
[1,28]:
Act. Carbon

CN + 0.5O2 (aq)

CNO

Act. Carbon

2H2 O + O2 + 2e

H2 O2 + 2OH

Act. Carbon

2CN + H2 O2 + 2OH

2H2 O + CNO

(3)
(4)
(5)

Alicilar et al. [3739] also studied the air oxidation of cyanide

in xed bed reactors packed with solid catalysts i.e. delrin and/or

Fig. 7. Removal of cyanide from solutions via catalyst assisted air oxidation
(0.27 l/min) over a period of 10 h (activated carbon dosage: 1020 g/l, [CN ]0 :
100 mg/l, [CuSO4 ]0 : 10 mg/l, [H2 O2 ]0 : 10 mg/l, and pH 10.511).

E.Y. Yazc et al. / Journal of Hazardous Materials 166 (2009) 13621366

1365

Table 1
Adsorption parameters of Thomas and Yoon-Nelson models for the removal of cyanide by plain (AC), copper- (ACCu) and silver-impregnated (ACAg) activated carbons and
rice husk (RH) ([CN ]0 : 100 mg/l and pH 11).
Adsorbent

ACAg
ACCu
AC
RH

qexp (mg/g)

16.426
6.032
3.516
0.401

Thomas

Yoon-Nelson

q0 (mg/g)

kT (104 l/(min mg))

R2

kYN (102 l/min)

 (min)

R2

18.094
6.389
2.568
1.957

0.65
1.59
2.58
19.99

0.9739
0.9748
0.9367
0.9784

0.65
1.59
2.58
19.98

603.122
212.969
85.596
65.225

0.9739
0.9748
0.9367
0.9784

V2 O5 , under co- or counter-current ow conditions. The authors

[37] reported that both delrin and V2 O5 were effective as catalysts
since over 95% of cyanide was removed under the conditions of both
co- and counter-current ows.
3.3. Adsorption of cyanide by activated carbon and agricultural
by-products in batch and column studies
Fig. 8 illustrates that activated carbon was more effective than
agricultural by-products for the removal of cyanide and impregnation of activated carbon with metals remarkably enhances the
extent of cyanide removal in the absence/presence of aeration. Aeration appeared to induce a profound effect on the extent of cyanide
removal for all type of adsorbents used in this study i.e. 3.2- to 25.6fold higher than that in the absence of air, in consistent with current
ndings (Fig. 8). This enhancement in the extent of cyanide removal
could be attributed to the catalytic activity of these adsorbents
and/or the air oxidation of cyanide [27]. The oxidation of surface
functional groups (i.e. chromene- and/or quinone-type functional
groups on carbon material such as activated carbon) in the presence of air could lead to the formation of positively active sites on
the adsorbents and to the increase in their adsorption capacity for
negatively charged ions such as cyanide [27,29].
Breakthrough curves produced in the column tests for the most
effective adsorbents (AC, ACCu and ACAg) are shown in Fig. 9.
The data for RH was also included for comparison with AC-based
adsorbents. Consistent with the earlier ndings (Fig. 8) metalimpregnated activated carbons had greater capacities than plain
activated carbon (and RH) with ACAg having the highest breakthrough capacity (500 ml, 50-bed volume). Adhoum and Monser
[26] also reported that the silver impregnation improved by 3.7-fold
the breakthrough capacity of activated carbon for CN adsorption.
Thomas (Eq. (6)) and Yoon-Nelson (Eq. (7)) models are widely
used to describe breakthrough curves for the removal of inorganic
and organic constituents [40,41]. In the current study, these mod-

Fig. 9. Breakthrough curves for cyanide adsorption by plain (AC), copper- (ACCu)
and silver-impregnated (ACAg) activated carbons and rice husk (RH) ([CN ]0 :
100 mg/l and pH 11).

els were used to describe breakthrough curves for the adsorption

of cyanide by plain (AC), copper- (ACCu) and silver-impregnated
(ACAg) activated carbons and rice husk (RH).
Ce
1
=
Co
1 + exp[kT (q0 m Co V )/]

(6)

Ce
1
=
Co
1 + exp[kYN ( (V/))]

(7)

where Ce (mg/l) and Co (mg/l) are the cyanide concentration of

efuent and initial solution, respectively; V (l) and  (l/min) are the
efuent volume and volumetric ow rate, respectively; q0 (mg/g)
and m (g) are the maximum capacity and mass of adsorbent, respectively; kT (l/(min mg)) and kYN (l/min) are the rate constant for
Thomas and Yoon-Nelson model, respectively;  (min) is the time
required for 50% cyanide breakthrough [40].
The parameters of Thomas (kT and q0 ) and Yoon-Nelson (kYN and
) models were determined using non-linear regression (Table 1).
Experimental capacities (qexp ) of the adsorbents were also presented to compare with the calculated capacities (q0 ) using Thomas
model. Both models were seemed to be consistent with the data as
indicated by high correlation coefcients (Table 1). It is also pertinent to note that these experimental capacities in the column
studies are lower than those previously determined values in equilibrium studies (e.g. 16.43 mg/g in column studies c.f. 29.6 mg/g in
the equilibrium studies of ACAg [27]). This can be attributed to
the increased contact time and probably to the positive effect of
aeration of the cyanide solution in the latter. In this regard, the performance of these adsorbents in the columns could be improved via
the aeration of cyanide solutions prior to the feeding to the column.
4. Conclusions

Fig. 8. Removal of cyanide by plain (AC), copper- (ACCu) and silver-impregnated

(ACAg) activated carbons, rice husk (RH), nut shell (NS) and activated nut shell
(ANS) over 10 h in the absence/presence of air (adsorbent dosage: 1 g/l, [CN ]0 :
100 mg/l, and pH 10.511).

This study has shown that non-oxidative removal of cyanide

induced by the decrease in pH is the leading mechanism in the
presence of aeration since the oxidation of cyanide by air is rather
limited. Oxidative removal of cyanide can be improved by supplying pure oxygen into the solution in the absence/presence of copper.

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E.Y. Yazc et al. / Journal of Hazardous Materials 166 (2009) 13621366

Furthermore, activated carbon was found to catalyse the oxidative

removal of cyanide in the presence of air. The catalytic effect of
the activated carbon appeared to be derived from the generation
of the strong oxidant, H2 O2 , in the presence of air resulting in the
enhanced oxidation of cyanide.
Adsorption studies have also shown that activated carbon and
agricultural by-products have relatively low capacity for cyanide
removal. However, adsorption capacity of activated carbons was
shown to be signicantly enhanced via impregnation with metals, silver (ACAg), in particular. Column studies have indicated
that ACAg has the highest breakthrough capacity (500 ml, 50bed volume) compared with plain activated carbon and agricultural
by-products. Breakthrough curves for plain and metal-impregnated
activated carbons and rice husk can be described by both Thomas
and Yoon-Nelson models.
Acknowledgements
The authors would like to express their sincere thanks and
appreciation to the Research Foundation of Karadeniz Technical
University for the nancial support (Project No. 2002.112.8.3), to
Erol Ylmaz (University of Quebec in Abitibi-Temiscamingue) and
Dr. Celal Duran (KTU) for their technical support and to the Newmont Mining Co. (Ovacik Gold Mine, Turkey) for kindly providing
the activated carbon samples.
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