Wat. Res. Vol. 30, No. 10, pp.

2309-2314, 1996

Pergamon
PII: S0043-1354(96)00119-4

Copyright 1996 ElsevierScienceLtd

Printed in Great Britain.All rights reserved
0043-1354/96 $15.00+ 0.00

OPTIMISATION OF A PURIFICATION METHOD

FOR METAL-CONTAINING WASTEWATER
BY USE OF A TAGUCHI EXPERIMENTAL DESIGN
E. BARRADO*, M. VEGA, R. P A R D O n , P. G R A N D E and J. L. DEL VALLE
Department of Analytical Chemistry, Faculty of Sciences, University of Valladolid,
E-47005 VaUadolid, Spain
(First received August 1994; accepted in revised form April 1996)

Abstract--A procedure for purifying waters polluted with metal ions has been designed. The method is
based on the precipitation of metals as magnetic ferrite from the alkalinised solution containing iron(II).
The working conditions were optimised by using a Taguchi L9(34)experimental design in order to minimise
the total resiidual concentration (TRC) of metal ions in solution. A statistical analysis of the experimental
data revealed the most influential factor to be the Fe(II)/metal concentration ratio (F), with a 29.5%
contribution, followed by pH (P, 5.2%) and time (H, 2.3%). On the other hand, temperature (T) had
little effect on the purification efficiency (1.0%), whereas noise (N, KMnO4) was found to contribute by
as much as 22.1%. Maximal purification efficiency (99.99%) is achieved when wastewater samples are
treated for 21h at 50C and pH 10 in the presence of iron(II) in a ratio Fe(II)/total metal of 15. In these
conditions, the process efficiencyis also the least influenced by variabilityin the sample composition, which
validates the proposed procedure. Copyright 1996 Elsevier Science Ltd
Key words---toxic metals, wastewater, decontamination, ferrite, optimisation, Taguchi parameter design

INTRODUCTION

The need to purify wastewater containing metal ions

arises from their toxicity and non-biodegradable
nature, which may pose serious problems on building
up at various stases during the eeobiological cycle
(Patterson and Pa,;sino, 1987; Ferguson, 1990).
Among the procedures used for this purpose,
those based on surface adsorption and precipitation
of various solids are worth special note. Thus,
Benjamin and Leckie (1981), Benjamin et al. (1982)
and Benjamin (1983) have studied adsorption by
iron oxides and metal-surface interactions involved
in the process. Also, Gadde and Laitinen (1974)
and Macchi et al. (1993) investigated more specific
processes such as the adsorption of lead from
industrial acidic batteries on iron(II) oxides in
alkaline medium, and Chen et al. (1991) assayed the
recovery of metal ions by adsorption on magnetic
iron oxides and their subsequent recycling by desorption with a view to their application by metal
refinining and electroplating industries.
Adsorption/desorption processes on hydrated iron
oxides have also been paid some attention, particularly as regards kinetic aspects and their utility
for purifying heavy metals (Theis et al., 1988;
Stollenwerk et al., 1985; Schultz et al., 1987;

*Author to whom all correspondence should be addressed.

Terashima et al., 1986; Edwards and Benjamin,

1989).
A very promising method for toxic metal removal
from wastewaters consists of the precipitation of
cations from an alkaline aqueous solution containing
ferrous ions. The magnetic ferrite precipitates are
formed by oxidising the solution by air or an
oxidising reagent at a temperature above 50C.
Using this procedure, a variety of heavy metals
can be simultaneously and effectively removed from
waste water. Katsura et al. (1977, 1979), Katsura and
Terada (1979), Ito et al. (1981) and Tamaura et al.
(1991a, b) amongst other authors, have studied the
adsorption of a variety of metals on a ferrite during
its formation under specific experimental conditions,
as well as potential mechanisms for metal incorporation into the ferrite structure. The main advantages
of this method are: (i) the formed ferrite sludge can
be readily separated from the clean solution by
m a g i . ic filtration and (ii) the solids obtained can be
reused, thus avoiding disposal and dispersal of heavy
metals in the environment.
These procedures, however, are in principle rather
costly for implementation on a large scale, so they
require optimisation in order to ensure an efficient
metal removal. For this reason, in this work we have
employed the Taguchi method to optimise the purification procedure by obtaining ferrites as described
by Tamaura et al. (1991a, b). The main thrust of
Taguchi methods is the use of a parameter design

2309

2310

E. Barrado et al.

which possesses the ability to design a p r o d u c t or

process to be robust against uncontrollable environmental changes, n a m e d noise factors (Ross, 1988;
Taguchi, 1991; Bendell et al., 1989). Optimisation o f
the process implies the use o f a strategically designed
experiment which deliberately introduces changes in
order to: (i) identify factors affecting the procedure,
(ii) estimate the factor levels yielding a n o p t i m u m
response a n d (iii) the most i m p o r t a n t , to decrease the
process variability without controlling or eliminating
causes o f variation.
MATERIALS AND METHODS
Apparatus and chemicals

The basic aim of this work was to purify wastewater from

training and research laboratories. Accordingly, the sample
chosen for the experiments was a mixture consisting of
various metal ions typically employed in analytical
chemistry laboratory exercises. The synthetic wastewater
sample contained the following 14 ions at a concentration
of 1000ppm except for AI(III), which was included at
500ppm: V(V), Cd(II), Co(II), Fe(II), Pb(II), Sb(III),
AI(III), Hg(II), Sn(II), Cr(III), Bi(III), Ni(II), Zn(II) and
Cu(II) and was prepared by dissolving adequate amounts of
the respective nitrate salt, except Sn(II) and Sb(III) which
were added as chloride salts and V(V) as sodium vanadate.
Iron(II) sulphate and sodium hydroxide (Panreac, reagent
grade) were added to aliquots of synthetic wastewater to
remove heavy metals by precipitation as magnetic ferrites.
Potassium permanganate (Panreac) was added to solutions
at different concentration levels to simulate the variability of
samples and simultaneously to ease the oxidation of iron(II).
The experimental set-up used for sample treatment
consisted of a 50 ml trunk-conical dual-wall reaction cell
connected to a Tamson TC-3 thermostat with adjustable
temperatures in the range 10-300C. A Crison micro-

Notation
F
T
H
P
N

pH 2002 pH meter furnished with a combined glass

electrode and a Ptl00 temperature probe was used for pH
measurement. Air was bubbled through the solutions by
means of an Auxten Capex MKI l air-dispensing pump to
promote the oxidation of Fe(II) ions to Fe(II1). A Metrohm
RNG 11 stirrer was used throughout the experiment to
ensure a homogeneous solution.
Metal ions in solution were determined on a sequential
Philips PU 7000-1CP Spectrometer.
Procedure

The purification procedure was optimised by applying a

Taguchi experimental design. Before the wastewater aliquot
was placed in the cell, the selected thermostat temperature
was set. After reaching such a temperature, 15 ml of
sample were transferred to the cell and diluted to 40 ml by
addition of distilled water. Then, the amounts of potassium
permanganate (noise factor) and ferrous sulphate needed to
adjust the level of each factor to that indicated in the
respective trial (see Tables 1 and 2) were added. After the
cell was closed, the electric stirrer, temperature probe,
pH electrode and air-feeding glass tube were connected,
and the pH adjusted to the selected value by addition
of concentrated sodium hydroxide. Both the pH and the
liquid volume in the cell were kept at their original values
throughout the purification process by addition of distilled
water and/or sodium hydroxide.
After the treatment interval had elapsed, the liquid was
separated from the solid ferrite by filtration through a
porous glass filter, diluted to 250 ml and its metallic content
analysed by ICP Spectrometry. On the other hand, the
resulting ferrites were desiccated at 100C for 1 h, puiverised
in an agate mortar and stored in glass vials for subsequent
studies.
RESULTS AND DISCUSSION
T h e steps for implementing the Taguchi experimental design are: (1) to select the o u t p u t variable to

Table 1. Factors and levels for the optimisation experiment

Factor
Level I
Level 2
[Fe(I1)]/[total metal in solution] ratio
2
7
Temperature (C)
25
50
Ageing time (h)
I
2
pH
8
l0
KMnO4 concentration (mol/I)
3.75 x l0 -3
3.75 x l0 -2

Level 3
15
75
3
12
7.50 x 10-2

Table 2. Experimental L9(34)orthogonal array with a three-levelnoise factor. Total remanent metal
concentration (TRC, in rag/l) has been determined
Control factors and levels
TRC (rag/l)
Trial
T
P
F
H
N~
N2
N3
S/N ratio
1

2.24
0.59
1.75
5.07
5.32
0.65
0,37
0.32
7.20
0,49
39,17
27.05
0.57
1,26

5.29
1.75
1.05
0.41
0.40
1.07
0.34
0.68
0.48
0.44
46.54
25.77
0.61
0.70

155.04
166.27
0.38
0.48
0.51
0.36
4.31
0.65
0.80
0.88
138.08
165.61
0.91
1.42

3.88
7.85
15.42
25.52

22.74
36.33
35.27
48.61

92.80
120.33
67.56
72.73

- 39.35
- 7.05
- 7.05
- 5.19
- 9.54
- 39.34
0.28

- 36.20
- 33.79

Purification of metal-containing wastewater

be optimised, (2) to identify factors and their interactions affecting the output variable and to choose
the levels to be tested, (3) to select the adequate
orthogonal array, (4) to assign factors and interactions to the colunms of the array, (5) to perform the
experiments, (6) to carry out a statistical analysis of
the data and the signal-to-noise ratio and determine
the optimum factor levels and (7) to conduct a
confirmatory experiment.
Total residual metal concentration (TRC) was
selected as the pa~rameter to be optimised as it is
directly related to tlae purification efficiency achieved.
TRC was calculated as the sum of the concentration
(in mg/l) of all metals (including Mn and Fe) in
solution after performing the purification process:

TRC = E ~"~'i

This parameter h,ts to be minimised in order to

ensure an optimum metal removal by ferrite sludge
formation.
The efficiency of the purification procedure and the
characteristics of the ferrites formed depend on
controllable experimental conditions such as pH,
ratio of Fe(II) concentration to total metal concentration in solution, ageing time and temperature
(noted P, F, H and T, respectively), pH is expected to
influence very strongly the precipitation of metal as
ferrite since in alkaline media the surface of iron
oxides is negatively charged and therefore can adsorb
cations (Benjamin, 1983; Tamaura et al., 1991a) and
besides, metal oxides can co-precipitate at alkaline
pH values (Smith and Martell, 1976). These phenomena improve with increasing pH, and also with
increasing adsorbent concentration. Therefore, high
levels of iron(II) we:re selected in order to obtain large
amounts of precipitated iron hydroxides. Ageing time
is also known to improve the adsorbent characteristics of the ferrite (Benjamin et al., 1982; Schultz
et al., 1987) and the stability of the precipitates by
enhancing their co~gulation. Increasing temperature
negatively affects the adsorptive properties of iron
oxide particles but improves the co-precipitation
phenomena, therefare its overall effect should be
evaluated for each particular situation.
Three levels for each control factor were chosen
(see Table 1) to detect any quadratic or non-linear
relation between the factors and the output variable,
and to obtain information over wider ranges of the
variables.
Changes in the solution composition will possibly
affect the effectiveness of the wastewater purification
process and the ch~.racteristics of the ferrite formed.
Because the composition of wastewater from
chemistry laboratories may vary over wide concentration ranges, the variability should be simulated in
some way as it can substantially alter the composition
of the unknown solution. Potassium permanganate
(noted henceforth N) was thought to be a suitable

2311

noise factor since is widely used in Practicals of

Chemistry and modifies the chemistry of the elements
and their oxidation states, thus simulating different
levels of redox properties of laboratory effluents. On
the other hand, potassium permanganate also
oxidises Fe(II) ions to Fe(III), then speeding up the
oxidation and formation of ferrite precipitates. Three
levels were selected for the noise factor ranging from
the lower to the higher potassium permanganate
concentration expected in wastewaters discharged in
typical laboratories.
Table 1 shows control and noise factors and their
selected levels. Four control factors at three levels
contain eight degrees of freedom, and can be fitted
to the L9(34) orthogonal array which provides the
greatest amount of information from the minimum
number of experiments. The design matrix used is
shown in Table 2. The nine different trials resulting
from this design were run at three noise levels
(Nj, N2 and N3) and duplicated in order to calculate
the residual error, so a total number of 54 purified
solutions were analysed by ICP to determine the
corresponding TRC (in ppm) as described above.
Experimental results of the 54 solutions are listed in
Table 2.
Statistical analysis

Because the selected Taguchi design L9(34) is

orthogonal, it was possible to resolve the effect
of each individual factor on the response and
control factor-noise factor interactions (enabling
optimisation of the process response), and on the
signal-to-noise ratio (which allows reduction of the
variability of the process, making it robust against
environmental variations).
Table 3 exhibits the results of the analysis of
variance (ANOVA) with pooled errors performed on
the experimental data. From the calculated variance
ratios F it can be inferred that all factors and interactions considered in the experimental design are
statistically significant effects at a 95% confidence
limit (in all cases calculated F is greater than the
critical value), then indicating that the variability of
experimental data must be explained in terms of
significant effects. The most influential factor is the
Fe/metal concentration ratio, which explains 29.5%
of the overall variance of the experimental data,
followed by pH (5.2%). Ageing time and temperature
have a minor effect (2.3% and 1.0% of the TRC
variation, respectively), whereas noise is highly
influential (22.1%). With regards to factor interactions, that between F and N was particularly
outstanding (33.0%), which can readily be understood taking into account that KMnO4 reacts with
Fe(II) increasing the amount of ferrite formed and in
consequence the removal of metals. The contribution
of the residual error to the TRC variability (2.6%)
indicates the goodness of the experimental design
used. As a rule, if such a contribution is smaller than
10-15%, the variance of the experimental data can be

E. Barrado

2312

et al.

Table 3. Pooled ANOVA table for the regular analysis

Variation source

Degrees of
freedom

Sum of
squares

Variance ratio~
(F)

2
2
2
2
2
4
4
4
4
27
53

1179
5744
32,156
2630
24,048
807
1608
36,024
2820
1418
108,434

11.2
54.7
306.1
25.0
228.9
3.8
7.7
171.5
13.4

T, Temperature
P, pH
F, Fe(ll)/metal ratio
H, Ageing time
N, Noise
Tx N
P x N
F x N
H x N
Residual
Total

Pooled sum
of squares

Pool
No
No
No
No
No
No
No
No
No
Yes

Contribution b
(%)

1074
5639
32,051
2525
23,943
597
1398
35,814
2610
2783
108,434

1.0
5.2
29.5
2.3
22.1
0.6
1.3
33.0
2.4
2.6
100.0

'Critical variance ratio for a 95*/, confidence level is 3.35 (2 d.f.) or 2.73 (4 d.f.).
bContribution is defined as 100 x (pooled sum of squares/total sum of squares).

said to be explained by the effect of factors and

interactions. In consequence, it can be asserted that
the experimental design used in this work took into
account all the variables affecting the response to
be optimised, and the levels tested were fit for the
purpose.
Figure IA shows the effects of control factor levels
on the output variable. TRC decreases strongly with
increasing F as the amount of metals adsorbedcoprecipitated on larger amounts of iron oxides also
increases. TRC also decreases slightly with increasing
H due to the enhancement produced on the
adsorptive properties of ferrite with time. An increase
of T level resulted in a weak diminution of the
purification efficiency (higher TRC) since adsorption
decreases with temperature, then demonstrating that
the ferrite formation method is not only a metal
precipitation process, but a combination of adsorption and co-precipitation mechanisms; level Tm led
to the best response. Finally, an increase of P from
pH 10 to 12 produced a slight increase in TRC since
some metal oxides can dissolve by formation
6O

0
I-

..f

20"

",,,

i:oo
.

TI 1"2 1"3 P1 P2 P3 I=1 [=2 F3 H1 H2 H3

F:

Factor ievel

Fig. 1. (A) Effects o f c o n t r o l factors T (temperature), P (pH),

F ( F e ( I I ) / t o t a l m e t a l c o n c e n t r a t i o n ratio) a n d H (ageing

time) on the mean response. (B) Effect of interactions control factor x noise factor on the mean response: (O) N3,
( x ) N2, (~) N, (C) Effects of control factors on the
signal-to-noise ratio.

of soluble hydroxylated complexes at high pH

values.
In order to verify if the differences between factor
levels are statistically significant, and to determine
those yielding a more pronounced effect on the
response, the Duncan test (Ross, 1988) was applied.
Significant differences were found (at a 95%
confidence level) between the three levels for factors
F, T and H, and also between levels P2 and P3, but
not between Pm and /'2 or P3, which were thus
equivalent.
Figure 1B exhibits the interactions between control
factors F, T, H and P and the noise factor N. In
all cases, level N3 yielded the poorer purification
efficiency whatever level of control factors, since
residual manganese in solution was also included in
the calculation of TRC. The only important interaction was F x N (see Table 3) and it can be observed
that level F3 leads to the same TRC value whatever
noise level chosen, which indicates that the purification procedure is insensitive to experimental noise
when the F3 level is used.
The statistical analysis thus revealed that the
F3-Pz--H3 combination is the most suitable for the
intended purpose, and any T,, /'2 or /'3 level would
be valid as they only introduce slight changes.
Taguchi employs the concept of the signal-tonoise (S/N) ratio to evaluate the variation of the
response around the mean value due to experimental
noise, and to obtain an optimum response with
smaller variations, which makes a method robust
against environmental variability. As the optimised
parameter TRC is a lower-is-better response, the
equation employed for SIN ratio calculation was
(Ross, 1988):

S/N

lOlog ~

y~

where N is the number of repetitions in each of the

nine trials (N = 6) and y, are the six experimental
values obtained for each trial. The calculated values
are listed in Table 2.
A pooled A N O V A of the S/N ratio values
(Table 4) revealed factor F to be the only significant

Purification of metal-containing wastewater

2313

Table 4. Pooled ANOVA table for the signal-to-noiseanalysis

Degrees of
Sum of
VarianceratioI Pooledsum
Variation source
freedom
squares
(F)
of squares
T, Temperature
2
57
P, pH
2
235
4.1
178
F, Fe(II)/Metatratio
2
1705
29.9
1649
H, Ageingtime
2
279
4.9
223
Residual
2
57
226
Total
8
2276
2276
'Critical varianceratio for a 95% confidencelevelis 19.00.
bContributionis definedas I00 (pooledsum of squares/total sum of squares).

Contributionb
(%)
7.8
72.5
9.8
9.9
100.0

factor responsible: for the variability in the SIR

ratio (72.5% contribution on the total variance),
whereas H (9.8%) and P (7.8%) do not have a
significant effect (calculated variance ratio < critical
value). Figure IC shows the effect that control
factors have on tbe average S / N ratio: the higher
S / N ratio was obtained for levels T~ or /'2, P~,
F3 and //2 or H3. The level of the only significant
factor ( F ) producing a more pronounced effect on
the S / N ratio was obtained by again applying the
Duncan test (Ross, 1988) and it was not found to
show significant differences between levels F2 and
F3, but these levels produced a higher S / N ratio
than F~.
In conclusion, statistical analysis of both raw data
and the S / N ratio showed that the combination of
parameter levels yielding a minimum TRC (maximum process efficiency), independent of uncontrollable variation of noise, was T2 (50C), P2 (pH 10), F3
(Fe(II)/total metal ratio of 15) a n d / / 3 (ageing time,
3 h). Temperature and ageing time, however, are
not too influential on the purification efficiency, but
the reproducibility of the results will increase with
increasing treatment time and decrease with increasing temperature in the event of a high variability in
the initial conditions.
It must be mentioned that the ferrite compounds
obtained in these conditions also had a markedly
magnetic character (Barrado et al., 1994).

character of ferrite compounds improve with

increasing temperature.
The alkaline medium is essential to achieve
quantitative precipitation of metals with intermediate
acidic character (Co(II), Ni(II), Cu(II), M n ( I V ) . . . ) ,
though too high pH values (pH > 10) cause very
acidic metal cations such as AI(III), Cr(III), Sn(IV) or
Zn(II) to form soluble hydroxy complexes thus
increasing the TCR. Optimum metal removal was
achieved for pH 10 (intermediate level tested).
Ageing time improves the physical properties of
precipitates, then enhancing both metal adsorption
and occlusion. In consequence, the higher level tested
resulted in the optimum purification process.

Chemical interpretation

Acknowledgements--Authors wish to thank the C.I.C.Y.T.

(proposal AMB 94-0938) and the Vicerrectorado de
Investigaci6n of the University of Valladolid for the
financial support provided for realisation of this work.

Fe(II)/total metal concentration ratio F is the

fundamental effect which can be readily understood,
taking into account that Fe(II) is precursor of
magnetic Fe304 precipitates; the amount of metals
collected on Fe(III) oxide by a dual adsorptionco-precipitation me,chanism increases with increasing
mass of oxide, whe~eas Fe(II) oxide is responsible for
the magnetic properties of the resulting ferrite. Both
metal recovery and magnetic characteristics (Barrado
et al., 1994) were optimal when the higher level F3 was
used.
Temperature combines two antagonistic effects:
increasing temperature improves the coagulation and
stabilisation of ferrite, and decreases the adsorptive
characteristics of iron oxides. This last effect is likely
to be dominant as the optimal TRC was obtained
for the lower T level (25C). Nevertheless, 50C
was selected because both stability and magnetic

Application of the optimised procedure

As can be verified in Table 2, the optimum
combination of factor levels T2-P~F3-H3 was not
previously tested, so in order to check their reliability
a series of checking experiments was carried out
by using the initial solution and the different noise
levels, as well as solutions from student laboratories.
The purification efficiency was found to be 99.99%
in every instance, which validates the proposed
conditions.
The optimised method is being successfully applied
to the purification of metal-containing wastewater
discharged by chemistry laboratories from the
University of Valladolid.

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