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Fuel Processing Technology 128 (2014) 111118

Contents lists available at ScienceDirect

Fuel Processing Technology


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

Optimization of the coal otation procedure using the PlackettBurman


design methodology and kinetic analysis
Dariuh Azizi, Mahdi Gharabaghi , Negar Saeedi
School of Mining Engineering, College of Engineering, University of Tehran, Iran

a r t i c l e

i n f o

Article history:
Received 17 July 2012
Received in revised form 23 June 2014
Accepted 24 June 2014
Available online 26 July 2014
Keywords:
Coal otation
Experimental design
Kinetic analysis
Optimization
PlackettBurman methodology

a b s t r a c t
In this paper, the otation method has been used for the preparation and beneciation of coal samples.
The PlackettBurman methodology has been applied to design of experiments and this experimental design
method is based on Hadamard matrix and ash content and efciency index have been considered as responses.
The operating conditions were chosen based on some screening tests. Results showed that ash content and efciency index could be 15.2% and 42.55 respectively when the values of collector, frother and solid percent were
5.29 kg/t, 78 g/t and 10% respectively. The effects of variables were studied by which increasing and decreasing of
responses could be transparently observed. Coal otation kinetic was studied and the results show that the
optimum time is 2 min to complete the otation process. In this investigation, the coal otation procedure was
optimized and the time of otation has been found by which energy consumption would be signicantly
reduced. Also, coal qualities could be improved by which needs of industry can be considerably satised.
2014 Elsevier B.V. All rights reserved.

1. Introduction
Coals are heterogeneous mixtures. The hydrophobicity of the former
depends upon the type of material [1] and the rank [2]. Microscopically,
coal has a crosslink network structure of polymeric molecules [3] and
macroscopically, it is made up of nely mixed discrete organic entities
known as macerals [4]. Coals are often highly variable even when
from the same source. So each time a bulk sample is received, a
complete set of experiments is conducted using the classical method
of treating one variable at a time. Coals are used for coke making in
steel industry around the world. Ash has high adverse effects on the
productivity and coke consumption in blast furnace. An increase in the
ash content of a coal concentrate by 1% over a critical limit results in
an increase in coke consumption by about 45% as well as decreasing
blast furnace productivity by about 36%; therefore there is always a
pressure on coal preparation plants to supply coal with very low ash
[5]. Because of this problem, it is necessary to nd some methods to decrease ash content of coal. Flotation as a mineral processing method is
used to produce low ash coal in some industrial plants. Flotation is
one of the most complex mineral processing operations as it is affected
by a very large number of variables. Many of these are beyond the control of the mineral engineer and some cannot be even measured
quantitatively with the available instruments. The relations between
measured and controlled variables are intricately related. Sometimes,
simultaneously changing various component settings will reinforce a

particular attribute. In addition, various component settings can cancel


or counteract each other if changes are not chosen wisely. For coal
nes (b 0.5 mm), froth otation is the most effective method of
separating ash forming mineral matter from the coals [6].
Many investigations about coal otation have been done through
which various methods and chemical materials have been introduced
to perform the otation procedure. Some investigations showed that if
otation is carried out with salt solutions, its performance could be
dramatically improved [712]. The seam-to-steam strategy offers an
entirely different solution for handling of ne coal [13] and the reverse
otation process had also been tested to desulfurize coal otation
concentrate [14,15]. Besides, characteristics of the otation procedure
can be determined by which this procedure could be perfectly
performed and some chemical materials have been found to carry out
otation. For more illustration, the otation studies performed with
low rank coals indicated that the mixtures of oils could be used to
improve otation recovery and selectivity [16]. Some studies have
shown that using surfactants can have inuences on coal otation
because surface of coal can signicantly be changed by surfactants
[1719] and many studies have been conducted to determine the effect
of particle size, shape and degree of particle locking (liberation) on coal
otation [20,21]. Miscellaneous investigations also tried to show the
effect of frother, collector, promoter, solid percent and other variables
on coal otation [2225].
2. Experimental design

Corresponding author at: School of Mining Engineering, College of Engineering,


University of Tehran, Tehran, Iran.
E-mail addresses: m.gharabaghi@gmail.com, gharabaghi@ut.ac.ir (M. Gharabaghi).

http://dx.doi.org/10.1016/j.fuproc.2014.06.021
0378-3820/ 2014 Elsevier B.V. All rights reserved.

One of the most effective techniques to study the process behavior is


the factorial designed test with analysis of variance [26,27]. There are

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D. Azizi et al. / Fuel Processing Technology 128 (2014) 111118

Cumulative passing (%)

100

where () is Kronecker product of matrices, which is:

80

1
B1
B
B1
B
B1
B
B1
B
B1
B
@1
1

60
40
20

1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1

1
1
1 C
C
1 C
C
1 C
C:
1 C
C
1 C
C
1 A
1

0
100

1000
Size (m)

100000

10000

Fig. 1. Cumulative passing at different sizes.

several advantages of statistical design of experiments over classical one


variable at a time method, where one variable is varied at a time. In
statistical design, experiments can be conducted in an organized manner and can be analyzed systematically to obtain much needed
information. The information can be utilized for optimization purpose.
The statistical techniques have been used to study the otation of
minerals [2830] and coal [31,32]. A review of coal processing literature
indicates a lack of statistically based studies on the application and/or
interaction of reagents with coals [33]. Naik et al. [34] carried out a 25
factorial design to study the effect of diesel oil, pH, MIBC, particle size
and sodium silicate on the otation of a low-rank on-coking coal. They
also carried out 23 factorial design experiments [35] on the inuence
of sodium metasilicate, kerosene and MIBC with a higher rank coal.
The PlackettBurman design as one of the most important method of
factorial design has been used as the experimental design. This method
is based on Hadamard matrix by which this experimental design
method has been created.
In an 1867 paper on simultaneous sign-successions, tessellated
pavements in two or more colors, and ornamental tile-work Sylvester
used self-reciprocal matrices, dened as a square array of elements of
which each is proportional to its rst minor [36]. This wide class of
matrices contains orthogonal rows and columns. In 1893 Hadamard
proved that such matrices attain the largest value of the determinant
among all matrices with entries bounded by unity [37]. After that paper
the matrices with entries equal to 1 and mutually orthogonal rows
and columns were called Hadamard. Originally there was an interest in
real Hadamard matrices, Hij|R, which found diverse mathematical
applications, particularly in error correction and coding theory [38] and
in the design of statistical experiments [39]. H8 (8 8 Hadamard
matrix) was chosen to design coal otation tests of this investigation
that it given by:

 
 

1 1
1 1
1 1


1 1
1 1
1 1

In this investigation, the main aim was the optimization of coal


otation in which the optimum point for this procedure and inuences
of variables has been studied. For this purpose, the PlackettBurman
design experiment method has been used by which this optimization
could be performed as correct as possible.

3. Materials and method


3.1. Material characterization
For this investigation, a representative sample of coal was taken
from the Hamkar mine, in Kerman province of Iran, and the entire sample was also crushed to a nominal minus 31.5 mm. The crushed sample
was sieved through which its properties can clearly be identied by
which this investigation could precisely be done. The result of sieves
analysis that has been shown in Figs. 1 and 2 shows characteristics of
the representative sample.

3.2. Experimental methods and procedures


The experiments were carried out using a Denver type otation
machine with an impeller speed of 1000 rpm. The volume of this machine
was considered 2.5 L for these experiments. 250 g of the representative
sample was used in each test and solid percent was 10% in these experiments. Moreover, fresh water was applied to prepare slurry for otation
tests and pH of experiments was 7.5. Wetting time and conditioning
time were considered to be 5 min and 90 s, respectively. In addition, different kinds of frother and collector were used to perform otation tests
which their optimum value can be precisely determined by which kinetic
and optimization experiments were carried out as correct as possible. For
doing optimization and kinetic tests, in the rst step, various chemical
materials were chosen to carry out otation tests based on obtained information from primary otation tests. Afterward, optimization and kinetic
tests were done based on chosen materials in the primary experiments.
These experimental results are denitely analyzed in the following sections of this paper.

30

Distribution
Content

Distribution (%)

25

70
60
50

20

40
15

30
10

20

10
0

0
25000

12000

6000

2360

1000

500

300

150

Size (m)
Fig. 2. Characteristics of the representative ash.

75

< 75

Content (%)

10

D. Azizi et al. / Fuel Processing Technology 128 (2014) 111118

80

yield
ash

32

40

10

20

Ash (%)

28

20

15

60

Yield (%)

Efficiency index

36

113

24

20
2EX20

Pine oil

A65

90

In the rst step of this investigation, needed chemical materials and


the operating conditions were determined by which optimization and
kinetic tests could be perfectly performed. For this purpose, different
kinds of frother and collector and various solid percents were analyzed
for which some primary tests were carried out. Consequently, needed
materials and the operating conditions can be completely chosen to
perform otation tests. This stage was done step by step through
which the rst step and considered target have been completely
satised.

Efficiency index

80

4.1. Primary otation tests

Pine oil

90

yield

80

70

70

60

60

50

50

40

40

efficiency index

30
ash

20
10

35

80

125

20
170

215

10

260

A65 (g/t)
90

90

yield

80

Efficiency index

80

70

70

60

60
50

50
efficiency index

40

40
30

30
20
10

20

ash
1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

5.5

10

Collector (kg/t)

Efficiency index Yield


3
ash content of tailings=ash content of clean coal:

90
80

Efficiency index

In the rst step of primary tests, the kind of frother must be chosen
and some tests were performed based on operating condition that it
has been exactly described in the previous paragraphs.
As shown in Figs. 3 and 4ab, A65 can be considered as suitable
frother to perform otation experiments, because the value of yield
and efciency index increased when this frother was used to perform
tests. In addition, some tests were carried out to determine effects of
A65 amount on efciency index, yield and ash value. These tests were
performed at the same operation conditions of previous tests that
they were done to nd the best frother.
When these gures were precisely studied, it is clearly obvious that
the change of frother amount has not had a signicant inuence on ash
content and yield, therefore, they cannot be considered for nding the
value of frother. However, if the curve of efciency index is maintained,
it can be concluded that this factor has been importantly inuenced by
frother dosage. Therefore, frother dosage has been determined based on
this curve and 78 g/t has been chosen for this variable which this decision can be denitely reasonable because of studied proofs.

2EX20

30

4.2. Determination of the operating condition


For doing this study, suitable kind and value of materials should be
found for which some otation tests were needed to be carried out.
For this aim, the special condition was considered for doing tests and
choosing materials. These tests were performed in natural pH, 10%
solid percent and an impeller speed of 1000 rpm. Also, 4 kg/t of gas oil
and fresh water was used to do tests. Wetting time and conditioning
time were 5 min and 90 s respectively. For each test, yield, efciency
index and ash content were studied by which effects of miscellaneous
materials were observed. Efciency index was calculated based on
ASTM Standard Test Method D5114-90, as follow:

H20

Frother type

Fig. 3. Effect of frother type on efciency index.

4. Results and discussion

Dowfroth

Yield or ash (%)

H20

Frother type

Yield or ash (%)

Dowfroth

90

yield

80

70

70

60

60

50

50
efficiency index

40

40

30

30

20
10

20

ash
5.8

7.0

8.2

9.4

Yield or ash (%)

A65

10.6

11.8

10.3

10
14.2

Solid content (%)


Fig. 4. Effects of (a) frother on the yield ash content, (b) A65 amount on the efciency
index, yield, and ash content, (c) collector amount on the efciency index, yield, and ash
content and (d) solid content on the efciency index, yield, and ash content.

Afterward, collector dosage was needed to be correctly determined;


therefore some otation tests were carried out. The same as previous
tests, solid percent and pH were 10% and 7 respectively and 250 g of

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D. Azizi et al. / Fuel Processing Technology 128 (2014) 111118

Table 1
Coded and actual levels of independent variables used in the experimental design.
Variable

Oil gas
A65
Solid content

Symbol

X1
X2
X3

Unit

kg/t
g/t
%

Role

Coded variable
level

Collector
Frother

+1

3.3
39
10

5.3
78
12

sample was used to perform tests. Furthermore, wetting time and


conditioning time were 5 min and 90 s respectively and gas oil and
A65 were considered as collector and frother. According to obtained
information in Fig. 4c, the value of collector should be 5.3 kg/t. Because
it was necessary to improve otation tests in efciency index and yield
which it can be obviously shown; if 5.3 kg/t of collector is used,
efciency index and yield could be signicantly increased and ash
content, on the other hand, could be declined. Next, solid percent should
be determined for which some otation tests were carried out and
operating conditions were similar to the previous steps despite the
fact that the value of collector and frother had been consider based on
the obtained results in the previous tests. For nding suitable and
optimum solid percent, relationships between solid percent and yield
and ash content and efciency index are needed to be analyzed by
which the value of solid percent could be perfectly found which is
applied to perform otation tests. For this purpose, solid percent versus
ash content, yield and efciency index were plotted in some curves in as
demonstrated in Fig. 4d.
By studying these graphs, it was concluded that if the value of solid
percent is considered to be close to 10%, satisfactory results could be
transparently obtained and ash content and efciency index could be
better than other conditions signicantly, although yield may be slightly
declined in this condition when it is compared with the value of
lower solid percent. Indeed, efciency index and ash content have
been prioritized to choose the best value of solid percent in optimization
tests.
4.3. Optimization of otation tests
To continue this investigation, nding optimum condition has been
considered and the relationship between miscellaneous variables and
optimum operating conditions has been illustrated by which the
otation procedure could be signicantly optimized. For this purpose,
Hadamard matrix was chosen as an effective method that it has been
known to design experiments. Since, the PlackettBurman (an experimental design method in DX7 software) design depends on Hadamard
matrix based on using the same as mathematic theory; it was applied
to optimize otation tests. By using this experimental design method
and three considered signicant variables to perform tests; some

experiments were designed. Table 1 lists design variables, and test


results are demonstrated in Table 2.
If all variables are assumed to be measurable then the Plackett
Burman can be expressed as
y f X1 ; X2 ; X3 Xi

where y is the output and Xi the variables of action called factors [40,41].
The results inserted to Design Expert (DX) software and a model
among several models were chosen and tted to the results. The nal
equations in terms of coded factors are selected as the following
equations:
y1 Ash content 16:150:65X2 0:075X3 0:28X2 X3

y2 Efficiency Index 34:90 3:13X1 2:7X2


2:35X3 2:23X1 X3 2:00X2 X3 :

Table 3 shows that prediction models of the efciency index and ash
content are signicant; because, P-value of models was under 0.05. Also,
inuences of collector, frother and solid percent were signicant.
Interactions between collector and solid percent and frother and solid
percent were signicant, while, other interactions didn't have a signicant effect on the efciency index.
As shown in Table 4, inuences of frother were signicant on the ash
content and there was an interaction between solid percent and frother.
As Fig. 5 shows the coefcient of multiple determinations (R2) tted
in them by the high value of R2 indicates that the equation is capable to
represent the system under the given experimental domain. Joglekar
and May suggested that for a good t of a model, R2 should be at least
0.80 [42]. R2 was found to be 0.9995 for efciency index and 0.8685
for ash content. The value of R2 shows that there is an acceptable
relationship between predicted and actual values; therefore, the models
were signicantly tted.
4.4. Inuence of miscellaneous variables on responses
The relationships between variables and ash content and efciency
index were studied and their effects on each other were found. In
order to determine these effects, experimental results have been
analyzed by software through which the model can signicantly be
selected and inuences of variable were perfectly portrayed. It was
concluded that the increase in solid content, collector dosage and
frother has increased efciency index. Moreover, interactions between
variables and their inuences on efciency index were maintained in
which some results could be obtained as demonstrated in Fig. 6.
If these interactions are studied, it can rmly be found that there are
interactions between solid content and frother and solid content and
collector dosage and these interactions happened when these variables

Table 2
PlackettBurman design of experiments for the study of three experimental factors in coded and actual levels with experimental results.
Run

1
2
3
4
5
6
7
8

Coded level of variable

Actual level of variable

X1

X2

X3

X1

X2

X3

+1
+1
+1
1
+1
1
1
1

1
+1
+1
+1
1
+1
1
1

1
1
+1
+1
+1
1
+1
1

5.3
5.3
5.3
3.3
5.3
3.3
3.3
3.3

39
78
78
78
39
78
39
39

10
10
12
12
10
12
12
10

Efciency
index

Ash content
(%)

33.3
42.5
39
36.9
37.3
32
35.8
22.4

17.3
14.9
15.6
16.1
16.3
15.4
16.9
16.7

D. Azizi et al. / Fuel Processing Technology 128 (2014) 111118

115

Source

Sum of
square

df

Mean
square

F value

P-value
prob N F

Model
X2
X3
X2X3
Residual
Cor total

4.03
3.38
0.045
0.61
0.61
4.64

3
1
1
1
4
7

1.34
3.38
0.045
0.61
0.15

8.81
22.16
0.3
3.97

0.0309
b0.0093
0.6158
0.1172

Signicant
Signicant

Ash (%)

Table 4
Analysis of variance of the developed models for ash content.

Table 3
Analysis of variance of the developed models for efciency index.
Sum of
square

Model
252.23
X1
78.13
X2
58.32
X3
44.18
X1X3
39.61
X2X3
32
Residual
0.13
Cor total 252.36

df Mean
square

F value

5
1
1
1
1
1
2
7

776.09
0.0013
1201.92 b 0.0008
897.23
0.0011
679.69
0.0015
609.31
0.0016
492.31
0.002

50.45
78.13
58.32
44.18
39.61
32
0.065
168.55

Fo

P-value
prob N F
Signicant
Signicant
Signicant
Signicant
Signicant
Signicant

are in high values. Indeed, it is clearly obvious that these interactions


could have signicant inuences on efciency index.
Subsequently, inuences of variables on ash content were determined. For this aim, solid percent and frother dosage were chosen as
signicant variables by which ash content could be changed. Results
showed that when frother dosage was increased, ash content was obviously declined; however, the change of solid percent does not have an
important effect on the amount of ash content. Furthermore,

rth
er

(g

/t)

o
Solid c

)
ntent (%

b
Efficiency index

Source

Sol
id

co n
ten
t (%
)

le c
Co l

tor

(kg

/t)

45

efficiency index

c
35

30

25

y = x + 2E-13
R2 = 0.9995

20
20

25

30

35

40

Efficiency index

Observed value

40

45

17.5

ash content

Sol
id

Observed value

17.0

16.5

Fro

the

r (g

/t )

Fig. 6. 3D plot of effect of the interactions (a) between solid percent and frother dosage on
the ash content, (b) between solid percent and collector dosage on the efciency index
and (c) between solid content and frother dosage on the efciency index.

16.0

15.5

15.0
15.0

co n
t en
t (%
)

y = x - 2E-12
R2 = 0.8685
15.5

16.0

16.5

17.0

17.5

Predicted value
Fig. 5. Relationship between predicted and observed values for efciency index and
ash content.

interactions among variables were maintained; it was found that


there has been an interaction between solid content and frother dosage
in the middle value of these studied variables approximately.
Afterwards, for doing a more complete study of the relationship
between variables, a 3D graph was needed to be portrayed in which
this aim could be realized. For this purpose, variables versus ash content
and efciency index were plotted in a 3D graph. This kind of graph can

116

D. Azizi et al. / Fuel Processing Technology 128 (2014) 111118

Table 5
Results of the process optimization and optimum levels of variables.
Case

Target

Collector

Frother

Solid content

Ash (%)

Efciency index

Desirability

Ash content
Variable
Efciency index

Minimum
In range
Maximum

5.29

78

10

15.2

42.55

show relationships between variables and more information can be


provided to understand the mechanism of the otation procedure.
It should be explained that interactions among important variables

have been seen in these 3D graphs. According to Fig. 6, increasing


solid content and decreasing frother dosage enhanced ash content.
In addition, when each variable was increased, efciency index was
signicantly inuenced through which the value of this important
parameter was sharply raised. In fact, this gure can describe inuences
of variables on ash content and efciency index when there were
interactions between them and it helped to understand this otation
process perfectly.

4.5. Finding of optimum condition


Finding optimum condition was one of the most important aims of
this investigation through which the performance of the otation
procedure can be signicantly improved. This possibility can be
provided by the PlackettBurman experimental design method which
depends on Hadamard matrices. The otation procedure could be
optimized in which the value of variables have been identied to
perform this procedure as ash content and efciency index have been
obtained in minimum and maximum values respectively as shown in
Table 5.
Understanding the condition of the procedure in optimum point can
help to describe otation tests that can be used to nd effective and
signicant variables in this process. For this aim, inuences of variables
on ash content and efciency index were needed to be maintained by
which increasing and decreasing of responses could perfectly be illustrated. According to signicant interactions among variables and their
inuences on efciency index and ash content, optimum point has
been studied and relationships between interactions and responses
have been portrayed in 3D plots as shown in Fig. 7.
If this gure is studied to understand the otation procedure,
anticipated optimum condition can be justied which can be predicted
by software. It is clearly obvious that inuences of interactions on responses can be understood and studied through which the enhancement

90
80

Cumulative yield (%)

70
60
50
40
30
20
10
0
0
Fig. 7. 3D plot of effect of the interactions (a) between solid percent and collector dosage
on the efciency index, (b) between solid percent and frother dosage on the efciency
index and (c) between solid percent and frother dosage on the ash content.

25

50

75 100 125 150 175 200 225 250 275

Time (s)
Fig. 8. Cumulative yield for coal in kinetic analysis test.

D. Azizi et al. / Fuel Processing Technology 128 (2014) 111118

of each variable has improved efciency index and increasing frother


dosage and decreasing solid content have increased ash content.
4.6. Kinetic analysis
From a practical point of view, the overall otation process can be
generally represented by a rst order system with lumped parameters,
assuming that the collection zone was perfectly mixed. Eq. (7) shows
the rst order model for a perfect mixed batch otation process [43]:
R
kt
1e
R

where R represents the mineral recovery at time t, R represents the


maximum otation recovery at innite time, and k is the kinetic rate
constant which involves all the microscopic sub-processes.
This has allowed a otation cell to be modeled using the chemical
reactor analogy; whereby the removal of solids from the pulp phase is
dened by a rst order rate equation. This means that a bank of cells
can be approximated by perfectly mixed CSTR's in series [44].
Subsequently, efforts have been made to accurately determine the so
called over-all otation rate constant (or k). This is not trivial, as k is
dependent on particle size, degree of liberation, air ow rate, agitation,
etc. To account for this, various continuous distribution functions of k
have been devised [45]; although previous reviews by Dowling et al.
[46] conclude that no single distribution model could sufciently
represent k; and Roesch et al. [47] suggest that attempts based on the
rst order kinetic assumption are approximative and hide secondary
details.
Determining the time of otation has been one of the most
substantial factors which should be known in every otation procedure.
In fact, it can be applied to nd optimum time in which recovery could
be when maximum value and time of otation would be sharply
declined. In this case, if the time of otation is not exactly observed,
more money and energy should be spent to perform otation. Finding
real otation time could help to decrease costs, because it can denitely
make spending time, consuming chemical materials and operating
conditions decrease transparently. Due to these reasonable proofs, the
kinetic of the otation procedure was studied to determine the otation
time. For this purpose, one otation test was carried out and operating
conditions were chosen based on optimum condition which has been
determined in optimization section. During the otation procedure,
several samples were taken to calculate yield in every sampling time
by which the kinetic could be precisely found. Yield versus time has
been plotted in one curve in which the trend of the kinetic has been
portrayed perfectly (Fig. 8).
Based on this curve, the kinetic rate constant (k) was 0.053 and it
can be understood that recovery has been stabilized in 120 s in which
recovery was 86.72%. It has been concluded that the otation procedure
has been completed in 120 s and if the otation time increases,
performance will never be improved and time, energy and chemical
materials will be surely wasted. Consequently, the otation time can
be optimized when the kinetic is analyzed and designing otation cell,
reagent consumption and choosing otation circuit can be signicantly
inuenced and they will be selected based on more information.
5. Conclusion
In this research work, the PlackettBurman methodology has been
used to optimize the coal otation process and nd important variables.
Representative sample of coal was taken from Hamkar coal mine, in
Iran. Experimental design, analysis of results, optimization and
modeling of the process were done by DX7 software. Predicted values
obtained using the model equations were in very good agreement
with the observed values (R2 value of 0.9995 for efciency index, R2
value of 0.8685 for ash content). Results of optimization showed that

117

ash content and efciency index could be 15.2% and 42.55 respectively
when the values of collector, frother and solid percent were 5.29 kg/t,
78 g/t and 10% respectively. Besides, the kinetic of the procedure was
studied through which the time of 120 s has been considered as the
optimum time and at this time the otation procedure could be rmly
completed.
Acknowledgment
This research work was partly supported by Iran National Science
Foundation (INSF) under contract number 92000649. The authors also
appreciate Mr. Arash Ashra for his help to this paper.
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