j m a t e r r e s t e c h n o l .

2 0 2 0;9(6):12654–12660

Available online at www.sciencedirect.com

https://www.journals.elsevier.com/journal-of-materials-research-and-technology

Original Article

Adsorption and desorption of butyl xanthate on

chalcopyrite

Cong Han ∗ , Dezhou Wei, Shuling Gao, Qingxiang Zai, Yanbai Shen ∗ , Wengang Liu
School of Resources & Civil Engineering, Northeastern University, Shenyang 110819, Liaoning, PR China

a r t i c l e i n f o a b s t r a c t

Article history: Reagent removal is an indispensable step to further separation of the copper sulfide ore
Received 16 March 2020 flotation mixed concentrate, and xanthate is one of the most commercially used collec-
Accepted 3 September 2020 tors for chalcopyrite flotation. In this work, the adsorption/desorption quantity of butyl
xanthate was measured by the spectrophotometric method. Three adsorption models of
Langmuir, Freundlich, and Temkin were used to fit the xanthate adsorption quantity dates.
Keywords: The results show that the adsorptions of sodium butyl xanthate on chalcopyrite match
Chalcopyrite the Langmuir model best in the experimental conditions. Sodium sulfide dosage, pH value,
Sodium butyl xanthate ultrasonic wave, and temperature all show effects on butyl xanthate desorption. Butyl xan-
Adsorption thate desorption can promote by increasing the dosage of sodium sulfide, ultrasonic wave
Desorption intensity, temperature, and acidity or alkalinity of pulp. The order of the effectiveness of
four conditions is sodium sulfide dosage, temperature, pH, and ultrasonic.
© 2020 The Author(s). Published by Elsevier B.V. This is an open access article under the
CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

[8–10]. Since chalcopyrite often intergrowth with other sulfide

1. Introduction minerals, different feeds need different beneficiation methods
applied.
Copper is an essential and irreplaceable metal resource, widely
To separate chalcopyrite from ores containing multiple sul-
used in material make, power transmission, metallurgy, and
fide minerals, the commonly used processing by far is that
other fields [1–5]. Chalcopyrite (CuFeS2 ) is the most plentiful
of selective flotation and bulk flotation [11,12]. Bulk flotation
copper-bearing mineral, accounting for about 70% of copper
is frequently used to treat copper ores with similar min-
mines. The efficient use of chalcopyrite ore has always been
eral floatability. To separate chalcopyrite more efficiently from
a hot issue in mineral processing [6,7]. Depending on the
these sulfide minerals is one of the hotspots and difficulties
nature of the treated ore, a different method used for copper
in flotation technology investigation [13–16].
raw ores processing, of which for the copper in the chalcopy-
Before chalcopyrite-other sulfide mineral flotation separa-
rite in the recovered ore is mainly by leaching and flotation
tion, the mixed concentrate needs to remove the adsorbed
collector [17–19]. The purpose of it aims to expose the orig-
inal surface of the minerals to enable carry out the following
∗
Corresponding authors. separation more efficiently. The effect of reagent removal
E-mails: hancong@mail.neu.edu.cn (C. Han), directly affects the index of separating chalcopyrite from
shenyanbai@mail.neu.edu.cn (Y. Shen). mixed concentrates and the quality of final concentrate.
https://doi.org/10.1016/j.jmrt.2020.09.021
2238-7854/© 2020 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12654–12660
Sodium (potassium) butyl xanthate is one of the most widely
used collectors for chalcopyrite flotation [20,21]. As universally
known, the transfer of xanthate from the liquid phase to the
surface of chalcopyrite is a chemical process. Many studies
found that the main xanthate-derived species on chalcopyrite
are copper xanthates and/or dixanthates [22,23]. Therefore,
to understand the adsorption characteristics of the chemical
species on the surface of minerals is significant for reagent
removal investigation. To clarify the effect law of the process
conditions such as chemical reagents, pH value, mechanical
energy input, and temperature on the desorption of xan-
thate pre-adsorbed on chalcopyrite, is of great significance for
guiding the research and application of chalcopyrite reagent
removal technology.
In this paper, Ultraviolet (UV)-visible spectrophotometry
was used for measuring the adsorption/desorption quan-
tity of sodium butyl xanthate (SBX) on chalcopyrite. The
basis on it drew the adsorption curve of SBX on chalcopy-
rite. Then, three adsorption models of Langmuir, Freundlich,
and Temkin were used to fit the adsorption data for ana-
lyzing the adsorption characteristics of SBX on chalcopyrite.
Additionally, the effect of conditions of sodium sulfide
dosage, pH value, the intensity of ultrasonic, and temper-
ature on desorption of SBX was investigated. The research
results can deepen the understanding of the adsorption char-
acteristics of butyl xanthate on chalcopyrite in flotation.
Simultaneously, it also can provide reference and guid-
ance on the technology research of chalcopyrite flotation
separation.
2. Experimental
2.1. Chalcopyrite sample
The chalcopyrite use for tests is produced from a mine in
Yunnan province, China. The raw ore was manually crushed
and then sorting to collect pure blocks. The pure blocks were
ground in a ceramic ball mill. Standard sieves used for screen-
ing the grinding products to get -0.1 + 0.043 mm fraction as
experimental chalcopyrite sample. Dilute hydrochloric acid
with a mass concentration of 0.5% was used to clean the col-
lected chalcopyrite in an ultrasonic cleaner to remove the
oxidized layer on the mineral surface. After acid pickling,
solid-liquid separation was performed. The upper clear liquid
is discarded, and the chalcopyrite was rinsed with deionized
water multiple times. The chalcopyrite sample after cleaning
was placed in a vacuum drying oven and dried at 25◦ C for 24 h.
The dried sample was placed in a jar with a rubber stopper and
stored as the final test chalcopyrite.
The X-ray diffraction (XRD) pattern of the chalcopyrite sam-
ple is presented in Fig. 1. The chemical analysis result shows
that the copper grade is 32.84%, indicating that the content of
chalcopyrite in the sample is 95.02% and the purity meets the
standard of the mono-mineral experiment. The SBX used in
the test is provided by the Tieling Flotation Reagents Co., Ltd
lab, China, in which purity is greater than or equal to 93%. The
other reagents used in the experiment are analytical grade, all
of which are commercial products of Tianjin Kemeiou Chem-
ical Reagent Co., Ltd.
12655
Fig. 1 – The XRD pattern of chalcopyrite sample.
2.2. Adsorption/desorption quantity measurement
Since the flotation of chalcopyrite using xanthate needs
to be carried out in alkaline, the adsorption test of xan-
thate on chalcopyrite was carried out at pH 8.0. The
SP-2000UV UV-visible spectrophotometer was used for mea-
suring the absorbance. Then the concentration of xanthate
determined by querying the corresponding absorbance on the
absorbance-concentration standard curve. Finally, the adsorp-
tion/desorption quantity was calculated.
Absorbance measurement for adsorption quantity calcu-
lation: weighted 2 g chalcopyrite and put it into a 50 mL
centrifuge tube, then add 30 mL deionized water (the pH had
been adjusted to 8.0 with HCl or NaOH solution priory) and SBX
into the tube. Then, put the centrifuge tube into a centrifuge
and centrifuge for 5 min at 5000 rpm. After that, the super-
natant was extracted from the centrifuge tube and measured
its absorbance.
Absorbance measurement for desorption quantity calcula-
tion: under the condition of SBX concentration of 20 mg·L−1 ,
the chalcopyrite sample for the desorption test was prepared
using the same method in the adsorption test treat to the
chalcopyrite. Then, added deionized water, Na2 S, and HCl or
NaOH into the centrifuge tube separately to deal with the
chalcopyrite. Tests of the effect of temperature and ultrasonic
intensity on the desorption of SBX pre-adsorbed on chalcopy-
rite tests were carried out in a KQ-600DE ultrasonic cleaner
with a heating function of the water bath. While tempera-
ture tests conducted, the ultrasonic function was turned off,
and the heating function was on. While ultrasonic intensity
tests were performed, the heating function was turned off. The
sample was treated for 5 min. Subsequently, put the centrifuge
tube into the centrifuge and centrifuge for 5 min at 5000 rpm.
Then, the supernatant was extracted from the centrifuge tube
and the absorbance was measured.
The adsorption quantity of the adsorbate was calculated
according to:
(C0 − C) × V
 = (1)
m
12656 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12654–12660
Fig. 2 – The curve of absorbance of SBX aqueous solution as
a function of wavelength.
Where  (mg· g−1 ) is the adsorption quantity, C0 (mg·L−1 )
is the initial concentration of adsorbate, C (mg·L−1 ) is the
concentration of adsorbate exists in the liquid phase after
adsorption, V (L) is the volume of solution, and m (g) is the
mass of adsorbent.
The desorption ratio of the adsorbate at different condi-
tions was calculated according to:
m − CV
=
m
Where  (%) is the desorption ratio,  (mg· g−1 ) is the
adsorption quantity, C (mg·L−1 ) is the concentration of adsor-
bate exists in the liquid phase after desorption, V (L) is the
volume of solution, and m (g) is the mass of adsorbent.
3. Results and discussion
3.1. Curve of SBX concentration and absorbance
The relationship curve between the absorbance and wave-
length of a SBX solution with 10 mg·L−1 concentration was
determined using deionized water as a reference, and the
result shows in Fig. 2.
Fig. 2 shows there are two distinct peaks appear at the
wavelengths of 225 and 299 nm, and the absorbance ratio of
the two peaks is approximately 1:2. The peak at 299 nm is the
best absorption peak of SBX, the peak at 225 nm is a shoulder
peak with valueless for measurement in this study [15–17].
Therefore, 299 nm is selected as the optimal absorption wave-
length for the SBX absorbance measurement.
At the wavelength of 299 nm, the absorbance of the solu-
tion with SBX concentrations of 1, 5, 10, and 20 mg·L−1 was
measured, respectively, and the result presents in Fig. 3.
It can be seen from Fig. 3 that the correlation coefficient
of the linear fitting equation is 0.997, indicating the excellent
linear relationship between the SBX concentration and the
absorbance, and the curve can be used for the determination
of the SBX concentration according to absorbance.
Fig. 3 – The curve of absorbance as a function of SBX
concentration.
(2)
Fig. 4 – The curve of the adsorption quantity on
chalcopyrite as a function of concentration at 16.9◦ C.
3.2. Adsorption characteristics of SBX on chalcopyrite
Many literatures have reported the pulp conditioning period
generally completed in 3–5 min, it is enough to make the min-
eral floatability reach the stable state in a specific collector
concentration [24–27]. Mineral surface hydrophobicity deter-
mines the floatability, and it is associated with the quantity of
the collector adsorbed on the mineral. Therefore, the adsorp-
tion quantion can be used to judge whether the floatability of
mineral reaches the stable state in pulp conditioning. It means
that, under flotation conditions, when floatability reaches the
steady-state, the distribution of the collector on the mineral
surface and liquid phase is in a dynamic equilibrium.
At the condition of pH is 8.0, and the pulp temperature
is 16.9◦ C, the relationship between adsorption quantity and
concentration was determined and presented in Fig. 4.
Fig. 4 shows that, in the period of pulp conditioning, the
curve of the adsorption quantity as a function of concentra-
tion conforms to type I isotherm. And in the low equilibrium
concentration range (below 0.89 mg·L−1 ), the adsorption quan-
tity of SBX rapidly increases. Then, its increase becomes to
slow down and gradually stabilizes, meaning the floatability
to reach a stable state. In this work, Langmuir mode [28], Fre-
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12654–12660 12657

Fig. 5 – The fitting curve of the Langmuir adsorption model.

Fig. 6 – The fitting curve of the Freundlich adsorption
model.

undlich model [29], and Temkin model [30] were used to fit the
experimental adsorption data to study the adsorption charac-
teristics of the collector on the mineral.

3.2.1. Langmuir model

Langmuir model is given as Eq. (3) can be transformed into
linear form as Eq. (4). Where C (mg·L−1 ) is the concentration
of SBX in the slurry phase as adsorption reaches dynamic
equilibrium,  (mg·g−1 ) is the adsorption quantity of SBX on
chalcopyrite at the dynamic equilibrium concentration(C) in
the slurry phase,  s is saturated adsorption quantity, and b is
adsorption constant. Taking the values of C/ as the ordinate
and C as abscissa, plot curve, and the result shows in Fig. 5.

bC
 = s × (3) Fig. 7 – The fitting curve of the Temkin adsorption model.
1 + bC

C 1 C
= +
 s b s
It can be seen from Fig. 5 that the correlation coefficient
(R2 ) of the fitting equation is 0.979, and the linear equation
isy = 2.554 + 2.375x. According to Eq. (4), it can be calculated
the values of  s and b are 0.42 and 0.93, respectively. Therefore,
the Langmuir adsorption equation of SBX on chalcopyrite at
16.9◦ C is  = 0.42 × 1+0.93C
0.93C
. the Freundlich adsorption equation of SBX on chalcopyrite at
3.2.2. Freundlich model
The Freundlich adsorption model may be expressed in terms
of Eq. (5), and its linear form shows as in Eq. (6). Where C
(mg·L−1 ) is the concentration of SBX in the slurry phase as
adsorption reaches the dynamic equilibrium,  (mg· g−1 ) is
adsorption quantity of SBX on chalcopyrite at dynamic equi-
librium concentration (C) in the slurry phase, A and n are
constants that relates to the properties of chalcopyrite and
SBX at a specific temperature. Taking the value of log as the
ordinate and logC as abscissa, plot curve, and the result shows
in Fig. 6.
(4)
1
log = log A + log C (6)
n
As shown in Fig. 6, the correlation coefficient (R2 ) of the
fitting equation is 0.903, and the linear equation isy = 5.177 +
0.615x. According to Eq. (6), it can be calculated the values of
A and n at 16.9◦ C are 1.504 × 105 and 1.625, respectively. Thus,
16.9◦ C is  = 1.504 × 105 · C1/1.625 .
3.2.3. Temkin adsorption model
The linear form of the Temkin model is written as Eq. (7).
Where C (mg·L−1 ) is the concentration of SBX in the slurry
phase as adsorption reaches dynamic equilibrium,  (mg·g−1 )
is adsorption quantity of SBX on chalcopyrite at dynamic equi-
librium concentration (C) in the slurry phase, a and b are
constants that relates to the properties of chalcopyrite and
SBX at a specific temperature. Taking the value of  as the
ordinate and logC as abscissa, plot curve, and the result shows
in Fig. 7.

 = AC1/n (5)  = a + b log C (7)

12658 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12654–12660

Table 1 – Fitting results of three adsorption models.

Adsorption model R2 Fitting equation
0.93C
Langmuir 0.979 16.9◦ C = 0.42 × 1+0.93C
Freundlich 0.903 16.9◦ C = 1.504 × 105 · C1/1.625
Temkin 0.882 16.9◦ C = 220.859 + 170.908 log C

Fig. 9 – Absorbance as a function of wavelength for the

Na2 S solution, desorption solution, and SBX solution.

Fig. 8 – The effect of Na2 S concentration on the residual

adsorption quantity of xanthate on chalcopyrite and the
desorption ratio.

Fig. 7 shows that the correlation coefficient (R2 ) of the fit-

ting equation is 0.882, and the linear equation is y = 220.859 +
170.908x. According to Eq. (7), it can be calculated the values of
a and b are 220.859 and 170.908, respectively. Accordingly, the
Temkin adsorption equation of SBX on chalcopyrite at 16.9◦ C
Fig. 10 – The effect of pH value on the residual adsorption
is  = 220.859 + 170.908 log C.
quantity of xanthate on chalcopyrite and the desorption
As Table 1 illustrates, the correlation coefficient of the
ratio.
Langmuir adsorption equation is the largest one among three
adsorption models, which implies that the Langmuir adsorp-
tion model is most reliable, the adsorption of SBX on the
chalcopyrite surface under the experimental conditions is
likely to be chemical monolayer adsorption [18,31].

3.3. Desorption characteristics of SBX on chalcopyrite

At the condition consistents with the adsorption experiment,

four terms of sodium sulfide dosage, pH value, ultrasonic
intensity, and temperature were selected to study the influ-
ence on the desorption characteristics of xanthate. The
chalcopyrite samples used for the desorption experiment
were prepared at the SBX concentration was 20 mg·L−1 . At
this concentration, the adsorption quantity of SBX is 0.2866
Fig. 11 – The effect of ultrasonic intensity on the residual
mg· g−1 . The desorption experimental results are presented in
adsorption quantity of xanthate on chalcopyrite and the
Figs. 8–12, where the value of the ordinate axe is the residual
desorption ratio.
adsorption quantity of the collector on chalcopyrite.
As can be seen from Fig. 8, as the Na2 S concentration
increases, the residual adsorption quantity of xanthate on
chalcopyrite gradually decreases. When Na2 S concentration desorption solution, Na2 S solution, and SBX solution were
reaches 66.67 mg·L−1 , the residual adsorption quantity of measured, and the results show in Fig. 9.
xanthate on chalcopyrite is only 0.0197 mg· g−1 , and the des- As shown in Fig. 9, the peak shape of the desorption
orption ratio is 93.13%. solution is consistent with the SBX solution, but there is a
In order to check the main product of the desorption difference between them. Although the absorbance of the
solution after Na2 S treatment, the UV-visible spectra of the desorption solution and SBX solution at 299 nm is not much
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12654–12660
Fig. 12 – The effect of temperature on the residual
adsorption quantity of xanthate on chalcopyrite and the
desorption ratio.
different, the absorbance of the SBX solution at 225 nm is
smaller than it at 299 nm, and the absorbance of the desorp-
tion solution at 225 nm is larger than it at 299 nm. It could be
attributed to the presence of Na2 S in the solution and the S-
bearing species produced during the desorption, which have
a strong absorption peak at 225 nm (Line 2 of Fig. 9). It can also
be seen from Fig. 9 that the absorbance of the Na2 S solution at
299 nm is close to zero. Therefore, it can judge that the peak at
299 nm of the desorption solution attributes to the xanthate
in the solution.
During the desorption process, it is inevitable that a few
amounts of xanthate will be transformed into other compo-
nents and move into the solution, resulting in the measured
desorption quantity is less than the actual one. Due to the
purpose of reagent removal is to expose the mineral surface
again, to determine the components in the liquid phase is
not the focus of the study. Moreover, because the absorbance
of the desorption solution and SBX solution at 299 nm is not
much different, to maintain the consistency of the tests, the
absorbance of the desorption solution is still measured at the
wavelength of 299 nm, and it assumes that all the compo-
nents desorbed from the chalcopyrite surface are in the form
of xanthate exists in solution.
As shown in Fig. 10, the xanthate easily desorbs from
the chalcopyrite while the mineral is in a strongly acidic or
strongly alkaline environment. Among them, in a strongly
acidic environment, the desorption ratio can reach 40.53% as
pH is 2.53; in a strongly alkaline environment, the desorption
ratio can reach 63.89% as pH is 11.42. It is considering that the
highly acidic slurry has strong corrosiveness to the pipeline
and equipment. Therefore, increasing the slurry alkalinity
compared to enhancing the acidity to remove the xanthate
is more feasible in actual production.
Fig. 11 illustrates that the ultrasonic can desorb xanthate
adsorbed on chalcopyrite, the higher the ultrasonic intensity,
the better the xanthate desorption ratio obtains. However,
the increase of desorption ratio is slow with the increasing
of ultrasonic intensity within the setting range of the test,
and the maximum value does not exceed 40%. The essence of
ultrasonic treatment is to increase the energy of the system.
However, ultrasonic treatment is difficult to achieve in practi-
12659
cal beneficiation process. Therefore, in practical applications,
the energy of the system could be increased by increasing the
mechanical stirring strength, thereby may achieve a similar
outcome to the use of ultrasonic treatment.
The results in Fig. 12 show that increasing temperature can
significantly promote the desorption of xanthate. The higher
the temperature, the better the desorption ratio obtains.
Within the temperature range in the experiment, the maxi-
mum desorption ratio is 67.06%.
4. Conclusions
Within the experiment concentration range, the absorbance
and the concentration of the xanthate solution presents an
excellent linear relationship. The adsorption quantity of xan-
thate on chalcopyrite increases with increasing the initial
concentration of xanthate.
The order of correlation coefficient of the linear equations
of three models is the Langmuir model (0.979), the Freundlich
model (0.903), and the Temkin model (0.882). At the conditions
of pH value is 8.0, pulp temperature is 16.9◦ C, the experimen-
tal agitation and contact time, the adsorption characteristic
of butyl xanthate on chalcopyrite is most consistent with the
Langmuir model. Butyl xanthate forms monolayer adsorption
on chalcopyrite.
Sodium sulfide, pH value, ultrasonic intensity, and temper-
ature all show an effect on the desorption of xanthate. Sodium
sulfide exhibits the best performance on xanthate desorp-
tion, and an up to 93.13% desorption ratio obtains while the
concentration of sodium sulfide is 66.67 mg·L−1 . Increasing
temperature, mechanical energy input, and pH value of pulp
may promote the desorption of xanthate when using sodium
sulfide, which will contribute to raising the desorption ratio
further or reduce the amount of sodium sulfide used.
Conflict of interest
The authors declare no conflicts of interest.
Acknowledgments
This research was supported by the Fundamental Research
Funds for the Central Universities (N2001008, N180408018),
the National Natural Science Foundation of China
(51674067, 51422402), Liaoning Revitalization Talents Pro-
gram (XLYC1807160), Liaoning BaiQianWan Talents Program
(201892127), and Open Foundation of State Key Laboratory of
Mineral Processing (BGRIMM-KJSKL-2019-12).
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