Minerals Engineering 45 (2013) 94–99

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Minerals Engineering
journal homepage: www.elsevier.com/locate/mineng

New source of unavoidable ions in galena flotation pulp: Components released

from fluid inclusions
Shaojun Bai a, Shuming Wen a,b,⇑, Yongjun Xian a, Jian Liu a, Jiushuai Deng a
a
Faculty of Land Resource Engineering, Kunming University of Science and Technology, Kunming 650093, PR China
b
Engineering Research Center for Efficient Utilization of Mineral Resources in Western of China, Kunming University of Science and Technology, Ministry of Education,
Kunming 650093, PR China

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

Article history: The present work investigated the trace and component release of fluid inclusions in natural pure galena.
Received 18 September 2012 The investigation results indicated that the composition of the inclusion trace was characterized by a
Accepted 1 February 2013 lower Pb content compared to the theoretical composition of galena; nonetheless, these inclusions were
Available online 5 March 2013
rich in lead and chlorine ion. The inclusions were liberated through a grinding process where their com-
positions were released into solution. It was found that the lead concentrations (CPbT) released from the
Keywords: inclusions through the grinding process reached 8.25  106 mol/L in the experiment with conditions of
Fluid inclusions
2 g galena placed into 40 ml pure deionized water under an inert environment, which was much higher
Component release
Natural galena
than the CPbT found through experimental dissolution (1.12  106 mol/L). Therefore, it was concluded
Dissolution that the release of Pb from the fluid inclusions in galena was an important new source of the Pb concen-
Unavoidable ions tration in the solution. This finding sheds new light on the source of unavoidable ions in the flotation
pulp. The residual position domain after the release of the inclusions causes the morphology difference
in the galena surface composition and roughness. This study provided a new understanding of the
unavoidable ion source that is found in the flotation theory and environmental geochemistry.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction
Galena (PbS) is one of the most intensively studied sulfide min-
erals because it is an important source of lead. In fact, natural and
synthetic lead sulfide are used for many practical applications
(Nowak and Laajalehto, 2000; Ralston, 1994). The beneficiation of
sulfide minerals requires a process known as froth flotation, which
separates sulfide minerals and gangue minerals based on their flo-
atability differences. However, when metal ions, such as Cu2+, Pb2+,
Zn2+, Ca2+ exist in the flotation pulp, the floatability differences
between the sulfide minerals and the gangues are reduced
(Chandra and Gerson, 2009; Ikumapayi et al., 2012; Peng et al.,
2012). These metal ions, known as ‘‘unavoidable ions’’, have signif-
icant effects on the flotation performance and lead to the metallic
sulfides and gangue particles being non-selectively activated dur-
ing the separation processes of metallic sulfide ores (such as
CuFeS2, PbS, ZnS, and FeS2). The source of these metal ions is not
explicitly known and several researchers have recently been inves-
tigating surface dissolution, surface dissociation and surface oxida-
tion during the grinding process of mineral ores to identify
⇑ Corresponding author at: Faculty of Land Resource Engineering, Kunming
University of Science and Technology, Kunming 650093, PR China. Tel./fax: +86 871
5153445.
E-mail address: shmwen@126.com (S. Wen).
potential sources for these ions (Finkelstein, 1997; Lin et al.,
2003; Zeng et al., 2000). However, the results of these investiga-
tions have been inconsistent with theoretical calculations based
on dissolution equilibriums of the minerals; almost all of the
experimental results reported have been much higher than those
of the theoretical calculations (Acero et al., 2007; Liu et al.,
2012). This inconsistency suggests that the theories, including sur-
face dissolution, surface dissociation and surface oxidation, as the
source of these ‘‘unavoidable ions’’ are still not applicable for the
comprehensive explanation for the occurrence of such ions and
its relation with froth flotation during the flotation process of
metallic sulfide ores.
Fluid inclusions are formed from the capture of diagenesis fluid
and mineralizing fluid during the ore-forming process and are
extensively found to exist in natural mineral crystals (Andrawes
et al., 1984; Gokce and Bozkaya, 2008; Wilkinson, 2001; Zhu et
al., 2007). Fluid inclusions represent relics of past hydrothermal
water in the Earth’s crust and are kept relatively stable because
they have low mobility within the mineral crystal. This occurs
because there is relatively no material exchange and/or no chemi-
cal reactions between the fluid inclusion and the host minerals.
This suggests that the fluid inclusion contains an accurate perfect
recording of the original physical and chemical information about
the ore-forming process (Abidi et al., 2010; Meissner and Wever,
1992; Robert et al., 1995; Wilkinson, 2010). For the foregoing

0892-6875/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.mineng.2013.02.001
 S. Bai et al. / Minerals Engineering 45 (2013) 94–99
reason, geological researchers examining ore deposits focus their
projects on the function of fluids during the ore-forming process
(Brannon et al., 1992; Bierlein et al., 1996; Polliand and Moritz,
1999; Farhad, 2012; Fairmaid et al., 2011). This includes the inves-
tigation of the age and temperature in which the ore formed and
the generation of the ore deposits (Canet et al., 2011; Philippot et
al., 2001; Xu et al., 2008). Although there is a considerable amount
of literature on fluid inclusions in mineral ores, little is known
about the effects of fluid inclusions on the flotation performance
of metallic sulfide ores. When the ores are crushed and ground
during the flotation process, it is likely that the fluid inclusions
in the mineral crystals will be liberated from the ore. This suggests
that the compositions of the fluid inclusions, such as the metal
ions, will be released into flotation pulp and may constitute the
‘‘unavoidable ions’’ in the pulp. The presence of these ‘‘unavoidable
ions’’ is expected to change the chemical compositions of the pulp
and may significantly affect the froth flotation performance of
metallic sulfide ores due to the non-selective activation of metallic
sulfide and gangue minerals. Therefore, an in-depth understanding
of the release of unavoidable metal ions from fluid inclusions is
expected to provide significant and important information about
the froth flotation process of mineral ores.
In the present study, infrared–ultraviolet microscope (IUM),
scanning electron microscope (SEM) and energy dispersive X-ray
spectroscopy (EDS) were employed to investigate the trace and
composition release of fluid inclusions in natural galena. The total
concentration of lead (CPbT) and chloride (Cl) ions released from
the inclusions were measured by inductively coupled plasma mass
spectrometry (ICP-MS) and ion chromatograph (IC). In addition, to
further verify the source of Pb in the aqueous solution, experimen-
tal dissolution of galena in pure deionized water was also
performed. The study in this paper therefore provides a new
understanding of the source of the ‘‘unavoidable ions’’ found in
the froth flotation pulp.
2. Experimental
2.1. Materials
The material used for the present study was from Huize area,
southwest Yunnan province of China, and a high purity galena
crystal was obtained from the material, after removal of gangue
minerals such as calcite and quartz by handwork. The XRD exper-
iments were performed using a Japan Science D/max-R diffractom-
eter apparatus with Cu Ka radiation (k = 1.5406 Å), an operating
Fig. 1. X-ray diffraction pattern of the galena.
95
Table 1
Chemical composition of galena used in experiments.
Element Pb S Fe Zn Cu SiO2
Mass fraction/% 84.71 13.42 0.33 0.04 0.015 1.32
voltage of 40 kV, and a current of 40 mA. The diffraction angle
(2h) was scanned from 10° to 90°. The X-ray diffraction pattern
and the chemical composition of the galena crystal are shown in
Fig. 1 and Table 1, respectively.
As shown in Fig. 1, the five strongest peaks appear at 25.96°,
30.07°, 42.39°, 51.13° and 64.02°. The strongest peaks are in agree-
ment with the values of the JCPDS card (No. 050592) (Mozafari and
Moztarzadeh, 2010). These values are also in agreement with the
crystal face of (1 1 1), (2 0 0), (5 1 1), (6 0 0) and (4 4 4), respectively.
From the values of lattice constants obtained with the XRD of the
galena, i.e., 5.936 Å  5.936 Å  5.936 Å, a = b = c = 90°, it was con-
firmed that this galena has a cubic structure. Chemical composition
of galena shows that the sample was found to have a high purity
with minor Fe and SiO2 impurities.
2.2. Methods and apparatus
2.2.1. IUM observation of galena fluid inclusion
The galena crystal was cut to a thin slice of double-sided pol-
ished and ground inclusion film, with a thickness of 90–150 lm
to increase light transmission. Then the morphology of fluid inclu-
sions in the crystal was observed with an infrared–ultraviolet
microscope (BX51, Fluid Inc., USA). The information obtained from
the observation was changed to data signal through infrared elec-
tronic induction, and after that the signal was treated with com-
puter software to output the picture of the fluid inclusion. The
IUM observation of samples was conducted by State Key Labora-
tory for Mineral Deposit Research Institute of Geo-Fluids.
2.2.2. SEM–EDS analysis of galena fluid inclusion
The morphology of galena fluid inclusion trace was determined
using SEM (SEM–EDS, FEI Holland, Philip). The sample was first
fixed on the SEM at low magnification for scanning until inclusions
trace appeared. Photography and spectrum analysis were then per-
formed on the position domain of inclusion trace.
2.2.3. Measurement of Pb and Cl released from galena fluid inclusion
The positive ions in the fluid inclusion of galena are usually
alkali metal ions, such as Na+, Mg2+, Ca2+, K+ and its intrinsic ion,
i.e., Pb2+; and the negative ions are mainly Cl, SO24  and F (Kesler
et al., 2007). In the field of geochemistry, numerous studies are
focused on the direct measurement technology for the chemical
composition and concentration of alkali metal ions and the nega-
tive ions in the fluid inclusion, as a result, it is relatively easy to
detect these ions; however, it is difficult to measure the concentra-
tion of its intrinsic ions in the inclusion directly, due to the lack of
proper techniques. Thus, an indirect method based on the grinding
of galena to release Pb in the fluid inclusions was used in the pres-
ent study.
For indirect measurement, the material was cleaned for 5 times
with ultrasonic and air-dried; the dried material was ground in a
mill (MM400, Retsch, Germany) with different times, at the same
vibration frequency of 900 min1, and then 2 g of the material with
40 ml pure deionized water was put into a centrifuge tube and
cleaned with ultrasonic for 1 min. When this cleaning process
was finished, a centrifuge (TL-4.7W, SCI, China) was used for
solid–liquid separation, with the separated liquid stored in closed
vials and analyzed for the total concentration of Pb and Cl by
96 S. Bai et al. / Minerals Engineering 45 (2013) 94–99
ICP-MS (ElAN-DRCII, PE, USA) and ion chromatograph (IC) (820–
413, waters, USA) directly with no acidification process.
All the above processes were conducted in a glove box under an
inert environment (i.e., argon saturated atmosphere), to avoid con-
tamination by atmosphere, and the experiments were carried out
at a room temperature of 25 °C. Pure deionized water with a resis-
tivity of 18 MX (Mill-Q5O, USA) was used throughout the
experiments.
2.2.4. Galena dissolution in pure deionized water
Before the dissolution, the material (4 g) from the largest grind-
ing time (12 min) was divided into two groups. One group (2 g)
was added to a centrifuge tube with 40 ml pure deionized water,
and then ultrasonic cleaning was performed for 1 min. The group
material after the ultrasonic cleaning process was performed in a
digital magnetic stirrer (DF-101S, Gongyi, China) with different
dissolution time for dissolution experiment. The other group
(2 g) with 40 ml pure deionized water was first centrifuged for
the solid–liquid separation, with the separated solid air-dried for
dissolution. Air-drying was conducted in a glove box under an inert
environment at a room temperature of 25 °C. With this process, the
Pb released from the fluid inclusion of galena during grinding was
removed and the effect of this Pb on the total concentration of Pb in
dissolution experiment was eliminated; then, the air-dried solid
with 40 ml pure deionized water was added to a 50 ml glass
beaker, followed by rapid magnetic stirring (1000 rpm) for the
dissolution experiment at different dissolution times. After the so-
lid–liquid separation, the separated liquid was stored in closed
vials and analyzed for the total concentration of Pb and Cl directly
with no acidification process.
Fig. 2. Morphology of galena from the infrared–ultraviolet microscope observation.
Fig. 3. SEM image of the galena inclusion traces.
The experiment process above was also conducted in a glove
box in an inert environment and carried out at a room temperature
of 25 °C and the pH of the pure deionized water is 6.80.
3. Results and discussion
3.1. Infrared–ultraviolet microscope imaging of galena fluid inclusion
The morphology of the fluid inclusion from the infrared–
ultraviolet microscope observation is shown in Fig. 2. In Fig. 2,
the surface and subsurface fluid inclusions traces of galena show
dark gray (Fig. 2b). Some microscopic minerals were generated
due to the reaction of the captured fluid and the host mineral;
these microscopic minerals easily absorbed infrared radiation, thus
causing the fluid inclusions to darken (Luders and Gutzmer, 1999).
The fluid inclusions trace presents itself as either oval shape with
clumping groups (Fig. 2a-1 and -2) or strip shape with isolated
position (Fig. 2b-3). Meanwhile, some of the inclusion trace has a
size of dozens of micron and are observable with naked eyes; how-
ever, some of the inclusions traces are small with a size of only a
few microns, and not observable even through microscope. Infra-
red–ultraviolet microscope imaging results show that fluid inclu-
sions do exist in this sample of galena and the number of fluid
inclusions is large.
3.2. SEM–EDS analysis of galena inclusion trace
The fracture surface morphology, after breaking the galena
inclusions, is shown in Fig. 3. There are numerous hollow regions,
which are caused by breaking the inclusions, present on the galena
 S. Bai et al. / Minerals Engineering 45 (2013) 94–99 97

fracture surface. These regions can be called the inclusion trace.
From the structure and morphology of the inclusion trace directly
observed using SEM, the galena inclusion traces present itself as
round shape, oval shape or irregular strip, which have a size range
from a few microns to dozens of micron. It can be concluded from
Fig. 3 that there are many fluid inclusions in this sample of galena.
Moreover, the results of SEM analysis are consistent with the re-
sults of IUM imaging with respect to the form and structure of nat-
ural galena fluid inclusion trace.
To prove that the hollow region present on the fracture surface
of galena is the inclusion traces, rather than scratches caused by
slicing the surface, EDS analysis was performed on the regions of

Fig. 4. EDS analysis results of galena inclusion traces for: (b) position (a) 1; (c) position (a) 2.
98 S. Bai et al. / Minerals Engineering 45 (2013) 94–99
the hollow. For comparison, region point analysis was performed
on the following locations: the flat area around the hollow regions
(Fig. 4a-1), and the hollow location (Fig. 4a-2), as shown in Fig. 4.
The EDS analysis results of galena inclusion traces indicated that
the flat area around the hollow regions consisted of Pb and S.
The mass fraction of Pb and S accounted for 85.25% and 14.76%,
respectively (Fig. 4b). These results were consistent with the theo-
retical composition of galena (Pb 86.40%, S 13.60%). The EDS anal-
ysis of hollow location found that Pb was the main composition
element, and accounted for 73.01% of the total elemental composi-
tion. The other composition elements consisted mainly of O and C,
respectively (Fig. 4c). For the composition of hollow location in
inclusion trace, the Pb content was found to be 13.39% less than
the theoretical composition of galena. Such a phenomenon may
be due to the possibility that the galena inclusion surface had been
oxidized and that the Pb entered into the fluid inclusion during the
ore-forming process of the galena. The EDS analysis results show
that the hollow regions were not caused by slicing the surface
but existed naturally and the hollow region was preserved after
breaking the inclusions. Fluid inclusions contain gas as well as li-
quid and that some ions are released into solution and others are
adsorbed on the inclusion interface after volatilization. Although
these conclusions have been obtained by many researchers, more
attention has been paid to the metallogenic conditions and pros-
pects for finding mineral resources (Charef and Sheppared, 1987;
Crawford, 1981; Czamanske et al., 1963). Therefore, there are not
many studies on the release of these ions from fluid inclusions in
galena and whether these ‘‘unavoidable ions’’ have effects on the
froth flotation solution. To address this issue, we investigated the
components released from fluid inclusions in galena in order to
evaluate a potentially important new source of the ‘‘unavoidable
ions’’ found in the galena flotation solution.
3.3. Concentration of Pb and Cl released from galena fluid inclusions
The ICP-MS and IC have been respectively used to measure the
concentration of lead released from the fluid inclusions and the
lead dissolved from galena and Cl released from the fluid inclu-
sions of galena during the grinding process. The results are shown
in Table 2.
As shown in Table 2, the total concentration of lead (CPbT) in the
aqueous solution increased with an increase in grinding time.
When the grinding time was increased from 4 to 12 min, the CPbT
increased from 2.13  106 to 8.25  106 mol/L. Numerous Cl
ions were also present in the aqueous solution. The absence of
Cl in the pure deionized water suggested that Cl must come from
the release of Cl ions in the fluid inclusions. The presence of Cl in
the aqueous solution provided powerful evidence for the release of
the fluid inclusion composition elements into the aqueous solu-
tion. The concentration of Cl in the solution decreased signifi-
cantly with the increase in grinding time. Such a phenomenon
may be explained by the formation reactions of lead-chloro com-
plexes. This process is expressed in Eq. (1) (Zheng, 1981).
2þ  60
Pb þ nCl ¼ ½PbCln 2n ðn ¼ 1; 2; 3Þ
Table 2
Concentration of Pb and Cl released from the galena fluid inclusions.
Grinding time (min) Concentration (106 mol/L)

Pb Cl
4 2.13 90.85
6 3.88 80.54
8 4.32 53.42
10 6.54 45.78
12 8.25 35.43
This suggests that Pb2+ in the aqueous chloride solution may be
present in the form of cationic, neutral or anionic chloro-com-
plexes, once the lead-chloro complexes formed, the element Cl
would no longer be detected by IC. This suggests that the lead con-
centration increased with the increase in the liberation degrees of
the fluid inclusion and the grinding fineness, while Cl concentra-
tion decreased with the increase in the liberation degrees of the
fluid inclusion. Therefore, it can be concluded that the lead dis-
solved from galena and components released from the fluid inclu-
sion can enter into flotation solution and become the ‘‘unavoidable
ions’’ found in the flotation pulp.
3.4. Dissolution of galena in pure deionized water
3.4.1. Effect of dissolution time
The dissolution experiments of galena were conducted in pure
deionized water (pH = 6.80) with a grinding time of 12 min and
in the absence of oxygen condition. The results of dissolution char-
acteristics based on different dissolution durations are illustrated
in Table 3. It can be seen from Table 3 that the experimental CPbT
decreased with the increase of dissolution time. The Pb may have
been derived from the dissolution of the galena or the release of
ions from the fluid inclusions. When the dissolution time was in-
creased from 0 to 300 min, the experimental CPbT decreased from
8.13  106 mol/L to 6.15  106 mol/L. The similar values of lead
released from the fluid inclusions (Table 2) and in the dissolution
experiments which include both the lead in fluid inclusions and ga-
lena lattice (Table 3) suggest that that the majority of Pb found in
the aqueous solution were released directly from the fluid inclu-
sions, rather than during the mechanical dissolution of the galena.
Therefore, it can be concluded that the Pb released from the fluid
inclusions is an important source of the ‘‘unavoidable ions’’ in
the flotation pulp.
3.4.2. Galena dissolution after removing released component of fluid
inclusions
In order to further verify the source of Pb in the aqueous solu-
tion, the dissolution of galena (ground for 12 min and after re-
moval of the components released from fluid inclusions) in pure
deionized water and in the absence of oxygen condition was inves-
tigated. As shown in Table 4, the CPbT and Cl concentration are
only 1.12  106 mol/L and 21.71  106 mol/L, respectively. How-
ever, the data in Table 2 indicated that the CPbT and Cl concentra-
tion in the aqueous solution at the same grinding time reached
Table 3
Dissolution experiments of galena (conditions: a grind-
ing time of 12 min and in the absence of oxygen).
Dissolution Concentration
time (min) (106 mol/L)
Pb
0 8.13
30 8.01
7.12
ð1Þ 180 6.84
300 6.15
Table 4
Experimental total concentration of Pb and Cl (conditions: a grinding time of 12 min
and in the absence of oxygen).
Grinding Dissolution pH Experimental Chloride
time (min) time (min) CPbT (mol/L) concentration
(106 mol/L)
12 180 6.8 1.12  106 21.71
 S. Bai et al. / Minerals Engineering 45 (2013) 94–99
8.25  106 mol/L and 35.43  106 mol/L. Both were much higher
concentrations than those found in the dissolution experiment.
Thus, it is concluded that the majority of Pb and Cl most likely
came from the release of mineral fluid inclusions rather than from
the galena dissolution.
4. Conclusions
On the basis of the results of the present investigation, the fol-
lowing conclusions have been drawn:
(1) Analysis results of IUM and SEM–EDS indicate many fluid
inclusions with a size range from a few microns to dozens
of micron exist in the galena; and the composition of galena
inclusion trace is characterized by lower Pb content compare
to the theoretical composition of galena.
(2) The compositions of fluid inclusions in galena are rich in Pb
and Cl, and they will be released into solution when the
fluid inclusions are liberated. The Pb concentration increases
and Cl concentration decreases with the increase in the lib-
eration degree of the fluid inclusion. These compositions
become ‘‘unavoidable ions’’ in the flotation pulp. The main
source of ‘‘unavoidable ions’’ in solution is not the dissolu-
tion of the galena, but the release of fluid inclusions in the
minerals.
(3) The component released from fluid inclusions presents an
important new source of unavoidable ions in galena flotation
pulp, and this provides a new understanding on the resource
of the unavoidable ions in the flotation pulp and also would
present a significant importance for the environmental
geochemistry.
Acknowledgements
This research project were supported by the Key Program of the
National Natural Science Foundation of China (Grant No.
u0837602) and the Analysis and Testing Foundation of Kunming
University of Science and Technology (Grant No. 2011-470), and
the authors are grateful to the State Key Laboratory for Mineral
Deposit Research Institute of Geo-Fluids in Nanjing University for
its technical support.
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