Professional Documents
Culture Documents
Department of Mining and Materials Engineering, McGill University, 3610 University Street, Montreal, Quebec H3A OC5, Canada
SGS Canada Inc., 185 Concession Street, PO 4300 Lakeeld, Ontario K0L 2H0, Canada
a r t i c l e
i n f o
Article history:
Received 18 October 2014
Received in revised form 24 March 2015
Accepted 13 April 2015
Available online 24 April 2015
Keywords:
Muscovite
Flotation
Zeta potential
QEMSCAN
Electroacoustics
Mica
a b s t r a c t
Muscovite mica is a naturally occurring phyllosilicate mineral with a wide range of industrial applications. This work investigated the separation of muscovite from unwanted gangue minerals in a mica
ore. Electroacoustic zeta potential measurements and single mineral otation tests were used to determine the effect of Custamine 8113 (collector) and Norlig-H (depressant) on muscovite. These results were
then compared to those of gangue minerals (feldspar and quartz). Muscovite showed an isoelectric point
(IEP) at pH 3.5. Feldspar and quartz did not have an IEP, having negative zeta potentials over the pH range
investigated (pH 310). This suggests that effective separation using a cationic amine collector, which
relies on electrostatic attraction as the basic mechanism of adsorption onto mineral surfaces, would
not be possible without the use of a depressant. Zeta potential measurements and single mineral otation
tests in the presence of both Custamine 8113 and Norlig-H indicate that reagent adsorption is controlled
by Custamine 8113 in the case of muscovite and by Norlig-H in the case of feldspar and quartz. This suggests that effective separation of muscovite from the gangue minerals present in the mica ore is possible.
These results were used to determine optimal otation conditions of the ore. Concentrates from the ore
otation were examined by QEMSCAN analysis, which showed that muscovite was effectively separated
from gangue minerals.
2015 Elsevier B.V. All rights reserved.
1. Introduction
1.1. Muscovite
1.2. Surface chemistry
Micas are a group of phyllosilicate minerals distinguished by
their close to perfect basal cleavage. They are widespread in
igneous, sedimentary and metamorphic rocks and their crystal
structure incorporates a large number of elements, leading to a
large and diverse mineral group. Of the many different minerals
in the mica family, muscovite (KAl2(AlSi3O10)(OH)2) is the most
common, and its physical properties render it useful in a wide
range of applications, such as: insulators; condensers; plastics;
cosmetics; and paints [13]. Muscovite is primarily separated from
common gangue minerals such as quartz and feldspar, taking
advantage of differences in physical properties [3]. These methods,
however, prove to be ineffective when dealing with small particle
sizes and therefore froth otation is used [1,3]. Froth otation may
217
Table 1
Reagents from the mica mine.
Reagent name
Reagent type
Manufacturer
Custamine 8113
Norlig-H
Cp-102a
Caustic
Collector/Frother
Depressant
Frother
pH Modier
ArrMaz
LignoTech
ArrMaz
OxyChem
218
Table 2
Particle size, surface area and electroacoustic measurement concentration for
muscovite, feldspar and quartz.
Mineral
d50 (lm)
Muscovite
Feldspar
Quartz
5.0
8.7
4.1
9.67
1.88
3.59
10.0
5.0
2.5
Table 3
Electroacoustic reagent dosages for muscovite, feldspar and quartz.
Mineral
Reagent
Dosage (g/g)
Dosage (g/L)
Dosage (g/m2)
Muscovite
Custamine 8113
Norlig-H
4.10 103
4.10 102
4.36 101
4.36 100
4.24 104
4.24 103
Feldspar
Custamine 8113
Norlig-H
4.10 103
4.10 102
2.07 101
2.07 100
2.19 103
2.19 102
Custamine 8113
Norlig-H
4.10 103
4.10 102
1.01 101
1.01 100
1.14 103
1.14 102
Quartz
found to be appropriate for muscovite, quartz and feldspar to represent the variation of zeta potential with pH. The condence
intervals indicate the degree of condence that the tted trendline
accurately represents the mean of the electroacoustic measurements. While this approach adequately describes the experimental
observations it was decided to utilize a prediction interval about
the trendline to be absolutely certain that observed deviations in
zeta potential were in fact signicant. The prediction interval
indicates the degree of condence (95% condence) with which
one may use the trendline to predict a future zeta potential measurement. Figs. 38 are reproduced in Appendix A (Figs. A4A9)
with the condence intervals about the trendlines replaced with
prediction intervals. Further explanation of the approach used
to calculate the prediction intervals is also included in the
Appendix.
Table 4
Conditions of mica ore otation tests.
Condition
Norlig-H (g/t)
1
2
3
500
500
250
1500
0
1500
2.5. QEMSCAN
In order to quantify the otation behavior of the mica and associated minerals of the ore body the mineralogy of concentrate and
tailings fractions should be measured. Quantitative evaluation of
materials by scanning electron microscopy (QEMSCAN) was used
in this work to determine the mineral abundance of muscovite
and gangue minerals in the feed and in the otation concentrates.
QEMSCAN is a mineralogical characterisation technique employing
an EVO 430 automated scanning electron microscope equipped
with four light-element energy-dispersive X-ray spectrometers
and iDiscover software for data and image processing. QEMSCAN
measures (and the iDiscover software processes) data from every
pixel across a sample with a pixel size dened based on the scope
of the analysis. The software assigns each pixel a mineral name
based on 1000 counts of energy dispersive X-ray spectral data
and backscatter electron intensities. If the minerals or constituent
phases comprising the sample are chemically distinct, QEMSCAN is
capable of reliably discriminating and quantifying minerals [63] by
comparing the data from each pixel to a set of mineral denitions
which are validated and rened to t the particular sample set
under investigation.
Samples prepared for QEMSCAN analysis included the feed as
well as representative samples of the combined concentrate from
each otation condition used during the ore otation experiments.
Each sample was screened and re-combined into three size fractions (+75 lm, 75/+38 lm, 38 lm) for a more detailed mineralogical determination to assess potential metallurgical
beneciation performance. These samples were prepared as polished sections and analyzed by QEMSCAN at the Advanced
Mineralogy Facility at SGS Canada (Lakeeld).
A micro-rifed, representative aliquot was obtained from each
fraction for whole rock compositional analysis by X-ray uorescence followed by preparation of the polished sections required
for QEMSCAN analysis. Graphite was added to disperse particles,
create random orientation and minimise density-induced particle
segregation, settling and preferred orientation. The samples were
mounted into an epoxy approximately 5 mm deep, and then backlled with epoxy. This shallow depth was selected to minimise
gravity separation during epoxy hardening. After hardening, the
sections were ground, polished, carbon-coated, and analyzed utilizing QEMSCAN. Two polished sections were prepared from the
+75 and one from each of the 75/+38 lm and 38 lm fractions
from each sample.
The samples were analyzed using the Particle Mineral Analysis
(PMA) QEMSCAN method. The PMA is a two-dimensional mapping
analysis aimed at resolving liberation characteristics of a set of particles. A pre-dened number of particles were mapped at a pixel
size of 3 lm. The QEMSCAN instrument was operated at a 25 kV
accelerating voltage and a 5 nA beam current. A reference mineral
list was developed using XRD (primarily to dene the major minerals) as well as a scanning electron microscope (SEM) equipped
with an energy dispersive spectrometer (SEMEDS). To verify the
broad mineral composition and improve the mineral database
SEMEDS analysis was employed as needed. For data validation
purposes, the calculated assays using QEMSCAN were compared
to chemical assays using X-ray uorescence (XRF). The chemical
analyses completed were conducted at SGS Canada (Lakeeld).
219
Fig. 1. Zeta potential trend of muscovite, feldspar and quartz in 103 mol/L KCl
(Error intervals shown are 99% condence intervals).
220
Fig. 2. Zeta potential trend of muscovite with and without Custamine 8113 and
Norlig H (Error intervals shown are 99% condence intervals).
Fig. 3. Zeta potential trend of feldspar with and without Custamine 8113 and Norlig
H (Error intervals shown are 99% condence intervals).
Fig. 4. Zeta potential trend of quartz with and without Custamine 8113 and Norlig
H (Error intervals shown are 99% condence intervals).
Fig. 5. Zeta potential trend of muscovite with and without both Custamine 8113
and Norlig-H. The order of reagent addition is reected in the names of the trends
(Error intervals shown are 99% condence intervals).
Fig. 6. Zeta potential trend of feldspar with and without both Custamine 8113 and
Norlig-H. The order of reagent addition is reected in the names of the trends (Error
intervals shown are 99% condence intervals).
Fig. 7. Zeta potential trend of quartz with and without both Custamine 8113 and
Norlig-H. The order of reagent addition is reected in the names of the trends (Error
intervals shown are 99% condence intervals).
8113 alone. This indicates that muscovite has a higher afnity for
the collector compared to the depressant, whereas Figs. 6 and 7
show that feldspar and quartz have a higher afnity for Norlig-H,
indicating that selective separation of muscovite from feldspar
and quartz is possible. It is also interesting to note that the order
of addition of the two reagents shows little change in the zeta
potential trends, indicating the strong selectivity of Norlig-H for
both feldspar and quartz.
3.2. Single mineral otation
Results from the otation of muscovite are shown in Figs. 8 and
9. They indicate that effective otation is possible using Custamine
Fig. 8. Single mineral otation results for muscovite with constant Norlig-H
concentrations and varying concentrations of Custamine 8113 and pH (Error bars
represent 95% condence intervals).
221
Fig. 10. Single mineral otation results for quartz with varying concentrations of
Custamine 8113 and Norlig-H at a constant pH 7.5 (Error bars represent 95%
condence intervals).
Fig. 9. Single mineral otation results for muscovite with varying concentrations of
Custamine 8113 and Norlig-H at the natural pH 7.5 (Error bars represent 95%
condence intervals).
Fig. 11. Pure mineral otation results of muscovite and quartz as a function of time
in the presence of 250 g/t Custamine 8113 and 1500 g/t Norlig-H at pH 7.5 (error
bars represent 95% condence intervals).
222
Fig. 12. Mass recovery, from muscovite otation tests, after collecting froth for 30,
60 and 300 s (error bars represent 95% condence intervals).
above 250 g/t, similar to the results obtained from single mineral
otation tests.
3.4. QEMSCAN
The mineralogy of the feed sample is provided in Table 5. The
sample consists of quartz (62.2%), K-feldspar (19.6%), muscovite
(9.1%), plagioclase (5.6%), and trace/minor amounts of other minerals. The bulk composition of the feed sample was validated by XRD
analysis.
Table 5
Modal mineralogy of the feed sample.
Fraction
Mass size distribution (%)
Calculated ESD particle size
Combined
+75um
75/+38um
38um
20
Sample
62.2
5.58
19.6
0.37
9.08
0.58
1.68
0.80
0.05
0.08
49.0
37
Sample
33.7
2.09
6.70
0.08
5.47
0.35
0.36
0.27
0.01
0.01
Fraction
68.7
4.26
13.7
0.17
11.2
0.72
0.73
0.56
0.02
0.02
26.0
24
Sample
16.6
1.79
5.52
0.13
1.42
0.11
0.22
0.16
0.00
0.01
Fraction
64.0
6.90
21.2
0.52
5.48
0.42
0.83
0.62
0.01
0.05
25.0
11
Sample
11.9
1.70
7.40
0.16
2.18
0.12
1.11
0.37
0.03
0.06
Fraction
47.5
6.78
29.6
0.62
8.74
0.47
4.44
1.46
0.14
0.26
100.0
26.0
100.0
25.0
100.0
Quartz
Plagioclase
K-Feldspar
Oxides
Muscovite
Biotite
Epidote
Tourmaline
Other silicates
Other
Total
100.0
49.0
Quartz
Plagioclase
K-Feldspar
Oxides
Muscovite
Biotite
Epidote
Tourmaline
Other Silicates
Other
21
21
18
12
14
14
9
11
7
6
40
38
36
13
24
21
24
22
10
9
25
26
23
17
12
12
9
11
6
7
11
12
11
9
7
8
7
8
6
5
223
Fig. 14. Particle maps of muscovite middlings associated with quartz/feldspars from the +75 lm fraction.
Fig. 15. QEMSCAN results for the combined concentrates of the muscovite otation tests for (a) combined particle size and (b) +75 lm, (c) 3875 lm and (d) 38 lm
fractions. Custamine concentrations used were 500 g/t (High) and 250 g/t (Low) with Norlig-H (Depressant) added at a concentration of 1500 g/t.
Fig. 16. (a) Total mass recovery, grade (solid line) and recovery (dashed line) of (b) muscovite, (c) quartz and (d) feldspar for three different size fractions. Custamine
concentrations used were 500 g/t (High) and 250 g/t (Low) with Norlig-H (Depressant) added at a concentration of 1500 g/t. Feed denotes the ore prior to otation.
224
Fig. 17. Cumulative water recovery by volume (error bars represent 95% condence
intervals).
grades of 87%, 49% and 26%, respectively. This indicates that the
majority of the gangue recovery is occurring at ner particle sizes.
It is also interesting to note that the recovery of coarse (+75 lm)
quartz and feldspar is elevated at high collector dosage in the
absence of depressant. This suggests that without the addition of
a depressant a signicant amount of coarse gangue is recovered,
most likely via the otation of non-liberated particles containing
both mica and gangue mineral phases. Combining these data with
the high volumes of water being recovered in the concentrates
(Fig. 17), it is proposed that the ne gangue particles are entering
the concentrate via entrainment rather than by true otation.
Adding a de-sliming step to remove nes or adding a cleaner otation stage may further concentrate the muscovite. The addition of
traditional entrainment treatments such as wash water may also
help to reduce the recovery of ne gangue.
4. Conclusions
This work investigated the separation of muscovite from
unwanted gangue minerals in a mica ore. The investigation
included zeta-potential measurements and single mineral otation
tests of pure muscovite and gangue minerals, feldspar and quartz,
to understand reagent interactions at mineral particle surfaces and
evaluate otation responses in the presence of an amine collector,
Custamine 8113, and depressant, Norlig-H. These results were then
Acknowledgements
The authors would like to acknowledge funding from the
Natural Sciences and Engineering Research Council of Canada
(NSERC) Discovery Grant: Mineral Processing Fundamentals. A.
Jordens acknowledges funding from the McGill Engineering
Doctoral Award as well as an NSERC Alexander Graham Bell
Canada Graduate Scholarship. The authors also gratefully acknowledge helpful discussions with Prof. J.A. Finch and Prof. G.A.
Whitmore regarding the display of zeta potential data.
Appendix A
The construction of condence and prediction intervals for electroacoustic zeta potential as a function of the pH level requires the
following two assumptions to hold:
Table A1
QEMSCAN results for the combined concentrates of the muscovite otation tests.
Flotation sample
Mineral
+75um
75/+38um
38um
Feed
Muscovite
Quartz
Plagioclase
K-Feldspar
Other
9.08
62.17
5.58
19.61
3.57
11.16
68.70
4.26
13.67
2.21
5.48
63.97
6.90
21.22
2.44
8.74
47.51
6.78
29.58
7.39
Muscovite
Quartz
Plagioclase
K-Feldspar
Other
27.45
38.11
3.82
25.14
5.48
62.62
21.56
1.17
9.60
5.06
17.36
43.78
4.56
28.55
5.74
11.13
45.56
5.06
32.61
5.63
Muscovite
Quartz
Plagioclase
K-Feldspar
Other
11.67
58.57
5.18
21.99
2.60
14.74
62.78
4.04
16.94
1.50
7.72
61.60
6.14
22.12
2.42
7.77
49.69
6.83
31.07
4.64
Muscovite
Quartz
Plagioclase
K-Feldspar
Other
52.68
16.57
2.02
20.22
8.51
86.66
3.70
0.04
3.02
6.57
48.80
16.47
2.12
22.92
9.68
25.95
27.24
3.63
33.49
9.69
Fig. A1. Zeta potential data for muscovite as a function of pH along with tted third
order polynomial trendline. Condence interval [CI] (99% condence) and prediction interval [PI] (95% condence) are shown about the trendline.
225
Fig. A5. Zeta potential trend of feldspar with and without Custamine 8113 and
Norlig-H (Error intervals shown are 99% prediction intervals).
Fig. A2. Zeta potential trend for muscovite at three different solids concentrations
(Error intervals shown are 99% condence intervals).
Fig. A6. Zeta potential trend of quartz with and without Custamine 8113 and
Norlig-H (Error intervals shown are 99% prediction intervals).
Fig. A3. Zeta potential trend for feldspar before and after heating (Error intervals
shown are 99% condence intervals).
Fig. A7. Zeta potential trend of muscovite with and without both Custamine 8113
and Norlig-H. The order of reagent addition is reected in the names of the trends.
(Error intervals shown are 99% prediction intervals).
Fig. A4. Zeta potential trend of muscovite with and without Custamine 8113 and
Norlig-H (Error intervals shown are 99% prediction intervals).
Fig. A8. Zeta potential trend of feldspar with and without both Custamine 8113 and
Norlig-H. The order of reagent addition is reected in the names of the trends. (Error
intervals shown are 95% prediction intervals).
226
Fig. A9. Zeta potential trend of quartz with and without both Custamine 8113 and
Norlig-H. The order of reagent addition is reected in the names of the trends. (Error
intervals shown are 95% prediction intervals).
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s2 Y 0 I XX 0 X X 0 Y=n k
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