Journal of Materials Processing Technology 74 (1998) 243 – 250

Rhenium recovery from Sarcheshmeh molybdenite concentrate

M.H. Shariat a,*, M. Hassani b
a
Department of Materials Science and Engineering, School of Engineering, Shiraz Uni6ersity, Shiraz, Iran
b
Training Department, Sarcheshmeh Copper Complex, Kerman, Iran

Received 17 September 1996

Abstract

Rhenium, in the form of ammonium perrhenate was recovered from Sarcheshmeh molybdenite concentrates by roasting the
concentrates with slaked lime. The effect of the roasting parameters, such as roasting temperature, roasting materials and gas
composition was investigated. The roasted materials were leached with water in order to separate the water-soluble calcium
perrhenate and the water-insoluble compounds, calcium molybdate and calcium sulfate, that were formed during roasting. Impure
rhenium-bearing solution was passed through a column of strong anionic quaternary resin (Dow IRA 410) for selective absorption
of rhenium ions from the solution. Stripping of the column was carried out with hypochloric acid. The resultant perrhenic acid
solution was exposed to hydrogen sulfide gas in order to precipitate rhenium heptasulfide. To produce ammonium perrhenate, the
sulfide was decomposed by ammonia in the presence of hydrogen peroxide. The solution was evaporated and ammonium
perrhenate crystals were formed. © 1998 Elsevier Science S.A.

Keywords: Ammonium perrhenate; Molybdenite concentrates; Roasting

1. Introduction conventional roasting of molybdenite concentrates un-

der normal conditions, rhenium converts to gaseous
Rhenium is recovered from molybdenite concentrates rhenium heptaoxide [7]. On the other hand the solids
through roasting or direct reduction of the concentrates products of the roasting of rhenium containing molyb-
[1]. Roasting of the concentrates can be carried out in denite with slaked lime are water-insoluble calcium
conventional roasting furnaces [2,3] or in muffle fur- sulphate CaSO4 and calcium molybdate CaMoO4 and
naces in the presence of slaked lime [4]. The conven- water-soluble calcium perrhenate Ca(ReO4)2. The possi-
tional roasting reactions are [5,6]: ble reactions that are taking place during roasting with
slaked lime are [4]:
MoS2 + 3O2 =MoO2 +2SO2 (1)
MoO2 +1/2O2 =MoO3 (2) MoS2 + Ca(OH)2 + 7/2O2 = CaMoO4 + 2SO2 + H2O
(6)
Re2S7 +10O2 =2ReO3 +7SO2 (3)
MoS2 + 2Ca(OH)2 + 4O2
ReS2 + 7/2O2 = ReO3 +2SO2 (4)
= CaMoO4 + CaSO4 + SO2 + 2H2O (7)
2ReO3 + 1/2O2 = Re2O7 (5)
Investigation of stability diagrams (Kellogg’s dia- MoS2 + 3Ca(OH)2 + 9/2O2
gram) for Mo –O –S and Re – O – S systems (Fig. 1) = CaMoO4 + 2CaSO4 + 3H2O (8)
show that MoO3 and ReO3 will form under normal
roasting conditions (the same PSO2, PO2 and T). Ac- Re2S7 + Ca(OH)2 + 21/2O2
cording to the diagram, MoS2 can not be converted to
= Ca(ReO4)2 + 7SO2 + H2O (9)
MoO3, and Re2S7 and ReS2 to Re2O7 directly. In the
Re2S7 + 2Ca(OH)2 + 11O2
* Corresponding author. = Ca(ReO4)2 + CaSO4 + 6SO2 + 2H2O (10)

0924-0136/98/$19.00 © 1998 Elsevier Science S.A. All rights reserved.

PII S 0 9 2 4 - 0 1 3 6 ( 9 7 ) 0 0 2 7 7 - X
244 M.H. Shariat, M. Hassani / Journal of Materials Processing Technology 74 (1998) 243–250

Re2S7 +8Ca(OH)2 + 14O2 Table 1

Chemical analysis of the Sarcheshmeh molybdenite concentrates
= Ca(ReO4)2 + 7CaSO4 +8H2O (11) (wt%)

2ReS2 +Ca(OH)2 +15/2O2 Element A B C

= Ca(ReO4)2 + 4SO2 +H2O (12)
Mo 52.22 56.78 54.72
2ReS2 +2Ca(OH)2 +8O2 Re 0.08 0.11 0.09
Fe 2.0 0.8 1.25
= Ca(ReO4)2 + CaSO4 +3SO2 +2H2O (13) Cu 1.4 0.7 1.15
Pb — 0.02 —
2ReS2 +5Ca(OH)2 +19/2O2 S 37.44 38.7 38.3
Insoluble 4.9 2.0 2.4
= Ca(ReO4)2 + 4CaSO4 +5H2O (14)
Oil Balance Balance Balance
The rhenium content of Sarcheshmeh molybdenite
Values are in wt.%.
concentrates is about 800 – 1100 ppm [8]. Table 1 illus-
trates three different analyses of the molybdenite con-
centrates (at different times). mesh (37m). The particle size of the lime and the slaked
lime used were also in the same range. They were mixed
in the desired proportion and were changed to a stain-
2. Experimental procedure less steel (316 l) rotating reactor with an internal diame-
ter of 10 cm and a length of 20 cm. The reactor
2.1. Materials and equipment capacity was about 400 g and was connected to a
low-gear electric motor with a 2.5 cm diameter stainless
The molybdenite used in this work was recovered steel tube and rotated at 20 rpm. Air or oxygen-en-
from copper concentrate by selective flotation in riched air, which could be passed through a pre-heat
Sarcheshmeh and its particle size was almost − 400 pipe, was fed to the reactor through a 0.3 cm 316 l
stainless steel tube. An electric furnace of 9 kW capac-
ity (Carbolite GPF 14/30) was used to heat the charged
materials in the reactor. A JEOL (JDX-8030 Model
DX-JE-2PC) X-ray diffractometer was used for chemi-
cal and mineralogical analysis, while a Varian A.A.
1275 analyzer was used for quantitative wet chemical
analysis. An ARL direct current plasma spectrometer
DCP (SS-7ARL) was used for quantitative wet chemi-
cal analysis, for high precision at lower limits, as re-
quired.

2.2. Roasting

The effect of various parameters such as the type of

reagent used (Ca(OH)2 or CaO), the composition of the
materials to be roasted, the roasting temperature and
the gas composition on the final product was investi-
gated. The temperature variations in the reactor were
recorded using an alumel chromel thermocouple and
are shown in Figs. 2 and 3. These variations showed
that for a particular furnace temperature, the tempera-
ture of the reactor increased almost linearly, but at
temperatures of around 500°C a little reduction in
reactor temperature was observed, probably due to the
decomposition of slaked lime according to the follow-
ing endothermic reaction:

Ca(OH)2 = CaO+ H2O (15)

This idea seems to be correct, because when lime was

used instead of slaked lime, this region disappeared
Fig. 1. The stability diagrams of Mo and Re. completely, as shown by comparison of Figs. 2 and 3.
 M.H. Shariat, M. Hassani / Journal of Materials Processing Technology 74 (1998) 243–250
Fig. 2. The temperature variation in the reactor when slaked lime is
used as a reagent (furnace temperature 550°C).
Subsequently, the temperature of the reactor increased
and reached a maximum that was greater than the
temperature of the furnace, due to the exothermic
roasting reactions occurring inside the reactor. At the
end of the reactions, the temperature of the reactor
decreased to the furnace temperature. The experiments
showed that the behavior of molybdenum and rhenium
in roasting reactions is alike, i.e. the products are either
calcium molybdate and calcium perrhenate or molybde-
num oxides and rhenium oxides. As the low rhenium
content of molybdenite concentrate is difficult to detect
with X-ray diffraction, it was assumed that, in composi-
tional analysis by XRD, if calcium molybdate is de-
tected, it means that calcium perrhenate has also been
produced; whilst if molybdenum oxides are detected, it
means that rhenium oxides have also been developed.
The roasted materials were composed of water-soluble
calcium perrhenate and water-insoluble calcium molyb-
date and calcium sulfate. Thus, they could be leached
with water to separate them. The parameters that were
altered during roasting were: (i) reagents, slaked lime or
lime; (ii) reagents ratio (Ca(OH)2:MoS2 or CaO:MoS2),
100, 150, and 200 wt.%; (iii) oxygen in roasting gas, 21,
40, 60, 80, and 97%; and (iv) roasting temperature, 550,
600, 650, 700 and 750°C.
Fig. 3. The temperature variation in the reactor when lime is used as
a reagent (furnace temperature 600°C).
245
2.3. Leaching
The roasted materials were mixed with water in a
suitable mixer to produce a slurry with the desired solid
density. The mixing time was dependent on the mixing
conditions, such as temperature, the rpm of the mixer,
and percentage of the solid materials in the slurry. This
time was found to be about 12 h at ambient tempera-
ture, for a slurry with 40% solid and vigorous stirring.
Higher temperatures needed less time. When leaching
was completed, the slurry was siphoned to a suitable
filter press. Air with a pressure about 15–20 kPa was
sent into the filter press chamber to filtrate the slurry,
until the produced cake was almost dried (about 10–
14% moisture). The cake was washed three to five times
and was filtered several times to remove any rhenium
ions trapped in the residue, and then was sent for
molybdenum trioxide production. The clarified solution
contained rhenium, calcium, molybdenum and copper
ions. Because of the high basicity of the solution due to
the presence of calcium ions, the presence of iron ions
in the solution was negligible, which helped the process
as the removal of iron from impure acidic solutions is
difficult. It is well known that to eliminate iron ions
from such solutions, it must be converted to a basic
solution by an alkali such as sodium hydroxide to
precipitate iron ions. For preventing the formation of
gelatinous iron compounds, the solution must be oxi-
dized [5,9]. However, as the leach solution is basic, all
of these steps are eliminated in the present study.
2.4. Ion exchange
The rhenium-bearing solution can be purified to ob-
tain a solution that can be converted to pure rhenium
salts. The pH of the solution must be about 9–12 [9]:
the higher this value, the more feasible is rhenium
absorption by the ion exchange process. A quaternary
strong anionic resin, Dow-IRA 410, was used for this
purpose. The resin absorbs rhenium ions more selec-
tively from the solution and the degree of absorption
increases with an increase in the basicity of the solu-
tion. Column preparation was started by: (a) weighing
a proper amount of dried resin; (b) soaking it in
deionized water for one or several days to achieve
maximum swelling of the resin; and (c) pouring the
resin into the column, which had layers of glass wool,
sea sand and glass wool at its bottom.
After charging the column it was be rinsed with 7 N
hydrochloric acid, distilled water and sodium hydroxide
(10% by wt.), respectively [9]. The clarified, impure, and
basic rhenium-bearing solution was vaporized to in-
crease the rhenium content to about 2 g l − 1. During
vaporization some calcium salts precipitated, the solu-
246 M.H. Shariat, M. Hassani / Journal of Materials Processing Technology 74 (1998) 243–250

tion was filtered to remove any calcium residue. The

solution was passed through the column at the rate of
4 cm3 cm − 3 of resin per h. The rhenium ions were
absorbed by the resin and the effluent was free from
any rhenium ions. When the rhenium break-through
point was reached, i.e. the resin was saturated with
rhenium ions, the column operation was stopped. This
point was determined by analyzing the effluent solution
for rhenium ions. The column was rinsed with sodium
hydroxide (10% by wt.) and distilled water to remove
any other ions that had been absorbed by the resin,
such as molybdenum ions, or ions entrapped mechani-
cally by the resin. In this step, as shown by analysis,
any rhenium removal was at the trace level. Thereafter
the column was stripped by means of a suitable acid,
e.g. sulfuric, nitric, hydrochloric or perchloric acid.
Perchloric acid was more efficient. Rhenium thus leaves
the organic phase and comes into solution again,
where, as the solution characteristic is acidic, perrhenic
acid is formed.

2.5. Chemical reactions

The product was pure perrhenic acid. To produce

other rhenium compounds, e.g. rhenium heptasulfide, it
was necessary to pass hydrogen sulfide gas through the
perrhenic acid solution. Consequently, rhenium hepta-
sulfide was precipitated according to the following reac-
tion:
2HReO4 + 7H2S= Re2S7 +8H2O
Increasing the solution temperature to about 70°C
increases the rate of the reaction and produces coarser
precipitates [8]. Increasing the acidity of the solution
also effectively increases the reaction rate. For this
purpose, an acid such as hydrochloric or sulfuric acid is
needed to acidify the solution. Hydrogen sulfide gas is
produced by the following reaction:
Na2S+ 2HCl= H2S +2NaCl
a flask with a capacity of 5 l was used. A suitable
amount of sodium sulfide was put into the flask, and
then a 2N hydrochloric acid solution was gradually
poured in. The hydrogen sulfide gas produced was
passed through a PVC pipe to the vessel containing the
solution. Subsequently, brownish rhenium heptasulfide
was formed, the mixture being filtered and washed with
distilled water. Thus rhenium heptasulfide residue was
separated from the solution. The rhenium heptasulfide
was converted to ammonium perrhenate by ammonia
in the presence of an oxidizing agent such as hydrogen
peroxide, nitric acid, and oxygen. Hydrogen peroxide
was used as oxidizing agent, the products being ammo-
nium perrhenate and ammonium sulfate. The ammo-
nium perrhenate was selectively crystallized from the
solution by evaporation, the remaining liquor being
Fig. 4. Flow sheet of the process.
(16)
separated by decanting and filtration, and returned to
the rhenium heptasulfide precipitation step for recovery
of any left-over rhenium. Ammonium perrhenate crys-
tals, which are usually the starting material for the
production of other rhenium compounds and metallic
powder [10], can be recrystallized to ensure higher
purity, the flow-sheet of this procedure being shown in
Fig. 4.
(17)
3. Results and discussion
As stated earlier, in these experiments roasting of
molybdenite concentrates was accomplished by the use
of lime or slaked lime with oxygen enriched air, thus
the rhenium remained in the solid phase instead of in
the gas phase.
3.1. Effect of temperature and reagent percentages
Samples were prepared, each consisting of 133 g of
molybdenite and slaked lime in the proportion of 1:1,
2:3 and 1:2. These samples were roasted at different
temperatures of 550, 600, 650, 700 and 750°C. During
roasting all the reactions Eqs. (6)–(14) could happen,
 M.H. Shariat, M. Hassani / Journal of Materials Processing Technology 74 (1998) 243–250 247

depending on the lime-to-concentrates ratio and also on

the amount of oxygen present in the reactor. A greater
lime-to-concentrates ratio would produce more calcium
sulfate and less sulfur dioxide. On the other hand with
a higher oxygen percentage in the inlet gas, other
reactions resulting in the production of molybdenum
oxides and volatile rhenium heptaoxide could occur
(Eqs. (1)–(5)). The products at this stage were calcium
molybdate and calcium sulfate, and a minor amount of
calcium perrhenate in the solid state, while in the gas
phase, water vapor, sulfur dioxide and nitrogen were
the main products. By analysing the effluent gases to
determine their sulfur dioxide content, the type of
reaction occurring during roasting was recognized, i.e.
if the percentages of sulfur dioxide in the exit gas was
only at the trace level, the reaction was according to
Eqs. (8), (11) and (14), if SO2 in the exit gas is about 10
to 12%, the reactions are probably Eqs. (6), (9) and
(12). All of the roasted samples were analyzed with
XRD to specify the chemical composition of the Fig. 6. Effect of roasting reagents on the rhenium recovery (in air at
600°C).
roasted materials. The best conditions for roasting the
samples were based on the final products being only
higher at lower temperatures and at a low slaked-lime
calcium molybdate, calcium sulfate, and calcium per-
ratio. By increasing the roasting temperature, the
rhenate. Fig. 5 illustrates the variation in rhenium
affinity of rhenium and molybdenum to form calcium
recovery in the roasted products of different composi-
tions as a function of temperature. If molybdenum salts increases. To investigate the effect of the type of
oxide is detected in the products, it possibly means that reagents used in roasting on rhenium recovery, a series
volatile rhenium heptaoxide is also formed and hence of experiments were carried out in which instead of
the rhenium recovery is reduced. As is shown in Fig. 5, slaked lime, lime was used. As shown in Fig. 6, the
the maximum recovery is related to sample SR 2060 rhenium recovery was reduced. Figs. 7 and 8 show the
(SR wxyz is a code for a sample in which slaked lime is effect of the oxygen content of the roasting gas on the
(wx/10) times that of the concentrates and the roasting rhenium recovery and the roasting time. It is clear that
temperature is (yz× 10)) [11]. This could be due to the both the recovery and the roasting time decreased as
affinity of rhenium to form heptaoxide possibly being the percentage of oxygen in the incoming gas increased.

Fig. 5. Effect of roast composition and reactor temperature on the Fig. 7. Effect of the incoming gas composition on the rhenium
rhenium recovery. recovery for SR 2060.
248 M.H. Shariat, M. Hassani / Journal of Materials Processing Technology 74 (1998) 243–250

Fig. 8. Effect of the incoming gas composition on the reaction time Fig. 9. Effect of the solution flow rate in the absorbing column on the
for SR 2060. rhenium recovery.

3.2. Leaching and aqueous chemical reactions tion is at only trace level, it increased gradually during
the time of operation, resin saturation being reached
The solution after leaching was evaporated and ana- when the rhenium content of the effluent solution be-
lyzed, a typical analysis is shown in Table 2. The basic came considerable. After loading the resin column, it
rhenium-bearing solution contained about 1 – 2 g l − 1 was washed with sodium hydroxide solution (10% by
rhenium was passed through the column of Dow IRA wt.) to remove any molybdenum ions, and was then
410 resin at the rate of 4 cm3 cm − 3 resin per h, losing washed with distilled water. The amount of rhenium
all of the rhenium and becoming almost free of rhe- lost in this step was negligible. For stripping, (elution)
nium ions. 800 cm3 of 0.5 N hypochloric acid solution was chosen.
The flow rate of the solution through the column has As the experiment showed the rate of stripping was less
an effective role on the amount of rhenium absorbed, than the rate of loading. A flow rate of 2 cm3 cm − 3 of
and hence on the rhenium content of the effluent resin per h was chosen for the eluent solutions. After
solution. The effect of the solution flow rate on the
rhenium content of the effluent solution was examined,
the results being presented in Fig. 9. It can be seen that
the lowest effluent concentration of rhenium is achieved
at a flow rate of 4 cm3 cm − 3 of resin per h. In order to
find the efficiency of Dow-IRA 410 in rhenium adsorp-
tion, 800 cm3 of rhenium-bearing solution was poured
over the resin column (30 cm high and 2.6 cm diame-
ter). Samples of 100 cm3 volume were collected from
the bottom of the column and analyzed. Fig. 10 illus-
trates the variation of the rhenium content in the
effluent solution with respect to the volume of the
solution passed. It can be seen that the first 300 cm3 of
the solution do not show any rhenium whilst the rest
did. Although the rhenium content of the effluent solu-

Table 2
Analysis of the rhenium-bearing solution for the SR 2060 sample

Element Re Mo Ca Fe Cu As

g l−1 1.63 0.2 8.1 0.05 0.06 0.00 Fig. 10. Rhenium content of the effluent solution during the rhenium-
absorbtion step.
 M.H. Shariat, M. Hassani / Journal of Materials Processing Technology 74 (1998) 243–250
the column stripping was completed, the resulting solu-
tion was analyzed, and the total rhenium content of the
solution was found. Under these conditions the maxi-
mum rhenium recovery from the rhenium bearing solu-
tion was about 90%. As hydrogen sulfide gas was
introduced into the produced perrhenic acid solution,
which latter was acidified with hydrochloric acid, rhe-
nium heptasulfide precipitates were formed rapidly. Af-
ter washing, filtering and drying the precipitates, they
were weighted and recovery of 92% was recorded. To
produce ammonium perrhenate, rhenium heptasulfide
was oxidized and decomposed by a suitable amount of
hydrogen peroxide and ammonium hydroxide solution,
after which the solution was evaporated to produce a
saturated solution of rhenium. The rhenium concentra-
tion of the solution was about 20 g l − 1, i.e. the solution
volume decreased to about 60 cm3. The saturated am-
monium perrhenate solution was cooled, which resulted
in the formation of the ammonium perrhenate crystals.
After the crystals had been collected, they were dried
and weighed. The weight of ammonium perrhenate
crystals was about 1.42 g, which shows that some of the
rhenium compounds remained in the solution. These
solutions are usually returned to the previous steps. The
total efficiency of rhenium recovery based on 900 ppm
rhenium content of concentrate and 1.42 g NH4ReO4
produced from 1600 g molybdenite concentrate is about
70%.
4. Discussion
As shown in Fig. 6 the rhenium recovery is reduced
when lime is used instead of slaked lime. Also, during
the conversion of calcium hydroxide to calcium oxide
at a roasting temperature of 600°C, the agitation result-
ing from water vapor may possibly enhance the kinetics
of the reactions. For this reason, if lime is used as the
reagent, owing to the lower rate of conversion of
rhenium sulfides to calcium perrhenate, other possible
reactions such as the formation of rhenium heptaoxide
formation can take place simultaneously and, hence,
the rhenium recovery will be reduced. If nitric acid is
used as the oxidizing agent, in the oxidization of the
rhenium heptasulfide, the products are ammonium per-
rhenate, ammonium sulfate and ammonium nitrate,
according to the following reaction:
Re2S7 +18NH4OH + 16HNO3
= 2NH4ReO4 +7(NH4)2SO4 +2NH4NO3 +17H2O
+ 7N2O
Since ammonium perrhenate and ammonium nitrate
have the same properties, separating them from each
other would be difficult. If oxygen or hydrogen perox-
ide is used, the products are only ammonium perrhen-
249
ate and ammonium sulfate according to the following
reactions, which can be separated easily:
Re2S7 + 16NH4OH+ 14O2
= 2NH4ReO4 + 7(NH4)2SO4 + 8H2O (19)
Re2S7 + 16NH4OH+ 28H2O2
= 2NH4ReO4 + 7(NH4)2SO4 + 36H2O (20)
As using oxygen as the oxidizing agent usually re-
quires a high temperature and pressure, its use is lim-
ited, so that hydrogen peroxide is used for the
oxidation of the rhenium heptasulfide.
5. Conclusion
This study has shown that the roasting of molybden-
ite concentrates in the presence of slaked lime in excess
of the stoichiometric amount (about twice the weight of
the concentrates) enables the recovery of the rhenium
content of the concentrates with the efficiency of 85–
90%, and has also shown that the best roasting temper-
ature is about 600°C. Excess oxygen has a negative
effect on the rhenium recovery in this process. In the
ion-exchange step, a resin other than the usually-used
resin, Dow IRA 400, was used successfully, i.e. Dow
IRA 410. The best flow rate of the influent was found
to be 4 cm3 cm − 3 of resin per h. Also, in converting the
rhenium heptasulfide to ammonium perrhenate, hydro-
gen peroxide was used instead of nitric acid as a
reagent, hence preventing the formation of ammonium
nitrate. Finally, the total rhenium recovery was evalu-
ated to be about 70%. However, at pilot or industrial
scale, the total recovery will be greater, as most of the
discard solutions after the ion-exchange step can be
recycled.
Acknowledgements
The authors wish to express their gratitude to the
management of the Sarcheshmeh Copper Complex for
their generosity in providing all of the materials, equip-
ment and financial support required for this research.
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