Brazilian Bauxite Residue Physical–Chemical
Characterization and Acidic Neutralization
Potential
Patricia Magalhães Pereira Silva, Andre Luiz Vilaça do Carmo,
Roseanne Barata Holanda, Fernando Gama Gomes,
Emanuele Nogueira, Raphael Vieira da Costa, Caio César Amorim de
Melo, Adriano Reis Lucheta, and Marcelo Montini
Abstract
Physical-chemical evaluation of Brazilian (Amazon
region) bauxite residue (BR) and analysis of its acid
neutralization capacity (ANC) using, hydrochloric (HCl),
sulfuric acid (H2SO4) and citric acid (C3H8O7) were
carried out to assess the potential application of BR as soil
ameliorant. Analysis indicated a particle size average size
(D50) of 6.04 lm, 1.65 g cm−3 density and 18.28 mS
cm−1 electrical conductivity. Mineral phases determined
by XRD showed hematite, aluminous goethite, anatase,
sodalite, gibbsite and quartz, in agreement with XRF (%)
elemental characterization: Fe (24.38), Al (11.20), Si
(7.91), Na (8.11), Ti (3.24), Ca (0.79), Zr (0.71), S (0.06),
V (0.07) and Mn (0.09). ANC analyses conducted after
21 days indicated a lower acid consumption and pH
equilibrium for H2SO4 and HCl (1.75 and 1.00 mol
H+ kg−1, respectively and *pH8) when comparing with
C3H8O7 (2 mol H+ kg−1). Results validate and provide
basis for an effective use of BR in agronomic
applications.





Keywords
Neutralization Bauxite residue Mineral
biotechnology Green mining Environment
P. M. P. Silva
A. L. V. do Carmo
R. B. Holanda
F. G. Gomes

E. Nogueira
A. R. Lucheta (&)
SENAI Innovation Institute for Mineral Technologies, Avenida
Com. Brás de Aguiar, 548, Belém, PA 66035-450, Brazil
e-mail: adriano.isi@senaipa.org.br
R. V. da Costa
C. C. A. de Melo
M. Montini (&)
Hydro Alunorte S.A, Rodovia PA-481 km 12, Distrito de
Murucupe, Barcarena, PA 68447-000, Brazil
e-mail: marcelo.montini@hydro.com
© The Minerals, Metals & Materials Society 2020
A. Tomsett (ed.), Light Metals 2020, The Minerals, Metals & Materials Series,
https://doi.org/10.1007/978-3-030-36408-3_16
Introduction
Bauxite residue (BR) is a by-product of the Bayer process,
the most widely used for alumina production, where bauxite
ore is digested under pressure, at temperatures around
180 °C, using sodium hydroxide (NaOH). For each ton of
alumina produced, around 0.9–1.5 tons of BR are produced,
depending on the initial bauxite-ore grade and the Bayer
process efficiency. It is estimated that annual global BR
production is about of 150 million tons and there is a
worldwide inventory of over 4.6 billion tons [1, 2].
The BR has different mineral phases depending on the
bauxite origins and the Bayer process conditions. However,
regardless of the differences in bauxite ore and process
conditions, all BR is characterized by high alkalinity
(pH > 10), high electrical conductivity (0.7–18.2 mS cm−1),
clay-like texture, elevated sodium content (69%) and high
density (2.5 g cm3) [3, 4]. Generally, the main mineral
phases present in the BR inherited from the mother ore are
hematite (Fe2O3), diaspore (a-AlO(OH), boehmite (c-AlO
(OH) or gibbsite (Al(OH)3); goethite (FeO(OH)), quartz
(SiO2), anatase/rutile (TiO2), among others.
In addition, the Bayer process conditions also include the
presence of alkaline phases such as sodium hydroxide
(NaOH), sodium carbonates (Na2CO3), sodium aluminate
(NaAl(OH)4). Besides, sodium silicate (Na2SiO3), zeolite
sodium hydrate and amorphous aluminosilicates. Desilica-
tion products (DSP) are formed within the Bayer process
through reactions with reactive silica (kaolinite) from the
bauxite ore. Bayer sodalite (Na6Al6Si6O24
Na2CO3
yH2O) is
the main DSP formed and it has a zeolite type structure able
to incorporate sodium salts, carbonate, aluminate, and
hydroxide ions, all of which are common anion impurities in
the Bayer liquor. Incorporated ions inside Bayer sodalite,
when leached, have buffering capacity from approximately
pH 11–8.3, while the buffering capacity of DSP is around
pH 8 [5]. General neutralization reactions are described
below:
115
116
OH þ þ H þ ! H2 O ðbuffers at  pH 10:3Þ
AlðOHÞ
4 þH
þ
! AlðOH Þ þ H2 O ðbuffers at  pH 10Þ
CO2 þ
! HCO
3 þH 3 ðbuffers at  pH 8:3Þ
DSP (e.g. sodalite) dissolution:
Na6 Al6 Si6 O24
Na2 CO3:
yH2 O þ 18H2 O þ 7H þ
 8Na þ þ 6AlðOHÞ3 þ 6SiðOHÞ4
þ HCO
3 þ yH2 O ðbuffers at  pH 8Þ
The high inherent BR alkalinity may cause equipment
corrosion and handling risks, thereby limiting its untreated
direct utilization in agriculture and as building materials. It is
also difficult to use as a secondary source of raw material for
iron, titanium or rare earth elements (REE) exploration. Partial
pH neutralization can change BR properties facilitating its
utilization [6]. However, prior to developing a neutralization
strategy, it is important to determine the BR acid neutraliza-
tion capacity (ANC), estimate the acid consumption and the
buffering levels. ANC is the capacity of a chemical system to
react after adding strong or weak acid. The mechanism is the
reaction between the acid and any Bronsted bases, such as:
 2þ
HCO 2
3 ; CO3 ; BðOHÞ ; AlðOHÞ ; AlðOHÞ4 or organic
acid anions that might be present in the system [7]. Thus, to
obtain the ANC for the BR, it is necessary to quantify how
many protons are needed to neutralize it as a function of the
added acid. The presence of buffering alkaline minerals (e.g.
sodalite, calcite, tricalcium aluminate) is the biggest struggle
for BR chemical neutralization. Snars and Gilkes [8] have
evaluated the ANC of BR samples from several countries over
a 28-day periods, including from Brazil. The buffering
capacity of the evaluated BR varied between pH 8.5 and 4.5
and it was a function of the mineral phases present and BR
origin (Bayer process conditions) [8].
In the present work, a Brazilian BR sample was physi-
cally, chemically and mineralogically characterized.
The ANC curves were determined using three acids (hy-
drochloric, sulfuric and citric). This study will generate basis
for the development of low-cost biotechnological neutral-
ization methods that may enable the future residue utilization
in agriculture as a soil conditioner.
Materials and Methods
Bauxite Residue (BR) Physic-Chemical
and Mineralogical Characterization
The BR sample was received at the SENAI Innovation
Institute for Mineral Technologies, in Brazil, where the
study was conducted. The sample was dried at 96 °C during
P. M. P. Silva et al.
24 h, disaggregated, and ground in an agate mortar and
pestle. Elemental composition was determined by energy
dispersive X-ray fluorescence (EDXRF) (Epsilon 3XLE,
PANalytical Spectrometer) using an X-ray Rhodium
(Rh) tube, and anode at 1.5 W. Mineral phases were deter-
mined by X-ray diffraction (XRD) (Empyrean; PANalytical
Diffractometer, Almelo, The Netherlands). Powder XRD
patterns were obtained (4°–75°2h, 40 mA, 40 kV, Ka
1.54 Å, step size 0.02°, 55 s/step). Particle size distribution
was determined by Laser Diffraction using a Mastersize
3000 (Malvern-PANalytical) equipment and water as dis-
persant (RI = 1.33), particle refractive index (RI) = 2.25,
and particle density = 1.56 g cm−3. Electrical Conductivity
(EC) and Hydrogen Potential (pH) were determined in a 1:1
(BR:distilled water, w/v) solution in a HI Edge 2020 EC
meter (Hanna Inst.) and in a Orion Star A211 pHmeter
(Thermo Scientific), respectively, whereas density was
determined by gravimetric method using a lab analytical
balance (Mettler Toledo).
Acid Neutralization Capacity (ANC)
The BR ANC curves were determined using hydrochloric
acid (HCl, 0.5 mol L−1), sulfuric acid (H2SO4, 0.25 mol
L−1), and citric acid (C6H8O7, 0.1667 mol L−1) separately,
according to a modified Snars and Gilkes [8] protocol. 30 g
of BR were weighed and transferred into 175 mL
polypropylene capped bottles. Deionized water and several
7.5 mL (0.025 mol L−1) acidic inputs were added to the
bottles to completed a 150 mL final volume, until reaching
150 mL of acid (2 mol H+ kg−1) (Fig. 1). A blank sample
was prepared by adding 150 mL of distilled water to 30 g of
BR, (Fig. 1). Suspensions were manually shaken for 1 min,
and then pH (Thermo Scientific, Orion Star A211 pHmeter)
was immediately measured. Subsequently, the flasks were
transferred to a mechanical agitator (Eppendorf, Innova 44)
operating at 130 rpm (30 °C), and supernatant pH was
measured after 4 h, 1 day, 3 days, 7 days, and 21 days.
Results and Discussion
BR Sample Characterization
A BR sample diffractogram is shown in Fig. 2. The main
phases identified in BR sample were: hematite (Fe2O3),
anatase (TiO2), sodalite (Na8(AlSiO4)6Cl2), gibbsite (Al
(OH)3), quartz (SiO2) and aluminous goethite ((Fe, Al)
OOH). Several studies shown that hematite is present in all
bauxite residues [9–11]; other minerals commonly found
are: boehmite (c-AlOOH), gibbsite (Al(OH)3), anatase,
rutile/anatase (TiO2), ilmenite (FeTiO3), perovskite
Brazilian Bauxite Residue Physical–Chemical Characterization …
Fig. 1 Schematic procedure of
ANC determination with crescent
acid concentrations
Fig. 2 XRD diffractogram of BR
from Brazil. Sdl sodalite, Gbs
gibbsite, Al-Gth aluminous
goethite, Ant anatase, Hem
hematite, Qz quartz
(CaTiO3), and quartz (SiO2). The two main phases formed
during the Bayer process are sodalite (Na8(Al6Si6O24)Cl2)
and calcite (CaCO3), where sodalite is the most common
DSP forming mineral during pre-desilication [12]. Calcite
was not identified in the evaluated BR sample at the method
detection limit. Calcite absence may be associated to low
calcium input during the process.
BR chemical analysis is presented in Table 1. The major
BR constituent element was Fe (24.38%), followed by Al
(11.20%), Na (8.11%), Si (7.91%) and Ti (3.24%). Other
elements were also detected in BR at a lower percentage
(e.g. Ca, Zr, Mn and S). The presence of these elements
corroborate with XRD results, being mainly associated to
hematite (Fe), gibbsite or aluminous goethite (Al), sodalite
(Na, Al, Si) and quartz (Si). Similar chemical composition of
Brazilian BR samples was found by Snars et al. [8] and
Braga et al. [13]. The elements Fe and Al where described in
higher concentrations by Snars et al. [8] and may probably
be associated to differences in bauxite origins and industrial
process conditions.
Bauxite residue particle size distribution (PSD) is shown
in Fig. 3. The PSD analysis indicated that the BR is
117
dominated by a mixture of very fine particles. It was found
that 90% (D90) of particles were smaller than 22.5 µm, 50%
smaller than 6.04 µm (D50) and 10% smaller than 1.65 µm
(D10). An important remark is that the dominance of small
particles and desegregated structure of BR may negatively
impact its performance for agronomical application as it,
may result in soil capillarity clogging or, cause difficult with
water absorption and plant roots penetration.
pH, EC and ANC
The BR determined pH and EC were 10.4 and 18.28 mS
cm−1, respectively. These data confirm the high alkalinity
characteristic of BR due to the addition of sodium hydroxide
(NaOH), and presence of anions such as OH−, CO32−/
HCO3−, AlðOHÞ4  /Al(OH)3(aq) and H2SiO42−/H3SiO4−
[12]. The EC values described in the literature ranges from
1.4 to 28.4 mS cm−1 and correspond to the EC found for the
BR [12].
Usually ANC curves are determined using a strong acid,
such as HCl, as described by Snars and Gilkers [8]. In this
118 P. M. P. Silva et al.

Table 1 Chemical composition, % Elem. BR (this work) Braga et al. [13] Snars and Gilkes [8]
expressed as percentage element
(%) in the Brazilian bauxite Fe 24.38 23.08 31.89
residue samples Al 11.20 11.38 7.99
Na 8.11 6.97 5.56
Si 7.91 8.93 7.29
Ti 3.24 2.82 2.57
Ca 0.79 0.86 0.83
Zr 0.71 – –
Mn 0.09 – 0.01
V 0.07 – –
S 0.06 – 0.08
LOI 7.99 10.80 9.30
LOI Loss on ignition

Fig. 3 Particle size distribution of bauxite residue
work, a modified protocol was developed to allow ANC
curve determination using also H2SO4 and C6H8O7. These
acids were evaluated due to our interesting in a future partial
neutralization of BR by using biotechnologically produced
sulfuric and organic acids by Acidithiobacillus sp. bacteria
and Aspergillus niger fungus, respectively [14, 15]. A pre-
vious study determined the A. thiooxidans biogenic H2SO4
maximum production in 0.8 mol of H+ after 12.5 days cul-
tivation with elemental sulfur as energy source [16]. The use
of biogenic produced acid for partial BR neutralization is an
alternative to reduce the process costs, making it economi-
cally viable, since it can potentially replace the need of
expensive pure chemical acids, such as HCl.
The buffering curves at different concentrations of HCl
(0–2 mol H+ kg−1) were showed in Fig. 4. A strong
decrease in pH (*pH 11.0 to pH 4.0) was observed after
only 1-min reaction, probably due to the neutralization of
free anionic species present in solution remaining from
Bayer process, such as NaOH. After 4 h incubation, the slow
chemical dissolution of the solid phases (e.g. sodalite) star-
ted to take place and new anionic species were released to
the solution raising the pH again. A buffering region around
pH 8.0 was observed along time for 1.0 and 1.8 mol
H+ kg−1 HCl concentration, probably generated by hydrox-
yls linked on the surfaces of oxides, mainly Fe and Al, as
well as sodium structure – sodalite type dissolution. Between
1.8 and 2 mol H+ kg−1 the pH decreased due to the sodalite
buffering capacity. Once sodalite/calcite is totally consumed
at pH 6–8, the pH will decrease until the next mineral phase
(e.g. iron and aluminum oxides) start to dissolve and buffer
pH below 2 [8]. The BR neutralization difficulty was
reported by Thornber and Binet [12] who observed a sig-
nificantly pH increasing along a time frame from 1 min to
5 days and a high equilibration time dependent buffering
curve [12].
XRD diffractograms of BR after 21 days treatment with
HCl acid were demonstrated in Fig. 5. After 21 days, the
calcite phase was identified in the treatment containing
0.75 mol of H+ kg−1, probably due to dissolution of Na2CO3
and NaOH which anions (CO32−/HCO3− and OH−) releasing
for the system reaction, promoting interactions with calcium
from Bayer process, contributing to calcite formation. The
calcite mineral phase was completely dissolved around pH 6
with 1.63 mol H+ kg−1 of HCl. Despite XRD being a
semi-quantitative method, we can observe a significant re-
duction of the sodalite peak, evidencing its dissolution at
2.0 mol H+ kg−1 of HCl, after 21 days incubation (Fig. 5).
Calcite and sodalite dissolution are the main cause of
Brazilian BR buffering around pH 6–8 [8].
Since BR will be tested in the future as a soil conditioner
to replace limestone application, we assumed that a partial
BR neutralization around pH 8.0 would be adequate to safe
management during soil application, remaining the soil
alkalinity power. Neutralization of bauxite residue to pH
around 8.0 is advantageous because the chemically adsorbed
Na is released to leaching, alkaline buffer minerals are par-
tially neutralized and metals such as: Cu, Cd, Pb, Zn, Ni, Hg
and Cr (i.e. environmental toxicity potentially) are insoluble
Brazilian Bauxite Residue Physical–Chemical Characterization … 119

Fig. 4 Bauxite residue pH

neutralization by different HCl
concentrations along 21 days

Fig. 5 XRD diffractogram of BR

solid phase after 21 days acid
treatment with concentrations of
hydrochloric acid of 0 mol
H+ kg−1 (blank sample),
0.25 mol H+ kg−1, 0.75 mol
H+ kg−1, 1.63 mol H+ kg−1 and
2.0 mol H+ kg−1. Sdl sodalite,
Gbs gibbsite, Al-Gth aluminous
goethite, Ant anatase, Hem
hematite, Cal calcite
120
at this pH [18]. Therefore, based on ANC, to keep pH 8.0 for
a longer time will require about 1 mol H+ kg−1 of solids,
evidencing the high BR buffer capacity (Table 2).
The ANC behavior when using H2SO4 acid was similar
to HCl acid (Fig. 6); however, other inflections points were
observed indicating dissolutions of minerals phases (mainly
sodalite). It was also observed a pH increasing after as soon
as 4 h reaction. A smooth slope was observed in the range of
1.40–1.80 mol H+ kg−1 and range of pH 6–9, in Fig. 6,
probably associated to the high proton consumption, since
this area is recognized as sodalite buffering region. Chevdov
et al. [18] argued that part of the buffering capacity of
bauxite residues between pH 9 and 6 could be attributed to
the titration of surface hydroxyl (OH−) groups from solid
phases [19]. As previously show the ANC to pH 8 increase
from about 0.5 H+ kg−1 mol H+ kg−1 solids at a 1 min to
1.75 mol H+ kg−1 solids at 21 days.
XRD diffractograms of ANC with H2SO4 were shown in
Fig. 7. The main buffering phases (sodalite and calcite) were
also identified, occurring the complete calcite and partial
Table 2 Concentration (Mol Mol H+ kg−1
H+ kg−1) of hydrochloric (HCl),
sulfuric (H2SO4) and citric Time HCl
(C6H8O7) acids necessary to 1 min 0.50
acidify bauxite residue to pH 8 to
over different times 4h 0.63
24 h 0.75
7 days 0.88
14 days 1.00
21 days 1.00
Fig. 6 Bauxite residue pH
neutralization by different H2SO4
concentrations along 21 days
P. M. P. Silva et al.
sodalite dissolution after 21 days incubation. Despite H2SO4
is also a strong mineral acid, HCl was most effective, under
the same H+ concentration, to promote sodalite dissolution.
ANC of C6H8O7 is shown at Fig. 8. Unlike the mineral
acids (HCl and H2SO4), even the highest concentration of
C6H8O7 tested was unable to acidify BR below pH 5.0 for
more than one minute (Fig. 8). Weaker organic acids, such
as citric, ascorbic, malic, are known to operate in a two-fold
manner concerning the dissolution of minerals. As reported
to Stumm [19], proton promoted dissolution can be
enhanced by the chelation of the released metal with excess
organic acids in solution thereby lowering the activity of the
free metal in solution. Alternatively, specific adsorption of
the organic acid to the surface of the solid can destabilize
bonds between the surface metal and the bulk mineral by
either ligand-to-metal or metal-to-ligand charge transfers that
ultimately promotes the dissolution of metals at the surface
[19]. Considering the target BR pH 8, would be necessary
more than 2 mol H+ kg−1 solid of C6H8O7 to keep it stable
for a longer time (Table 2).
H2SO4 C6H8O7
0.50 0.88
0.63 1.00
0.88 1.00
1.00 1.5
1.25 >2.00
1.5 >2.00
Brazilian Bauxite Residue Physical–Chemical Characterization … 121

Fig. 7 XRD diffractogram of BR

solid phase after 21 days acid
treatment with concentrations of
Sulfuric acid of 0 (blank sample),
0.25 mol H+ kg−1, 0.75 mol
H+ kg−1, 1.63 mol H+ kg−1 and
2.0 mol H+ kg−1. Sdl sodalite,
Gbs gibbsite, Al-Gth aluminous
goethite, Ant anatase, Hem
hematite, Cal calcite

Fig. 8 Bauxite residue pH

neutralization by different
C8H8O7 concentrations along
21 days
122 P. M. P. Silva et al.

Fig. 9 XRD diffractogram of BR

solid phase after 21 days acid
treatment with concentrations of
citric acid of 0 (blank sample),
0.25 mol H+ kg−1, 0.75 mol
H+ kg−1, 1.63 mol H+ kg−1 and
2.0 mol H+ kg−1. Sdl sodalite,
Gbs gibbsite, Al-Gth aluminous
goethite, Ant anatase, Hem
hematite, Cal calcite

XRD diffractograms of BR samples treated with C6H8O7
were demonstrated in Fig. 9. Calcite was completely dis-
solved under C6H8O7 concentration of 0.75 mol H+ kg−1,
even better than H2SO4. However, sodalite phase seems to
remain unchanged (Fig. 9). Citric acid is unable to transform
the chemical speciation of Na structure [20]. Kong et al. [20]
described BR cancrinite and calcite dissolution after C6H8O7
reaction, by decreasing protonation and surface adsorption
of H+, a primary buffering effect [20].
Table 2 summarizes the amount of acid necessary to
partially neutralize BR to pH 8 along 21 days experiment.
As expected, a lower concentration of HCl was required for
partial neutralization of BR to pH 8 compared to H2SO4 and
C6H8O7. However, there are many negative points by con-
sidering using HCl in large scale BR neutralization, such as
elevated costs, dangerous transport, storage and handling
and absence of biotechnological routes for its production.
The determined BR ANC confirmed that sodalite and
calcite dissolution were the main responsible for pH
buffering. In general, Brazilian’s BR are richer in sodalite
than calcite, and as observed, calcite is primarily solubilized,
hence sodalite is the main challenge to BR alkalinity
neutralization.
Conclusions
The BR evaluated sample was mainly composed by he-
matite, aluminous goethite, gibbsite, sodalite, anatase, with
their associated elements: Fe, Al, Na, Si and Ti.
The ANC results indicate that BR partial alkalinity neu-
tralization was most effective with HCl > H2SO4 > C6H8O7.
HCl reached pH below 5.0 even after 21 days reaction.
Acid BR treatment showed a pH buffering between pH 6 and
8, were calcite and sodalite are most soluble.
If we consider a long term partial biological BR alkalinity
neutralization to pH 8.0, adequate to the soil conditioners
development, bacterial and fungal cultures will need to
produce at least 1.5 mol H+ of H2SO4 and >2.0 mol H+ of
C6H8O7 per kg. These results indicate how efficient the
microbial bioreactors for biogenic sulfuric and citric pro-
duction would be will be to allow partial BR neutralization.
Brazilian Bauxite Residue Physical–Chemical Characterization …
Acknowledgements The authors are grateful for the financial support
of this study by Hydro Alunorte S/A and all technical and logistical
support from Hydro’s R&D team.
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