Journal of Water Process Engineering 15 (2017) 43–48

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Journal of Water Process Engineering

journal homepage: www.elsevier.com/locate/jwpe

Utilization of raw and dried Victorian brown coal in the adsorption of

model dyes from solution
Galuh Yuliani a,c,∗ , Gil Garnier a , Alan L. Chaffee b
a
Bioresource Processing Research Institute of Australia (BioPRIA), Department of Chemical Engineering, Monash University, Clayton Campus, VIC 3800,
Australia
b
School of Chemistry, Faculty of Science, Monash University, Clayton Campus, VIC 3800, Australia
c
Chemistry Department, Faculty of Mathematics and Science Education, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154,
Indonesia

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

Article history: Being plentiful and readily available in many parts of the world, brown coal is probably one of the most
Received 10 December 2015 potential substitutes for activated carbon. Many reports include the brown coal drying stage prior to
Received in revised form 10 May 2016 adsorption despite the fact that it may lead to coal shrinkage and reduction of its pore volume, thus
Accepted 7 June 2016
diminishing its adsorption capacity. In this study, various types of raw (wet) brown coal were investi-
Available online 20 June 2016
gated as adsorbents for anionic and cationic dyes in aqueous solution. The adsorption capacities of these
raw brown coals were compared with those of oven dried brown coals and also with activated carbon. It
Keywords:
was found that raw brown coals exhibit high adsorption capacities for cationic dye, but very low capac-
Brown coal
Cationic dye
ities for anionic dyes, suggesting the involvement of a cation-exchange mechanism. Additionally, the
Adsorption capacity cation exchange capacities correlate positively with its cation adsorption capacity highlighting the major
role of strongly acidic groups in the adsorption process. Drying the brown coal significantly reduces its
adsorption capacity for cationic dye, supporting the hypothesis of coal shrinkage and the consequent
reduced pore volume upon drying. These findings suggest that raw (wet) brown coal may perform as
well as activated carbon for the removal of positively charged species in aqueous solution. Regeneration
of the used adsorbent may also not be necessary, since the used brown coal can be simply burnt as fuel
or composted.
© 2016 Elsevier Ltd. All rights reserved.

1. Introduction to 60%) leads to inefficiencies for this purpose. Hence, alternative

Activated carbons are generally regarded as the most effective
adsorbents used in water treatment processes due to their high
surface area, microporous structure and high degree of surface
reactivity. Activated carbons have been widely used in purification,
decolorisation, deodorisation, dechloronation and separation pro-
cesses [1]. However, the problems associated with high activation
and regeneration costs are disadvantageous. As a result, relatively
cheap alternative materials derived from industrial waste, agricul-
tural waste, minerals and coal have been intensively investigated
as alternatives for activated carbon [2,3].
Brown coal deposit in many parts of the world are vast and this
provides the basis for power generation industries in many places
[4]. Unfortunately, the high moisture content of the brown coal (up
∗ Corresponding author at: Chemistry Department, Faculty of Mathematics and
Science Education, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Ban-
dung 40154, Indonesia.
E-mail addresses: gyuliani@gmail.com, galuh@upi.edu (G. Yuliani).
applications of brown coal are sought in order to make economic
use of a cheap and locally available material [5].
Brown coal has some similarities to activated carbons, namely
high porosity and high surface area. Brown coal has been used to
prepare commercial activated carbons via energy intensive pyroly-
sis and activation procedures [6]. The use of raw brown coal itself, as
well as sorbents derived from it, for colour and metal removal from
aqueous solutions have also been reported [7–12]. It is commonly
accepted that high adsorption capacities of brown coal for metal
ions and dyes are mainly due to the cation-exchange mechanism of
some oxygen containing groups on the coal surface [3,9,12]. How-
ever, the effects of moisture content and brown coal pre-treatment
prior to adsorption, such as drying, are still poorly understood.
When considered as an abundant and cheap material, brown coal
optimisation for wastewater treatment processes is an attractive
proposition.
The primary objective of this study is to characterise and
optimize brown coal as a potential low-cost high-performance
industrial adsorbent for aqueous process effluents. A series of Vic-
torian brown coals, adsorbing either an anionic or a cationic dye

http://dx.doi.org/10.1016/j.jwpe.2016.06.004
2214-7144/© 2016 Elsevier Ltd. All rights reserved.
44 G. Yuliani et al. / Journal of Water Process Engineering 15 (2017) 43–48

Table 1 in order to reduce the possibilities of differences in the ratio against

The moisture contents, ash yields and ultimate analyses of brown coals.
the background of the KBr pellets.
Adsorbent Moisture content (%) Ash Yield Ultimate Analysis (% db) FTIR spectra of the dried brown coals are provided in Fig. 2. The
important functional groups, phenols and carboxylic groups, give
Carbon Hydrogen Nitrogen
clear bands in the FTIR spectrum of the raw brown coal. The band
LYNA 34 5.1 62.5 4.0 0.5
at 1710 cm−1 is the C O stretching due to the carbonyl and car-
MV 30 2.0 66.3 4.4 0.5
LY 12 6.2 62.7 4.3 0.67 boxyl groups. The absorption at 1630 cm−1 is dominated by (C· · ·C)
YL 55 2.2 64 4.7 0.51 stretching of aromatic rings, unsaturated olefinic bonds and poly-
AC 6 12.6 83.3 0.5 0.4 aromatic structures, and C O stretching of quinones bridged to
acidic hydroxyl [13].

were selected as model systems. The performance of brown coal

was compared to coal-derived activated carbon. A secondary objec-
tive is to understand the mechanism of adsorption and to study the
effect of pre-treatment (drying) on the adsorption efficiency.
2. Material and methods
2.1. Materials
Brown coals used in this experiment were Loy Yang high sodium
(LYNA), Loy Yang (LY), Yallourn (YL) and Maryvale (MV) brown
coals. All brown coal samples were mined from the Latrobe Val-
ley region of Victoria, Australia. The bulk samples were coned and
quartered to obtain representative samples, sieved and particles
sizes between 150 ␮m to 212 ␮m were chosen. Dried brown coals
were obtained by drying under nitrogen at 105 ◦ C for 3 h.
For comparison, an activated carbon was also studied. The
activated carbon was coal-derived and purchased from Activated
Carbon Technology Australia with particle sizes between 150 ␮m
to 212 ␮m.
The moisture contents, ash yields and ultimate analyses of the
adsorbents investigated are supplied in Table 1. The ash yields and
the C,H and N analyses were performed by the HRL Technology Pty.
Ltd., Mulgrave, Victoria. The ash yields were determined accord-
ing to the HRL Method No. 1.6 and the C,H and N analyses were
determined on the Leco Truspec CHN analyser according to the
HRL Method No.1.4. The nitrogen sorption (at 77.15 K) and car-
bon dioxide sorption (at 273.15 K) measurement was performed
using a Micromeritics ASAP 2010 surface area analyser. Cationic and
anionic dyes are safranin-O (SO) and alizarin red (AR), respectively.
Their structures are given in Fig. 1.
2.3. Batch adsorption
Known amounts of adsorbent were added to dye solutions in a
batch reactor system and shaken for 20 h at 20 ◦ C to attain equilib-
rium. The aqueous phase was filtered using a 0.45 ␮m syringe filter
and then was analysed for residual concentration of dye using a
UNICAM 8625 UV/vis spectrometer. The absorbance measured was
then converted to concentration using calibration curves for each
dye.
Due to the nature of brown coal, the addition of both raw and
oven dried brown coal decreased the solution pH. For SO, the
absorption at 516 nm did not change significantly as the pH of
dye solutions changed. The absorption difference when the pH was
changed from 6.5 to 2.5 is below 3% and is still acceptable. The solu-
tion pH after addition of raw and oven dried brown coal ranged from
3.8to 4.8. For AR, the absorption at 425 nm changed dramatically as
the solution pH changed from 3 to 6.5. However, the addition of
brown coal did not considerably change the solution pH. The pH of
various concentrations of AR solution in distilled water was in the
range 3.9–4.5 and, after addition of brown coal, was still in the range
3.8–4.2. When activated carbon was used, the pH of the solution
was adjusted to 4 using an aqueous solution of 0.1 M H2 SO4 .
2.4. Cation exchange capacity analysis
All of brown coal samples used were analysed by the HRL
Technology Pty Ltd., Australia for their effective cation exchange
capacity (ECEC). The adsorbents were first dried, ground and sieved
to less than 212 ␮m before submitted for the analysis of “Exchange-
able bases” according to Method 15D3 on the Australian Handbook
of Soil and Water Chemical Methods [14,15]

2.2. FTIR analysis 2.5. Theory and analysis

The FTIR analysis was conducted to identify the lignite’s func- The adsorption capacity (qe ) represents the amount of dye
tional groups. All lignite samples were dried at 105 ◦ C under N2 molecules adsorbed per gram of adsorbent (mg/g) and can be cal-
for 5 h to reduce the intensity of OH bands. The KBr pellets were culated using equation 1.
obtained using 1 part of coal and 200 parts of KBr. The FTIR spectra
were collected using a Perkin-Elmer Spectrum 100 FT-IR spectrom- V
qe = (C0 − Ce )( ) (1)
eter. The analyses for all samples were performed at the same time m

(a) (b)
Fig. 1. Chemical structure of model dyes: (a) SO (cationic) (b) AR (anionic).
 G. Yuliani et al. / Journal of Water Process Engineering 15 (2017) 43–48 45

layer) of sorbent (mg/g) and KL is the adsorption energy constant

of Langmuir isotherm (L/mg).
The Freundlich model can be expressed as follow [17]:

log qe = log KF + (1/n) log Ce (3)

whereKF is adsorption capacity (mg/g) and n is Freundlich constant

related to adsorption intensity.

3. Results and dicsussion

3.1. Adsorption isotherm

Fig. 2. FTIR spectra of brown coals. Fig. 3 shows the equilibrium adsorption of SO, a cationic dye,
on brown coal and coal-derived activated carbon. LYNA coal and
500 YL exhibited higher adsorption capacities than the coal-based acti-
450 vated carbon. MV coal had lower adsorption capacity than activated
400 carbon and LY coal had the lowest adsorption capacity for the
cationic dye. The initial adsorption slope was higher for activated
350
carbon than for coals, indicating faster uptake of dye molecules. For
qe (mg g-1)

300
LYNA LYNA, YL and MV, the initial dye uptake rates were similar.
250 The upper limits of the adsorption capacities of the brown coal
YL
200 samples for safranin dye were mostly above 150 mg/g. This is higher
AC
150 than some alternative adsorbents reported in the literature for the
MV
100 same dye. For example, the adsorption capacity of adsorbent pre-
LY pared from rice husk for safranin adsorption when calculated with
50
the Langmuir adsorption isotherm was only 35.8 mg/g[18], while
0
adsorption capacities of kaolinite and alumina for the similar dye
0 20 40 60 80 100
Ce (mg L-1)
were reported to be equal to 53.7 mg/g and 0.01 mg/g, respectively
[19].
Fig. 3. Adsorption of SO dye on brown coal and activated carbon as a function of The adsorption data were fitted with the Langmuir and Fre-
equilibrium concentration in solution. undlich isotherm models (Fig. 4) to provide insight on the nature
of the interaction between dye and adsorbent. All adsorption data
whereC0 is the initial concentration of the dye solution (mg/L), Ce is fit the Langmuir isotherm better than the Freundlich isotherm
the equilibrium concentration of the dye solution (mg/L), m is the (Table 3), as indicated by the correlation coefficients (R2 ) greater
amount of adsorbent used (dry basis, g) and V is the volume of dye than 0.99. The Langmuir model characterises the adsorption in
solution (L). terms of a monolayer interaction between the adsorbate molecules
Some models are available to correlate the experimental adsorp- and the adsorbent surface. The agreement between experimental
tion data and may provide useful information on adsorption data (for all brown coal samples) and the Langmuir isotherm sup-
behavior and the heterogeneity of adsorbent surface. The isother- ports the concept of a strong monolayer interaction; this would
mal equilibrium sorption data obtained from the batch experiment be expected from a cation-exchange mechanism. The maximum
was processed according to Langmuir and Freundlich models. The adsorption capacities (Q 0 ) of LYNA and YL coal for safranin were
Langmuir equation is represented as follow [16,17]: similar when calculated using the Langmuir equation (Table 2).
The overall trend of the adsorbents’ performance in removing
Ce Ce 1
= 0 + 0 (2) cationic dye from aqueous solution was: LYNA > YL > Activated car-
qe Q Q KL
bon > MV > LY.
whereCe is the concentration of the dye remaining in the solution The adsorption capacity of all brown coals for the anionic dye
(mg/L), qe is the amount of dye adsorbed per gram of adsorbent (alizarin red) decreased significantly (Fig. 5). In contrast, activated
(mg/g), Q 0 is the maximum surface coverage (formation of mono- carbon maintained high capacities for both dyes. While the adsorp-

0.8 3
0.7 2.5
0.6
LYNA 2
Ce/qe (g L-1 )

0.5
AC
log qe

YL
0.4 1.5
AC LYNA
0.3
1 YL
0.2 MV
0.5 MV
0.1 LY
LY
0 0
0 50 100 150 -1 0 1 2 3
Ce (mg L-1) log Ce

(a) (b)
Fig. 4. (a) Langmuir and (b) Freundlich isotherms for SO adsorption on activated carbon and brown coal.
46 G. Yuliani et al. / Journal of Water Process Engineering 15 (2017) 43–48
Table 2
Surface area of brown coals and coal-based activated carbon.
N2 sorption BET Surface area (m2 /g coal db)
CO2 sorption Surface area (m2 /g coal db) (Dubinin-Radushkevic)
Pore volume (cm3 /g) (Mercury intrusion porosimetry) [15]:
Micropore (<2 nm)
Mesopore (2–50 nm)
1200
1000
AC
800 YL
qe(mg g-1)
MV
600
LYNA
400
LY
200
0
0 50 100 150
Ce (mg L-1)
Fig. 5. Adsorption of AR dye on brown coal and activated carbon as a function of
equilibrium concentration in solution.
tion capacity of activated carbon for anionic dye was higher than
that for cationic dye, the adsorption capacity of the brown coal for
anionic dye was less than 15% of that for cationic dye. The adsorp-
tion of the anionic dye adsorption onto brown coals did not fit the
Freundlich model at all. Therefore, only the Langmuir model was
used to plot the adsorption data (Fig. 6).
The maximum adsorption capacities (Q 0 ) of brown coals for
alizarin red dye adsorption were insignificant when compared to
activated carbon (Table 3). The Q 0 values for all coals were less
than 4% of that for coal-based activated carbon. Also the Langmuir
isotherm fits are relatively poor and the K values are very low. How-
ever, the overall trend of the brown coals’ performance in removing
anionic dye from aqueous solution was: LY > YL > MV > LYNA.
Most activated carbons have a very large specific surface area,
typically above 800 m2 /g, with micropores contributing over 80%
of the total surface area groups [16]. This provides ample adsorp-
tion sites for the dye molecules to establish physical interactions
with the adsorbent’s surface (physisorption). Additionally, acti-
vated carbons possess functional groups with both basic and acidic
properties. The acid functional groups are carboxylic, lactonic, and
phenolic, while the basic functional groups include ketonic and
pyronic oxygen-containing species [20]. These functional groups
may play a role in the adsorption mechanism such as increasing the
interaction of activated carbon with polar adsorbates. However, the
density of these functional groups is low, typically between 0.54
to 14.9 group nm−2 , with the total functional groups concentra-
tion of around 1 mmol g−1 [21]. Because of their low concentration,
they are probably not the main factor influencing the high capac-
ity of activated carbon for either anionic or cationic species in the
wastewater.
The higher adsorption capacity of activated carbon for alizarin
red compared to safranin may be due to the bulkier molecular
structure of safranin (Fig. 1.). Molecular dynamics1 simulations
1
Molecular dynamics simulations were carried out for each of the adsorbate ions
at 298 K for 100 ps using the Forcite module and the Compass forcefield of the Mate-
AC LY Brown coal
LYNA MV YL
1235 ± 20 2.0–2.5
837 202 234 237 242
0.38 0.062 0.068
0.36 0.052 0.058
were used to predict the van der Waals surface of the dyes
[22]. The volumes occupied by the safranin and alizarin red ions
averaged 305.4 Å3 and 243.3 Å3 , respectively at 298 K. Therefore,
activated carbon can accommodate more alizarin red molecules
within its micropores than safranin. It is also likely that the smaller
alizarin red molecules can penetrate smaller pores from which the
safranin would be excluded. This suggests physisorption as domi-
nant adsorption mechanism for activated carbon. In physisorption,
the surface area and pore volume typically govern the adsorption
efficiency. The activated carbon has high surface area and pore
volumes for both micro and mesopores (Table 2).
The surface areas of the brown coal samples are roughly one
quarter of the activated carbon (Table 2). Despite their lower
surface areas, brown coals have considerably higher adsorption
capacities for the cationic dye (Table 3). This suggests that an addi-
tional mechanism, such as cation-exchange, is enhancing cationic
dye adsorption. Chemisorption appears to be the dominant mech-
anism for safranin adsorption.
The adsorption capacities of brown coal for anionic dye were
considerably less than a quarter of those of activated carbon,
as expected from pure physisorption (proportional to surface
area) (Table 2). The negatively-charged adsorbate molecules were
unable to access the available pores of the brown coal surface.
The negatively-charged surface might prevent the adsorbates from
adsorbing onto the available pores on brown coal structure. This
also suggests the predominant role of chemisorption in the adsorp-
tion process using brown coal.
3.2. Effect of brown coal drying
Raw brown coal having a moisture content between 55 and 57%
was reported to have Langmuir isotherm saturation capacity of
286–370 mg/g for methylene blue adsorption [15]. On the other
hand, the adsorption capacities of dry and pyrolysed brown coal
for methylene blue were only 45 mg/g and 25 mg/g, respectively
[23,24]. The dry and pyrolysed coals exhibited lower adsorption
efficiency and effectiveness presumably due to surface shrinkage
and possible preoxidation and crosslinking during the drying pro-
cess.
In this study, three Victorian brown coals (LYNA, MV and YL)
were dried under N2 for 3 h and the adsorption capacities for
the cationic dye solution before and after drying were compared
(Fig. 7). It can be seen that the adsorption capacities of all coal sam-
ples were diminished as a result of drying. Additionally, positive
correlation between the adsorption capacities (Q 0 ) of raw brown
coals and moisture content (Table 1) was observed. Coal sample
having the lowest moisture content, LY, had the lowestQ 0 . This
supports the role of water molecules occupying the coal pores in
maintaining the active site for adsorption and the hypothesis of
rials Studio® suite of programs (Accelrys, San Diego). The occupied volume was
determined from the Connolly surface which uses the van der Waals radii of the
atoms in the structure.
 G. Yuliani et al. / Journal of Water Process Engineering 15 (2017) 43–48 47

Table 3
Langmuir and Freundlich isotherm constants and correlation coefficients for SO and AR dyes adsorption on brown coal and activated carbon.

Adsorbent Langmuir Isotherm SO(cationic) dye Freundlich Isotherm SO(cationic) dye Langmuir Isotherm AR (anionic) dye

Q 0 (mg/g) KL (L/mg) Correlation coefficient (R2 ) KF (mg/g) n Correlation Coefficient (R2 ) Q 0 (mg/g) KL (L/mg) Correlation coefficient (R2 )

LYNA 476 0.58 0.9998 167 3.2 0.9033 5.76 0.01 0.8806
YL 476 0.5 0.9982 209 5.3 0.9788 30.4 0.01 0.658
MV 357 0.82 0.9995 157 4.6 0.9411 10.4 0.02 0.9779
LY 139 0.27 0.9829 48 4.1 0.9007 34.7 0.04 0.9902
AC 357 56 0.9998 293 13 0.7318 1000 0.91 0.9091

12 macrostructure. Factors contributing to the level of shrinkage are

coal rank and lithotype [27,28].
YL
10
MV 3.3. Role of cation-Exchange capacity (CEC)
8
Ce/qe (g/L)

LY
Brown coal has many of the oxygen containing groups associ-
6
LYNA ated with its structure, present as carboxyl and phenolic groups
4 [29]. When added to water or dye solutions, these acidic groups
lose their hydrogen ions due to ionization that result in lowering
2 the pH of water or solutions. This mechanism forms a negatively
charged layer on the surface that leads to its ability to interact well
0 with positively charged molecules. The presence of these carboxyl
15 65 115 165 groups and, to a lesser extent, the phenolic groups possibly aug-
Ce (mg/L) ments the adsorption of positively charged dye onto brown coal
[30].
Fig. 6. Langmuir isotherm adsorption for AR on brown coals.
Coal-COOH Coal-COO− + H+ (i)
+ −
Dye + nCoal-COO = (Coal-COO-Dye) (ii)
surface shrinkage and pore collapsing of brown coal upon drying
[25]. To confirm the role of oxygen containing groups and cation
The removal of water from brown coal is always accompanied exchange mechanism in brown coal’s adsorption, the cation-
by shrinkage even at low temperature (30 ◦ C) in vacuum [26]. Sig- exchange capacity of the raw coal is plotted versus the adsorption
nificant levels of pore collapsing and crosslinking occur during capacity for cationic dye (Fig. 8). The adsorption capacity of coal
drying at 105 ◦ C, the standard temperature for drying coal [25]. generally increased as the cation-exchange capacity increased. The
During evaporation, water molecules occupying the large pores are low adsorption capacity of LY (Fig. 3 and Table 3), for example,
lost first, followed by water in the smaller pores. Coal shrinkage may be due to its low cation exchange capacity. This result sup-
occurs, but the structural changes are relatively small at this point ports the involvement of oxygen functionalities in cation-exchange
due to the ordered arrangement and the rigidity of the coalified mechanism of positively charged dye adsorption.

500 500

400
qe (mg g-1 db)

400
qe (mg g-1 db)

300 300 YL
MV
200 200 YL dried
MV dried
100 100

0
0
0 50 100
0 50 100
Ce (mg L-1) Ce (mg L-1)

500
qe (mg g-1 db)

400
300
LYNA
200 LYNA dried
100
0
0 10 20 30 40
Ce (mg L-1)

Fig. 7. Equilibrium adsorption of cationic dye (safranin) onto raw and dried brown coal.
48 G. Yuliani et al. / Journal of Water Process Engineering 15 (2017) 43–48
40
LYNA
Effecve caon exchange capacity,
35
30
ECEC (meq/100g, db)
25
20
15 MV YL
10
5
LY
0 [10] C.J. Butler, A.M. Green, A.L. Chaffee, Remediation of mechanical thermal
0.3 0.8 1.3
Adsorpon capacity (qe , mmol/g)
Fig. 8. Relationship between cation exchange capacity of brown coal to adsorption
capacity for cationic dye solution.
4. Conclusions
Adsorption studies performed on brown coal and coal-based
activated carbon to cationic and anionic dyes revealed the adsorp-
tion mechanism followed by the brown coal. Coal based activated
carbon showed consistent performance in adsorbing both cationic
and anionic dyes with high adsorption capacities for both dyes.
On the contrary, the adsorption capacity of the brown coal for
an anionic dye was significantly lower than that for the cationic
one. Strong acidic group content, reflected by the cation-exchange
capacity of coal, correlated positively with its adsorption capacity
for cationic dye solution. This confirms the major role of hydroxyl
and carboxyl groups in the brown coals in attracting the positively
charged dye molecules and suggests chemisorption as one of the
adsorption mechanisms involved. The study also demonstrated the
loss of adsorption capacity of coal upon drying due to the pore
collapse and consequent changes in the coal structure. The result
suggests the potential of (wet) brown coal as a replacement for acti-
vated carbon in removing positively charged contaminants in the
wastewater. Neither pretreatment nor regeneration will be neces-
sary since the coal can still be used as fuel after use.
Acknowledgements
This project was funded by the Department of Primary Indus-
try (Victoria) under the Energy Technology Innovation Strategy
(ETIS) programin which the project partners wereMonash Univer-
sity, Keith Engineering, Kimberly Clark Australia, Gippsland Water,
and GHD Ltd. The authors acknowledge Mr Greg Knowles for tech-
nical advice with instrumental analysis.
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