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International Journal of Coal Geology 73 (2008) 3 18

www.elsevier.com/locate/ijcoalgeo

Composition and mode of occurrence of mineral matter in some

Colombian coals
Ins Carmona Lpez a , Colin R. Ward b,
b

a
School of Materials Engineering, Faculty of Mines, Universidad Nacional de Colombia, Sede Medelln, Colombia
School of Biological, Earth and Environmental Sciences, University of New South Wales, Sydney, NSW 2052, Australia

Received 27 December 2006; received in revised form 26 March 2007; accepted 28 March 2007
Available online 21 April 2007

Abstract
The minerals in a range of Colombian coal samples, selected to represent the principal coal-mining regions, have been
investigated using low-temperature ashing and quantitative X-ray diffraction techniques, and the results compared to information
from chemical analysis and Mssbauer spectroscopy studies. Kaolinite, illite, interstratified illitesmectite and quartz are the
dominant mineral matter components in almost all of the coal samples, with small but significant proportions of pyrite (up to
around 15% of the mineral matter) being present in around half of the samples studied. Other minerals present in particular samples
include chlorite, muscovite, paragonite, ankerite, dolomite, calcite and siderite, along with phosphate minerals apatite and goyazite.
Jarosite and coquimbite are also noted in some of the pyrite-bearing coals, probably representing oxidation products of the pyrite
developed with exposure or storage. Bassanite is present in the low-temperature ash of some coals, and in one sample occurs along
with significant concentrations of hexahydrite, alunogen, tschermigite and paraluminite, all of which were probably derived from
interaction of inorganic elements in the organic matter with organic sulphur during maceral oxidation.
Quantitative analysis of the minerals in the low-temperature ash of the coal samples using Rietveld-based X-ray diffraction
techniques provides results that are consistent, at least for the most abundant elements, with the chemical composition of the coal
ash as determined by standard analysis procedures. The evaluation of mineral-rich concentrates by Mssbauer spectroscopy also
provides results consistent with the XRD data, especially as regards pyrite and some of the sulphate components. Optical
microscopy indicates that much of the pyrite, and in some cases also the carbonates, occurs as anhedral crystals, finely
disseminated in the maceral components, as aggregates of crystals (including pyrite framboids), as fine-grained crystals replacing
liptinite, and as fracture fillings. Some sub-angular to rounded quartz grains are also present, possibly of detrital origin, but most
other minerals, including the clay minerals, occur mainly as aggregates of intimately admixed mineral and maceral constituents.
2007 Elsevier B.V. All rights reserved.
Keywords: Coal characterisation; Colombia; Mineral matter; Petrography; X-ray diffraction; Mssbauer spectroscopy; Chemical analysis

1. Introduction

Corresponding author. Fax: +61 2 9385 1558.

E-mail addresses: icarmona@unalmed.edu.co (I. Carmona),
C.Ward@unsw.edu.au (C.R. Ward).
0166-5162/$ - see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.coal.2007.03.005

Colombia has coal resources of varying quality that

are distributed throughout the country (Jamieson, 1985;
INGEOMINAS, 2004), with potential to supply national
demand for several hundred years. Colombia is also
currently the world's fourth largest thermal coal

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

Fig. 1. Distribution of coal-bearing areas in Colombia, showing regions from which samples were taken.

exporter, with a contribution representing more than 5%

of the total export market.
The most important coal-bearing units are the
Paleocene Cerrejn Formation, located in the province
of La Guajira, the Los Cuervos Formation, also of
Paleocene age, located in the provinces of Cesar and
Norte de Santander, the upper Maastrichtian to

Paleocene Guaduas Formation, located in the provinces of Cundinamarca and Boyac, the Campanian
to Maastrichtian Umir Formation, located in the
western parts of the provinces of Cundinamarca,
Boyac, and Santander, and the OligoceneMiocene
Amag Formation located in the province of
Antioquia.

El Playn-El Tambo
La Jagua de Ibirico
El Cerrejn Zona Norte
Suesca-Albarracn
50.47W
42.72W
30.09W
10.82W
2 25 08.91N
9 34 31.03N
11 1 13.62N
5 34 17.28N
OligoceneMiocene
Paleocene
Paleocene
MaastrichtianPaleocene

76 47
73 18
73 18
73 16

Checua-Lenguazaque
Checua-Lenguazaque
Sogamoso-Jeric
El Hoyo-Mosquera
Amag-Sopetrn
Amag-Sopetrn
San Jorge
Aranzazu-Santa gueda
15.59W
25.26W
14.30W
60.00W
34.62W
02.22W
02.93W
44.32W

Longitude

73 43
73 43
73 00
77 05
75 12
75 12
75 48
75 28
5 19 34.81N
5 19 42.73N
5 36 54.87N
2 11 59.98N
5 53 29.66N
5 54 20.33N
7 59 47.15N
5 15 59.95N

Latitude
Age

MaastrichtianPaleocene
MaastrichtianPaleocene
MaastrichtianPaleocene
Mid EoceneMid Miocene
OligoceneMiocene
OligoceneMiocene
Miocene
MiocenePliocene

La Honda Vereda Seguengue

La Jagua, M-27
Cerrejn Manto 140
Escaln Veta Grande
0322
0330
0334
1083

Cauca
Cesar
Guajira
Boyac

JB09, Mina El Rub, M-La Grande

JB10, Mina El Bosque, M-120
Cooprisa, M-Galeras
El Hoyo-Pata, M-BG 19B
Hulleras Manto 4
La Coquizada
Puerto Libertador M-L
Aranzazu M-5
0034
0035
0036
0048
0056
0057
0066
0137

Formation
Regin

Central
Central
Central
Pacfica
Atlntica
Atlntica
Atlntica
Central

Province

Cundinamarca
Cundinamarca
Boyac
Cauca
Antioquia
Antioquia
Crdoba
Caldas

Sample number Mine

Table 1
Location of coal samples

Guaduas
Guaduas
Guaduas
Guachinte
Amag
Amag
Cerrito
Secuencia Volcaniclstica
de Aranzazu
Pacfica Mosquera
Atlntica Los Cuervos
Atlntica Cerrejn
Central
Guaduas

Area

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

Palynological, stratigraphic, sedimentological and

petrographic studies indicate that the majority of the
coals were formed in deltaic and transitional environments (Azpiritxaga and Casas, 1989; Sarmiento, 1992;
Quetame and Sarmiento, 2004; Bayona et al., 2004),
but some show evidence of significant terrestrial
influence (Guzman, 1991). The physical, chemical
and petrographic characteristics of the coals vary
significantly, depending on these influences, with
rank ranging from lignite to bituminous coal and
anthracite.
Although some preliminary studies have been carried
out using different techniques (Carmona et al., 2003),
little information has been published on the mineral
matter in Colombian coals, including the nature and
relative proportions of the individual minerals, the
modes of mineral occurrence, and the associations
between the different groups of minerals present within
the coals.
The nature and distribution of the mineral matter in
coal is significant in the technology of preparation and
use, as well as in the environmental impact of mining,
utilization and waste management (e.g. Raask, 1985;
Vassilev et al., 1995; Gupta et al., 1999; Reifenstein
et al., 1999; Ward, 2002). Relevant aspects include the
mode of occurrence and the mineral matter, its behavior
when the coal is used, and the association of trace elements with particular mineral components (e.g. Gluskoter et al., 1977; Swaine, 1990; Finkelman, 1994; Ward
et al., 1999, 2005; Huggins, 2002; Dai et al., 2005,
2006).
2. Samples studied
Twelve samples of coal were selected for mineralogical study, representing materials from the different
coal-bearing regions of the country (Fig. 1). To facilitate
microscopic evaluation of mineral occurrence, the samples from each region were chosen to include coals with
significant ash percentages.
The samples for analysis, taken from exploration
activities ahead of mine workings, were supplied by
INGEOMINAS (the Colombian Institute of Geology
and Mining), belonging the Department of Mines and
Energy of the Republic of Colombia. Table 1 indicates
the sources of the samples, along with their stratigraphy
and mining associations. Table 2 provides a summary of
the basic coal properties.
The quantity of sample supplied from each seam was
approximately 200 grams. A representative fraction of
150 g of each sample was obtained by cone and quartering,
and this was then reduced to a size passing 20 mesh

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

Table 2
Proximate analysis and other data for the coal samples (Minercol, 2001)
Sample
number

Total
moisture

Equilibrium
moisture

Residual
moisture

Ash

Volatile
matter

Fixed
carbon

Total
sulphur

CV
(cal/g)

FSI

ASTM
classification

0034
0035
0036
0048
0056
0057
0066
0137
0322
0330
0334
1083

2.35
7.34
5.71
10.22
3.57
12.62
16.62
37.65
7.52
4.63
14.43
7.45

1.92
1.34
5.92
6.64
2.70
5.86
21.61
30.64
18.48
16.20
13.62
8.15

1.11
0.81
4.74
4.15
1.79
4.42
14.01
28.24
2.05
3.22
9.79
6.04

13.20
10.83
13.01
31.50
13.73
12.81
11.02
9.88
20.40
8.90
4.28
13.61

30.48
25.03
36.31
32.26
32.28
26.22
35.19
37.15
37.89
36.80
34.36
36.31

55.21
63.33
45.94
32.09
52,20
56.55
39.78
24.73
39.66
51.08
51.57
44.04

1.38
0.50
1.04
0.47
2.34
1.36
1.68
0.44
2.97
0.82
1.23
0.88

7341
7657
6489
4586
6885
6620
5121
3832
6280
7063
6633
6313

5
8
1
0
6
0
0
0
2
2.5
0
0

hvBa
mvB
hvBa
hvBc
hvBa
mvB
subC
ligA
hvBc
hvBc
hvBc
subA

Note: Proximate analysis, sulphur and CV on air-dried (residual moisture) basis.

(850 m) but retained on 60 mesh (250 m) for preparation

of the samples for the different analysis procedures.
3. Analytical program
3.1. Chemical analysis
Representative portions of the coal samples were ashed
at high temperature (750 C), and the ashes subjected to
chemical analysis according to the procedures outlined by
ASTM D3174. The chemical analysis of the ashes was
performed in the Coal Laboratory of the Faculty of Mines
at the Universidad Nacional de Colombia, Sede Medelln,
with other data provided by INGEOMINAS. The results
of the ash analyses are summarised in Table 3.
3.2. X-ray diffraction analysis
Representative portions of each coal were more finely
ground in a ring-grinder mill, and oxidised at low

temperature (around 120 C) in an IPC four-chamber

oxygen-plasma asher, following procedures outlined
by Standards Australia (2000). The resulting lowtemperature ash (LTA) residues were subjected to X-ray
powder diffraction using a Philips X'pert system, with
CuK radiation. Samples were run from 2 to 60 2, with
a step increment of 0.02 and a counting time of 2 s per
step, and the relevant data (2900 steps per sample) stored
in digital form. The minerals in each case were identified from the diffractograms by reference to the ICDD
Powder Diffraction File.
Quantitative analyses of the minerals present in
each LTA were made using Siroquant, commercial
interpretation software (Taylor, 1991) based on the Rietveld
(1969) full-profile XRD analysis technique. Rietveldformat XRD data (.hkl) files were prepared using Siroquant
for each mineral present in the samples, drawing on a
comprehensive collection of crystal-structure information
in the Siroquant database. A task (.tsk) file was set up for
each individual analysis, with a listing of the minerals

Table 3
Chemical analysis of coal ashes (wt.%)
Sample

SiO2

Al2O3

Fe2O3

CaO

MgO

K2O

Na2O

P2O5

TiO2

0034
0035
0036
0048
0056
0057
0066
0137
0322
0330
0334
1083

59.48
65.47
65.90
58.25
47.57
48.35
47.07
34.66
71.50
77.45
73.00
70.48

26.63
27.01
28.85
33.50
26.97
16.06
28.33
15.68
15.20
14.73
8.20
23.73

5.27
1.17
2.93
3.35
15.71
9.94
13.29
8.91
8.60
1.37
11.90
1.41

1.58
1.23
0.59
1.70
1.14
7.98
3.01
20.01
2.50
1.09
1.97
0.60

0.58
0.38
0.50
1.08
1.57
4.28
1.54
3.96
1.15
0.53
2.22
0.54

1.45
1.06
0.55
0.49
1.01
1.01
0.65
0.57
0.57
1.37
0.57
1.02

0.73
0.65
0.23
0.30
0.27
0.32
0.32
0.98
0.46
0.70
2.10
0.88

1.31
0.80

1.21
1.45

SO3
0.51
0.04

0.12
0.11
0.11
0.13

1.14
0.85
0.97
0.82

2.46
10.15
3.67
13.74

0.11

1.23

0.22

Total
98.75
99.26
99.55
98.67
97.96
99.05
98.96
99.46
99.98
98.80
99.96
98.66

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

Table 4
Mineralogy of LTA residues (wt.%), based on X-ray powder diffraction and Siroquant
Sample Number
LTA (wt.%)
Quartz
Kaolinite
Illite
Interstratified Clay
Muscovite
Paragonite
Chlorite
Albite
Calcite
Dolomite
Siderite
Ankerite
Apatite
Goyazite
Pyrite
Jarosite
Coquimbite
Bassanite
Boehmite
Total

0034

0035

0036

0048

0056

0057

0066

0137

0322

0330

0334

1083

13.2
22.8
35.4
7.4
28.2

11.7
24.0
48.7
11.1
14.6

11.0
21.9
57.3
9.7
10.2

34.8
6.2
63.2
19.1
8.2

14.7
10.8
41.0
9.9
22.6

14.0
23.8
19.7
10.3
19.2
3.8

12.8
13.1
39.4
30.9

15.4

23.1
41.6
23.4
11.1
6.7

10.5
47.5
24.5
16.6

3.0
54.2
16.9
9.4

10.0
32.4
41.0
10.9
14.8

8.8

12.9

0.9

2.0

3.5
3.2

7.2
3.3
0.9
1.5

0.9
3.2

1.2

0.3

1.4
11.9

0.9

13.4

0.6
100.0

99.90

100.0

100.0

1.5
100.1

expected to be present (i.e., the .hkl files to be used in the

analysis) and the relevant sample XRD pattern. Corrections
were made to remove the background from the sample
XRD trace, after which a calibration function was applied
(Matulis and Taylor, 1992) to compensate for the effects of
the goniometer geometry on the X-ray diffraction pattern.
Details of these and other procedures are given by Ward
et al. (1999, 2001).
The operation of Siroquant involved interactive adjustment and best-fit matching of the combination of
synthetic XRD profiles for the individual minerals in
each task file to the observed X-ray powder diffraction
pattern. The results of the Siroquant analysis (Table 4)
represent the final output from each task, when the best
possible fit had been achieved between the observed and
synthetic XRD patterns.

1.7

1.0

8.4
2.7
2.9
2.5

100.0

99.9

N
O
T

10.1
1.2

Q
U
A
N
T
I
F
I
E
D

2.6
1.9

1.9

100.0

99.9

100.1

100.0

mode, with a 57Co/Rh source. The spectra were taken at

room temperature, with adjustments using the MOSF
program (Vandenberghe et al., 1994). The spectrometer
was calibrated with crystalline hematite. The results of
the Mssbauer study are presented in Table 5.
3.4. Petrographic analysis
Petrographic analysis was carried out on polished
sections of particulate grain mounts of each coal sample,
based on the material passing 20 mesh and retained on
60 mesh sieves. Analysis was performed using a Leitz
reflected light microscope, with special reference to
description of the minerals and their different modes of
occurrence in the coal samples. Table 6 summarizes the
petrographic composition of the coals, based on this
microscopic study.

3.3. Mssbauer spectroscopy

4. Ash chemistry and mineral matter
Mineral concentrates for Mssbauer spectroscopy
were obtained using a float-sink process, with a zinc
chloride solution of RD = 1.50 g/cm3 as the separating
medium. The coal particle size was less than 840 m
and more than 250 m. Each separation used 100 g of
coal and 150 ml of separating medium. The samples
were analyzed in the Solid State Physics Laboratory in
the Faculty of Sciences at the Universidad de Antioquia,
with the assistance of Dr Alvaro Morales. The Mssbauer experiments were carried out in transmission

4.1. Chemistry of coal ash from different regions

The chemical composition of the coal ash (Table 3)
shows some degree of variation among the coals of
the different regions. The coals of the provinces of
Cundinamarca and Boyac (Checua-Lenguazaque,
Sogamoso-Jeric and Suesca-Albarracn), represented
by Samples 0034, 0035, 0036, 1083, have ash with high
percentages of SiO2 and Al2O3. The samples from the

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

Table 5
Mossbauer spectroscopy data (hyperfine parameter) for coal samples
Sample (mm/s) (mm/s) (mm/s) Rel area (%) Mineral
number
phase(s)
0034

0.6

0.33

0.3

0.93

2.8
1.6
0.52
2.5
1.6
0.58

1.33
1.34
0.08
1.22
1.31
0.29

0.33
0.33
0.54
0.5
0.56
0.34

0.023
0.045
0.41
0.3
0.28
0.88

2.9
1.7
0.64
2.8
1.7
0.61

1.22
1.31
0.35
1.19
1.31
0.29

0.42
0.75
0.40
0.35
0.44
0.35

0.07
0.05
0.56
0.28
0.16
0.86

0066

1.2
2.6
1.6
0.66
0.24
2.2
1.7
0.58

0.33
1.31
1.41
0.28
0.78
1.22
1.31
0.29

0.11
0.61
0.2
0.38
0.3
0.6
0.4
0.33

0.01
0.07
0.02
0.67
0.0005
0.23
0.08
0.86

0137

1.2
2.8
1.7
0.55

0.37
1.11
1.31
0.30

0.29
0.52
0.59
0.37

0.09
0.03
0.02
0.77

0322

1.0
2.9
1.6
0.56

0.95
1.22
1.31
0.29

0.42
0.48
0.6
0.32

0.001
0.19
0.04
0.86

0.91
2.9
0.64
1.2
2.8
2.3
0.63
0.82
2.7
0.88
0.62
0.98
2.8
1.5

0.35
1.51
0.33
0.38
1.22
1.22
0.29
0.47
1.31
1.31
0.30
0.95
1.22
1.31

0.36
0.41
0.35
0.33
0.55
0.1
0.35
0.39
0.47
0.24
0.37
0.42
0.48
0.6

0.1
0.017
0.56
0.25
012
0.06
0.88
0.11
0.004
0.09
0.77
0.001
0.19
0.04

0035

0036

0048

0056

0057

0330

0334

1083

Pyrite +
Kaolinite
Kaolinite
Ankerite
Kaolinite
Kaolinite
Ankerite
Pyrite +
Kaolinite
Kaolinite
Ankerite
Kaolinite
Kaolinite
Ankerite
Pyrite +
Kaolinite
Jarosite
Kaolinite
Ankerite
Kaolinite
Jarosite
Kaolinite
Ankerite
Pyrite +
Kaolinite
Jarosite
Kaolinite
Ankerite
Pyrite +
Kaolinite
Jarosite
Kaolinite
Ankerite
Pyrite +
Kaolinite
Jarosite
Kaolinite
Kaolinite
Jarosite
Kaolinite
Ankerite
Pyrite
Jarosite
Kaolinite
Ankerite
Kaolinite
Jarosite
Kaolinite
Ankerite

NOTE: r = quadrupole deployment, = isomeric deflection, referred to

the isomeric deflection of Fe, = width of line for each doublet, Rel
area = relative spectral area (%).

provinces of Antioquia and Crdoba (Amag-Sopetrn

and San Jorge), Samples 0056, 0057, 0066, have ash
with low percentages of SiO2 but high percentages of

Al2O3 and Fe2O3. The coals from the province of La

Guajira (Cerrejn), represented by Sample 0334, and the
province of Cesar (La Jagua; Sample 0330) both have
ash with high percentages of SiO2 and low percentages
of Al2O3. The coals from the different sequences in the
province of Cauca (Samples 0048, 0322) have ash with
markedly contrasting SiO2 and Al2O3 percentages.
The coal from the province of Caldas (Aranzazu;
Sample 0137) has ash with a low percentage of SiO2 but
high percentages of Fe2O3 and CaO. This ash is different
to that of all the other coals studied, possibly due to
the volcaniclastic character of the sediment associated
with the coal seams (Castao and Gmez, 2001). However, the coal in that sequence is also a low-rank coal
(Table 2), and, as discussed further below, the unusual
ash chemistry more probably reflects the presence of
high proportions of non-mineral inorganic elements
(cf. Ward, 2002), occurring either in the pore water or as
part of the organic matter.
4.2. Minerals in LTA residues
The overall proportion of LTA isolated from the coal
samples (Table 4) was typically between 10 and 15%.
One sample (0322) had a slightly higher LTA yield of
23%, and another (0048) a yield of around 35%. The
remaining sample, from the Cerrejon mine (0334), had a
very low proportion of mineral matter, with an LTA
yield of only 3%.
As indicated in Table 4, the most abundant minerals
in the LTA of the coal samples are quartz, kaolinite, illite
and interstratified illitesmectite (I/S). Together with
micaceous material (muscovite and/or paragonite) in
two samples and a trace of chlorite in one sample, these
typically make up at least 85% of the total mineral
Table 6
Petrographic composition data (%) for samples studied. (Minercol,
2001)
Sample
number

Vitrinite

Liptinite

Inertinite

Minerals

Vitrinite
reflectance

0034
0035
0036
0048
0056
0057
0066
0137
0322
0330
0334
1083

68.4
68.0
59.6
52.2
66.4
65.6
74.1
59.6
51.4
68.8
78.4
84.4

2.4
3.6
6.4
10.0
5.2
3.6
9.9
26.6
12.2
2.8
2.8
2.0

21.6
22.0
27.2
0.8
16.8
21.2
2.0
2.7
11.0
19.2
12.4
12.2

7.6
6.4
6.8
37.0
11.6
9.6
14.0
11.1
25.4
9.2
6.4
1.4

0.69
0.86
0.41
0.52
0.75
1.26
0.39

0.43
0.44
0.41

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

Table 7
Inferred composition of coal ash from Siroquant data
Sample

0034

0035

0036

0048

0056

0057

0066

0330

0334

1083

LTA %
SiO2
Al2O3
Fe2O3
MgO
CaO
Na2O
K2O
P2O5
SO3
Total

13.2
64.35
28.39
3.35
0.28
0.58
0.22
2.13
0.33
0.36
100.00

11.7
66.22
30.55
1.03
0.15
0.10
0.11
1.83
0.00
0.00
100.00

11.0
65.22
32.39
0.66
0.10
0.07
0.08
1.48
0.00
0.00
100.00

34.8
56.34
38.98
0.00
0.09
2.15
0.06
2.38
0.00
0.00
100.00

14.7
54.28
32.21
10.20
0.46
0.48
0.18
2.19
0.00
0.00
100.00

14.0
60.34
24.58
5.06
3.58
3.11
0.15
2.56
0.00
0.63
100.00

12.8
52.82
30.05
8.69
0.00
1.09
0.00
3.44
0.00
3.92
100.00

10.5
76.42
20.63
0.00
0.00
0.00
0.10
2.85
0.00
0.00
100.00

3.0
72.74
10.96
10.46
0.00
1.35
0.00
0.93
0.00
3.55
100.00

10.0
70.41
26.79
0.65
0.15
0.10
0.11
1.79
0.00
0.00
100.00

matter. The remainder is represented by pyrite, which

constitutes more than 10% of the LTA in some samples
but is absent from the LTA in others, or by carbonate
minerals: siderite, calcite, dolomite and ankerite.
Other minerals identified from the XRD data, typically in low concentrations, include feldspar (albite), the
bauxite mineral boehmite (Al.O.OH), phosphates such
as apatite and goyazite, and sulphate minerals such as
jarosite, coquimbite and bassanite. Although many of
the sulphates may be derived from oxidation of pyrite
(Rao and Gluskoter, 1973), either with sample storage or
during low-temperature ashing, at least some of the
sulphate minerals, particularly the bassanite, may represent artifacts of the low-temperature ashing process
(Ward, 2002), produced by interaction of organically
associated inorganic elements with the organic sulphur
during oxidation of the maceral components.
The coals from the Cretaceous to Early Tertiary
Guaduas Formation, in the provinces of Cundinamarca
and Boyac, mostly have LTA with relatively low pyrite
contents, and the mineral matter consists almost entirely
of quartz and the clay minerals. Quartz typically makes
up 2030% of the LTA isolated from these coals, and
kaolinite (3555%) usually makes up the bulk of the
clay mineral fraction. Traces of siderite are also present
in some samples. The LTA of the coal from the middle
Tertiary Guachinte Formation (0048) in the province of
Cauca has a similar mineralogy, but has a significantly
lower proportion of quartz and a higher proportion of
kaolinite and illite than the LTA of the Guaduas Formation samples.
The LTA of the coals from the OligoceneMiocene
Amag and Mosquera Formations, in the provinces of
Antioquia and Cauca, and the coal from the Cerrito
Formation in the province of Crdoba, mostly contain
significant proportions of pyrite. In the sample from the
Cerrito Formation (0066) the pyrite is accompanied by
the iron sulphate minerals jarosite and coquimbite. As

discussed above, the jarosite and coquimbite may

represent oxidation products of the pyrite, formed either
by exposure of the coal to the atmosphere during sample
storage or possibly by exposure of the pyrite to activated
oxygen in the low-temperature ashing process. The
absence of these minerals from the LTA of the other
pyrite-rich coals in the same group (0056 and 0322),
however, suggests that oxidation of the pyrite during
ashing is less likely to be involved.
One of the Amag Formation samples (0057) contains a significant proportion of ankerite (ferroan dolomite), along with a trace of siderite. Traces of dolomite
are also noted in the LTA of some other coal samples
from this group (0056 and 0322).
The LTA of the low-ash sample from the Cerrejn
Formation (0334) has a high proportion (14%) of pyrite
and a significant proportion (3.5%) of coquimbite. The
LTA of this coal also has a relatively high proportion
(54%) of quartz, and lower proportions of clay minerals,
kaolinite, illite, and especially I/S, than most of the other
coal samples studied. The LTA of one of the samples
from the Mosquera Formation (0322) also has a relatively high quartz content.
Mica minerals identified as muscovite and paragonite
(Na mica) are present in the LTA of the sample from the
Palaeocene Los Cuervos Formation in the province of
Cesar. These minerals have a significantly different
XRD pattern from the illite more commonly found in the
coal samples. The formation of paragonite by thermal
metamorphism of an otherwise low-rank Indonesian
coal has been described by Susilawati and Ward (2006).
However, there appear to be no unusual heat sources,
such as igneous intrusions, associated with the coals of
the Los Cuervos Formation, and in the absence of any
such effects the paragonite is assumed to represent
material of essentially detrital origin.
The LTA of the coal from the MiocenePliocene of the
Aranzazu area (sample 0137), contains a range of sulphate

10

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

Fig. 2. Plots showing comparison between proportions of major element oxides in coal ash inferred from Siroquant data to proportions of the same
oxides determined directly by ash analysis. A) SiO2; B) Al2O3; C) Fe2O3; D) CaO; E) MgO; F) K2O. The diagonal line on each plot represents
equality of the two estimates.

minerals, including bassanite (CaSO41 / 2H2O), alunogen

(Al 2 (SO 4 ) 3 17H 2 O), hexahydrite (MgSO 4 6H 2 O),
tschermigite (NH4Al(SO4)212H2O) and paraluminite
(Al4SO4(OH)1010H2O), along with a small proportion
of quartz. The sulphate minerals probably all represent
artifacts of the low-temperature ashing process, produced by interaction of inorganic elements in the organic
matter, as well possibly as nitrogen in the coal, with
organic sulphur during oxidation. Such artifacts are
common in the LTA of lignites and other lower-rank
coals (cf. Ward et al., 2001), and their occurrence in the

LTA of this sample is consistent with the rank of the coal

(lignite A) as indicated in Table 2. Some of these
minerals are not in the current Siroquant database, however, and hence evaluation of their relative proportions
could not be carried out as part of the present study.
4.3. Relation of minerals to ash chemistry
The chemical composition of the coal ash implied by
the quantitative analysis of the mineral matter from the
XRD study was calculated for each coal sample, based on

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

Fig. 3. Comparison of proportion of LTA determined by oxygenplasma ashing (wt.%) with proportion of minerals identified by point
counting (vol.%).

the proportions of each mineral indicated by Siroquant and

stoichiometric data or typical published chemical analyses
for the minerals in question (Ward et al., 1999). The
results, after allowance for loss of H2O, CO2 and other
constituents from the minerals during ashing (Table 7),
were compared to the actual (high-temperature) ash anal-

11

ysis data for the same coal samples (Table 3), determined
using atomic absorption techniques.
Graphic plots illustrating the comparison for each
major oxide are given in Fig. 2. Linear regression lines
are shown for each plot, together with the equation for
each regression line ( y = ax + b) and the relevant
correlation coefficient (R2). A diagonal line is also
drawn on each graph, representing the line along which
the points would fall if the proportions of the relevant
oxide estimated from the Siroquant data were exactly
equal to those determined directly by chemical analysis.
For a perfect correlation, all points would plot along this
line, and the correlation equation parameters would be:
a = 1, b = 0, and R2 = 1.0.
Fig. 2 suggests a good level of agreement for SiO2
(Fig. 2A), with seven of the ten points falling very close
to the diagonal equality line. Although the correlation
coefficient is quite high (R2 = 0.87), the parameters of
the regression equation (a and b) depart slightly from
the ideal values due to the influence of three low-silica
data points with outlier characteristics. Extrapolation of
the regression line including these outliers results in an

Table 8
Modes of mineral occurrence as indicated by microscopic analysis
Sample
number

Area

0034

ChecuaLenguazaque

0035
0036

0048

0056
0057

0066

0330
0334
1083

Mineral association

Pyrite occurs as framboids, anhedral crystals, and finely disseminated pyrite completely surrounded by vitrinite. The quartz
occurs as rounded grains. The carbonates are fine-grained replacing liptinite. Aggregates of minerals and macerals (see
Fig. 4).
ChecuaPyrite occurs as disseminated anhedral crystals and as framboids. The quartz occurs as sub-rounded and angular grains in
Lenguazaque vitrinite and inertinite. Aggregates of minerals and macerals. (see Fig. 5A and B).
SogamosoPyrite occurs as finely disseminations crystals in the coal grains, as anhedral crystals, as framboids and aggregates of
Jeric
framboids, and as grained pyrite filling microfractures. There are also fine-grained minerals replacing liptinite macerals (see
Fig. 5C and D).
El HoyoPyrite occurs as anhedral crystals and as finely disseminated particles in the coal grains. The carbonate occurs as crystals and
Mosquera
fine-grained spheroidal aggregates with vitrinite and pyrite. There are also aggregates of minerals and macerals (vitrinite and
liptinite). This sample also has abundant aggregates of individual minerals (see Fig. 5E).
AmagPyrite occurs as massive aggregates, as finely disseminated pyrite, as framboidal aggregates, and as crystals filling
Sopetran
microfractures and pores of inertinite. There are also fine-grained aggregates of carbonate, pyrite and vitrinite (see Fig. 6).
AmagPyrite occurs as finely disseminated material replacing liptinite, as fine-grained aggregates filling microfractures, as
Sopetran
framboids, and in fine-grained reniform aggregates (bunch of grapes structure). Carbonates in fine-grained aggregates, as
fine-grained disseminated and partial replaced of liptinites. There are also aggregates of minerals and macerals (see Fig. 7A
and B).
San Jorge
Pyrite occurs as fine-grained finely disseminated crystals and as framboidal aggregates. The carbonates occur as finegrained aggregates, as fine-grained disseminated crystals in vitrinite, as fillings of pores in sclerotinite, and partially
replacing liptinite. Minerals (framboid pyrite and fine-grained) and macerals aggregates.
La Jagua de
Pyrite occurs as fine-grained disseminated crystals in vitrinite, as framboids, and as fine-grained aggregates filling
Ibirico
microfractures. The carbonates occur as fillings of microfractures. Minerals and macerals aggregates (see Fig. 7C,D,E).
Cerrejn Zona Pyrite occurs as fine-grained disseminations, as anhedral grains, as framboids and framboidal aggregates with
Norte
carbonate and fragmental vitrinite, as fine-grained aggregates in vitrinite, and filling microfractures.
SuescaPyrite occurs as anhedral grains, as fine-grained disseminations in vitrinite, as framboids pyrite, as irregular
Albarracn
aggregates, and filling the pores of inertinite. The carbonates occur as fine-grained masses partially replacing liptinite,
as infillings of pores in inertinite, as infillings of microfractures, and as minerals and macerals aggregates (see Fig. 8).

12

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

intercept on the y-axis (b value) higher than suggested

by the points covering most of the determinations.
The correlation coefficients and regression line
parameters for Al2O3 (Fig. 2B) are close to the ideal
values, although the overall comparison suggests a very
slight over-estimation of Al2O3 by the XRD data for
most of the samples. The proportion of Fe2O3 indicated
by calculation from the XRD data (Fig. 2C), on the other
hand, appears in all cases to be slightly lower than the
directly-analysed values. The difference may reflect
omission of Fe from the chemical composition data used
for illite and illite/smectite in the calculation of the
inferred ash chemistry (cf. Ward et al., 1999). The illite
composition used in the present calculations was that of
a diocathedral mineral with Al and no significant Fe.
Some Fe may, however, be substituted for Al in the illite
and I/S structures in the LTA residues of these particular
coal samples, providing a possible explanation for the
higher inferred Al2O3 and lower inferred Fe2O3 percentages relative to the direct determinations. Alternatively, some of the Fe in the coals may occur in a noncrystalline form, such as poorly-crystallized iron oxides,
or as a component of the organic matter. Residues of

such materials are not likely to be detected by XRD

techniques.
Fig. 2 also suggests that the chemistry inferred from
the XRD data generally under-estimates the CaO and
MgO contents of the ash samples. Although the proportion of CaO in most cases is relatively close to the
equality line (Fig. 2D), one sample (0057) represents an
outlier, with only around half of the CaO identified by
direct ash analysis apparently represented by Ca-bearing
minerals identified in the XRD study. The (high-temperature) ash of this sample has an unusually high proportion of SO3 (Table 3), but the LTA has only a low
proportion of crystalline bassanite (Table 4). It may be
that much of the Ca associated in this sample is associated with the organic matter and provided a site for
sulphur fixation, but that only poorly-crystallized
bassanite was formed as an artifact in the LTA residue
and as such was not detectable by XRD techniques. For
MgO (Fig. 2E), the sample with abundant ankerite
(Sample 0057) plots close to the equality line, suggesting that most of the Mg, at least in this sample, occurs in
the carbonate component. The Mg in the other samples,
however, may also occur as mainly a component of the

Fig. 4. Modes of mineral occurrence in coal sample 0034: A) aggregates of macerals and minerals, PPL; B) aggregates of macerals and minerals,
XPL; C) pyrite in fine-grained aggregates, PPL; D) pyrite in fine-grained aggregates, XPL; E) pyrite filling pores in inertinite, PPL; F) carbonate
filling fractures, PPL. All photomicrographs taken on polished surfaces under oil immersion, 500.

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

13

Fig. 5. Modes of mineral occurrence in coal samples: A) aggregates of macerals and minerals in sample 0035, XPL; B) quartz in sample 0035, PPL; C):
framboids of pyrite in sample 0036, XPL; D) Pyrite filling fractures in sample 0036, PPL; E) aggregates of macerals and minerals in sample 0048, PPL.
All photomicrographs taken on polished surfaces under oil immersion, 500.

organic matter, and form essentially non-crystalline

artifacts in the LTA residues of the coal samples.
Estimates of K2O provide a more scattered correlation (Fig. 2F), possibly due to variations in the saturation
of K+ in the illite and illite/smectite constituents. This
is difficult to allow for in stoichiometric calculations
(Ward et al., 1999). Although it represents a significant
component of the coal ash (Table 3), Na2O is not represented to any great extent in the stoichiometric composition of the minerals identified by XRD. It was
therefore not plotted as part of these correlations. Table 3
also indicates that Na2O is also less abundant than K2O
in most of the samples studied. Some Na may occur in
association with the organic matter, for example as ions
dissolved in the pore water, in which case it would not be
expected to appear as crystalline phases in the LTA
derived from the coal samples.
4.4. Relation between XRD and Mssbauer spectroscopy
data
Mssbauer spectroscopy has been used by a number of
researchers on coal samples (e.g. Gracia et al., 1999;
Ahmed et al., 1999, 2003), mainly to investigate the ironbearing phases. Interpretation of the Mssbauer spectra
obtained for the present study (Table 5) indicates the

presence of pyrite in those samples for which XRD analysis

(Table 4) shows its occurrence in measurable proportions
within the mineral matter. These include samples 0034,
0036, 0056, 0066, 0322 and 0334. Samples producing LTA
in which no or very little pyrite was identified (samples
0035, 0048, 0057, 0330 and 1083) do not display
recognizable pyrite patterns in Mssbauer spectral studies.
It is perhaps significant to note that samples 0036, in
which pyrite was identified from the Mssbauer data,
and 1083, in which it was not identified, both have LTA
containing similar, relatively low proportions of pyrite
(0.9%), as indicated by the XRD data (Table 4). Pyrite
was not, moreover, identified by Mssbauer studies in
sample 0035, for which XRD analysis indicates that the
LTA contains around 0.3% pyrite. This may reflect the
occurrence of the pyrite in sample 0035 as fine particles
within the organic matter, not readily liberated by grinding
for the float-sink concentration used in the Mssbauer
evaluations. It thus appears that, for the experimental
conditions used in the present study, a lower limit probably
exists at around 1% pyrite in the mineral matter for
identification of pyrite in Colombian coals by Mssbauer
techniques.
The presence of jarosite is indicated in a number of
samples by the Mssbauer data, but only in four samples,
0066, 0322, 0330 and 0334, is the relative area as listed in

14

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

Fig. 6. Modes of mineral occurrence in coal sample 0056: A) aggregates of macerals and minerals, PPL; B) aggregates of macerals and minerals,
XPL; C) carbonate, PPL; D) carbonate, XPL; E) framboids of pyrite, PPL; F) aggregates of pyrite framboids, PPL; G) pyrite filling fractures.
All photomicrographs taken on polished surfaces under oil immersion, 500.

Table 5 greater than around 0.1%. Jarosite and/or the

slightly more dehydrated iron sulphate coquimbite are indicated in the LTA of two of these samples (0066 and 0334)
by the X-ray diffraction data (Table 3), suggesting consistency between the XRD and the Mssbauer interpretation. The X-ray diffraction data indicate a relatively high
proportion of pyrite in the LTA of sample 0322, and hence
the jarosite indicated by Mssbauer studies in this sample
may be derived from oxidation of pyrite prior to the
Mssbauer determinations. For sample 0330, however, no
pyrite and no iron sulphate materials are indicated by the
XRD study.

Identification of jarosite in samples 0066, 0322 and

0334 by the Mssbauer technique, which was applied
to mineral concentrates and not to LTA residues, also
indicates that the iron sulphate minerals found in the LTA
of the same samples were products of pyrite oxidation with
exposure or storage, and were not formed by oxidation of
the pyrite in the coals during the plasma ashing process.
5. Modes of mineral occurrence
As indicated in Table 6, the coals are typically richer in
vitrinite than inertinite macerals, with over 60% vitrinite

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

15

Fig. 7. Modes of mineral occurrence in coal samples: A) partial replacement of liptinites by minerals in sample 0057, PPL; B) rounded grains quartz in
vitrinite, sample 0057, PPL; C) carbonate finely disseminated in vitrinite, sample 0030, PPL; D) pyrite filling pores in inertinite, sample 0030, PPL;
E) Pyrite filling pores in inertinite, sample 0030, PPL. All photomicrographs taken on polished surfaces under oil inmersion, 500.

and 1220% inertinite in most of the samples studied.

Those coals with lower proportions of vitrinite (e.g. 0048
and 0322) have high proportions of mineral components,
and would have significantly greater proportions of vitrinite
if the analyses were expressed to a mineral-free basis.
Liptinite usually makes up only a small fraction
(b5%) of the maceral material. It is, however, relatively
abundant in four of the coals studied (0048, 0066, 0322
and 0137). Liptinite is particularly abundant, especially
as a fraction of the maceral components, in sample 0137,
from the Aranzazu volcaniclastic sequence. Castao and
Gomez (2001) consider that the coals of this sequence
were generated in a limnic depositional environment,
with open marsh to clastic marsh settings and a high
density of herbaceous vegetation, under a temperate
climate and possibly rheotrophic conditions.
The volumetric proportion of visible minerals in the
coals studied ranges from 1 to 37% (Table 6). As indicated
in Fig. 3, this percentage is broadly similar to, although
mostly somewhat lower than, the proportion of LTA
isolated from the same coal samples. Since the density of
the minerals in coal is usually around twice the density of
the maceral components, the proportion of visible

minerals, which is expressed as a volume percentage,

would be expected to be around half the weight
percentage of the same mineral fraction isolated by lowtemperature ashing. Fig. 3, however, suggests a relationship somewhat closer to equality. This may be due to
intimate admixture of macerals and minerals within the
coals, so that a certain amount of organic matter is also
included with the identified mineral masses, or possibly
due to differences in the sample splits actually examined
in the separate laboratories involved.
The mode of occurrence of the visible mineral components is described briefly in Table 8, and photomicrographs of representative coal specimens showing some
of the key mineral occurrences are given in Figs. 48.
Although its presence is not always recognised by
XRD or Mssbauer spectroscopy (Tables 3 and 4), at
least traces of pyrite are visible under the microscope in
all of the coal samples studied. The high reflectance of
the material and the contrast to the maceral components
serve to facilitate recognition, even at low concentrations, in polished sections of such coal samples.
The pyrite in the coals displays a wide range of
textures, including occurrence as individual grains

16

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

Fig. 8. Modes of mineral occurrence in coal sample 1083: A) carbonate filling fractures, PPL; B) carbonate filling fractures, XPL; C) aggregates of
minerals, PPL; D) partial replacement of liptinite by minerals, PPL; E) aggregates of minerals, XPL. All photomicrographs taken on polished surfaces
under oil immersion, 500.

disseminated inside the macerals, as crystalline aggregates (framboids and coarser grained aggregates), as
infillings of pores (including lumens in sclerotinite), and
as replacements of the maceral components. These
indicate mainly a syngenetic origin. In some samples the
pyrite also occurs as fracture infills, suggesting also an
epigenetic origin.
The carbonate minerals, where present, have a
similar mode of occurrence to the pyrite, with crystals
and fine-grained aggregates, maceral replacements
(especially of liptinite) and fracture fillings. In sample
0057, for example, the carbonates occur as fine-grained
aggregates, as fine-grained disseminated minerals, and
as partial replacements of liptinite macerals.
Quartz occurs as sub-angular and rounded particles
that probably represent material of detrital origin. Much
of the other mineral material, mainly representing the
clay minerals identified by the XRD study, appears to
occur as intimate admixtures with the maceral components (mineral-maceral aggregates), with a mode of
origin that cannot readily be interpreted from microscopic studies.

6. Conclusions
The minerals in Colombian coals are chiefly
represented by kaolinite, illite, interstratified illite/
smectite and quartz. Pyrite is also relatively abundant
in some cases, making up to around 10% of the mineral
matter in several coal samples, but even though it is seen
under the optical microscope in most coal samples it is
not always present in sufficient concentrations to be
identified by XRD or Mssbauer spectroscopy studies.
Micas, including the sodium-bearing variety paragonite, carbonates (calcite, dolomite, ankerite and/or
siderite) and phosphates (apatite and goyazite) are also
present, although typically in low concentrations, in
some coal samples.
A range of sulphate minerals has been identified in
the LTA of some coal samples. Some of these sulphates,
such as jarosite and coquimbite, probably represent
oxidation products of pyrite, developed during exposure
or storage. Others, such as bassanite, probably represent
products of interactions between organically associated
inorganic constituents during the plasma ashing process.

I. Carmona, C.R. Ward / International Journal of Coal Geology 73 (2008) 318

The LTA of the lignite sample from the Aranzazu volcaniclastic sequence contains an abundance of such
sulphate artifacts, including a range of aluminium and
ammonium sulphate components.
Quantitative analysis of X-ray diffraction data by
Rietveld techniques provides estimates of the mineral
percentages in the LTA residues that are for the most part
consistent with the chemistry of the high-temperature
ash as determined by independent chemical analysis.
Comparison of the XRD data with the Mssbauer spectroscopy interpretations suggest that the lower limit of
pyrite concentration at which the mineral can be identified by the Mssbauer techniques used in the study is
around 1% of the total mineral fraction in the coal
samples.
The minerals observed by microscopic study are
intimately associated with the organic constituents of the
coals. Pyrite, and in some cases carbonates, occur as
anhedral crystals, finely disseminated in the maceral
grains, as aggregates of crystals (including pyrite framboids), as fine-grained crystals replacing liptinite, and as
fracture fillings. Some sub-angular to rounded quartz
grains are also present, possibly of detrital origin, but
most other minerals, including most of the clay minerals, occur mainly as aggregates consisting of intimately admixed mineral and maceral constituents.
This study has provided a general overview of the
range of mineral matter found in coals from the different
regions and sequences of Colombia, as a basis for
characterizing the coals in relation to materials from
other countries. It also provides a reference data-set for
further investigating relationships between mineral
matter and other geological factors within the various
coal-bearing regions. Extension of such studies to a
wider range of samples from individual coalfields, seams
and mine sites may be of value in further understanding
the mineralogical characteristics of the coals in the
different coal-bearing regions of Colombia, and in
relating key coal characteristics more specifically to
different aspects of utilisation and environmental impact
assessment.
Acknowledgements
This work was completed with the support of
Investigation Direction of the Universidad Nacional de
Colombia, Sede Medelln, the Colombian Institute of
Geology of Mining (INGEOMINAS) and of the School
of Biological, Earth and Environmental Sciences at the
University of New South Wales. Special thanks are
expressed to Prof Alvaro Morales, of the Faculty of
Sciences at the Universidad de Antiquia, for execution

17

of the Mssbauer spectroscopy analyses. Thanks are

also extended to Dr Zhongsheng Li, of UNSW, for
assistance with the plasma ashing and XRD analysis,
and to Frank Stoddart and David French, as well as the
referees, for their helpful advice on different aspects of
the paper.
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