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A more accurate method for estimating in situ coal density and mineral
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Article  in  International Journal of Coal Geology · November 2016

DOI: 10.1016/j.coal.2016.11.007

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 International Journal of Coal Geology 168 (2016) 237–252

Contents lists available at ScienceDirect

International Journal of Coal Geology

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

A more accurate method for estimating in situ coal density and mineral
matter from ash and specific energy determinations
Eric Robeck a,⁎, Dennis Huo b
a
Weir International, Inc., 1431 Opus Place Suite 210, Downers Grove, IL 60515, USA
b
Peabody Energy Australia, 100 Melbourne Street, South Brisbane, Queensland 4101, Australia

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

Article history: The estimation of in situ coal density has been the subject of extensive research due to its importance for coal re-
Received 8 April 2016 serve estimation. However, despite decades of studies, a universal method for density estimation that can be ap-
Received in revised form 9 November 2016 plied to all coal deposits still does not exist. Traditional ash-based methods are inaccurate because ash is a
Accepted 10 November 2016
combustion product that does not contain the volatile mineral components which are lost upon combustion.
Available online 14 November 2016
Coal is composed of three primary constituents: organic macerals, inorganic mineral matter, and moisture. Un-
Keywords:
derstanding the properties of the mineral matter is particularly critical for accurate density estimation. The meth-
Coal od described herein improves the accuracy of density estimates by first estimating the mineral matter percentage
Ash of each sample using only ash and specific energy analyses, both of which are performed on the large majority of
Density exploration samples. A least-squares hyperbolic formula is derived from the dry coal and mineral properties in
Specific gravity order to estimate the dry sample density. The formula accepts two in situ moisture percentages, for both coal
In situ and rock, in order to estimate in situ density for coal and other lithologies.
Mineral matter This method has several advantages over existing techniques. It is valid for all values of ash, with no loss in accu-
Macerals
racy outside a limited range. The scatter caused by mineral volatiles is reduced, resulting in a much higher corre-
Moisture
lation coefficient. Coal and mineral densities derived from the formula may also provide insight into the coal
Petrography
maceral and mineral types present within a project, as well as changes in mineralogy with ash content.
© 2016 Elsevier B.V. All rights reserved.

1. Introduction
Reliable estimates of density are essential to the valuation and oper-
ation of coal mines, as they are used to quantify reserves and resources,
calculate stripping ratios, estimate recovery, and in some jurisdictions
determine royalty or tax payments. Even small errors in density
estimates can add or remove many millions of tons of reserves, and
discrepancies may be difficult to catch before production begins. In
the last couple of decades, a great deal of research has gone into the in-
vestigation of new methods for calculating in situ density, particularly in
Australia (Ryan, 1990; Smith, 1991; Preston and Sanders, 1993; Fletcher
and Sanders, 2003; Sanders, 2003; Meyers et al., 2004; Preston, 2005).
This is partly in response to increasing regulatory scrutiny and the de-
velopment of rigorous international mineral reporting codes.
Public companies must submit resource and reserve reports pre-
pared by independent experts (referred to as Qualified Persons or Com-
petent Persons) based on the international reporting standard accepted
by the relevant stock exchange. The Committee for Mineral Reserves In-
ternational Reporting Standards (CRIRSCO) has established standards
⁎ Corresponding author.
E-mail address: erobeck@gmail.com (E. Robeck).
for national codes that are recognized and adopted worldwide for
market-related reporting and financial investment, including the Aus-
tralasian Code for Reporting of Exploration Results, Mineral Resources
and Reserves (JORC Code), Canadian National Instrument 43-101 (NI
43-101) and South African Mineral Resource Committee (SAMREC). In
June 2016, the United States Securities and Exchange Commission
(SEC) proposed revisions to its own rules governing property disclo-
sures for mining registrants, which would also bring them into compli-
ance with CRIRSCO and significantly increase the level of scrutiny
applied to coal resource and reserve estimates for U.S. based mining
companies. Because reserve tonnage is extremely sensitive to changes
in density, regulatory agencies require that the calculations be per-
formed as accurately as possible.
Testing coal and non-coal plies within workable seams for relative
density (RD), also referred to as specific gravity, is an important best
practice for routine sample analysis in coal exploration and mining pro-
grams. However, many companies (particularly in the U.S.) test only a
fraction of the total samples for RD, and often exclude non-coal plies
within the planned working section. Some companies have begun to
rely on Apparent Relative Density (ARD) testing (Australian Standard
1038.26) for reserve estimation. However, ARD data are unsuitable for
density estimation because they are performed on lump samples

http://dx.doi.org/10.1016/j.coal.2016.11.007
0166-5162/© 2016 Elsevier B.V. All rights reserved.
238 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252

which have not been crushed and analyzed for moisture. The unknown Table 1
moisture content makes it impossible to accurately determine the coal List of abbreviations.

and mineral particle densities. Sparsely sampled or incomplete RD Parameter Subscript

data may cause significant errors in reserve estimation. In standard geo- ρ Density (g/cm3) Constituent Sulfur form
logical models, the coal seam density models become decoupled from r Mineral matter ratio c coal org organic
more closely sampled parameters, such as ash, with the result that ϕ Void porosity (air-filled) m mineral pyr pyritic
local variations in density are not represented by the model. When esti- A Ash s sample sul sulfate
C Carbon w water tot total
mating coal reserves and quality, it is critical that RD be estimated for all
D Relative density (unitless) Moisture basis
samples, not just coal, because the density of coal is approximately half E Specific energy is in situ
that of most minerals. For working section composites that include out- H Hydrogen ad air dried
of-seam strata, thickness-weighted average values only account for M Moisture d dry
about 50 to 70% of the total non-coal material. S Sulfur daf dry, ash free
V Volatile matter dmmf dry, mineral matter free
Coal density is correlated to three primary constituents: macerals
(organic units composing the coal mass), minerals, and moisture. In
situ density can be estimated by knowing the properties and relative
proportions of each constituent. Traditional ash-based methods to esti- Coal macerals have relatively low densities (generally 1.2–1.6 g/cm3)
mate density are imprecise because ash is a combustion residue that while most minerals have much higher densities (2.2–5.0 g/cm3). For
does not contain all of the original mineral matter, as volatile compo- calculation purposes, it may be assumed that a sample (excluding mois-
nents of the minerals are lost upon combustion. However, the mineral ture) is represented by a two-phase mixture of pure coal with density ρc
matter content is rarely analyzed in coal analysis programs. In order to and pure mineral with density ρm. Pure “coal” consists entirely of
significantly improve the accuracy of coal density estimates, it is neces- macerals and thus has a mineral matter percentage (md) of zero,
sary to determine mineral matter content using alternate techniques while for all minerals the value of md is 100. The density of a particular
that are inexpensive, available for a large fraction of exploration sam- sample can be estimated by the following formula:
ples, and applicable to the historical samples which comprise the bulk
of many mine databases. 100ρc ρm
ρd ¼ ð1Þ
This paper reviews several previously-published approaches to the ρc md þ ρm ð100−md Þ
estimation of mineral matter and in situ density, and then describes a
new method for the estimation of coal and rock density. Techniques where
are developed to estimate mineral matter percentage using only data
for RD, ash, and specific energy (SE) (expressed as Btu/lb, kcal/kg or ρd sample density (g/cm3), dry basis
MJ/kg). These common parameters are used to establish a least- ρc pure coal density (g/cm3)
squares regression equation between RD and mineral matter percent- ρm pure mineral density (g/cm3)
age. Among the outputs of the regression are the average maceral and md mineral matter percentage, dry basis.
mineral densities, which can be validated against common values listed
in this paper. Once the initial regression is established, only ash and SE When plotted as a function of mineral matter percentage, sample
data are required to estimate the dry RD of each sample, and realistic ap- density takes the form of a hyperbola with values ρc at md = 0 and ρm
proximations can be made using only ash data. In situ RD is calculated at md = 100 (Fig. 1).
by applying the in situ moisture percentage for coal (and another for The simplistic two-phase “coal/mineral” mixture is complicated by
rock, if desired), which can be estimated using various methods (e.g. the (a) mineral composition, (b) relative proportions of the different
Fletcher and Sanders, 2003; Meyers et al., 2004). Even in the absence macerals, (c) coal rank, and (d) presence of water- and air-filled
of RD measurements, this method makes it possible to generate a fully
deterministic relationship between density and ash for various coal
and rock types using reasonable estimates of coal petrography, mineral-
ogy, and in situ moisture. m

Examples are presented using data from multiple coal seams in the
late Permian Ulan Coal Member of the Illawarra Coal Measures, in
New South Wales, Australia. The coal is primarily dull with minor bright
bands, high in ash, low in sulfur, and of high volatile A bituminous rank.
Density (dry basis)

Interburden and non-coal plies are characterized by tuffaceous

claystone, carbonaceous claystone, siltstone, and rare sandstone lenses.
The dataset consists of a total of 3969 samples with air-dried RD data, of
which 1266 samples were also analyzed for air-dried SE; the latter were
used to develop a site-specific regression formula for in situ density
against dry ash. In addition, there are 96 samples with extended analysis
data (including ultimate analysis) which were used for comparison
with empirical formulas developed by other researchers (Fletcher and
Sanders, 2003; Meyers et al., 2004; Smith, 1991).
A number of terms are used develop the theoretical framework and
mathematical methods for coal density estimation. While these terms
are defined in the text, they are contained in Table 1 for reference. c

0 100
2. Coal and mineral matter

Coal is a heterogeneous material composed of solid particles, liquids, Fig. 1. Sample density as a function of mineral matter percentage, demonstrating the
and gases. The particles consist primarily of various coal macerals hyperbolic relationship between a two-phase mixture of pure coal (maceral) and
(metamorphosed organic matter, or kerogens) and inorganic minerals. mineral, each with a constant density.
 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252 239

pores. The nature and relative abundance of the individual minerals and
macerals within a given coal sample may vary widely, and thus a simple
model with single density values for the (total) minerals and (total) or-
ganic matter is only an approximation.
In addition to the organic material in coal, which is represented by
various coal macerals, some volatile matter is lost from the minerals
upon combustion, e.g. water of hydration from clay minerals, CO2
from carbonates, sulfur from sulfides and some sulfates, and chlorine
from any salts that may be in the coal (Ward, 1984). As a result, the per-
centage of ash (solid residue) is less than the mass of the original min-
erals (Fig. 2).
Because most minerals contain some volatile matter, the ash per-
centage is almost never 100%, even in samples lacking carbonaceous
material. The proportion of original mineral matter relative to the ash
percentage is represented by the “mineral matter ratio” which is de-
fined as follows:
md
r¼
Ad
where
Ad ash, dry basis
md mineral matter, dry basis
r mineral matter ratio.
The terms density and RD (or specific gravity) are often used inter-
changeably, but they have different units. Density is the mass per unit
volume, often expressed as grams per cubic centimeter (the units
used in this paper). RD is the mass of a substance relative to the mass
of water displaced by the sample and is therefore unitless. For practical
and theoretical purposes most formulas in this paper refer to density, al-
though the results of laboratory analyses are reported as RD. Conversion
Surface Moisture
Total
Moisture
Inherent Moisture
Ash
Mineral
Mineral
from one to the other is simple:
ρs
D¼ ð3Þ
ρw
where
D sample RD (unitless)
ρs sample density (g/cm3)
ρw density of water at 4.0 °C (g/cm3).
The percentage of ash produced by a sample upon combustion
depends on the total mineral content and the nature of those min-
erals. The ash yield excludes any volatiles lost from the mineral mat-
ter in the ashing process (Fig. 2). The proportion of volatiles
produced is highly variable and depends upon the mineral composi-
tion. Minerals that produce significant volatiles have large mineral
matter ratios (r) because the mass of the original minerals is high rel-
ative to the residual ash (Eq. (2)). Average densities and mineral
ð2Þ
matter ratios are shown for a few minerals commonly found in coal
in Table 2.
While individual mineral densities vary, most of the minerals in
Table 2 have a density between 2.5 and 2.8 g/cm 3 . The value of r
can range from 1.0 to nearly 2.0 depending on the proportions of
constituent minerals, but aggregate sample values above 1.5 are
rarely observed. Similarly, the dry, mineral matter free (dmmf) den-
sity of coal macerals can range from 1.0 to 1.7 g/cm3 although aver-
age distributions usually range from 1.2 to 1.6 g/cm 3 (Table 3).
Examples of density distribution in four coal lithotypes are shown
in Fig. 3.
Smith (1991) and Sanders (2003) noted that ρc is a function of
rank, increasing with the degree of coalification. As rank increases
and volatile elements (H, N and O) are lost, the average density of
the organic matter increases, although the change in density from
lignite to low volatile bituminous rank is generally b0.1 g/cm3
(Mahajan, 1982). Thus, ρc is more strongly correlated to the coal
type, or overall maceral distribution (Table 3), which is largely inde-
pendent of rank (O'Keefe et al., 2013). Coal seams within a particular
deposit may have distinct density “signatures” based on the compo-
sitional differences resulting from their unique depositional
environments.
The relationship between ash and float/sink gravity in washabili-
ty analysis is similar to that of ash and RD values in untreated coal
samples, and provides an important validation of the hyperbolic re-
lationship described above. The RD of each washed fraction may be
approximated as the midpoint of the heavy liquid float and sink
Table 2
Mineral matter densities (ρm) and ratios (r) for common minerals (Ryan, 1990; Vassilev
et al., 2010).

Mineral Chemical composition ρm r Mass

(g/cm3) loss
Organic
(%)

Quartz SiO2 2.65 1.00 0

Pure Kaolinite Al2Si2O5(OH)4 2.16–2.68 1.16 14.0
Coal Illite KAl4(AlSi7O20)(OH)4 2.6–2.9 1.05 4.5
(Macerals) Montmorillonite (½Ca,Na)0.7(Al,Mg,Fe)4[(Si,Al)4O10]2 1.7–2.0 1.05 5.0
(smectite) (OH)4·nH2O
Chlorite (Mg,Al,Fe)12[(Si,Al)8O20](OH)16 2.6–3.3 1.26 20.4
as received

Fixed Pyrite/marcasite FeS2 4.88–5.01 1.50 33

air-dried

Carbon Calcite CaCO3 2.71 1.79 44

Siderite FeCO3 3.96 1.61 38
1.79a
dry

Ankerite Ca(Mg,Fe,Mn)(CO3)2 3.05 44

Dolomite CaMg(CO3)2 2.84 1.91 48
Gypsum CaSO4·2H2O 2.31 1.26 20.9
Plagioclase NaAlSi3O8–CaAl2Si2O8 2.62–2.76 1.00 0
Fig. 2. Relationship between the various constituents of coal and reporting bases (Ward,
K feldspar KAlSi3O8 2.55–2.63 1.00 0
1984). Total moisture is equivalent to in situ moisture, pure coal is composed entirely of
a
macerals, and minerals release volatile matter upon combustion to ash. Assumes an average ankerite composition of 54% Ca, 24% Mg, 20% Fe and 2% Mn.
240 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252

Table 3 1/ m
Typical dmmf coal densities (ρc) for various bituminous rank coal macerals (Crelling, 100
1994).

Group Maceral ρc (g/cm3)

Vitrinite Vitrinite 1.27–1.33

Inertinite Inertinite (all) 1.35–1.60
Semifusinite 1.35–1.50
Fusinite 1.50–1.60
Liptinite Bituminite 1.15–1.24
Sporinite 1.15–1.22
Alginite 1.05–1.12
Resinite 1.03–1.10

gravities; e.g. a fraction with sink and float gravities of 1.35 and 1.40,
respectively, would have a RD of approximately 1.375. The relation-
ship between the fraction ash and midpoint fraction density can then
be used to estimate theoretical yield and product ash percentage for
preparation plants operating at different circuit cutpoints. For this
purpose, the ash percentage is traditionally plotted as a function of
the specific volume, or volume per unit of mass (the reciprocal of
density) (Anonymous, 1966):
0

 1/ c
100ρm ρc 1 100ρm
Ad ¼ − ð4Þ
ρc −ρm ρ ρc −ρm
Fig. 4. Mineral matter percentage as a function of specific volume, showing the linear
Because Eq. (4) fails to account for mineral matter volatiles lost upon relationship observed in coal washability analysis.
combustion, it is in fact an equation for estimating mineral matter, not
ash. The relationship is linear, with a slope of 100ρmρc/(ρc − ρm)

500 80

(a) 70
(c)
Mass Recovered (mg)

400
Mass Recovered (mg)

60

50
300
40

200 30

20
100
10

0 0
1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7
Density (g/cm3) Density (g/cm3)

200 175

175
(b) (d)
150
Mass Recovered (mg)
Mass Recovered (mg)

150
125

125
100
100
75
75
50
50

25 25

0 0
1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7
Density (g/cm3) Density (g/cm3)

Fig. 3. Coal maceral density profiles (Crelling, 1994). (a) A density profile of a humic coal. The main peak represents the vitrinite group macerals, the low density shoulder represents the
liptinite group, and the high density shoulder represents the inertinite group. (b) A density profile of an inertinite-rich Gondwana coal. The highest peak represents vitrinite but the bulk of
the sample consists of inertinite macerals on the high side of the vitrinite. (c) A density profile of a fusain lithotype containing only inertinite macerals. The low density peak is semifusinite
and the high density peak is fusinite. (d) A density profile of a resinite-rich coal from the western United States. The major peak is the vitrinite maceral group and the smaller, very low
density peak is resinite.
 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252
(Fig. 4). With md substituted for Ad, Eq. (4) is algebraically equivalent to
Eq. (1).
3. Estimating mineral matter
Coal and rock density is highly correlated to the minerals contained
in the coal and non-coal lithologies within each sample. For this reason,
it is important to characterize the nature and relative abundance of the
mineral species and any non-coal organic elements. Data from plasma-
ashing, XRD and similar evaluations for a few representative materials
in the sample suite could be used to establish more clearly what min-
erals are actually present, and in what abundance. Significant benefits
would be gained by direct evaluation of the nature of the mineral matter
in at least some of the coal and non-coal samples within a specific coal
seam. In multi-seam deposits, samples should ideally be taken from
each coal seam, as depositional environments frequently vary between
seams, potentially resulting in very different mineral assemblages.
Unfortunately, the nature of the mineral matter is rarely analyzed di-
rectly in a laboratory. This paper explores several techniques for quanti-
fying the percentage of mineral matter in the untreated sample, even if
its composition cannot be precisely determined. Detailed mineralogical
data were not available for the present project, so only broad mineral
groups (silicates, aluminosilicates, and carbonates) could be identified,
based upon the inorganic volatile yield of large groups of samples. How-
ever, as will be demonstrated, even such general information can im-
prove the accuracy of density estimates.
3.1. Parr formula
The simplest and most commonly used method to estimate mineral
matter is the original Parr formula (Rees, 1966):
md ¼ 1:08Ad þ 0:55Stot
where
Stot total sulfur, dry.
The Parr formula was derived from the observation that mineral
matter is composed primarily of aluminosilicates (clays), silicates
(quartz, feldspar), pyrite and calcite. The clays lose water of hydration,
pyrite (FeS2) is converted to Fe2O3 and sulfur oxides, and calcite liber-
ates CO2. The overall proportion of calcite in coal is assumed to be
small, so there is no correction for the loss of CO2 as used in other
methods (described below). The percentage of ash is multiplied by
1.08 to restore the water of hydration lost during ashing. This is an aver-
age value based on mineral matter data from Illinois and Eastern U.S.
coals, which are composed primarily of kaolinite, quartz, pyrite and illite
(Rees, 1966). The correction for sulfur is based on the assumption that
all of the sulfur is present as pyrite. During the ashing process, sulfur
atoms are replaced by oxygen atoms as the FeS2 is oxidized to Fe2O3,
resulting in the loss of 33% of the pyrite mass. It should be noted that
the Parr formula applies specifically to the mineral matter in the coal it-
self, not non-coal plies, which may contain very different mineral as-
semblages (Table 1).
The density of the coal mineral matter may vary significantly, par-
ticularly in pyritic coals. A knowledge of this variability is useful for
determining when the in situ density may be higher than suggested
by the ash percentage alone. The proportion of mineral matter in re-
lation to ash, referred to herein as the mineral matter ratio (Eq. (2)),
is useful for comparing multiple samples and comparing the results
of the Parr formula with other methods for estimating mineral mat-
ter, which are described below. For the Parr formula, the mineral
matter ratio may be estimated by substituting Eq. (2) into Eq. (5)
241
and solving for r:
1:08Ad þ 0:55Stot 0:55Stot
r¼ ¼ 1:08 þ ð6Þ
Ad Ad
For typical Ad and Stot percentages, r values derived from the Parr for-
mula range between 1.08 and 1.20. Because the Parr formula uses total
sulfur, significant proportions of organic sulfur or sulfate sulfur may in-
troduce bias. For high ash samples with moderate to high sulfur content,
values of md calculated by the Parr formula may exceed 100%, indicating
that the coefficients are incorrect. Samples with high sulfur percentages
may return unreasonably high r values because all sulfur is treated as
pyrite, which has a density of approximately 5.0 g/cm3 (Table 2). Ryan
(1990) suggested that the Parr formula can be improved by replacing
total sulfur (Stot) with pyritic sulfur (Spyr); however, pyritic sulfur deter-
mination is rarely performed on individual samples.
3.2. King-Maries-Crossley (KMC) formula
The King-Maries-Crossley (KMC) formula, developed by King et al.
(1936) for European coals, is more comprehensive than the Parr formu-
la and accounts for most of the volatile mineral matter. The formula as
revised by British Coal (Ward, 2002) is
md ¼ 1:13Ad þ 0:5Spyr þ 0:8CO2 þ 2:85Ssul −2:85Sash þ 0:5Cl ð7Þ
where
Sash sulfur in coal ash
Spyr pyritic sulfur in coal
Ssul sulfate sulfur in coal
Cl total chlorine in coal
CO2 mineral carbon dioxide yield from coal.
ð5Þ The various coefficients correct for the loss in weight due to loss of
water of hydration in clay minerals, oxidation of pyrite to ferric oxide
and sulfur dioxide, the loss of carbon dioxide from mineral carbonates,
and the fixation of sulfur in the ash. The 1.13 Ad coefficient corrects for
the loss of water of hydration at high temperatures due to the decompo-
sition of clay minerals (King et al., 1936). The original value of 1.09 pro-
posed by King et al. (1936) was revised to 1.13 in 1971 based on analysis
of 80 British coals (Given and Yarzab, 1978), indicating significant vari-
ability between datasets. The 0.5 Cl coefficient is based on the assump-
tion that half the chlorine is in mineral form (Speight, 2005).
The extra terms in the KMC formula should give more accurate re-
sults, provided that the 1.13 Ad coefficient is a suitable approximation;
however, the KMC formula requires significantly more analyses, making
it unsuitable for routine use. Although mineral matter was calculated for
1402 samples in the present project using the Parr formula, none had
sufficient data for use of the KMC formula in mineral matter
calculations.
3.3. Choudhury-Ganguly formula
Another formula proposed by Choudhury and Ganguly (1978) at-
tempts to account for the effect of carbonate minerals on the volatile
matter of coals:
md ¼ 1:1Ad þ 0:7CO2 ð8Þ
This formula attempts to correct for the most obvious weakness of
the Parr formula (the loss of carbon dioxide from carbonates) but it
completely ignores the oxidation of pyritic sulfur. The formula was em-
pirically derived from samples of low-sulfur coals in the Jharia coalfield
of India. Its usefulness is limited because CO2 is generally only analyzed
on clean coal composites and therefore cannot accurately characterize
the mineral matter of in situ coal resources. Also, the contribution of
242 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252

pyrite to volatile mineral matter cannot be ignored for many coal- mineral matter (both on a dry basis) is given by
bearing regions.
100−md
Ed ¼ Edmmf ð10Þ
100
3.4. Direct determination of mineral matter

There are two primary methods of directly determining mineral where

matter in a sample: acid demineralization and low temperature ashing
(LTA). Ed specific energy, dry basis
Edmmf specific energy, dry mineral matter free basis
md mineral mater, dry basis.
3.4.1. Acid demineralization Substituting Eq. (2) into Eq. (10), this can be expressed as
A more reliable technique for determining the mineral matter
content of coal is that of acid demineralization (Bishop and Ward, 100−rAd E rA
1958), which is the only method for mineral matter determination Ed ¼ Edmmf ¼ Edmmf − dmmf d ð11Þ
100 100
in coal currently covered by international standards (ISO 602-
1983). The sample is treated with 40% hydrofluoric (HF) acid at
50–60 °C. A solution of hydrochloric (HCl) acid is applied to the sam- From this, it can be seen that a least-squares linear regression of Ed
ple before and after the HF treatment in order to prevent accumula- against Ad should have a y-intercept of Edmmf and slope of − Edmmf r/
100 (Gray, 1983). If for a given dataset Ed is plotted against Ad, the aver-
tion of calcium fluoride. The method requires that residual pyrite,
residual ash, and the small amount of retained chloride (assumed age Edmmf value can be estimated from the y-intercept. Solving for r:
to be HCl) be determined separately (Bishop and Ward, 1958). The
mineral matter content is calculated by 100ðEdmmf −Ed Þ
r¼ ð12Þ
Edmmf Ad

1
md ¼ wt loss þ HCl þ ðFeS2 Þ þ residual ash ð9Þ A graphical approach can be used to estimate Edmmf. The starting
3
point is a plot of dry SE against dry ash for the coals in question
(Fig. 5). A line is then drawn from the point representing 100% ash
The acid demineralization technique can be applied to coals of all and zero SE to the projected y-axis intercept of a line just above the up-
ranks and requires no assumptions about the nature of the mineral permost range of the data points. The SE value at that intercept (i.e., the
matter (Given and Yarzab, 1978). However, the technique provides extrapolated SE at 0% ash) would (presumably) represent the Edmmf
no information on the nature of the mineral matter, which is impor- value. The lines for r = 1.1 and r = 1.5 could then be added for compar-
tant in assessing water of hydration and other volatile mineral com- ison, running from that value on the y-axis to values of 91.0% and 66.7%
ponents. The technique is slow and complex, and has not been ash on the y-axis, respectively.
widely used. The Gray method has several important advantages for estimating
mineral matter content:
1. Unlike in the Parr and KMC formulas, md cannot exceed 100%.
3.4.2. Low temperature ashing
2. Only ash and SE determinations are needed, making the method suit-
Another method for directly determining mineral matter in coal
able for most exploration data.
samples is low-temperature oxygen-plasma ashing (Gluskoter,
1965), as prescribed by Australian Standard (AS) 1038.22. The proce-
9,000
dure is faster than that of acid demineralization and appears to be re-
Edmmf n
liable for high rank, low sulfur coals. However, closely specified
conditions of ashing must be adhered to, including the radiofrequen- 8,000
cy power level and treatment of low rank or high sulfur coals with r
possibly dilute HCl acid to remove calcium and sodium cations and 7,000 r
reduce sulfur fixation (Given and Yarzab, 1978). Such cations are r
nevertheless also part of the mineral matter, and should not be ig- 6,000
nored. If they are to be removed before ashing the proportions also oxidized
need to be evaluated by analysis of the leachate produced, and the coal
5,000
data fed back into the evaluation. HCl may also dissolve carbonate
minerals (e.g. calcite and siderite), which are present in some
lower-rank coals. Non-mineral Fe is also an important component 4,000
in the mineral matter of many lower-rank coals.
The radiofrequency ashing technique (AS1038.22) was used by 3,000
Fletcher and Sanders (2003) to correlate relative density to mineral
matter as described in Section 4.2. 2,000 r=
1.
0
3.5. Gray method 1,000 100( dmmf d)
=
r=

r=

dmmf d
1.5

1.

Two methods for determination of r from the relationship be-

1

0
0 10 20 30 40 50 60 70 80 90 100
tween specific energy (SE) and ash and volatile matter vs. ash, re-
Ash (% dry basis)
spectively, were developed by Gray (1983). The SE-based method,
herein called the Gray method, is the most robust because it has Fig. 5. SE vs. ash, showing an abundance of clay and silicate minerals at low to moderate
few input parameters and SE is more strongly correlated to ash ash and more carbonate-rich samples at high ash. The r = 1.0 line should be placed
yield than to volatile matter. The relationship between SE and above all SE values, with the y-intercept corresponding to the Edmmf value.
 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252 243

3. Because both ash and SE are often analyzed on all samples, including
non-coal plies, the method can be applied to samples with the full
range of mineral matter percentages.
4. Expensive, time-consuming laboratory tests are not required.
5. A much wider range of mineral volatiles can be accounted for than
allowed by empirical formulas such as the Parr formula (Eq. (5)).
6. Because the Gray method is not empirical, the mineral matter esti-
mates are specific to each sample population, thereby minimizing
bias.
7. Changes in the nature of the mineral matter with increasing ash can
be observed, if present.
This approach works well for the present dataset, which embraces
seams of similar rank and composition that in theory have similar values
of Edmmf. Deposits in which the rank of the coal varies (e.g. due to chang-
es in depth, thermal alteration or tectonic features) would have more
variable Edmmf values. SE is also affected by coal petrography, further in-
creasing the spread of Edmmf values. In these cases, the data should be
grouped by seam or coal type prior to analysis.
It is important that the Edmmf value be estimated as accurately as
possible. For this reason, the interactive approach adopted in Fig. 5 is
preferable to least-squares linear regression. Weathered samples have
lower SE and may substantially decrease the average least-squares
Edmmf value, potentially resulting in unrealistic values of r b 1.0 for
some samples. In contrast, samples containing high proportions of rela-
tively volatile minerals may steepen the regression line and lead to an
overestimate of Edmmf. Even small errors in the site-specific Edmmf
value may significantly bias the calculated r values, particularly for
low-ash samples.
A plot of r against ash is useful for comparing the average propor-
tion of mineral-derived volatiles for each sample to that of the most
common mineral types (Fig. 6). As r increases on the vertical axis, the
proportion of mineral-derived volatiles also increases, resulting in a
“100% mineral” curve beyond which such a mineral cannot exist. The
relative coal/mineral content is indicated by the position between
the y-axis and the “100% mineral” curve, while the space to the
right of that line approximates the percentage of inorganic volatile
matter. Fig. 6 can be used to:
1. Compare the r value of coal or rock samples to that of several com-
mon minerals.
2. Interpret trends in mineralogy with increasing ash.
3. Estimate the potential error introduced by scatter in the SE vs. ash
relationship.
4. Identify obvious laboratory errors (r values well below 1.0).
5. Compare the Gray method values to Parr formula values to assess the
possibility of bias.
A particular r value cannot be used to determine a unique mineral
composition because many possible assemblages could result in the
same value. For example, a sample with r = 1.26 could contain a miner-
al content of pure chlorite (Table 2) but is far more likely to contain a
mixture of kaolinite, pyrite, quartz, and other constituents. Also, sample
lithology is not a reliable guide to the mineral matter ratio. A silica-
cemented sandstone would be expected to have a low r; however, the
r of a calcite-cemented sandstone might be quite high. For pure kaolin-
ite, r = 1.16, while for quartz and feldspar, r = 1.00 (Table 2). Therefore,
a 50/50 mixture of kaolinite with quartz/feldspar would be expected to

2.00
Dolomite
1.91
Weathered Calcite,Ankerite
1.79
Samples
Siderite
1.61 Samples Cannot Exist
1.50 and Sulfate Minerals Pyrite, Marcasite
10
0%
mi
ne
ral
(r)

Gypsum,Chlorite
1.26
Kaolinite
1.16

1.05 Increased Smectite

Illite
1.00
Silicate and Aluminosilicate (Clay) Minerals Quartz,
Feldspar,
Plagioclase
0.80 Lab Errors

0.60 r (Parr formula)

r (Gray method)
0.40 common minerals
meanr (r = 1.106)
± 1.0% error interval
0.20 mineral matter = 100%
aluminosilicate minerals
0.00
0 10 20 30 40 50 60 70 80 90 100
Ash (% dry basis)

Fig. 6. Mineral matter ratio against ash, compared to r values for common minerals. Distinct changes in mineralogy occur with increasing ash, although individual minerals cannot be
distinguished. A difference of 1.0% (for example) between the average or calculated Edmmf and the actual Edmmf for each sample would increase uncertainty in the r estimate by the
amount shown by the dashed black lines. However, the average value should be similar, and the uncertainty rapidly diminishes with increasing ash.
244
have an r value of approximately 1.08 — equal to the baseline (zero sul-
fur) Parr value. On the other hand, samples with an abundance of illite
(r = 1.05) or silicates may have r values lower than those predicted
by the Parr formula. This is the case for most samples between 30 and
60% ash in the present dataset.
One disadvantage of the Gray method is that scatter increases with
decreasing ash. For low ash samples, scatter due to changes in oxidation,
petrography, oxidation, or rank may steepen the line from the y-
intercept (the average Edmmf) to the sample data (Ad, Ed). The SE value
is correlated to the volatile matter and fixed carbon content of the or-
ganic matter, which are sensitive to oxidation, thermal alteration, and
maceral composition. Such errors in Edmmf estimates will reduce the ac-
curacy of r values at low ash percentages, but the error potential rapidly
diminishes with increasing ash (Fig. 6). The Parr formula is subject to
the same uncertainty, as shown by the divergence in values below ap-
proximately 15% ash in Fig. 6. At very low ash percentages, the sample
mineral matter ratio may be better approximated by the mean mineral
matter ratio (r) for the total dataset.
4. Estimating density
The search for reliable methods to relate density to ash has occupied
geologists and mining engineers for decades, resulting in a number of
different approaches. The appeal of ash-based methods is that nearly
all untreated coal and non-coal ply samples are analyzed for ash yield.
This section reviews the most common methods for estimating in situ
RD as a function of ash yield, although it is by no means exhaustive.
The resulting discussion is used as a foundation for developing a new,
more accurate method for estimating density based on mineral matter
content.
4.1. Least-squares polynomials
The most common approach to estimating the RD from sample ash
percentage involves least-squares polynomial functions (usually first-,
second-, or third-order). However, it has long been recognized that
these polynomials do not honor the shape of the data distribution across
the full range of ash values. Depending on the degree of the polynomial,
3.0
2.9 RD values (n = 1,266)
2.8
2.7
2.6
Relative Density (dry basis)
2.5
2.4
2.3
2.2
2.1
2.0
1.9
1.8
1.7
1.6
1.5
1.4
= 1.24 + 1.41 × 10 2 d 1.73 × 10 4 d 2 + 2.26 × 10
1.3 d d
1.2
0 10 20 30 40
Ash (% dry basis)
Fig. 7. Polynomial least-squares regression equations for the project data, showing
divergence from data values at low, middle and high ash percentages.
E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252
density may be over- or underestimated for different ash ranges (Fig. 7).
Workarounds have been developed for this. A common approach is to
exclude samples above a certain ash percentage (e.g. 40%) before devel-
oping a least-squares regression for the remaining samples. However,
such equations do not accurately represent the densities of high-ash
roof, floor, or parting materials. If regression equations are used to esti-
mate RD from ash, they can underestimate the non-coal sample density
(and therefore the impact of dilution). Density for out-of-seam mate-
rials is often modeled using constant “waste” values, which fail to cap-
ture the characteristics of all rock types or account for their moisture
content.
The first-order polynomial shown in Fig. 7 is clearly a poor fit to the
project dataset, severely underestimating the density of both high and
low ash samples while overestimating densities in the center of the
chart. The second- and third-order polynomials appear more reasonable
and have similar R2 values, but they diverge sharply at low ash yields.
The estimated RD values for “pure” coal (i.e. the density of dry, ash
free organic matter) are 1.38 and 1.24 for the second- and third-order
equations, respectively — which covers a huge range of coal types.
Also, there is no way of knowing which RD is the most reasonable for
high ash materials, as scatter increases to the right and only two sam-
ples exceed 90% ash.
Often, the polynomial regressions are derived from the original air
dried or as received laboratory RD data. However, moisture introduces
an independent variable, thereby increasing scatter and reducing the re-
liability of the least-squares regression equation. Unless the as-analyzed
moisture is considered equivalent to the in situ moisture, it is more ac-
curate to convert the data to dry basis before performing the regression;
estimated RD values can subsequently be converted to in situ basis at
the desired moisture content.
A first-order polynomial formula widely used in the U.S. coal min-
ing industry is: Dis = 1.25 + Ad/100. Many U.S. coal mining compa-
nies rely on this formula almost exclusively in lieu of RD testing,
despite the potential for serious error. This formula has the advan-
tage of being simple and is a reasonably good fit to some low ash,
low moisture Appalachian coals, for which it was developed. Howev-
er, the formula cannot be applied to coals of different rank, petrology,
or mineralogy. As with the first-order polynomial shown in Fig. 7, the
formula is also inaccurate for non-coal lithologies and should not be
used when more accurate data or methods are available.
4.2. Fletcher and Sanders, ACARP C10041
ACARP Project C10041 (Fletcher and Sanders, 2003) was a compre-
hensive study conducted to determine the best techniques for estimat-
ing in situ moisture in coal seams. In addition, ten empirical equations
were proposed to estimate in situ RD (Dis) from other coal quality
data, i.e. without first estimating in situ moisture. A series of regressions
were carried out in order to estimate Dis using up to five independent
variables on datasets of 16 to 60 samples. All but one of the recommend-
ed formulas require air-dried or dry RD as an input, so they are not rel-
evant to this discussion. The remaining formula proposed by Fletcher
and Sanders (2003, p. 53) requires only values for mineral matter and
dry, mineral matter free organic hydrogen:
d = 1.15 + 1.43 × 10 2
d
Dis ¼ 0:0074md −0:0324H o;dmmf ð13Þ
2
= 0.9142
d = 1.38 + 1.53 × 10 3 d + 1.41 × 10 2
d
2 where
2
= 0.9519
third-order polynomial
6 3 Ho,dmmf organic hydrogen, dmmf (%)
2
= 0.9560 Dis relative density, in situ.
50 60 70 80 90 100
The formula was derived from a dataset containing only 17 sam-
ples, and mineral matter was determined using the radiofrequency
ashing technique (AS1038.22) (Fletcher and Sanders, 2003). Al-
though this formula was not recommended due to the lack of other
 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252 245

analytical parameters, the equation type was classified as “best” (rel- 3.0
ative to other regression equations) due to a relatively low standard 2.9 RD values, at 6% moisture (n = 1,266)
error of 0.017 and R2 value of 0.95. However, there appears to be an 2.8
error in this formula. For the present dataset, the equation yields 2.7
Dis values of − 0.093 and 0.213 at minimum and maximum md values 2.6
of 10.49 and 48.84, respectively. No further comparison was lignite

Relative Density (dry basis)

2.5
performed.
2.4
2.3
2.2
4.3. Meyers Secondary Model No. 1, ACARP C10042
2.1
Meyers et al. (2004) describe an empirical formula, referred to as the 2.0
Meyers Secondary Model No. 1, for estimating in situ RD. The model is 1.9
referred to as “secondary” because it does not require air-dried RD as 1.8
an input, and was derived by least-squares regression on 52 samples, 1.7
with a standard error of 0.0076 and R2 value of 0.9945. Minimum and 1.6
maximum Ad percentages for the samples were 3.91 and 46.53, 1.5
respectively.
1.4
1.3

Dis ¼ 2:582  10−5 A2d þ 6:251  10−3 Ad þ 8:608  10−5 V 2daf 1.2
0 10 20 30 40 50 60 70 80 90 100
−2
−1:32  10 V daf −6:447  10−4 C 2daf þ 9:253  10 −2
C daf −1:602 Ash (% dry basis)
ð14Þ
Fig. 9. Plot of in situ relative density against dry ash for coals from the project area,
showing fit to equations proposed for coals of different rank by Smith (1991).
where

Vdaf volatile matter, daf (%) 4.4. Smith method

Cdaf carbon, daf (%).
Smith (1989, 1991) was among the first researchers to recognize
The present dataset contains 96 samples with ultimate analysis data, that the relationship between RD and ash was hyperbolic. Based on
each of which was also tested for RD. The Dis value was calculated for all analysis of coal samples from Alberta, he proposed empirical equations
96 samples using the Meyers equation, then plotted against Ad to devel- to quantify in situ RD for different ranks, with the general form
op Fig. 8. The linear regression equation for the calculated Meyers values
has a R2 value of 0.8956; however, the equation is a poor fit to the real 100
RD values, almost all of which fall above it. Also, this second-order mul- Dis ¼ ð15Þ
a þ bAd
tivariable polynomial equation fails to represent the hyperbolic density-
ash relationship at higher ash percentages.
Four pairs of coefficients were proposed for the following ranks:
1.70
• low and medium volatile bituminous: a =75.436, b = − 0.402
• high volatile bituminous: a =76.925, b = − 0.417
1.65
• subbituminous: a = 80.150 , b= −0.451
1.60
• lignite: a = 82.634 , b= −0.476
Relative Density (in situ basis)

1.55
Because, as discussed above, the density-ash relationship is hyperbol-
1.50 ic, the equations approximate the data distribution over a much wider
range than polynomial equations (Fig. 9). However, the high volatile bi-
1.45 tuminous curve significantly overestimates the RD values for this project,
which are converted to a 6% moisture basis, consistent with this project's
1.40 coal type. The subbituminous curve, while a better fit, is not representa-
tive of the rank or moisture content of the present dataset. Clearly, em-
1.35 pirical relationships derived from the Alberta coals studied by Smith
(1991) cannot be applied indiscriminately to other coal deposits.
1.30 The Smith method suffers from a number of limitations. A dry, ash-
RD values, at 6% moisture (n = 96)
free coal density (including associated closed pores) of 1.33 g/cm3 was
1.25 assumed for all ranks and coal types. The method fails to distinguish be-
least-squares regression (Meyers)
tween ash (a byproduct of combustion) and mineral matter, referring to
1.20 “ash density” and “volume of ash including empty pores.” The “ash den-
0 10 20 30 40 50
sity” is arbitrarily fixed at 2.90 g/cm3 (significantly higher than that of
Ash (% dry basis)
most minerals) and it was assumed that “ash contains 3% moisture by
weight” for all ranks (Smith, 1989). The equations are based on data
Fig. 8. Plot of in situ relative density against dry ash for coals from the project area,
calculated by the Meyers Secondary Model No. 1 equation. The calculated values and
from Alberta coal mines only. No procedures were proposed for deriving
least-squares regression compare poorly to the actual RD values at 6% moisture. these coefficients from other project datasets.
246 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252

4.5. Ryan method 1. Improve the correlation coefficient (R2) and reduce the standard
error of the estimate.
The theoretical approach taken by Ryan (1990) is similar to that 2. Minimize bias introduced by samples with high r, which may in-
taken by Smith (1991) and also results in a hyperbolic relationship be- crease scatter, lift the regression curve, and overestimate tonnages.
tween RD and ash. However, instead of generalizing RD vs. ash relation- 3. Capture the ranges of ρc and ρm values. These are often indicative of
ships for coals of various ranks, Ryan used the statistics program particular maceral and mineral assemblages and may serve as a “fin-
CURVEFIT to test 25 different equations for a single dataset (Ryan, gerprint” of a particular deposit or seam.
1990). The equation with the highest R2 value was hyperbolic, taking 4. Validate the reasonableness of the regression curve against the coal
the form of Eq. (15), in general agreement with the theoretical develop- maceral and mineral properties described in this paper.
ment of Smith (1991). Ryan's (1990) paper appears to be the first paper
Eq. (16) contains several errors that must be corrected before pro-
to introduce in situ moisture and air-filled void porosity as variables and
ceeding. The units are not consistent due to (a) failure to account for
to use mineral matter ratio to increase the accuracy of RD estimates.
the density of water, (b) substitution of unitless RD for density and
Values of a and b were calculated for several seams at a single site, re-
(c) improper use of a volumetric percentage for air-filled voids (ϕv) as
vealing subtle variations with increasing depth and rank.
moisture and ash are mass percentages. In addition, the equation is
The general in situ RD equation proposed by Ryan (1990) is
only accurate when Mis = 0% (i.e., on the dry basis). Although the equa-
tion returns the correct a value, thereby approximating the in situ den-
100ρc ρm sity at Ad = md = 0, the b value does not account for Mis and increasingly
Dis ¼
ðM is þ ϕv Þρc ρm þ ð100−Mis Þρm þ ðρc −ρm ÞrAd overestimates in situ density with increasing mineral matter content.
or A correction to Eq. (16) is presented here. Void porosity (ϕv) is re-
moved because in saturated coal seams gas is typically adsorbed to
100 the surface of the coal, not present as free gas (Aminian, 2005). To main-
Dis ¼
 ð16Þ
100−Mis ρc −ρm tain unit consistency, Mis is divided by ρw, thereby maintaining unit con-
M is þ ϕv þ þ rAd
ρc ρc ρm sistency (previously it was assumed to be 1 g/cm3 and ignored). Finally,
the b coefficient is modified to account for the effect of moisture on in
where situ rock density.

Mis in situ moisture 100

ρis ¼

 ð18Þ
ϕv air-filled void porosity. M is 100−Mis 100−Mis ρc −ρm
þ þ rAd
ρw ρc 100 ρc ρm
This can be further reduced to the form of Eq. (15), where
This gives the corrected coefficients
100−Mis
a ¼ M is þ ϕv þ
ρc M is 100−M is
a¼ þ ð19Þ
ρw ρc


ρc −ρm
b¼ r


ρc ρm 100−M is ρc −ρm
b¼ ð20Þ
100 ρc ρm
Despite the strong theoretical foundation and elegance of Ryan's
(1990) formula, it was never widely used and does not appear to be Eq. (18) describes the fundamental relationship between in situ
cited outside of the original paper. density and that of the constituent macerals, minerals and moisture.
The unit returned is in situ density (ρis, as mass per unit volume), not
4.6. Mineral matter method RD. Mis and md are mass percentages, so a and b have units of specific
volume (1/ρ).
The mineral matter method is a new framework proposed in this Dry sample density can be estimated by using Eq. (17) and setting
paper for estimating the density of coal and its constituent mineral com- the moisture term in coefficients a and b to zero. In that case, the coef-
ponents. The approach uses standard laboratory analyses of raw coals to ficients are
develop an empirical, site-specific equation for all values of ash. The
technique can also be used to generate a fully deterministic relationship 100
a¼ ð21Þ
between density and ash; given reasonable estimates of in situ mois- ρc
ture, petrography, and mineralogy, in situ density can be estimated
even for deposits where only ash data exist. ρc −ρm
b¼ ð22Þ
To the authors' knowledge, the mineral matter method is the first ρc ρm
statistical procedure for fitting a least-squares hyperbola to a density
vs. mineral matter relationship to be published. This method builds and the dry coal and mineral densities are given by
upon the work of Ryan (1990) and also uses the Gray method
(Eq. (12)) to calculate a value of r for each sample so that it becomes 100
ρc ¼ ð23Þ
an independent parameter and not part of the b coefficient, as is the a
case for the Smith (1991) formula (Eq. (15)). The general form of the
density equation is 100
ρm ¼ ð24Þ
a þ 100b
100
ρ¼ ð17Þ
a þ brAd In order to estimate in situ relative density (RD) for the purpose of
determining coal and rock tonnages, it is not necessary to use units of
The goals of deriving the regression of average particle density specific volume for the coefficients. When both sides of Eq. (17) are di-
against mineral matter, rather than against ash, are to: vided by ρw, the coefficients lose their units and the general form of the
 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252
relative density equation becomes
100
D¼ ð25Þ
a þ brAd
In order to convert the dry RD values to in situ moisture basis, the
in situ moisture values must be as accurate as possible. Estimating in
situ moisture is difficult because samples can never be analyzed in
situ; the act of recovering a sample disturbs it, in the process remov-
ing moisture or adding moisture that wasn't initially present. As re-
ceived RD data (analyzed before the sample is allowed to air dry)
may approximate the initial moisture content, but it is difficult to de-
termine if samples have drained or been contaminated with drilling
fluid. Porosity, and a sample's ability to retain moisture, may increase
due to decompression or fracturing. Also, samples are rarely ana-
lyzed before drying due to the difficulty of working with wet sam-
ples. In Australia, RD analysis is usually performed on an air-dried
basis (AS1038.21.1).
Over the years, a number of methods have been proposed to esti-
mate in situ moisture (e.g. Fletcher and Sanders, 2003; Meyers et al.,
2004). A full discussion is beyond the scope of this paper, but Fletcher
and Sanders (2003) provide two simple formulas that may have broad
applicability in both Australia and North America:
Mis ¼ 1:1431  MHC þ 0:348 ð26Þ
Mis ¼ 1:117  EQM þ 0:317 ð27Þ
where
MHC Moisture Holding Capacity, high rank coals (AS1038.17)
EQM Equilibrium Moisture (ASTM D1412).
These equations rely on relatively common tests, already performed
at many mines in order to predict the moisture of raw feed or product
streams. It should be noted that these are empirical formulas derived
from a range of black coal samples, and do not apply to all basins or
coal types. Rigorous testing should be performed before they are applied
to a particular coal mine or deposit. Often, a project has been in develop-
ment long enough that the in situ moisture is fairly well defined, and the
use of untested formulas is not required.
Average moisture for samples of other lithologies can be estimated
using as-received moisture data from non-coal ply or overburden sam-
ples, taking into account differences in porosity, induration, and relative
abundance. Coal moisture decreases with increasing rank as volatiles
are driven out and pore spaces close. In high-rank coals, the difference
between the moisture contents of coal and other lithologies may be
negligible and is often ignored. However, low-rank coals often contain
more moisture than the non-coal plies contained within the same
seams. In this case, applying the same moisture percentage to both
low ash and high ash samples could introduce error to non-coal sample
density estimates. Eqs. (19) and (20) may be modified to accept average
moisture values for coal and mineral fractions (Mc and Mm, respective-
ly). In such a two-moisture scenario, factors a and b are calculated as
follows:
Mc 100−M c
a¼ þ ð28Þ
ρw ρc
100−M m 100 þ M c ðρc −1Þ−ρc Mm
b¼ − ð29Þ
100ρm 100ρc
Factor a is unchanged, as Eqs. (19) and (25) are equivalent, but b is
more complex. Another option is to first convert ρc and ρm to in situ
values by the Preston and Sanders (1993) formula (as ρc,is and ρm,is, re-
spectively) based on their separate moisture contents, then substitute
the in situ values in Eq. (18) for the dry basis values. With this approach,
247
no additional moisture is required, so Mis is set to zero, resulting in
100
ρis ¼ ! ð30Þ
100 ρc;is −ρm;is
þ md
ρc;is ρc;is ρm;is
Thus, the in situ a and b coefficients are equivalent to the dry basis
versions and can be derived from the in situ densities using Eqs. (21)
and (22). Regardless of how the in situ a and b coefficients are derived,
Eqs. (23) and (24) can then be used to determine the average in situ coal
and mineral densities, assuming that saturation is 100%.
5. Methodology
The preceding concepts were used to develop a set of procedures
that were then applied to the exploration sample data from the project
area, as described below. The same procedures can be applied to sam-
ples from any other exploration program provided that adequate SE
and RD data are available.
5.1. Convert all parameters to dry basis
In the Australian coal industry, the standard method for converting
RD values between moisture bases is the Preston and Sanders formula
(Preston and Sanders, 1993). While it is also widely used international-
ly, the formula is relatively unknown in the U. S. coal industry. The for-
mula was developed from first principles and laboratory tests support
the validity of the equation (Fletcher and Sanders, 2003). The default
formula when converting RD from moisture M1 to moisture M2
(Preston and Sanders, 1993) is:
100−M1
D2 ¼ D1  ð31Þ
100 þ D1 ðM2 −M 1 Þ−M 2
If converting from air-dried to dry basis, this simplifies to
100−Mad
Dd ¼ Dad  ð32Þ
100−Dad M ad
and from dry to air-dried basis
100
Dad ¼ Dd  ð33Þ
100 þ Mad ðDd −1Þ
The Preston and Sanders formula was applied to all of the samples in
the present dataset prior to subsequent analysis, in order to improve the
correlation between the other parameters.
5.2. Use the Gray method to estimate mineral matter ratio
All 1405 samples with SE data were plotted against ash, as shown
in Fig. 5. No variation in coal rank could be observed among the indi-
vidual seams for this project, as there was limited variability in the SE
values at low ash levels. The average Edmmf was determined graphi-
cally from Fig. 5, then r was calculated for all samples having SE
data using Eq. (12). The mean value for r (r) was calculated (1.10),
which can be substituted for r in samples lacking SE data.
5.3. Plot RD against mineral matter and exclude any weathered samples
A total of 1266 samples with both RD and SE data were plotted as Dd
vs. md in Fig. 10. Samples lacking SE data were not plotted because the
mineral matter ratio could not be calculated.
248 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252

3.0
RD values (n = 1,266)
2.9
least-squares regression
2.8
2.7
2.6
2.5
2.4
2.3
2.2
2.1
2.0
1.9
1.8
1.7
1.6
1.5 2
=0 .9784
1.4
100 100
1.3 d = =
+ d 76.45 0.3864 d

1.2
0 10 20 30 40 50 60 70 80 90 100

Fig. 10. Relative density values against mineral matter percentage, showing a reduction in scatter and bias. The distribution of values around the least-squares regression, as represented by
the 95% confidence and 95% prediction intervals, indicates the variability in petrography and mineralogy within the sample population. For low ash samples, the absolute difference
between ash and mineral percentages is fairly low, so most variability is due to differences in petrography, oxidation, or rank. High ash samples, in contrast, are more likely to contain
carbonate and other high-volatile minerals, which are responsible for much of the scatter around the regression.

5.4. Perform least-squares regression to calculate the average dry coal and
mineral densities 3.0
2.9 RD values (n = 1,266)
The Solver add-in of Microsoft Excel was used to minimize the 2.8 least-squares regression (r = 1.10)
sum of squares of the residuals by optimizing coefficients a and b 2.7
in Eq. (17). The results were compared to those obtained by apply- 2.6
ing the same technique against ash (with no correction for r).
2.5
Relative Density (dry basis)

Converting ash percentage to mineral matter percentage prior to re-

2.4
gression analysis increased R 2 from 0.9504 to 0.9784 and reduced
2.3
the standard error from 0.0665 to 0.0439 (a decrease of 34%)
(Table 4). 2.2

The best-fit dry coefficients are a = 76.45 and b = −0.3864, both 2.1

with units of cm3/g. Eq. (17) was used to derive the project-specific 2.0
1.9
1.8
1.7
1.6 2
=0 .9504
1.5
1.4 100
Table 4 =
d
Least-squares regression statistics. 1.3 76.45 0.4253 d

Statistic Ash Mineral matter 1.2

0 10 20 30 40 50 60 70 80 90 100
Sum of squares of the residual 5.59 2.43 Ash (% dry basis)
Total sum of squares 112.80 112.80
Standard error 0.0665 0.0439
Fig. 11. Relative density against ash percentage, showing the regression equation
Correlation coefficient, R 0.9749 0.9891
converted to a dry ash basis with r ¼ 1:10 . The variability in sample mineralogy
Coefficient of determination, R2 0.9504 0.9784
introduces noticeable bias and scatter to the relationship that are not present in Fig. 10.
 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252 249

dry basis regression equation: Preston and Sanders formula for the same moisture and dry densi-
ties.

100 100
ρd ¼ ¼
a þ b  rAd 76:45 cm3 =g−ð0:3864 cm3 =gÞ rAd 100 100
ρc;is ¼ ¼ ¼ 1:28 g=cm3
The average densities for pure coal (ρc) and mineral matter (ρm) a 77:86 cm3 =g
were calculated using Eqs. (23) and (24) as follows: 100 100
ρm;is ¼ ¼
a þ 100b 77:86 cm3 =g þ 100ð−0:3633 cm3 =gÞ
100 100 ¼ 2:41 g=cm3
ρc ¼ ¼ ¼ 1:31 g=cm3
a 76:45 cm3 =g
100 100
ρm ¼ ¼
a þ 100b 76:45 cm3 =g þ 100ð−0:3864 cm3 =gÞ
100 It is perhaps worth nothing that a Mis value of 6% does not imply a
¼ ¼ 2:64 g=cm3 porosity of 6% as moisture and ash percentages are mass-weighted. At
37:85 cm3 =g
constant moisture, the porosity must increase with increasing ash due
to the higher mineral density. In this example, a constant 6.0% moisture
These average endpoint densities are similar to those of common corresponds to coal and mineral porosities of 7.7% and 14.4%,
coal macerals and minerals. A fully deterministic model assuming respectively.
endmembers of vitrinite (ρc ≈ 1.30 g/cm3; see Table 3) and quartz
(ρm = 2.65 g/cm3; see Table 2) would have produced nearly the same 5.7. Estimate in situ relative density for all samples
equation.
The dry basis regression equation is plotted in Fig. 10. The y- For samples already having RD data, the only conversion per-
intercepts at zero and 100% mineral matter represent the average formed was from an air-dried moisture to an estimated in situ mois-
ρc and ρm values. The statistical distribution is shown by the 95% con- ture basis using the general Preston and Sanders (1993) formula
fidence and 95% prediction intervals. The former indicates the uncer- (Eq. (31)). All other RD values were estimated using the in situ a
tainty regarding the mean value, which due to the large size of the and b coefficients calculated above in the form of Eq. (25):
dataset is very low. The latter represents the probability that any
sample value will fall within a certain distance of the regression 100 100
equation. Dis ð6%Þ ¼ ¼
a−b rAd 77:86−0:3633 rAd
Variance typically increases to the right in an “RD trumpet”
(Sanders, 2003), caused by the greater variation in mineral types
The value of r varies by sample and is calculated solely from the ash
which occurs in high-ash materials (Fig. 11). However, the scatter
and SE data. Although it is also possible to use the project average r for
of RD values is much lower relative to mineral matter than to ash
all samples, this is not recommended for samples with SE data. All esti-
(Fig. 10). By comparison, the least-squares regression equation is
mated densities would fall on the regression line, masking the natural
plotted against dry ash in Fig. 11, using the r value of 1.10 to convert
distribution and biasing the results. Fig. 12 shows the actual and esti-
md to Ad. Deviation from the least-squares regression occurs when
mated in situ RD values together with the regression equation at 6%
RD is plotted vs. ash due to systematic changes in mineralogy with
moisture.
increasing ash. No such bias can be observed when RD is plotted
against mineral matter (Fig. 10).
6. Summary of mineral matter method
5.5. Estimate in situ moisture
The mineral matter method is easy to perform using spreadsheets
and can be reduced to 12 steps. Performing these steps will result in
For this dataset, MHC or EQM data were not available, so the authors
the most accurate in situ RD estimates for all exploration samples,
used a constant Mis of 6% for the sample coal fraction, consistent with
thereby providing the highest accuracy and spatial resolution for re-
local studies. Based on non-coal ply quality data and the characteristics
serve and resource estimation.
of the surrounding lithologies, the same moisture was used for the sam-
ple mineral fraction as well. 1. Convert all RD, ash and SE data to dry basis using the Preston and
Sanders (1993) formula.
5.6. Derive in situ equation coefficients and determine in situ coal and rock 2. Plot SE (Ed) for all samples against ash (Ad).
densities 3. Graphically determine the dry, mineral matter free SE (Edmmf).
4. Estimate r for each sample:
The estimated in situ moisture of 6% was used in combination with
the average dry ρc and ρm densities estimated earlier to calculate the 100ðEdmmf −Ed Þ
r¼
in situ a and b coefficients by Eqs. (19) and (20). Edmmf Ad

M is 100−Mis 6 100−6 5. Calculate the mean value for r (r) as ∑r/n; for samples lacking SE
a¼ þ ¼ þ ¼ 6 cm3 =g
ρw ρc 1:00 g=cm3 1:31 g=cm3 data, set r ¼ r.
þ71:86 cm3 =g ¼ 77:86 cm3 =g 6. Calculate mineral matter as md = rAd for all samples.
7. For samples with both SE (Ed) and RD (Dd) data, plot Dd against md.




 8. Exclude all weathered and outlier samples.
100−M is ρc −ρm 100−6 1:31 g=cm3 −2:64 g=cm3
b¼ ¼ 9. Use the Solver add-in of Microsoft Excel to minimize the sum of
100 ρc ρm 100 1:31 g=cm  2:64 g=cm
3 3

 squares of the residuals, ∑(ρest − ρd)2, by optimizing the dry a
−1:33 g=cm3 and b coefficients:
¼ 0:94 ¼ −0:3633 cm3 =g
3:46 g2 =cm6
100
ρ¼
Eqs. (23) and (24) were used to calculate the in situ densities. The a þ bmd
results were found to be identical to those calculated with the
250 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252

3.0
2.9 all RD values, at 6% moisture (n = 3,969)
(n = 1,666)
2.8 r = 1.10)
2.7
2.6
2.5
2.4
2.3
2.2
2.1
2.0
1.9
1.8
1.7
1.6
1.5
1.4
100 100
1.3 is (6%) = =
d 77.86 0.3633 × × d

1.2
0 10 20 30 40 50 60 70 80 90 100

Fig. 12. In situ relative density at 6% moisture against dry ash, comparing the distributions of the estimated values (for samples with SE data) against all RD values (including those which
lack SE data). The regression equation was converted to in situ basis at a moisture of 6% using Eqs. (19) and (20). The estimated values follow the distribution of the actual values, falling
below the regression line for silicate-rich samples and rising above it for carbonate-rich samples (see Fig. 6).

10. Calculate the average pure coal (ρc) and mineral (ρm) densities: 12. Use the Preston and Sanders (1993) formula to convert the RD data
to in situ basis; for all other samples
100
ρm ¼ 100
a þ 100b ρis ¼
a þ brAd

100
ρc ¼
a 7. Accuracy

11. Apply the estimated in situ moisture (Mis) content to calculate the One of the most surprising outcomes from the mineral matter method
in situ coefficients: is how closely the estimated RD values match the analyzed values. To a
large extent, real and estimated RD values share the same distribution,
particularly at high ash percentages (see Fig. 12). This captures much of
M is 100−Mis
a¼ þ the natural variability in mineral content and may reveal trends not cap-
ρw ρc
tured by the regression equation. In this project, the RD of very high (N


 70%) ash samples is often greater than that estimated by the regression
100−Mis ρc −ρm equation, possibly due to the loss of mineral volatiles liberated from
b¼
100 ρc ρm carbonate-cemented sandstones. In contrast, the RD of moderately high
ash (40 to 60%) samples tends to be lower than predicted by the regres-
sion equation, possibly due to an abundance of claystones and tuffaceous
If using separate in situ moisture values for coal (Mc) and rock (Mm)
sediments. If a constant value for r is used, all estimated values to fall on
the formulas are:
the regression curve and the extra precision is lost, as is the case for the
polynomial, Smith and Ryan methods. However, the regression curve is
M c 100−Mc still a good fit to the data, and in practice is unlikely to introduce signifi-
a¼ þ
ρw ρc cant bias.
Laboratory errors are rarely the primary source of scatter in coal sam-
100−Mm 100 þ Mc ðρc −1Þ−ρc M m ples. Minor differences in rank, oxidation, maceral type and mineral com-
b¼ − position affect sample SE values to a greater degree, particularly at low
100ρm 100ρc
ash percentages. It is difficult to accurately estimate r for very low ash
samples because r is a function of the slope of the line connecting the
 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252 251

projected Edmmf and the sample data point (Eq. (12)). To the extent that
the sample Edmmf (which cannot be measured) differs from the average
(or estimated) Edmmf, the value of r will be incorrect. This source of uncer-
tainty is represented by the “1.0% error interval” in Fig. 6, which becomes
asymptotic as md approaches zero, because the slope of a line connecting
two Ed values with the same md value is infinite. For this reason, it is im-
portant to confirm that all samples are of similar rank and exclude weath-
ered or oxidized samples, which will have artificially high r values (Fig. 6).
A problem shared by most multivariate empirical formulas, including
those developed by Meyers et al. (2004) and Fletcher and Sanders (2003),
is that exploration samples usually are not analyzed for the additional re-
quired parameters. This severely limits the applicability of the equations
and makes them unsuitable for estimating out-of-seam dilution. Another
problem, which is shared by the Smith (1991) method, is that empirical
equations are derived from small datasets that do not represent all de-
posits or coal types. Blindly applying these empirical equations to a new
dataset can result in significant bias. In contrast, the mineral matter
method uses the common parameters ash, RD, and SE to generate a
project-specific least-squares regression equation. Estimating RD using
this formula requires only ash data, although accuracy improves signifi-
cantly if SE data are also used to estimate r. That makes this method suit-
able for all coal and rock samples, provided sufficient RD and SE data are
available to perform the initial regression analysis.
In order to compare the accuracy of the methods reviewed in this
paper, histograms of relative error were prepared for six of the empirical
equations described earlier (Fig. 13). Because this list includes the Meyers
Secondary Model No. 1 (Eq. (14)) (Meyers et al., 2004), which requires ul-
timate analysis carbon values, the comparison is limited to the 96 samples
with extended coal quality data. This further constrains the range of dry
ash percentages to between 3.91 and 46.53%.
The Smith (1991) high volatile bituminous and Meyers Secondary
Model No. 1 equations were derived from sample datasets from Alberta,
Canada and Queensland, Australia, respectively, and clearly are a poor
analogue to this project.

Mineral Matter Method 1st Order Polynomial

0.35 0.35
Mean -0.005 Mean -0.020
0.30 Median -0.002 0.30 Median -0.008
St. Dev. 0.032 St. Dev. 0.053
Relative Frequency

Relative Frequency
0.25 Skewness -1.43 0.25 Skewness -3.31
Kurtosis 5.45 Kurtosis 17.53
0.20 0.20

0.15 0.15

0.10 0.10

0.05 0.05

0.00 0.00
-0.12 -0.10 -0.08 -0.06 -0.04 -0.02 0 0.02 0.04 0.06 0.08 0.10 0.12 -0.12 -0.10 -0.08 -0.06 -0.04 -0.02 0 0.02 0.04 0.06 0.08 0.10 0.12
Residual (g/cm3) Residual (g/cm3)

Meyers Secondary Model No. 1 2nd Order Polynomial

0.45 0.35
Mean -0.051 Mean -0.048
0.40
Median -0.041 0.30 Median -0.047
0.35 St. Dev. 0.035 St. Dev. 0.054
Relative Frequency

Relative Frequency

Skewness -3.06 0.25 Skewness -1.84

0.30
Kurtosis 16.36 Kurtosis 8.96
0.25 0.20

0.20 0.15
0.15
0.10
0.10
0.05
0.05

0.00 0.00
-0.12 -0.10 -0.08 -0.06 -0.04 -0.02 0 0.02 0.04 0.06 0.08 0.10 0.12 -0.12 -0.10 -0.08 -0.06 -0.04 -0.02 0 0.02 0.04 0.06 0.08 0.10 0.12
3
Residual (g/cm ) Residual (g/cm3)

Smith (1991) - High Vol. Bituminous 3rd Order Polynomial

0.35 0.35
Mean 0.021 Mean -0.014
0.30 Median 0.027 0.30 Median -0.007
St. Dev. 0.048 St. Dev. 0.048
Relative Frequency

Relative Frequency

0.25 Skewness -3.58 0.25 Skewness -3.27

Kurtosis 20.62 Kurtosis 18.06
0.20 0.20

0.15 0.15

0.10 0.10

0.05 0.05

0.00 0.00
-0.12 -0.10 -0.08 -0.06 -0.04 -0.02 0 0.02 0.04 0.06 0.08 0.10 0.12 -0.12 -0.10 -0.08 -0.06 -0.04 -0.02 0 0.02 0.04 0.06 0.08 0.10 0.12
3
Residual (g/cm ) Residual (g/cm3)

Fig. 13. Histograms comparing the accuracy of the six most density estimation techniques reviewed herein, applied to the 96 samples with extended quality data.
252 E. Robeck, D. Huo / International Journal of Coal Geology 168 (2016) 237–252
The polynomial regression equations are derived from the full popula-
tion of 1266 RD samples, not the 96 samples used to generate the histo-
grams in Fig. 13. In general, the first-order polynomial provides a
reasonable fit to the data, as shown in Fig. 7. However, accuracy of the
second-order polynomial decreases, despite the increase in polynomial
degree, because the second-order equation sharply diverges from the
data at low ash (Fig. 7), as a parabola is a poor fit to the full hyperbolic
density-ash relationship. The other polynomials diverge less sharply, but
each only honors the data over a limited range. This underscores how sen-
sitive polynomial regressions are to the input data distribution and the
polynomial degree.
By every statistical measure, the mineral matter method is the most
accurate method for estimating the relative density of the coal quality
data for this project.
8. Conclusions
Reserves and resources should always be estimated using in situ den-
sity values derived from exploration data. The best practice is to perform
relative density analysis on each sample, including non-coal plies, and
convert the values to the appropriate in situ moisture basis using the
Preston and Sanders (1993) formula. However, for many historical
datasets, relative density data do not exist or are incomplete. It is impor-
tant that sufficient data to calibrate the relationship of density and miner-
al matter to ash be obtained as early as possible in order to report resource
tons accurately, beginning at the reconnaissance drilling stage. This will
keep expectations about a resource as realistic as possible and reduce sur-
prises for both mining companies and their investors.
The mineral matter method for in situ density estimation proposed
in this paper is ideal for exploration datasets because it allows data
from all coal and rock samples to be used for density and tonnage esti-
mation. It is unnecessary to extrapolate sparse RD data through samples
lacking these data, use constant coal or rock densities, or rely on least-
squares polynomials or untested empirical formulas developed by
other researchers.
The mineral matter method has several advantages relative to the
other methods reviewed in this paper:
1. Only ash, RD, and SE data are needed to derive the RD vs. mineral
matter regression equation.
2. Once the site-specific regression equation has been calculated, only
ash data are needed to estimate RD, although accuracy improves
with the use of SE data as well.
3. The equation requires only two coefficients, making it easy to use in
calculations.
4. There is no loss of accuracy outside a limited range of ash
percentages.
5. Uncertainty in high ash samples caused by mineral volatiles is
reduced.
6. Different in situ moisture values can be applied for coal and rock
samples.
7. The pure coal and mineral densities at 0% and 100% mineral matter,
respectively, can be compared to common maceral and mineral den-
sities in order to check their reasonableness.
8. The range of coal maceral and mineral densities can be graphically
evaluated using the RD vs. mineral matter chart (Fig. 10).
The mineral matter method has been developed from the funda-
mental properties of coal macerals and minerals. Formulas may be de-
rived empirically (from the statistical techniques presented in this
paper), for projects with adequate RD data, or deterministically (from
reasonable estimates of maceral and mineral types), for projects with
limited to no RD data. Maceral and mineral densities predicted by the
formula can be validated against petrographic analysis results, core de-
scriptions, and geophysical logs. The ranges of ρc and ρm values serve as
View publication stats
a useful guide to the variability within the deposit and may indicate
compositional or rank differences between seams.
Acknowledgements
The authors would like to express their gratitude to John Rusnak for
his support of this research at Peabody Energy and to Alan Best for
reviewing the formulas. Special appreciation is due to Professor Colin
Ward of the University of New South Wales for providing valuable in-
sights and revisions which significantly improved the quality of this
paper. The authors also thank Peabody Energy for providing the data
and granting permission to publish these results.
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