PERGAMON Journal of Asian Earth Sciences 17 (1999) 255267

Oil-generating potential of Tertiary coals and other organic-rich

sediments of the Nyalau Formation, onshore Sarawak
Abdullah Wan Hasiah
Department of Geology, University of Malaya, 50603 Kuala Lumpur, Malaysia
Received 8 December 1997; accepted 1 July 1998

Abstract

The oil-generating potential of coals and other organic-rich sediments from the Late OligoceneEarly Miocene Nyalau
Formation, the oshore extension of which is believed to be a major source rock, is evaluated. Coals of the Nyalau Formation
are typically dominated by vitrinite, with moderate and low amounts of exinite and inertinite, respectively. Signicant amounts
of clay minerals are present in these coals and those containing between 15 to 65% mineral matter by volume are termed
carbargilite. The samples analysed range from sub-bituminous to high-volatile bituminous rank, possessing vitrinite reectance in
the range 0.42% to 0.72%. Tmax values range from 42584508C which is in good agreement with vitrinite reectance data. Good
oil-generating potential is anticipated from these coals and carbargilites with moderate to rich exinite content (1535%). This is
supported by their high hydrogen indices of up to 400 mgHC/gTOC, PyGC (S2) pyrograms with n-alkane/alkene doublets
extending beyond nC30, and their being in the early to mid-mature oil-window range. Petrographically, the most signicant
evidence of the oil-generating potential of these coals is the generation of petroleum-like materials (exsudatinite) visible under
the microscope. Exsudatinite is a secondary maceral, commonly considered to represent the very beginning of oil generation in
coal, which is shown here to also have an important role to play in hydrocarbon expulsion. The precursor of exsudatinite in
these coals is the maceral bituminite which readily expels or mobilizes to hydrocarbon-like material in the form of oil smears
and/or exsudatinite as observed under the microscope. The maceral bituminite is considered to play a major generative role via
early exsudatinite generation, which is considered to facilitate the overall expulsion process in coaly source rocks. # 1999
Elsevier Science Ltd. All rights reserved.

1. Introduction source rock to have been deposited in peat swamp en-

The sediments under investigation constitute part of
the Nyalau Formation outcropping in the Bintulu
area, onshore Sarawak (Fig. 1a). The Tertiary strati-
graphy within the study area and the gross deposi-
tional facies are summarized in Fig. 1b. The Nyalau
Formation was deposited during OligoceneEarly
Miocene times (Wolfenden, 1960). This formation is of
particular importance as it is an onshore extension of
Cycles I and II in the Balingian Province oshore
Sarawak and are considered to contain important
source and reservoir rocks for oil and gas (Du Bois,
1985). In oshore areas, the sediments consist of u-
vial and estuarine channel sands with overbank clays
and coals. Selected crude oils from the Balingian
Province are waxy (high proportion of nC20+) with
high pristane/phytane ratio of >3.0 suggesting the
vironment of deposition (Awang Sapawi et al., 1991).
The onshore Nyalau Formation is made up of a simi-
lar lithological sequence of sandstoneshalemudstone
and also contains coal seams. These seams are gener-
ally thin, about 2030 cm thick and rarely exceeding
1 m (Fig. 2). Examples of such onshore successions are
found in the Bintulu area. The total thickness of the
Nyalau Formation is approximately 18000 ft (Liechti
et al., 1960) and coals are mainly present in the middle
and upper parts of the formation. The whole sequence
represents shallow marine, tidal and coastal plain
deposits and is only moderately folded.
In this study, the oil-generating potential of the
coals and other organic-rich sediments, which include
shales and carbargilites, were evaluated by means of
organic petrological and organic geochemical methods.
The samples analysed were collected around the

1367-9120/99 $ - see front matter # 1999 Elsevier Science Ltd. All rights reserved.
PII: S 0 7 4 3 - 9 5 4 7 ( 9 8 ) 0 0 0 4 3 - 9
256 A. Wan Hasiah / Journal of Asian Earth Sciences 17 (1999) 255267
Fig. 1a. Location of the study area.
Bintulu area, mainly along the BintuluMiri road and
BintuluTatau road.
2. Experimental
Detailed petrographic study was carried out on a
total of 30 samples, several of which were further ana-
lysed by Rock-Eval pyrolysis (as described by Espitalie
et al., 1977) and total organic carbon (TOC) determi-
Fig. 1b. Stratigraphy of the BintuluTatau area (after Wolfenden,
1960; Bait and Asut, 1991).
nation using a LECO carbon analyzer. The coals that
were analysed by Rock-Eval and TOC are from kilo-
meter 27 to 32, BintuluTatau road and at Kampung
Jepak, while the carbargilites and the shales are from
kilometer 16 to 17, BintuluMiri road. Among these
samples, a coal and a carbargilite were also analysed
by PyGC (pyrolysisgas chromatography; as
described by Bjory et al., 1985) and by GCMS (gas
chromatographymass spectrometry) using a Hewlett
Packard mass spectrometer instrument. An attempt
was made to isolate the bituminite/exsudatinite mac-
erals from the vitrinite matrix. Complete separation of
these macerals was not possible due to their intimate
association, however, more than 50% of bituminite/
exsudatinite material present was recovered (veried
microscopically). This material constitutes sample M16
upon which PyGC was performed.
Samples for microscopic assessment were crushed to
approximately 2 mm in size and mounted in slow-set-
ting polyester (Serix) resin mixed with resin-hardener
in mounting cups. Upon hardening, the blocks were
ground on a water-lubricated diamond lap until the
surface was at and free of irregularities. The samples
were then polished using successively ner grades of
silicon carbide and nally, alumina. Water is used as a
lubricant for all these polishing stages. Microscopical
examination was carried out under oil immersion in
 A. Wan Hasiah / Journal of Asian Earth Sciences 17 (1999) 255267 257

Fig. 2. Logged sections at (a) Sungai Selad, BintuluTatau Road and (b) Km 16, BintuluMiri Road.

plane-polarised reected light, using a Leica DMRXP
microscope photometry system equipped with uor-
escence illuminators. The lter system consisted of BP
340-380 excitation lters, a RKP 400 dichromatic mir-
ror and a LP 425 suppression lter. Maceral compo-
sitions, based on a 1000 point count, were determined
under both normal reected `white' light and UV
(ultraviolet) light. Random vitrinite reectance
measurements in oil immersion (%Ro) were carried
out in reected `white' light using a MPV SP photo-
meter head. The Windows-based MPVGEOR software
package was used to acquire the vitrinite reectance
data.
3. Results and discussion
Based on relative abundance of organic matter com-
pared to mineral matter (MM), three organic-rich rock
types are identied petrographically, comprising coals
258 A. Wan Hasiah / Journal of Asian Earth Sciences 17 (1999) 255267
Table 1
Geochemical data summary
Organic facies parameters Coal
% R0 0.420.70
TOC (% wt) 73.583.1
HI 292343
Tmax 425450
Kerogen assemblage Type III/II
(MM <15%), carbargilites (MM between 15%65%)
and shales (MM >65%). The variation in the pro-
portions of the organic versus the inorganic content is
also reected in the TOC content, whereby the coals,
carbargilites and shales, in general, possess TOC
>70%, between 70%20%, and <20%, respectively.
A summary of vitrinite reectance (%Ro) and geo-
chemical data for the samples analysed is presented in
Table 1.
3.1. Maceral/kerogen assemblage
The maceral composition of the coals and carbargi-
lites is plotted on a ternary diagram in Fig. 3.
Vitrinite, generally classied as type III kerogen, is the
most abundant maceral in the coal and carbargilite
samples (58%78% and 40%45% by volume, re-
spectively). All samples, however, contain signicant
amounts of type II liptinite macerals (15%35% by
volume). The most common liptinitic constituents in
the coals are resinite and sporinite with minor amounts
of bituminite and liptodetrinite. The liptinitic material
in the carbargilites, in contrast, is dominated by bitu-
minite and exsudatinite, with relatively minor amounts
of resinite and sporinite. The microscopic features and
Fig. 3. Maceral and mineral matter distributions in coals (.) and car-
bargilites ().
Carbargilite Shale
0.460.72 0.50
50.067.5 1.72
325400 50
425450 426
Type III/II Type III/IV
origin of all these liptinite macerals were described by
Wan Hasiah (1997b). In support of the petrological
data, the S2 PyGC pyrograms of the coals and
carbargilites (examples of which is shown in Fig. 4a)
display mixed kerogen ngerprints of predominantly
n-alkane/alkene doublets and aromatic compounds. In
sample M16, where the bituminite/exsudatinite content
is greater than the vitrinitic constituent, the pyrogram
is dominated by n-alkane/alkene doublets that extend
beyond nC30 indicative of the aliphatic-rich, oil-prone
nature of these macerals. In this sample the n-octene
to xylene ratio is 1.1 while in samples R2-16 and
SB32B, a carbargilite and a coal, respectively, a
slightly lower ratio of 0.8 is obtained.
The relatively higher value of hydrogen indices (HI)
of about 400 mgHC/gTOC in the carbargilites com-
pared to the coals (see Table 1) is likely to be due to
the higher abundance of the macerals bituminite and
exsudatinite in the carbargilite, and suggests that the
carbargilites possess greater oil-generating potential
than the coals. This is illustrated by the HI-Tmax dia-
gram shown in Fig. 5. The shales are dominated by
type III and IV kerogen (vitrinite and inertinite)
suggesting poor oil-generating potential. This is sup-
ported by the relatively low hydrogen index of 50
mgHC/gTOC possessed by these samples.
3.2. Biomarker distribution
GCMS analysis was performed on the saturate hy-
drocarbon fraction of a carbargilite (R2-16) and on a
coal (SB32B) sample. The TIC (total ion current), m/z
191 and m/z 217 chromatograms for the two samples
are shown in Fig. 4b and Fig. 4c. Not all of the peaks
in these traces were identied. The peaks that were
identied (based on retention times and previously
published literature e.g. Armanios et al., 1994;
Sosrowidjojo et al., 1994) are listed in Table 2.
The TIC traces of the coal and the carbargilite dis-
play a waxy appearance, being depleted in the nC10
nC15 range and are dominated by heavier members
(nC25+). The samples analysed show the presence of
humps of unresolved complex compounds suggesting
that the samples are possibly biodegraded, thus
accounting for the depletion of the n-alkanes, in par-
 A. Wan Hasiah / Journal of Asian Earth Sciences 17 (1999) 255267 259

Fig. 4a. PyGC (S2) pyrograms of a coal (SB32B) and carbargilite samples (R2-16 and M16).
260 A. Wan Hasiah / Journal of Asian Earth Sciences 17 (1999) 255267

Fig. 4b. TIC traces of a coal (SB32B) and a carbargilite (R2-16) saturated hydrocarbon fractions.
 A. Wan Hasiah / Journal of Asian Earth Sciences 17 (1999) 255267

Fig. 4c. m/z 191 and m/z 217 mass fragmentograms of a coal (SB32B) and a carbargilite (R2-16) saturated hydrocarbon fractions.
261
262 A. Wan Hasiah / Journal of Asian Earth Sciences 17 (1999) 255267

be abundant in the saturated hydrocarbon fractions of

crude oils from SE Asia (Grantham et al., 1983; van
Aarssen et al., 1990, 1992) which are generally con-
sidered indicative of terrestrially-derived source. Both,
the coal and carbargilite samples show biomarker dis-
tributions of typical terrigenous organic matter input
characterized by a very high hopane/sterane ratio
(>10), high Tm/Ts ratio, dominance of C29 steranes
over C28 and C27 steranes, low diasteranes and high
bicadinanes compounds. 18a (H)-oleanane, although
present in both samples, is higher in relative abun-
dance in the carbargilite, possessing a higher oleanane/
C30 hopane (ol/30) ratio compared to the coal sample
(Fig. 4c). Based on these biomarker assemblages, Wan
Hasiah et al. (1995) correlated these two potential
sources (bituminite/exsudatinite-rich carbargilite and
bituminite/exsudatinite-poor coal) to the two main oil
types in the Balingian Province, oshore Sarawak.
Since the coals only contain minor amounts of bitumi-
nite (<5% by volume), some other hydrogen-rich con-
stituents must also contribute to the oil-proneness of
the Nyalau Formation coals.
Fig. 5. Hydrogen Index/Tmax diagram.
The possible presence of cadalene, the diaromatic
counterpart of cadinane (tentatively identied by van
ticular the lower end member series. Isoprenoids, in Aarssen et al., 1992 in several SE Asia crude oils),
particular pristane and phytane, occur in high relative detected in the S2 PyGC pyrograms, may represent
concentrations, possessing pristane/phytane (Pr/Ph) one other terrestrial marker compound, particularly in
ratios >3.0. These features are similar to those sources of low thermal maturity. It is interesting to
described by Awang Sapawi et al. (1991) for Balingian note that this compound occurs in lower concentration
Province oils. (based on cadalene to xylene ratio) in the coal sample
The m/z 191 mass fragmentograms of the carbargi- of mid-maturity (0.7%R0) which is low in mineral
lite and coal samples show abundant pentacyclic triter- matter content and bituminite/exsudatinite macerals,
panes. The m/z 217 mass fragmentograms are than in carbargilite sample of low thermal maturity
dominated by bicadinanes (bc), a group of resin-de- (0.45%R0) which is rich in bituminite/exsudatinite as
rived triterpenoid pentacyclic hydrocarbons found to well as clay minerals. A plausible explanation of this
interaction between maturity eect, organic matter
type and presence of clay minerals needs further
Table 2 detailed investigation.
Peak assignments in the m/ z 191 and m/ z 217 mass fragmento-
grams
3.3. Thermal maturity
Peak Compound
The coals and carbargilites possess vitrinite reec-
24 C24 tetracyclic terpane tance values ranging from 0.42 to 0.72% and therefore
Ts 18a(H),22,29,30-trisnorneohopane
are of sub-bituminous C to high volatile bituminous B
Tm 17a(H),22,29,30-trisnorhopane
29 C29 17a(H),21b(H)-hopane rank. Tmax values range from 42584508C and are thus
29 m C29 17b(H),21a(H)-moretane in good agreement with the vitrinite reectance data.
ol 18a(H)-oleanane Shale samples possess vitrinite reectance values of ap-
30 C30 17a(H),21b(H)-hopane proximately 0.5%. All samples analysed are therefore
30 m C30 17b(H),21a(H)-moretane in the early mature to mid-mature range. The level of
31 S 17a(H)-homohopane (22 S)
31R 17a(H)-homohopane (22R) thermal maturity attained by these samples is also
32 S 17a(H)-bishomohopane (22 S) reected in their biomarker distributions. The coal
32R 17a(H)-bishomohopane (22R) sample (SB32B) with R0 of 0.7% possesses lower mor-
bc trans-trans-trans-bicadinane etane to hopane (30 m/30) and Tm/Ts ratios compared
bc? Bicadinane (unidentied structure)
to the carbargilite sample (R2-16) with R0 of 0.45%,
C29 steranes 5a(H),14a(H)17a(H)&5a(H),14b( H),17b(H)20(S + R)
C29 steranes and the latter sample shows incomplete isomerisation
of the 22R to 22 S of the C32 hopane (see Fig. 4c).
 A. Wan Hasiah / Journal of Asian Earth Sciences 17 (1999) 255267
The generation of petroleum in most source rocks is
considered to begin in the sub-bituminous A coal
stage, which is equivalent to approximately 0.5%R0
while the actual expulsion of hydrocarbons begins
later, in the high volatile bituminous coal stage which
approximately equivalent to 0.7%R0 (Hood et al.,
1975; Tissot and Welte, 1984). However, there have
been a number of workers that have observed an early
phase of hydrocarbon generation from coals at a
maturity generally regarded as immature (e.g.
Khorasani and Murchison, 1988; Zhao et al., 1990;
Khorasani and Michelsen, 1991; Wan Hasiah et al.,
1995). Coals and carbargilites of the Nyalau
Formation in the Bintulu region also show evidence of
this early generation phenomenon, and its relevance
with regard to the nature of oil generation and expul-
sion is discussed below.
3.4. Oil generation and expulsion
The mechanism of petroleum generation and expul-
sion from coals and related terrestrially-derived or-
ganic matter is still poorly understood. It appears to
involve a great number of factors such as maceral
type, maceral association (microlithotype), coal micro-
texture and hydrocarbon saturation thresholds (e.g.
Bertrand, 1989; Littke et al., 1989; Hunt, 1991;
Snowdon, 1991; Stout, 1994; Scott and Fleet, 1994).
These factors are complexly interrelated and are a pro-
duct of the original precursor material (coal-forming
ora), depositional environment, degree of preser-
vation of organic matter (inuence of microbial ac-
tivity), and association with mineral matter. To what
extent diering tectonic styles, climate, geology and
time inuence the petroleum potential of these sedi-
ments is still unclear.
Although it is now generally accepted that terrest-
rially-derived organic matter is capable of generating
oil in commercial volumes e.g. Kutei and South
Sumatera Basins, Indonesia (Thompson et al., 1985;
Sosrowidjojo et al., 1994), Gippsland Basin, SE
Australia (Thomas, 1982), the nature of the terrestrial
organic matter responsible is generally unspecied. The
recognition that terrestrial organic matter is a contri-
butor to oil accumulation has come from a range of
geochemical techniques such as biomarker research
(see Philp, 1994) and pyrolysisgas chromatography
(e.g. Powell and Boreham, 1994; Stout, 1994). Since
oil-source characterization studies are generally organic
geochemical in nature, sucient attention is not always
given to the microscopical assessment of the source
material. This study is an attempt to incorporate both
organic petrological and organic geochemical methods.
The organic petrographic study revealed an early
phase of petroleum-like material (exsudatinite) being
generated in the Nyalau Formation coaly source rocks
263
(Figs. 69). It was possible to directly identify the orig-
inal precursor of this exuded material as the maceral
bituminite, regarded here as the most oil-prone organic
constituent of the Nyalau Formation coals/carbargi-
lites. This is illustrated by its readiness to expel hydro-
carbon-like material in the form of oil smears and/or
exsudatinite as observed under the microscope (Figs. 7
and 9). Although exsudatinite is presently in the form
of solid bitumen, the microscopic texture clearly indi-
cates mobility under geological conditions. The readi-
ness of exsudatinite to disproportionate into free
hydrocarbons in the form of oil droplets is clearly vis-
ible under the microscope, especially when irradiated
with UV or blue light (Fig. 8). Some of these petro-
graphic features, indicative of oil generation from
these coals and carbargilites, were presented elsewhere
(Wan Hasiah, 1997b). The apparent ease with which
the maceral bituminite expels liquid hydrocarbon,
suggesting it has reached its saturation threshold, can
also be observed under normal reected `white' light
(Fig. 9). The oil-proneness of this maceral is conrmed
from the PyGC (S2) pyrograms of sample M16,
which is dominated by n-alkane/alkene doublets
extending beyond nC30.
It is important to note that the generation mechan-
ism described here is a low maturity phenomenon.
Coals and carbargilites possessing relatively low vitri-
nite reectance (0.450.55%) have generated a mobile
petroleum phase, either as a disproportionate product
of exsudatinite or by direct expulsion from the bitumi-
nite precursor. By a vitrinite reectance of about 0.7%
(or slightly higher), exsudatinite occurs only as an
inert residue in the form of a micrinite-like maceral
(Fig. 10). At this maturation level, the remnant exsu-
datinite only uoresces faintly or not at all, suggesting
that it has expelled most of its hydrogen-rich com-
ponents.
The question most often debated in relation to oil
generation and expulsion from coals is whether the hy-
drocarbon that has been generated can be expelled out
of the coal. Among the factors highlighted with
regards to hindrance of migration from coal is its
adsorptive capacity, a phenomenon thought to largely
prevent the release of generated liquid hydrocarbons,
except from certain boghead and cannel varieties
(Hunt, 1991, 1996). It is described and demonstrated
in this study that one possible mechanism of expelling
petroleum from a coaly source is via the formation of
exsudatinite. The formation of exsudatinite has long
been regarded as representing the very beginning of
hydrocarbon generation in coal (Teichmuller, 1974).
However, it is felt that the role and signicance of
this maceral in petroleum expulsion has not been
fully appreciated. Its characteristic behaviour of form-
ing a crack network, as illustrated in Fig. 12 and
Fig. 13 (see also Wan Hasiah, 1997a), suggests that it
 264
A. Wan Hasiah / Journal of Asian Earth Sciences 17 (1999) 255267

Fig. 6. (F6). Extrusion of hydrocarbon in the form of exsudatinite (e) from the precursor bituminite (b); UV light excitation; mag. 125  .

Fig. 7. (F7). Bituminite displaying characteristic properties of low reectance, coloured internal reection and lack of any characteristic shape or structure (same eld of view as Fig. 6); reected
`white' light; mag. 125  .

Fig. 8. (F8). Occurrence of oil droplets representing free hydrocarbon in exsudatinite; UV light excitation; mag. 160  .

Fig. 9. (F9). The maceral bituminite readily expelling liquid hydrocarbons in the form of oil smears and exsudatinite maceral; reected `white' light; mag. 160  .
 A. Wan Hasiah / Journal of Asian Earth Sciences 17 (1999) 255267

Fig. 10. (F10). A micrinite-like inert residue, formed once the exsudatinite has expelled all of its hydrogen-rich components; reected `white' light; mag. 125  .

Fig. 11. (F11). At an early stage of exsudatinite generation from its precursor maceral, bituminite (uoresces dull brown) expelling hydrocarbons preferentially along the shaly layers of carbargi-
lites; UV light excitation; mag. 125  .

Fig. 12. (F12). As more of the exsudatinite material is generated, it forms cracks perpendicular (as well as parallel) to the shaly layers within the carbargilites and begins to intrude into the
`pure' coal part of the rock; UV light excitation; mag. 125  .
265

Fig. 13. (F13). Exsudatinite forming a crack network and brecciating the coal/carbargilite; UV light excitation; mag. 125  .
266 A. Wan Hasiah / Journal of Asian Earth Sciences 17 (1999) 255267
has a great role to play in hydrocarbon expulsion into
a carrier bed. At an early stage of exsudatinite gener-
ation from its precursor maceral, the preferred path of
extrusion seems to be along the shaly layers of carbar-
gilites (Fig. 11). As more of the exsudatinite material is
generated, it forms cracks perpendicular to the shaly
layers and begins to intrude into the `pure' coal part
of the rock (Fig. 12) subsequently brecciating the rock
(Fig. 13). It appears that the generation of petroleum
in the form of exsudatinite is enhanced in the carbargi-
lite more than in the `pure' coal as the presence of the
shaly layers (predominantly silty shale) provide a more
ecient conduit for expulsion. On a larger scale, thin
coals and carbargilites interbedded with the shales and
sandstones of the Nyalau Formation, would provide
favourable conditions for short range migration.
4. Conclusions
Coals are a very varied and complex group of source
rocks. A number of factors inuence the timing (and
therefore phase) of petroleum generation and expul-
sion from coals/carbargilites. The relative importance
of these factors will vary from formation to formation
and under dierent geological situations. As for the
Nyalau formation coals and carbargilites, the maceral
type (its abundance and their association), microtex-
ture (e.g. exsudatinite crack network) and mineral mat-
ter association are among the important factors
inuencing petroleum generation and expulsion mech-
anism.
Based on this study, good oil-generating potential is
anticipated from the coals and carbargilites of the
Nyalau Formation, owing to their exinite-rich nature
(type II kerogen supported by high HI) and of favour-
able maturity. Carbargilites have slightly better genera-
tive and expulsive potential compared to the coals, on
account of a more extensively developed exsudatinite
crack network, and by being nely interbedded with
shaly layers, which better facilitates migration within
the source rock and subsequent expulsion (i.e. primary
migration) into conduit beds. Poor oil-generating po-
tential is anticipated from the shales as the kerogen is
predominantly of type III and IV.
The organic matter type identied to be the most
crucial in the oil generation/expulsion process in this
formation is bituminite, by virtue of its ability to gen-
erate signicant amounts of the secondary maceral
exsudatinite. The development of an exsudatinite crack
network at a relatively low maturity (0.450.55 %R0)
is believed to facilitate expulsion of later generated
hydrocarbons. Thus, it appears that exsudatinite rep-
resents more than just the beginning of oil generation
in coals, but also plays a signicant role in hydro-
carbon expulsion.
Acknowledgements
The authors would like to thank Petronas Research
and Scientic Services Sdn. Bhd., Exxon Production
Research Company and Geolab Nor for technical as-
sistance and University of Malaya for providing
Research Grant No. F484/97. The author would also
like to thank Mr Ching Yu Hay for drafting Fig. 1a
and 2. Comments by Mr P. Abolins, Mr R.C. Davis
and Dr C. Schiefelbein are acknowledged and very
much appreciated.
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