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PETROLEUM EXPLORATION AND DEVELOPMENT

Volume 44, Issue 1, February 2017


Online English edition of the Chinese language journal

Cite this article as: PETROL. EXPLOR. DEVELOP., 2017, 44(1): 32–39. RESEARCH PAPER

Significance of source rock heterogeneities: A case study


of Mesoproterozoic Xiamaling Formation shale in North
China
WANG Xiaomei1, 2, *, ZHANG Shuichang1, 2, WANG Huajian1, 2, SU Jin1, 2, HE Kun1, 2, WANG Yu1, 2,
WANG Xiaoqi2
1. Key Laboratory of Petroleum Geochemistry, China National Petroleum Corporation, Beijing 100083, China;
2. PetroChina Research Institute of Petroleum Exploration & Development, Beijing 100083, China

Abstract: Taking Mesoproterozoic Xiamaling Formation, Northern China as an example, the heterogeneities of source rock in different
scales and hydrocarbon microscopic occurrence are studied based on observation of outcrops and observation with microscopy, and geo-
chemical analysis. The large scale heterogeneities of source rocks are considered to be controlled by the plate movement and pa-
leo-latitude location, while the micro-scale might be controlled by climate changes driven by the astronomical orbit. The constant exis-
tence of heterogeneities includes the differences of organic matter, debris sources and porosities. The heterogeneities of source rock
should be seriously treated during the evaluation of oil and gas resources, especially the unconventional oil and gas. This kind of hetero-
geneous source rocks provides excellent source-reservoir assemblage of oil and gas generation, expulsion and accumulation, and new ref-
erence indexes for the economic evaluation of unconventional oil and gas. Therefore, quantitative study of the heterogeneity of source
rock is of great significance for investigating formation mechanism and resource estimation of unconventional oil and gas.

Key words: shale; source rock; heterogeneity; organic laminae; source-reservoir assemblage; unconventional oil and gas resources
evaluation; Mesoproterozoic; Xiamaling Formation

Introduction fore, explorationists and scientists set their eyes on source


rock once again, and they tried to find out the factors control-
In more than one hundred years since the birth of petroleum
ling the organic matter enrichment, formation of source rock,
industry, sources rocks have become the second circle of aca-
demic and industrial focus. The first time was in the 1970s, and source-reservoir types from the biogeochemical process
when the theory of “kerogen generating hydrocarbon” was experienced by the source rocks, and the perspective of “at-
first put forward by Tissot et al., in this theory, the argilla- mosphere-continent-ocean interaction”[811].
ceous rocks and shale, rich in organic matters, are regarded as In recent years, some researchers have found that high
hydrocarbon sources[1], and so comes the petroleum explora- quality source rocks are generally laminated organic-matter-
tion concept of “hydrocarbon sources controlling hydrocarbon rich shale and organic-matter-poor siliceous rock and carbon-
accumulation”. The second time was in the 1990s, triggered ate, for example, the Mesoproterozoic Xiamaling Formation
by the technological breakthrough made by the Americans in in North China[11], the Permian Dalong Formation in South
the exploration of unconventional petroleum accumulations, China[12], the Early Jurassic Blue Lias Formation in the
and this time the theory that argillaceous rocks and shale southeastern England[13], and the worldwide Cretaceous Cam-
could act as reservoirs was advanced[23], subsequently, a new panian organic-matter-rich shale[14]. Further research shows
understanding of "source-reservoir in one" have been reached. that the heterogeneity of source rocks, rather than chaotic, has
In over a decade, major oil and gas fields have been found in some explicit regularity. The sedimentary records reveal that
the deep strata and ancient marine strata around the world[47], the source rocks have regular patterns in spatial distribution
making us wonder what’s the formation limit, depth limit and and developing time. The spatial distribution pattern of source
potential limit of hydrocarbon exploration once again. There- rocks is attributed to the Wilson Cycle of tectonic move-

Received date: 04 Jul. 2016; Revised date: 19 Dec. 2016.


* Corresponding author. E-mail: wxm01@petrochina.com.cn
Foundation item: Supported by the Key Fund of National Natural Science Foundation of China (41530317); the China National Science and Technology Major
Project (2016ZX05004); the Scientific Research and Technological Development Project of China National 565 Petroleum Corporation (CNPC 2016A-0204).
Copyright © 2017, Research Institute of Petroleum Exploration and Development, PetroChina. Published by Elsevier BV. All rights reserved.
WANG Xiaomei et al. / Petroleum Exploration and Development, 2017, 44(1): 32–39

ment[15], also influenced by the ancient latitude and geo-


graphic location[11]; whereas the developing time span of
source rocks is considered to be controlled by the climatic
cycle driven by the orbital force[11]. Wagner et al. studied the
Cretaceous source rocks on both sides of the Atlantic, and
found out that source rock heterogeneity was clearly influ-
enced by ancient climatic changes and the Milankovitch Cy-
cles[9,14,16]. Recent research on the Xiamaling Formation dem-
onstrates that the Mesoproterozoic source rocks are also in-
fluenced by the Milankovitch Cycles[11]. The source rock het-
erogeneity has different time scales: the large cycle is of 110
million years, shown as source rock development in different
geologic ages; the medium cycle is of 10100 thousand years,
shown as interbeds of organic-matter-rich shale and or-
ganic-matter-poor sediments; and the small cycle is less than a
thousand year in time span, shown as the alteration of or-
ganic-matter-rich layer and clastic layer observed under mi-
croscope. Thus, the macroscopic cyclicity and heterogeneity
of source rock is clearly related with the tectonic movements Fig. 1. Outcrop distribution of Xiamaling Formation in North
China (Modified from literature [18]).
of the lithosphere, the orbital force, and the ancient latitude,
whereas the microscopic heterogeneity of organic matter layer showing the Xiamaling Formation is of the Mesoproterozoic
development is related with the periodic changes of climate. age, and it is thus estimated that the ancient sedimentary rate
The sedimentary record of recent 0.64 million years reveals then was approximately (6.6±1.4) mm/ky[11]. The Xiamaling
that the ancient climatic change, which controls the primary Formation, deposited in the Xiahuayuan area, Zhangjiakou, is
productivity of both the continent and the ocean, is of mon- in unconformable contact with the Jurassic Strata above, and
soon type. The climatic change is actually composed of sev- Tieling Formation below, 470 m in thickness, and low in ma-
eral cycles of different time scales, including smaller cycles of turity (with a EasyRo of 0.6%), and the cumulative thickness
several decades, and larger cycles of several hundred years to of organic-matter-rich shale with total organic carbon content
several thousand years, which are influenced by solar radia- of more than 1% is over 200 m. The middle to lower part of
tion and ocean current[11]. Thus, the macroscopic and micro- the Xiamaling Formation encompass interbeds of siliceous
scopic heterogeneity of source rocks are probably influenced rock and black shale, in which the black page-like shale has
by the inherent forces of the Earth itself. It is the above con- the highest TOC of 24%, chloroform asphalt content of over
trolling factors of different time scales that eventually give 8 800 μg/g, and oil content of over 10%, reaching the stan-
rise to the source rock heterogeneity of different scales. dard of oil shale[19].
The above researches provide us a new way to evaluate
1.1. Characteristics of the outcrop
source rock heterogeneity and cyclicity quantitatively, sur-
passing early qualitative source rock assessment from a few This set of low-maturity source rock in the Xiamaling For-
parameters such as primary productivity, preservation condi- mation shows distinct heterogeneity on the outcrops, include-
tions, and sedimentary rate[17]. But few researches have been ing sedimentary cycles of two different time scales. On the
carried out on the quantification and hydrocarbon accumula- large time scale, Unit 1 is composed of alternations of or-
tion significance of source rock heterogeneity of different ganic-matter-poor layers and organic-matter-rich layers from
time scales, especially in the unconventional hydrocarbon top of the formation to the base; Unit 2 is rich in organic mat-
exploration. Taking the Mesoproterozoic Xiamaling Forma- ter; Unit 3 is composed of alternations of organic-matter-poor
tion of North China as an example, the source rock heteroge- layers and organic-matter-rich layers; and Unit 4 is poor in
neity and its significance in hydrocarbon accumulation have organic matter. Thus, the 350 m sedimentary strata of Xiama-
been discussed from the perspective of organic petrology, ling Formation is divided into four units (Fig. 2). On the small
geochemistry, and hydrocarbon migration in this paper. time scale, each unit displays rhythmic sedimentary charac-
teristics of minor difference. Unit 1 (075 m) is mainly com-
1. Heterogeneity of the Xiamaling Formation
posed of alternations of black and green shale, and green silty
shale
mudstone and marl. Unit 2 (75242 m) is mainly composed of
The Xiamaling Formation is mainly distributed in the Yan- alternations of black shale and thin-layer gray shale or green
liao Depression in North China (Fig. 1). The age of tuff and mudstone. Unit 3 (242305 m) is mainly composed of alter-
bentonite samples were determined by high-precision zircon nations of black shale and siliceous rock or green mudstone.
data are (1 384.4±1.4) Ma and (1 392.2±1.0) Ma respectively, Unit 4 (305350 m) is mainly composed of red mudstone and

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WANG Xiaomei et al. / Petroleum Exploration and Development, 2017, 44(1): 32–39

Fig. 2. Heterogeneity characteristics of sediments in the Xiamaling Formation in the Xiahuayuan area, Zhangjiakou (TOC).

green silty mudstone. Except for Unit 4, black shale is ubiq- smaller time cycles of several thousand to tens of thousand
uitously distributed in the Xiamaling Formation, alternating years. Such sedimentary cycles are considered to be related to
with other types of sedimentary layers. Based on the sedi- the Milankovitch Cycles driven by orbital force and the Had-
mentary rate of Unit 3 of approximately (6.6±1.4) mm/103 a, ley Cell controlled by ancient latitude distribution[11]. The
it is estimated that the lasting time of the four sedimentary spatial distribution of effective source rock is more controlled
cycles are 11.4 Ma, 25.3 Ma, 9.5 Ma, and 7.0 Ma, respectively, by basin structure, for example, black shale of the Xiamaling
whereas the centimeter-thick black shale and interlayers are of Formation is mainly distributed in the slope and basin facies

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WANG Xiaomei et al. / Petroleum Exploration and Development, 2017, 44(1): 32–39

in the depression (Fig. 1). spectrum analysis reveal that organic bands can be seen
clearly in the black shale, with a thickness of 1020 μm (ap-
1.2. Microscopic characteristics
proximately half the thickness of the alternating clastic band).
Orthogonal polarization microscopic observation reveals For example, Point a in Fig. 4, located in the organic band,
bedding and texture structure are both widely developed in the has a percentage of carbon atom of more than 70%, whereas
Xiamaling Formation. The organic matter rich laminae are the percentage of carbon atom of the clastic band is below 1%;
generally black, brown, and dark brown under reflected light, while Point b has a high silicon atom percentage of 27.4%, a
around 10150 μm thick in single lamina, in continuous or ratio of atomic silicon to oxygen of approximately 1:2.48,
discontinuous ripple shape and fold shape. In contrast, the lower than quartz (1:2.0), but higher than silicate (1:3.0), in-
alternating clastic layers poor in organic matter are generally dicating Point b should be clay minerals with certain amount
yellow or khaki, with quartz crystals and cubic pyrite crystals of silicate. The observation results also reveal that the organic
clearly seen. In the organic-matter-rich black shale (Fig. bands are tight, with low porosity, and pores mostly less than
3a-3b), the organic laminae are generally black, thick in single 5 μm and microscale or nanometer scale; whereas pores and
lamina, with much higher organic content than the clastic micro-fractures are much more developed in the alternating
laminae, and high alternating frequency. In comparison, in the clastic layers, and mostly micrometer scale (Fig. 4). Although
organic-matter-poor siliceous rock (Fig. 3c-3d), greyish-green micro-fractures and pores in the clastic layers are irregular,
mudstone (Fig. 3e) and green mudstone (Fig. 3f), the organic they can connect with each other laterally into interlayer pores
laminae are generally brown and khaki, thinner in single lam- and micro-fractures.
ina, and much higher in organic content than the clastic layers, Based on the charged effect of the electron beam of the
with slightly lower alternating frequency. Microscopic obser- oil-bearing samples, and utilizing the method of back scatter-
vation also shows that transitions among different lithofacies ing cross section secondary imaging of focusing ion beam–
exhibit obvious distinction in the number of organic laminae scanning electron microscope (FIB-SEM), the in-situ distribu-
and the crystal characteristics of clastic minerals (See Fig. 2 tion of free hydrocarbons in the black shale of the Xiamaling
thin sections). The above observations indicate that the mi- Formation has been observed. With a spatial resolution of
croscopic heterogeneity of the Xiamaling Formation derives nanometer scale (< 106 m), and detection limit of 1012 mol,
from the difference in organic matter content and sedimentary this method is better than the conventional fluorescence and
source. Such microscopic heterogeneity in the time cycle of energy spectrum analysis in both detection effect and limit,
several years to several decades might represent the influence and can overcome the poor representativeness of analyzed
of climatic changes on primary productivity, sedimentary clast area caused by sample heterogeneity, thus achieving the goal
source, and preservation conditions. of in-situ imaging of free hydrocarbons in trace amount[20].
Scanning electron microscopic observation and energy The results show that free hydrocarbons occur mainly in the

Fig. 3. Organic petrologic characteristics of the source rock in Xiamaling Formation.

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WANG Xiaomei et al. / Petroleum Exploration and Development, 2017, 44(1): 32–39

Fig. 4. Interbedded deposits and pore characteristics of organic


matter layer of gray-black shale (290.4 m) and debris layer (a
energy spectrum measurement points of organic matter layer,
benergy spectrum measured points on debris layer).

form of bands or block bright patches (Fig. 5). The block


bright patches are mostly less than 5 μm, and sporadic in
space distribution, which might represent the accumulation of
free hydrocarbons in the organic bands and micro-pores in the
clastic layers. The band bright patches are several microme-
ters, and crystals of detrital minerals are widely existed, which
may be accumulations of free hydrocarbons in micro-fractures
of the clastic layers. At transitions between black shale and
siliceous rock, or near micro-fractures, the accumulations of
Fig. 5. Occurrence of free hydrocarbons in sediments of Xiama-
free hydrocarbons could be clearly observed (Fig. 5a, 5c), ling Formation.
with much higher amount of hydrocarbons than the retained
hydrocarbons in the black shale, which indicates that free than one centimeter thick, which represents a depositional
hydrocarbons generated by organic matter had begun to mi- time span of 2050 thousand years, close to the precession
grate from black shale to the adjacent clastic layers or frac- (20 thousand years), obliquity (40 thousand years) and eccen-
tures, but due to the low maturity of organic matter, the tricity (50 thousand years) in modern Milankovitch Cycles,
amount of free hydrocarbons generated by the black shale is thus this might represent cyclic changes composed of several
still limited, and still in the early migration stage. Therefore, cycles of different time scales. Thus the cyclic changes of
the distributions of free hydrocarbons and organic bands re- organic matter and clastic mineral composition are the most
flect the source rock heterogeneity and features of hydrocar- typical features of source rock heterogeneity.
bon generation and migration. Geochemical analysis also reveals that source rock hetero-
geneity lead to the combination of hydrocarbon generation
1.3. Geochemical characteristics
and expulsion. Taking the one-meter-thick sedimentary cycle
High-resolution geochemical analysis of the Xiamaling in Fig. 6 for example, the average TOC of black shale is
Formation reveals that characteristics of the geochemical data 4.49%, whereas the TOC of alternating siliceous rock is only
have similar trend with sedimentary rock type. Taking the 0.51%. The hydrogen index value of black shale (averaging
most typical Unit 3 as an example, in this unit, black shale 287.0 mg/g) is approximately twice that of the siliceous rock
with TOC of over 3.0% alternates frequently with siliceous (averaging 143.6 mg/g). However, the hydrocarbon index
rock with TOC of less than 1%, which is consistent with the (averaging 20.4 mg/g) and productivity (averaging 0.13) of
changing pattern of hydrocarbon generation potential index the siliceous rocks are much higher than that of the black
HI and TOC (Fig. 6). The content of SiO2 can reflect clastic shale (averaging 9.0 mg/g, 0.03). But both the black shale and
quartz or silicate mineral composition, which has opposite siliceous rock have a Tmax value of 440 C, and similar car-
changing tendency with TOC. The content of TOC and SiO2 bon isotopic composition of kerogen (δ13Ck) (33.7‰ 
reflect the organic layers alternating with clastic mineral lay- 33.8‰), which indicate they have the same organic matter
ers, just like the microscopic observation. Such alternating source and thermal history, or same hydrocarbon generation
sedimentary cycles could occur for more than 30 times within process and hydrocarbon index theoretically. The reason for
one meter. The single organic-matter-rich shale layer is less the higher hydrocarbon index and productivity of the siliceous
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WANG Xiaomei et al. / Petroleum Exploration and Development, 2017, 44(1): 32–39

Fig. 6. High-resolution geochemical parameters of the 1m-thick sediments in unit 2 of the Xiamaling Formation.

rock should be the short distance migration of free hydrocar- rock, and result in inaccurate estimations in petroleum re-
bons from black shale to the adjacent siliceous rocks. This sources assessment. Research has proved that the main con-
phenomenon is consistent with FIB-SEM observation that tribution for oil and gas generation are the organic-matter-rich
hydrocarbon generated by the black shale tends to migrate to shale and mudstone layers[21], while the alternating layers poor
adjacent siliceous rock. in organic matter just provide pathways for hydrocarbon mi-
gration and space for hydrocarbon accumulation[9]. The high
2. Source rock heterogeneity and its significance
quality source rock are actually the thin-layered dark brown or
for hydrocarbon accumulation
black laminae, with extremely high content of organic matter
Source rock heterogeneity adds difficulty to petroleum re- (carbon atom percentage of higher than 70%) and hydrogen
source assessment. In conventional source rock evaluation, index, thus are the true sources responsible for hydrocarbon
the organic-matter-rich shale and the alternating clastic rock generation (Fig. 7a). In contrast, the clastic rock or carbonate
or carbonate are taken as a whole set of source rock, which with very low content of organic matter actually generates
might obscure the true information of hydrocarbon source insignificant amount of hydrocarbons, or no hydrocarbons,

Fig. 7. The hydrocarbon generation and expulsion processes and reservoir characteristics of the heterogeneous shale black shale.

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WANG Xiaomei et al. / Petroleum Exploration and Development, 2017, 44(1): 32–39

thus should not be regarded as hydrocarbon source rock. It is hydrocarbon generation, shale with TOC of approximately 7%
also found that, compared to homogeneous mudstone deposits can lead to 4.9% rise in porosity at the price of consuming
with large thickness, the black shale with strong heterogene- 35% organic carbon[3]. The organic matter content and poros-
ity actually has higher hydrocarbon generation potential. Tak- ity of Sha 3 of the Shahejie Formation in Zhanhua Depression
ing the major source layer, Member Chang 7 in Ordos Basin are positive correlated[25], but the increased porosity is mainly
as an example, the black shale interbedded with tuff has come from the alternating clastic rocks and carbonate, not the
higher effective carbon, hydrogen index, and degradation rate organic-matter-rich layers, which is the reason that or-
than the mudstone of the same thickness with weaker hetero- ganic-matter-poor interlayers have much better production
geneity[22], and hydrocarbon generation potential 5  8 times performance than the organic-matter-rich layers[26].
that of the homogeneous mudstone. Based on the above dis- In summary, the clastic or carbonate layers interbedded
cussion, source rock heterogeneity, such as the thickness of between source rock layers should be main reservoir space for
single source rock layer, scale of cycles, and hydrocarbon shale hydrocarbons, and the distribution and development of
generation potential of each cycle, should be taken into con- interlayers would determine the shale oil and gas reserves.
sideration to achieve more accurate estimation of petroleum During the exploration and development of unconventional oil
resources. and gas resources, besides basin structure[27] and secondary
From the view of hydrocarbon expulsion and accumulation, biodegradation[28], more attention should be paid to the search
the heterogeneous lithological association is better than the of source rock with high organic carbon content, suitable ma-
homogeneous one. The organic-matter-rich layers, as hydro- turity, and combinations of strongly heterogeneous shale and
carbon sources, can generate massive oil and gas, but low in clastic rocks or carbonate.
porosity, and thus low in storage capacity. The generated hy- 3. Conclusions
drocarbons can only be absorbed on the surface of organic
matter and mineral crystals, or accumulate in the nanometer The influence of source rock heterogeneity on hydrocarbon
scale organic pores and intercrystalline pores. In contrast, the generation and accumulation should be re-examined. Espe-
alternating clastic rock and carbonate layers, rich in fractures cially the selected parameters and calculation methods for
and pores, with the reservoir capacity over a hundred times petroleum resource assessment should be modified to some
that of the organic-matter-rich shale, act as effective reservoirs extent. In conventional source rock evaluation, the or-
for migrating hydrocarbons from adjacent shale (Fig. 7b), in ganic-matter-rich shale and the alternating clastic rock or car-
addition, the interlayer fractures can act as migration paths in bonate are combined together as a whole set of source rock,
the process of hydrocarbon expulsion, giving rise to excellent which may obscure the true information of hydrocarbon
source rock, and result in inaccurate estimations in petroleum
source-reservoir combination (Fig. 7c). For example, the shale
resources assessment. Meanwhile, the reservoir capacity and
layers in Sha 3 and Sha 4 of Shahejie Formation in the Jiyang
migration potential of the alternating clastic layers and car-
Depression, are rich in organic matter, and high in hydrocar-
bonate layers are neglected, which would bring great uncer-
bon generation potential, the generated oil only needed to
tainty to petroleum resources assessment, and lower the con-
migrate a short distance to accumulate in the interlayer, so,
trollable estimates for unconventional hydrocarbons. This
these interlayers should be considered as the focus in petro-
study shows that alternating shale and clastic rock or carbon-
leum exploration[23]. Therefore, the reservoir space of uncon-
ate layers, with strong heterogeneity can act as excellent
ventional shale oil and gas is not limited to the traditional
source-reservoir combinations. Organic-matter-rich layers can
large size fractures and pores, or the nanometer-scale pores in
generate massive hydrocarbons, the pores and fractures in
the organic layers[24], but includes the micrometer-scale pores
interlayers can provide space for hydrocarbon accumulation
and fractures in the interlayers between strongly heterogene-
and paths for hydrocarbon migration, and the alternating sili-
ous source rock. The interlayer pores and structures can act as
ceous rock or carbonate layers are effective reservoirs respon-
paths for hydrocarbon migration to let oil and gas out besides
sible for hydrocarbon accumulation. In the exploration and
reservoir space.
development of unconventional oil and gas, more attention
The strong heterogeneity shale combinations are conducive
should be paid to the source rock heterogeneity and interlayer
to reservoir modification and hydrocarbon current formation.
modification. Quantitative evaluation of source rock hetero-
On one hand, the interlayers, rich in brittle minerals and car- geneity and study on interlayer modification would definitely
bonate minerals, only adsorb few hydrocarbons, leading to beneficial for petroleum resource assessment, and exploration
high portion of free hydrocarbons; on the other hand, large and development of unconventional oil and gas.
amount of water-soluble organic acid anion and phenols are
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