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Coal Reservoir Laboratory of National CBM Engineering Center, School of Energy Resources, China University of Geosciences (Beijing), Beijing 100083, China
Coalbed Methane Resources and Reservoir Formation Process Key Laboratory of Ministry of Education, China University of Mining and Technology, Xuzhou 221116, China
CNOOC Energy Technology & Services-Oileld Engieering Research Institute, Tianjin 300452, China
a r t i c l e
i n f o
Article history:
Received 3 March 2013
Received in revised form 14 May 2013
Accepted 16 May 2013
Available online 25 May 2013
Keywords:
Geochemistry
Rare earth elements
Paleoenvironment
Oil shale
Dahuangshan
a b s t r a c t
The Dahuangshan oil shale, located in the northern Bogda Mountain, on the southern margin of the Junggar
Basin, was deposited in a Late Permian lacustrine environment. A combined investigation of element and
organic geochemistry was performed to dene the source rock potential, the paleoenvironment, and source
of the organic matter. Thick sequences of oil shales with an average thickness of 638 m were deposited in
Lucaogou Formation which mainly consists of oil shale, argillaceous dolomite, silty claystone, tuff, limestone,
and dolomitic marl. A spot of plant stem fossils and abundance of pyrite crystals, shtail and sh skeleton can
also be found there.
Analyzed oil shale samples from Dahuangshan area are characterized by high total organic carbon (TOC) contents (5.634.75%), S2 (22.65199.25 mg HC/g rock), hydrogen index (HI, 3591068 mg HC/g TOC), and oil
yield (4.926.6%), indicating the oil shales have excellent source rock potential. Tmax values (433453 C)
show an early to medium maturation stage of organic matter, which is supported by organic geochemical
maturation parameters. All of the obtained kerogen types are types II and I, with oil prone source rock potential.
Dahuangshan oil shale samples are rich in SiO2 (68.59%), followed by Al2O3 (10.18%) and Fe2O3 (5.43%). Compared with average shale and North American Shale Composite (NASC), analyzed oil shale samples are obviously
enriched in P (0.71%). There is a signicant correlation between Al2O3 and Fe2O3, MgO, K2O, MnO, Cu, Ba, Co, and
Ni for their association with clay minerals. Besides, the signicant correlations between Fe2O3 and MnO, Co, and
Ni are considered to result from their similarity on geochemical behavior. All selected oil shales are characterized
by distinctly sloping light rare earth elements (LREE) trends (LaN/SmN = 2.705.95) accompanied by at heavy
rare earth elements (HREE) trends, with distinct Eu negative anomalies (0.600.73). Two slightly different patterns of REEs in the oil shale samples are distinguished by the difference in Ce depletion and Nd anomaly.
In addition, Dahuangshan oil shale samples are characterized by short- to middle-chain n-alkanes, low carbon
preference index (CPI) values (0.931.24), single peak composed of nC20 or nC22, low Pr/Ph (0.410.91), relatively
high Homohop index (0.0610.99), and high concentrations of C27 sterane, indicating reducing, deep-water, and
moderate saline environment with prevalent contribution of algae and microorganisms to organic matter
accumulation.
2013 Elsevier B.V. All rights reserved.
1. Introduction
With rapid increases in consumption of energy and chemicals, oil
supply and demand imbalances are intensifying so as to become
a restraining factor on economic growth in China. China had imported
about 179 million (Fu et al., 2010) tons of crude oil in 2008 and over
250 million tons in 2011. Oil shale, one of the substantial unconventional
Corresponding author at: Coal Reservoir Laboratory of National CBM Engineering
Center; School of Energy Resources, China University of Geosciences (Beijing), Beijing
100083, China. Tel.: + 86 10 82322011.
E-mail address: peach888@163.com (S. Tao).
0166-5162/$ see front matter 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.coal.2013.05.004
fossil resources that can be produced and converted to liquid fuels, has
received increasing attention. The Third Chinese Oil and Gas Resource Assessment and the 2007 World Energy Survey showed that a total oil shale
resource of some 720 Gt is located across 22 provinces, 47 basins, and 80
deposits. The shale oil resource has been estimated at some 48 Gt, which
is highly signicant for alleviating the pressure of petroleum supplies (Liu
et al., 2007; WEC, 2007). At present, retorting and combustion for power
generation are the main patterns of oil shale application. In 2011, shale
oil production by retorting technology was about 1.46 million tons all
over the world, of which about 650,000 t were produced in China, including 7 oil shale retorting plants located in 5 provinces (Li, 2012). Estonia,
the biggest electricity producer from oil shale in the world (Hamburg,
42
2. Geological setting
Bogda Mountain is situated in the eastern part of Tianshan Mountain
range and is located on the southern margin of the Junggar Basin which
is a large, organic-rich foreland basin in northwest China (Jiao et al.,
2007; Tao et al., 2012a). Thick sequences of organic-rich lacustrine oil
shales are exposed in the foothills of Bogda Mountain (Carroll, 1998),
including 13 different oil shale mining areas, and eight of them have
been studied by us in recent years (Fig. 1A) (Tao et al., 2010, 2011,
2012a,b,c). Carroll et al. (1992) documented three Upper formations
that contain organic-rich mudstones. From oldest to youngest, they are
the Jingjingzigou, Lucaogou, and Hongyanchi formations, among which
extremely rich and oil-prone oil shales are discovered in Lucaogou
Formation.
The Dahuangshan region is located in the eastern part of Bogda
Mountain oil shale belt (Fig. 1A). The Permian Jingjingzigou, Lucaogou,
and Wutonggou formations are the major outcropping seams in this
area (Fig. 1B). The Lucaogou Formation consists of a sequence of dolomitic mudstone, dolomitic marl, argillaceous dolomite, limestone, silty
claystone, tuff, and oil shale (Fig. 2). In Dahuangshan area, the thickness
of the Lucaogou Formation (average 845 m) is larger than that of other
Fig. 1. (A) Simplied map showing geological setting of northern Bogda Mountain, and the location of the study area. (B) Simplied geological map of the Dahuangshan oil shales,
showing three oil shale proles, and two boreholes.
43
44
(Littke et al., 1998; Peters and Cassa, 1994; Tissot and Welte, 1984). The
extremely low PI-values (0.0040.037) indicate immature organic
matter whereas elevated Tmax values (433453 C) (Table 1) imply an
early to medium maturation stage.
Table 1
Results of Rock-Eval/TOC analysis and calculated parameters.
Sample no.
TOCa
(wt.%)
S1b
(mg HC/g)
S2 c
(mg HC/g)
S3 d
(mg CO2/g)
HIe
(mg HCi/g TOC)
OIf
(mg CO2/g TOC)
PIg
(S1 / S1 + S2)
Tmaxh
(C)
O-01
O-02
O-03
O-04
O-05
O-06
O-07
O-08
O-09
O-10
O-11
O-12
O-13
O-14
O-15
O-16
O-17
O-18
O-19
O-20
O-21
O-22
O-23
O-24
O-25
O-26
O-27
O-28
O-29
O-30
O-31
O-32
O-33
O-34
O-35
O-36
O-37
O-38
O-39
O-40
O-41
O-42
9.71
7.45
13.20
21.12
13.90
5.86
11.00
9.12
7.86
13.92
31.17
12.56
17.77
12.35
9.35
8.51
7.67
15.11
10.16
17.81
29.02
6.01
14.39
9.38
6.69
11.41
5.60
27.06
31.99
9.30
11.85
32.23
7.13
10.61
15.69
7.44
10.22
13.33
34.75
6.31
9.58
13.59
0.50
0.40
1.70
0.90
1.09
0.35
0.43
1.16
1.06
1.14
1.89
1.21
1.47
1.75
0.46
0.33
0.33
1.03
0.54
2.81
2.84
0.35
0.65
0.72
0.79
1.02
0.29
2.96
3.29
0.59
1.26
1.71
0.40
0.97
2.16
0.35
0.66
2.18
0.96
0.64
0.66
1.96
56.16
30.45
95.67
133.16
80.45
39.88
53.54
53.37
29.03
75.19
199.25
58.73
88.49
69.03
43.77
86.16
39.92
81.65
46.25
108.54
180.49
35.38
114.88
53.55
29.49
99.92
24.65
144.86
198.88
39.3
71.64
184.03
41.07
53.65
109.14
32.78
109.13
57.50
194.39
22.65
60.21
74.69
4.72
3.51
6.30
3.70
3.40
2.56
2.63
1.57
1.44
3.16
5.90
2.27
3.29
1.86
4.23
4.23
2.69
2.32
2.86
4.47
5.33
3.09
3.43
2.46
2.15
2.67
2.94
4.65
1.67
3.63
1.95
6.56
2.28
5.79
4.28
5.73
4.03
2.79
3.67
1.72
3.73
6.70
578
409
725
630
579
681
487
585
369
540
639
468
498
559
468
1012
520
540
455
609
622
589
798
571
441
876
440
535
622
423
605
571
576
506
696
441
1068
431
559
359
628
550
49
47
48
18
24
44
24
17
18
23
19
18
19
15
45
50
35
15
28
25
18
51
24
26
32
23
53
17
5
39
16
20
32
55
27
77
39
21
11
27
39
49
0.009
0.013
0.017
0.007
0.013
0.009
0.008
0.021
0.035
0.015
0.009
0.020
0.016
0.025
0.010
0.004
0.008
0.012
0.012
0.025
0.015
0.010
0.006
0.013
0.026
0.010
0.012
0.020
0.016
0.015
0.017
0.009
0.010
0.018
0.019
0.011
0.006
0.037
0.005
0.027
0.011
0.026
439
438
441
440
441
440
441
441
437
437
447
438
441
439
440
440
438
441
442
440
445
440
441
443
439
443
441
440
454
437
438
454
436
434
435
436
441
433
453
436
442
443
a
b
c
d
e
f
g
h
i
Fig. 3. Plot of TOC wt.% versus S2 mg HC/g rock indicating the kerogen types.
(NASC; Gromet et al., 1984); while, Al2O3, MgO, TiO2 and K2O contents
are lower than both of them; MnO contents of oil shale samples vary
from 0.09% to 0.29%, and the average being 2.57%, close to average
shale (0.36%), but much lower than that of NASC (2.98%).
Particularly, Dahuangshan oil shale is obviously enriched in P,
with a mean value of 0.71%, which is much higher than that of average shale (0.19%) and NASC (0.13%). This phenomenon is probably
caused by the input of the volcanic ash which is indicated by a tuffaceous composition of the interbedded mudstone and carbonate layers
(Fig. 5). Volcanic ash provided ample nutrients for growth of algae
leading to formation of a reducing depositional environment favorable
for preservation of organic matter. As a result, the oil yield values of
the Dahuangshan oil shale samples are relatively high, with an average
of 15.0%, which is even higher than the mean value of the Green River
oil shales (11.44%, Ruhl, 1982). The analysis results indicate that SiO2
is the dominant constituent of the outcrop samples, the variation of
which inuences directly on the contents of other elements (Table 3);
therefore, due to a dilution effect SiO2 exhibits a negative correlation
with most major elements and trace elements, which is so-called
Diluent Effect of SiO2.
Al2O3 is also an important component in surface sediments, the
contents of Al2O3 and SiO2 always change in the reverse direction.
45
Fig. 4. Plot of Tmax C versus HI mg HC/g TOC identifying the kerogen types.
4.5.1. n-Alkanes
Aliphatic hydrocarbons are dominated by n-alkanes. Gas chromatograms of saturated hydrocarbons from Dahuangshan oil shales
46
Table 2
Concentrations of ash, oil yield, total sulfur, organic sulfur and major elements in samples from the Dahuangshan oil shale (unit in %).
Sample no.
Oil yield
Ad
St,d
So,d
SiO2
Fe2O3
Al2O3
CaO
MgO
K2O
Na2O
TiO2
P2O5
MnO
O-04
O-11
O-13
O-20
O-21
O-28
O-29
O-32
O-35
O-39
Ave.
Ave. shalea
NASCb
7.8
4.9
9.9
12.2
20.5
26.6
15.1
17.5
9.4
26.2
15.0
52.35
64.33
55.08
67.14
65.45
62.37
71.03
64.18
56.91
50.2
60.90
0.88
0.48
0.89
0.59
0.32
0.35
0.31
0.34
0.52
0.58
0.53
0.31
0.21
0.3
0.15
0.13
0.09
0.09
0.18
0.23
0.23
0.19
66.14
69.01
63.84
64.7
71.09
71.5
76.78
70.14
65.42
67.29
68.59
64.21
64.8
6.68
4.96
6.84
5.34
5.18
4.32
4.76
4.76
5.98
5.46
5.43
6.71
5.66
12.39
10.26
12.88
11.3
8.6
7.82
6.37
9.4
12.69
10.12
10.18
17.02
16.9
1.33
3.14
3.8
5.02
3.41
4.1
3.3
3.7
3.6
3.96
3.54
3.44
3.63
2.34
1.97
2.08
2.09
1.84
1.81
1.73
1.86
2.63
1.98
2.03
2.7
2.86
2.52
2.34
2.82
2.76
2.05
1.82
1.5
2.14
2.75
2.12
2.28
3.58
3.97
2.2
0.7
1.93
2.28
0.61
0.56
0.44
0.73
1.46
1.23
1.21
1.44
1.14
0.68
0.58
0.64
0.55
0.51
0.48
0.41
0.5
0.62
0.6
0.56
0.72
0.70
0.86
1.15
0.98
0.3
0.42
0.48
0.36
0.78
0.86
0.92
0.71
0.19
0.13
0.22
0.14
0.29
0.13
0.18
0.11
0.09
0.18
0.25
0.20
0.18
0.5
0.06
Ad, ash yield, dry basis; St,d, total sulfur, dry basis; So,d, organic sulfur, dry basis.
a
From Clarke (1924).
b
From Gromet et al. (1984).
Td
Do
Td
Td
Q
Ta
Sd
Do
200 m
Td
Ta
200m
Td
Td
Q
Td
Qa
Td
200m
200m
Ta
Fig. 5. Minerals in the Dahuangshan prole samples (existing as thin bed or thin interbedded with oil shale), Thin section, Polarized light. A limestone with tuff debris (Td), tuffaceous matrix (Ta), and quartz (Q); B dolomite with tuff debris, dolomite (Do), quartz, and siliceous debris (Sd); C tuffaceous mudstone with tuff debris and tuffaceous matrix;
D tufte with tuff debris, tuffaceous matrix, quartz, and authigenic quartz (Qa).
47
Table 3
Correlation coefcient values of major elements and trace elements.
SiO2
Al2O3
Fe2O3
CaO
MgO
Na2O
K2O
TiO2
P2O5
MnO
Ba
Sr
V
Cu
Co
Ni
SiO2
Al2O3
Fe2O3
CaO
MgO
Na2O
K2O
TiO2
P2O5
MnO
Ba
Sr
Cu
Co
Ni
1.000
0.951
0.735
0.087
0.715
0.850
0.954
0.870
0.455
0.730
0.867
0.412
0.287
0.898
0.872
0.843
1.000
0.847
0.150
0.836
0.836
0.959
0.928
0.564
0.819
0.787
0.333
0.041
0.946
0.952
0.905
1.000
0.402
0.690
0.792
0.739
0.854
0.451
0.858
0.429
0.032
0.154
0.881
0.903
0.786
1.000
0.260
0.061
0.053
0.372
0.378
0.257
0.353
0.469
0.838
0.132
0.228
0.132
1.000
0.660
0.762
0.767
0.395
0.656
0.697
0.478
0.001
0.876
0.904
0.739
1.000
0.830
0.751
0.148
0.547
0.696
0.130
0.148
0.852
0.835
0.633
1.000
0.812
0.415
0.703
0.892
0.390
0.147
0.874
0.867
0.825
1.000
0.687
0.809
0.600
0.146
0.074
0.896
0.900
0.900
1.000
0.619
0.179
0.013
0.297
0.452
0.465
0.773
1.000
0.431
0.301
0.008
0.803
0.843
0.816
1.000
0.601
0.422
0.737
0.696
0.638
1.000
0.609
0.320
0.330
0.228
1.000
0.143
0.050
0.051
1.000
0.988
0.881
1.000
0.860
1.000
4.5.2. Terpanes
The distribution and relative abundances of pentacyclic and tricyclic
terpanes obtained from m/z 191 ion chromatograms are shown in Fig. 8
and their parameters are given in Table 5. Triterpenoids are relatively rare
in Dahuangshan oil shale samples. Traces of unsaturated triterpenes
are found in most of the samples. The hopanoids are dominated by the
presence of C30-hopane, C29-norhpane, 17(H)-trisnorhopane (Tm),
and a considerable quantity of homohopanes (C31C35) (Fig. 8).
Hopanes are ubiquitous constituents of sedimentary organic matter
(Piedad-Snchez et al., 2004; Zumberge, 1987). They are derived from a
degraded bacteriohopane C35 (Ourisson et al., 1979). As shown in Fig. 8,
the hopane C30 is the highest whereas the relative abundance of
Table 4
Rare earth element contents (in g/g) in samples and associated geochemical parameters.
Element
O-4
O-11
O-13
O-20
O-21
O-28
O-29
O-32
O-35
O-39
La
Ce
Pr
Nd
Sm
Eu
Gd
Tb
Dy
Ho
Er
Tm
Yb
Lu
Y
V
Ni
Sr
Ba
Cu
Co
REE
L/H
(La/Yb)N
Ce
Eu
(La/Sm)N
18.1
33.8
4.80
19.9
4.21
0.84
4.22
0.68
3.68
0.79
2.12
0.32
2
0.31
20.7
65.7
41.2
129
221
68.20
13.41
95.77
5.78
6.10
0.87
0.61
2.70
6.27
11.7
1.47
5.67
1.16
0.25
1.30
0.20
1.19
0.26
0.85
0.13
0.88
0.16
8.25
101
36.6
110
97.2
48.67
8.58
31.49
5.34
4.80
0.93
0.62
3.40
21.9
42.8
5.31
21.2
4.40
0.92
4.33
0.69
3.87
0.77
2.30
0.33
2.04
0.32
21.1
128
43.5
146
268
69.81
13.28
111.18
6.59
7.24
0.96
0.64
3.13
16.5
36.6
4.03
16.8
3.35
0.74
3.53
0.58
3.11
0.67
1.79
0.28
1.64
0.27
17.2
184
39.7
185
340
63.25
11.57
89.89
6.57
6.78
1.08
0.66
3.10
23.0
35.5
4.79
26.2
2.91
0.63
3.44
0.52
3.03
0.63
1.95
0.28
1.82
0.28
17.9
133
37.8
163
195
52.87
9.74
104.98
7.78
8.52
0.81
0.61
4.97
13.4
25.4
3.17
12.7
2.60
0.56
2.95
0.46
2.57
0.56
1.73
0.26
1.69
0.26
16.4
143
37.2
170
212
52.69
9.23
68.31
5.52
5.35
0.94
0.62
3.24
9.68
17.4
2.24
8.8
1.83
0.44
1.86
0.30
1.70
0.37
1.08
0.17
1.05
0.16
9.59
86.3
41.5
133
235
55.76
10.05
47.08
6.04
6.22
0.90
0.73
3.33
17.6
25.3
2.85
14.7
1.86
0.41
1.89
0.29
1.71
0.36
1.10
0.17
1.11
0.17
10
120
38.4
198
191
52.10
9.82
69.52
9.22
10.69
0.86
0.67
5.95
17.6
34.5
4.56
18.3
3.72
0.84
4.08
0.65
3.90
0.88
2.61
0.38
2.51
0.39
24.7
147
42.9
237
322
71.24
13.89
94.92
5.16
4.73
0.93
0.66
2.98
12.6
28.3
2.98
11.2
2.30
0.46
2.36
0.35
1.99
0.42
1.30
0.19
1.35
0.22
11.9
189
41.5
176
207
62.08
11.28
66.02
7.07
6.29
1.11
0.60
3.45
L/H = LREE/HREE; (La/Yb)N, (La/Sm)N; subscripts N stands for chondrite-normalized value (Boynton, 1984); Ce/Ce* = CeN/(LaN PrN)0.5; Eu/Eu* = EuN/(SmN GdN)0.5; subscripts N
stands for chondrite-normalized value (Boynton, 1984).
48
Fig. 6. Distribution patterns of rare earth elements in oil shale samples by chondrite-nomalized. REE patterns.
In general, Pr/nC17 and Ph/nC18 ratios would decrease along with the
increasing in maturity of organic matter (Moldowan et al., 1985). The
Pr/nC17 ratios range between 0.31 and 1.04, and Ph/nC18 ratios vary between 0.45 and 1.45 (Table 5), which are lower than those of immature
oil shale in the central Tibetan plateau (Wang et al., 2011), showing the
early maturation stage of oil shale in Dahuangshan area. This result is
consistent with the relatively high Tmax values as discussed above.
4.5.3. Steranes
The steranes composition could be correlated with the type of
environment (Huang and Meinschein, 1979). They proposed that a
dominance of C27 sterols (steranes) mainly derive from algae, while
the C29 sterols are more typically associated with land plants. Volkman
(1986) indicated that the low C28 levels are typical of limnic environments. However, they also considered that microalgae or cyanobacteria
can also be important sources of C29 sterols. From the m/z 217 mass chromatograms of our samples, the relative abundances of the C27, C28, and
C29 steranes and their 20S and 20R epimers have been determined
(Fig. 8; Table 5). Dahuangshan oil shale samples show a higher proportion of C27 (2455%) compared to C29 (2647%) and C28 (1329%)
steranes, except sample O-04 having C29 > C27 steranes distribution,
reecting a high contribution of aquatic algae (Peters and Moldowan,
1993), which is consistent with the n-alkanes distribution. The predominance of C29 steranes in sample O-04 may reect a high contribution of
bacteria or/and microorganisms (Riboulleau et al., 2007; Vandenbroucke
and Bchar, 1988).
Moreover, 20(S)/(20S + 20R) and /( + ) sterane ratios
increase with increasing maturity of organic matter (Hunt, 1996;
Goodarzi et al., 1989; Seifert and Moldowan, 1980). As shown in
Table 5, 20(S)/(20S + 20R) and /( + ) ratios are in the range
0.20.34, and 0.150.32, respectively, indicating the early maturation
stage of organic matter (Grantham, 1986; Goodarzi et al., 1989).
5. Conclusions
(1) Two types of facies sequences are developed in section No.2.
from Dahuangshan area. The middleupper part of the section
consists of dark-black oil shale interbedded by thin-bedded argillaceous dolomite, silty claystone, tuff, limestone, and dolomitic
marl, containing a spot of plant stem fossils, and an abundance
Fig. 7. Mass chromatograms (m/z = 85) for the saturated alkanes of selected samples from the Dahuangshan oil shale.
49
Fig. 8. m/z 191 and m/z 217 ion fragmentograms of the saturated fractions showing the distribution of the terpanes and steranes for selected oil shale samples.
50
Table 5
Organic geochemical data for extracts of samples from the Dahuangshan oil shale.
Sample no.
CPI
Pr/Pha
Pr/nC17
Ph/nC18
Gammacerane indexb
Homohop indexc
20(S)/(20S + 20R)d
/( + )
O-04
O-11
O-13
O-20
O-21
O-28
O-29
O-32
O-35
O-39
1.12
0.98
1.24
1.08
0.93
1.01
1.05
0.99
1.16
1.01
0.41
0.59
0.82
0.60
0.91
0.56
0.57
0.61
0.42
0.52
0.97
0.59
0.45
0.31
0.91
0.56
0.37
0.72
1.04
0.82
1.24
1.02
0.98
0.47
0.56
1.02
0.45
0.67
1.45
0.85
0.09
0.23
0.26
0.18
0.36
0.11
0.13
0.08
0.12
0.15
0.112
0.066
0.061
0.077
0.084
0.106
0.109
0.990
n.d.
0.145
0.21
0.23
0.28
0.24
0.34
0.31
0.21
0.29
0.20
0.22
0.19
0.24
0.32
0.18
0.28
0.20
0.15
0.26
0.17
0.18
%C27f
%C28g
%C29h
24
55
37
50
48
44
53
47
46
52
29
14
27
24
16
25
13
22
22
20
47
31
36
26
36
31
34
31
32
28
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