Hydrocarbon Generation Kinetics of a Heterogeneous Source Rock

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Hydrocarbon generation kinetics of a heterogeneous source rock system: - Example from the Eocene-Oligocene Shahejie Formation, Bohai Bay Basin in eastern China Zhuoheng Chen, Maowen Li, Tingting Cao, Xiaoxiao Ma, ZHiming Li, Qigui Jiang, Zheng Li, and Chunqing Jiang Energy Fuels, Just Accepted Manuscript • DOI: 10.1021/acs.energyfuels.7b02361 • Publication Date (Web): 03 Nov 2017 Downloaded from http://pubs.acs.org on November 3, 2017

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Hydrocarbon generation kinetics of a heterogeneous source rock system:

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- Example from the Lacsutrine Eocene-Oligocene Shahejie Formation,

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Bohai Bay Basin, China

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Zhuoheng Chen1, Maowen Li2, Tingting Cao2, Xiaoxiao Ma3, Zhiming Li2, Qigui Jiang2, Zheng

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Li4 and Chunqing Jiang1 1

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Geological Survey of Canada, 3303-33 Street NW Calgary，Alberta T2L 2A7，Canada;

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China State Key Laboratory of Shale Oil and Shale Gas Resources and Effective Development,

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Sinopec Petroleum Exploration and Production Research Institute，31 Xueyuan Road，Haidian

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District， Beijing 100083，China;

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China University of Petroleum (Beijing), 18 Fuxue Road，Changping District, Beijng 102249，

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China; 4Sinopec Shengli Oilfield Company, 3 Liaocheng Road, Dongying, Shandong 257015,

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China

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Abstract

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Source rock heterogeneity is a common and important feature that requires

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attention in shale oil resource evaluation. The Eocene-Oligocene Shahejie Formation

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in the Jiyang Super-basin, Bohai Bay Basin, has been studied to investigate vertical

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variations in source rock characteristics and their thermal decomposition behaviours

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in a relation to lacustrine shale oil resource potential. Fifty-four core samples from

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Luo 69 Well were analyzed using Rock-Eval 6 equipment and the resulting FID

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(Flame Ionization Detector) hydrocarbon pyrograms were examined to study their

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generation kinetics. Differences in bulk geochemical characteristics, petroleum

ACS Paragon Plus Environment

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generation capacities and petrophysical properties allow for sub-division of the

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samples into three “homogenous” groups: a) a stratigraphically higher facies,

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corresponding to samples with HI value around 600 mg HC/g TOC and high S1/TOC

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(either due to exogenous hydrocarbon input or thermally less stable kerogen, or both;

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b) stratigraphically a facies in the middle of the section, representing thermally more

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stable facies group with similar generation potential, but much lower S1/TOC; and c)

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a stratigraphically lower facies, corresponding to source rock with low TOC (100 mg HC/g TOC) (Fig. 3b). The

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samples with the lowest Tmax values (Group III) occur in the deepest part of the well

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and show the lowest HI values (Figs. 3c, 3b and 4). It appears that samples in Group I

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and II align in a single straight line on a TOC-S2 cross plot (Fig. 3d), indicating

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similar generation potential. Samples in Group III fall along another trend with lower

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generation potential than those in Groups I and II, which are supported by the

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Tmax-HI plot in Fig. 3c The samples with lowest Tmax values in Group III are

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typical Type III kerogen by their low hydrocarbon generation potential (fig. 3c) and

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low HI and relative high OI values (Fig. 3 b).

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Figure 3. Cross-plots of various Rock-Eval parameters showing geochemical characteristics of the

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Es3x samples from Luo 69 Well.

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Figure 4a is a composite diagram displaying geochemical data and petrophysical

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properties derived from well logs against depth to reveal the variation of these

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attributes in vertical direction. Figure 4b links typical petrophysical log responses to

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organic rich rock types, showing the diversity of mineral components and texture in

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the source rock unit in the study. The stratigraphic interval can be divided into five

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sub-lithological-geochemical units: a) organic-rich laminated argillaceous limestone

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(sub-unit A: 2990 – 3020m); b) calcareous mudstone with variable clay mineral

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contents (sub-unit B: 3020 - 3040 m); c) organic-rich laminated argillaceous

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limestone (sub-unit C: 3040 – 3068 m); d) low porosity massive to thin bedded

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limestone (sub-unit D: 3068 – 3123 m); and e) calcareous mudstone/shaly limestone


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(sub-unit E: 3123-3130 m). The geochemical characteristics of samples from sub-unit

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A and C show similarities and differences. Samples in sub-unit A have much higher

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S1/TOC ratios than those in sub-unit C though TOC and S2/TOC are comparable;

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while the carbonate content and Tmax in the upper part are lower. Petrophysical

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differences between the A and C sub-units are observable, slightly higher Gamma Ray

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as indicated by higher clay content, higher density and lower sonic transit time shown

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by lower porosity estimates, and lower resistivity indicated by the separation of

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measured and calculated sonic (the second last column of Fig. 4a) in sub-unit A than

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those of sub-unit C.

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The sub-units D and E contain low organic content with TOC lower than 2%

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with variable remaining generation potentials and relatively high percentage of free

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hydrocarbon content (S1). The lithology is different from the overlying sub-units

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indicated by low estimated porosity and lack of obvious ∆T separation (the second

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last column of Fig. 4a).

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Figure 4a. Depth profiles of Rock-Eval and petrophysical parameters showing different

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geochemical and petrophysical characteristics of the source rock at different depths. The ∆T

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separation is the difference between measured sonic transit time and estimated sonic transit time

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from resistivity log proposed by Passey et al.24. Large separation indicates potential good source

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rock interval. Porosity curves are smoothed to show the general trends.


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Figure 4b Composite profile of petrophysical well logs with Photomicrographs showing

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vertical source rock heterogeneity in the source rock interval of Sha3 Member (Es3) of

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Shahejie Formation in this study. GR (column 1) indicates relative abundance in clay content;

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SP (spontaneous potential) indicates relative permeability; PE (photoelectronic Index, red

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solid in second column) show carbonate content (3-5 from dolomite to calcite); Resistivity:

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oil and gas (organic matter) indicator; Porosity logs (column 4). Photomicrographs showing a)

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organic-rich muddy limestone. Thin clay-rich and carbonate layers interbedded with

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TOC>2%; b) organic-rich laminated argillaceous limestone containing solid bitumen in

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inter-granular pores of calcite grains (3057.6 m); c) thin carbonate layer with organic-rich

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laminae. Organic matter shown as solid bitumen in horizontal fractures (3 059.35 m); d)

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interbedded clay and carbonate thin layers (3104.4m) and TOC is 600 mg HC/g TOC from Group I, which is typical of

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immature Type I/II source rock from a lacustrine setting in China.

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requires higher temperature to convert to hydrocarbons, and the generation


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. While in

Type I kerogen

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temperature is expected to be even higher under a high heating rate at 3°C/millions in

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this study. The 50% conversion at about 175°C is reasonable for the Group I.

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Composite Generation Kinetics

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A single immature sample represents a specific facies and contains little

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information on the diversity of organic matters from different facies. A hydrocarbon

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generation kinetics model based on a single immature sample, therefore, may not be

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able to capture the variation in kinetic properties due to source rock heterogeneity. In

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contrast, multiple samples from either vertically stacked or laterally extended

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stratigraphic sections offer better chance to reveal the diversity in organic matter and

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allow for characterization of their variability spatially. The proposed composite

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kinetics model addresses the issue of source rock heterogeneity by using a synthetic

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pyrogram of aggregated samples from vertically stacked or/and laterally extended

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sections that represent the diversity in organic matters due to facies change and

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variable terrestrial inputs. Because samples in sub-units A and D+E are either in early

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hydrocarbon windows or partly contaminated by exogenous hydrocarbons, they

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cannot be used for construction of a kinetic model without corrections40, 41. As such,

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the immature samples of 22 pyrograms from post-solvent extraction replicates in

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stratigraphic sub-unit C (Group I) have been used to construct a composite kinetics

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model to demonstrate its application to a heterogeneous source rock system.

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Under laboratory constant heating rate (25 °C/min), the calculated hydrocarbon

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generation rates are similar among the 22 samples in sub-unit C (Figs. 13a). The

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transformation ratios show a moderate variation (maximum 25 °C) at onset of


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massive hydrocarbon generation (TR=10%). The difference in temperature becomes

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small (only 5 °C) when TR reaches 90% (Figs. 13b). However, when geological

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heating rate is applied (3 °C/million years), the generation rates behaved differently

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(Fig. 13c), and show two distinct groups (Figs. 13c), one with the peak rates of around

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165 °C and the other about 175 °C. The transformation ratios also show two distinct

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groups, with one displaying onset temperature of massive generation at about 150 °C

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and offset at 175 °C, and the other group with onset at about 160°C and offset at

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180 °C (Figs. 13d). The maximum differences in temperature at the onset and offset

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of generation among the 22 samples are 30 °C (150-180 °C). The offset temperature

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at geological heating rate does not seem to converge as those derived from laboratory

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heating rate (Fig. 12b), and large difference remains (Fig. 13d). In the proposed

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composite model, the overall average behaviour of thermal degradation is expressed

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as the mean production (conversion) rate and mean transformation ratio as shown in

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Figure 13, while the maximum temperature difference in generation is shown by a

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temperature envelope defined by the lower and upper boundaries. The temperature

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difference of onset (and offset) hydrocarbon generation among the samples in Group I

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can be up to 15 °C, indicating a kinetically heterogeneous source rock (Fig. 13d). For

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a geothermal gradient of 30 °C/km, this translates to 500 meters of difference in burial

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depth for onset hydrocarbon generation for the same source rock unit in the extreme

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case.


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Figure 13. Source rock kerogen conversion for the non-contaminated samples in this study; a) and

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b) observed from laboratory pyrolysis at a heating rate of 25 °C/min; and c) and d) inferred for

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geological conditions at a heating rate of 3 °C/million years. Kinetics estimation was made by

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optimization of both frequency factor A and activation energy Ea.

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Discussion

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Implications for Facies Change and Maturity

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In a study of source rock thermal maturity of the Bakken Formation in North

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Dakota, Nordeng42 demonstrated that, a) samples from the same source rock with

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similar thermal maturity in a single well follow a linear relationship between mean E

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and log(A); b) samples at different thermal maturities fall into different trends; and c)


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all the trends are roughly parallel showing a systematic shift from low to high

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maturities (Fig. 14). Thermal maturation results in kinetic parameters shifting to high

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activation energies; while the observed spread of samples from the same well along a

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trend-line may indicate a combined effect from laboratory random errors and the

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source rock heterogeneity due to seasonal changes, terrestrial inputs, water condition

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and others.

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by random laboratory error has been discussed by many authors

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rule-of-thumb for this effect on the kinetic parameter estimation is that an error of 1

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kcal/mol in E is compensated by a factor of 2 error in A and that a random 2 °C

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temperature measurement error may cause a spread of 4 kcal/mol in E

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geochemistry laboratory of Geological Survey of Canada, a finely powdered (< 212

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µm) Cretaceous Second White Speckled shale sample with a 5.1% TOC and 441 oC

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Tmax has been used as a standard rock sample for the purpose of QA/AC of the

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Rock-Eval procedure. The statistics of 11542 standard samples analyzed from 1998 –

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2016 show a mean of 441 °C and a standard deviation of 1.0 °C in Tmax. For a

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normally distributed measurement errors with a standard deviation of 1 °C in Tmax,

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the 99% confidence interval is 4 °C in temperature. This could translate to 8 kcal/mol

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in E, meaning that there is a 99% possibility that the spread of data point along the

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log(A)−E straight-line due to laboratory errors would not be greater than 8 kcal/mol in

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E.

The spread of data points along a log(A)−E compensation line as caused 34, 43, 44

. A simple

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. At the

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In the Luo 69 well, the sampling depth interval spans about 130 metres, and

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thermal maturity should be similar or slightly increase with increasing depth.


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However, Tmax values of the samples do not follow a systematic order (Fig. 3c and 4),

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indicating different generation kinetics rather than exogenous input affecting the

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thermal indicator of the samples as suggested by results from the extracted replicates

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(Figs. 9 and 10). Each sub-unit shows slight difference in lithology and thus small

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change in kinetics are expected. However, samples from the same stratigraphic

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sub-units A and D+E do not align in straight lines in a semi-logarithmic cross-plot of

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Ea and log10(A) (Figs 15a and c). Additional factor, such as maturity overprints due

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to source rock heterogeneity, is apparent.

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Figure 14. Comparison of sample thermal maturity expressed as kerogen decomposition path (a)

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versus kerogen generation kinetics (b). Source of data is Table 1 of Nordeng.42


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Figure 15. Estimated kinetic parameters for samples in different sub-stratigraphic units showing

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variation in kinetic properties as well as maturity overprints, a) samples in sub-unit A; b) in

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sub-unit C; c) in sub-units D+E; and d) comparison of all samples.

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Lamination and Source Rock Heterogeneity

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Lamination is a common feature and unique to shale. Two alternative functional

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characters of self-sourcing and self-retaining make heterogeneity special in shale oil

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reservoir. The two mutual competing (exclusive) capacities rely on alternations of

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vertically stacked sedimentary rocks of different characteristics within a single source

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rock unit. Organic-rich lamina are the primary sources of hydrocarbon generation in a

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shale. In contrast, in a coarse grained segment embedded in the laminar, the rock has

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more storage capacity with reduced generation capacity and serves as ideal storage for

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expelled hydrocarbons from the organic-rich lamina. Oil generated from the lamina


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likely migrate to and are stored in coarser, more porous, but organic-leaner thin beds

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and lenses within the shale. The “contamination” by self-generated in the same shale

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unit affects pyrolysis experiments, resulting in false high S1 peak with a retarded S1b

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hump in default S2 temperature regime on their hydrocarbon pyrogram and

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suppressed Tmax. 13, 445

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On the other hand, the coarse-grained thin layer or lens is deposited in an

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alternative environment or the same environment with more terrestrial input, leading

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to a mixture of indigenous organic matter with more terrestrial organic matter

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Alternation in lithology results in changes in not only organic matter mixing and bulk

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kerogen components, but also porosity and permeability, which can lead to permeable

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zones within source rock unit that are likely connected with more mature source rocks.

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Therefore, an additional cause for high S1 and retarded S1b humps could be

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exogenous oils generated from thermally mature source rock by up-dipping migration.

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Effects of Free Hydrocarbons versus Varying Kinetic Property

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Tmax value has been regarded as thermal indicator in source rock study, particularly

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in marine source rock evaluation. However, caution should be exercised when applied

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to source rock with mixed kerogen types. When comparing thermal maturity of a

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heterogeneous source rock, absolute value of Tmax, Ro% or temperature (depth) may

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not be appropriate and the rate of kerogen conversion to hydrocarbon could be a better

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term to use. This is because thermally less stable source rock may start to generate,

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while thermally stable source rock remains unchanged under the same thermal stress


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.

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level. Thermally less table samples convert more kerogen to hydrocarbons, thus have

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higher thermal maturity level than those of thermally stable samples.

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For example, in Luo 69 well, the samples in Group III from deepest part of the well

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show the lowest Tmax value among the samples from all three groups. Although the

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lowest in Tmax, samples in Group III show the highest PI and S1/TOC values. The

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low generation potential (HI600 mg HC/g TOC) and low OI suggest

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that the samples in Group I contain primarily Type I kerogen. The narrow activation

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energy spectrum indicate unitary kerogen (Figs 11) and more thermally stable source

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rock (Fig. 12). Although Tmax values are the highest, source thermal maturity

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remains lowest in Group I. The kinetic model (Fig. 12) represented by sample # 97 97

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and 85 indicate an immature nature for the samples in Group I, consistent with the

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Rock-Eval data interpretation.

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Conclusions

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Data analyses suggest considerable variations in geochemical and petrophysical

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characteristics in the lower part of the Es3 Member of the Shahejie Formation in Luo

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69 well, which led to a subdivision of the unit into three stratigraphic segments for

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characterization of the heterogeneity. Source rock samples seem to have similar bulk

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geochemical characteristics and petrophysical properties within each segment, but

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differ considerably across segments. Source rock heterogeneity shows in not only

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organic richness, type of organic matter and hydrocarbon generation potential, but

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also in their kinetic properties.

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Characterization of source rock heterogeneity in shale oil reservoir is challenging

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because of the two mutually competing properties of self-sourcing and -retaining.


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Exogenous oil contamination from self-generated oil may blur source rock’s true

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generation capacity and kinetic properties. Identification of the overprints from

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contamination is an important step in characterization of the heterogeneity.

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The composite generation kinetics study shows a temperature variation of about

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25 °C from 10% to 90% transformation ratios in geological time scale for the

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apparently “homogeneous” source rock in sub-unit C (Group I). The kinetic models

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also indicates a more unitary and thermally resistant kerogen composition in samples

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from Group I than those from the other two Groups.

735

Acknowledgements

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The authors acknowledge the financial support of China Major Science 973

737

Project (No. 2014CB239101) and Sinopec Key Laboratory of Petroleum

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Accumulation Mechanisms Open Funds, and Sinopec management for permission to

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publish this work. This represents an output from Geoscience for New Energy Supply

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Program of Natural Resources Canada and is partly supported by PERD funding.

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Hydrocarbon Generation Kinetics of a Heterogeneous Source Rock

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