Transformation of the Pore Space during the Simulation of the … · 2016. 1. 21. · MOSCOW UNIVERSITY GEOLOGY BULLETIN Vol. 70 No. 5 2015 TRANSFORMATION OF THE PORE SPACE DURING

ISSN 0145�8752, Moscow University Geology Bulletin, 2015, Vol. 70, No. 5, pp. 446–453. © Allerton Press, Inc., 2015.Original Russian Text © D.R. Gilyazetdinova, D.V. Korost, 2015, published in Vestnik Moskovskogo Universiteta. Geologiya, 2015, No. 5, pp. 78–85.

446

Processes that are related to the primary migrationof hydrocarbons (HC) from the parent rocks, espe�cially those that promote the beginning of the move�ment, have been insufficiently studied. The study ofthese processes is possible when conditions similar totabular ones are created. Therefore, most studies thatdeal with the primary migration processes are purelyexperimental.

Due to the increased interest in the study of thestructure, composition, and oil and gas potential ofunconventional hydrocarbon sources, studies on thetransformation of the pore space of rocks during thegeneration of hydrocarbon fluids are again of interest.

Conventional HC resources are decreasing. In thisregard, there is a need to develop new unconventionalHC sources. One example of these sources is thedomanik oil material strata, which contains a hugehydrocarbon mass. Study of the conditions and pro�cesses of HC generation, the formation and transfor�mation of the pore space in these rocks is necessary tounderstand the mechanisms of oil formation anddetermine the optimal and cost�effective ways for theirindustrial exploitation.

The generation and primary migration of hydro�carbons in nature are controlled by a variety of param�eters, viz., the temperature, pressure, and organic

matter type and content. The influences of most ofthese parameters have been studied and demonstratedin experimental works [Beletskaya, 1990, 2007; Tisot,1967; Rudkiewicz et al., 1994; Lafargue et al., 1993;Kobchenko et al., 2011]. However, there are a fewstudies that deal with the influence of the textural fea�tures of rocks, as well as the quantitative content ofHCs on the transformation of the pore space. There�fore, we selected these parameters to study the pro�cesses of the primary migration.

MATERIALS AND METHODS

Rocks with a high bitumen content that are knownas domanikites or domanikoids, which contain dis�persed organic matter (OM) of the sapropelic type(Corg = 5–20%), are among the potential HC sourcesin the territory of the Volga�Ural oil and gas province.

Domanikites include clay, clay�carbonate, sili�ceous�clay�carbonate, and siliceous rocks. In the eastof the Eastern European platform, domanikites aredeveloped in the Perm and Samara regions, Tatarstan,and Bashkortostan.

Domanikites occur in the volume from the horizonof the Srednefranskii substage of the Upper Devonianto the Kizel horizon of the Tournaisian substage of the

Transformation of the Pore Space during the Simulation of the Generation of Hydrocarbon Fluids in the Domanik Horizon

of the South�Tatar Crest as an ExampleD. R. Gilyazetdinova and D. V. Korost

Department of Geology, Moscow State University, Moscow, 119991 Russiae�mail: [email protected], [email protected]

Received March 23, 2015

Abstract—The main purpose of this paper is to study the factors that control changes in rock structure duringcatagenetic transformation of organic matter. Hydrocarbon generation and primary migration can be con�trolled by numerous parameters; the most important are temperature, pressure, hydrocarbon composition,and organic matter type and content. The influences of most of these parameters have been studied andexperimentally demonstrated. However, there are a few works that are dedicated to the investigation of thetexture features of rocks, as well as the quantitative content of the organic matter on the pore space transfor�mation of rocks. Therefore, these parameters are the most important when studying the primary migrationprocesses. It was found experimentally that the rock pore space after each stage of heating is transformed,forming new pore spaces and channels that connect the primary pores. A sample with a relatively low contentof organic matter has been found to undergo fewer changes in pore�space morphology in comparison to rockthat is saturated in organic content. It has been found that that the change of pore�space morphology dependson the original structure of the rocks. Most of the structural changes were observed during rock heating within260–430°C; the most intense formation of hydrocarbons was revealed within this interval.

Keywords: primary migration, pyrolysis, CT scanning, organic matter, Domanik depositions

DOI: 10.3103/S0145875215050051

MOSCOW UNIVERSITY GEOLOGY BULLETIN Vol. 70 No. 5 2015

TRANSFORMATION OF THE PORE SPACE DURING THE SIMULATION 447

Lower Carboniferous and form a bituminous clay–sil�iceous–carbonate formation [Ananiev et al., 2007].

Domanikoid deposits were formed in basins anddeflections that were undercompensated by precipita�tion and originated at stages of the geological develop�ment of the basin when the rate of tectonic subsidenceexceeded the rate of sedimentation. This situationoccurred in the east of the Russian plate in semilux(domanik) time to form a vast unloaded paleodepres�sion that occupied almost the entire territory of themodern Volzhsko�Kamskaya anteclise. In the LowerDevonian�Tournaisian, the sizes of the depressionswere gradually reduced to relatively narrow troughs ofthe Kamsko�Kinelskaya system. The domanik basinwas an epicontinental marine reservoir with a depth of100–300 m with normal salinity. The high HC contentwas related to the enrichment of the water of thedepression in zooplankton.

The primary enrichment of zooplankton by lipidspromoted high HC accumulation. Free silica was sup�plied from the east, from the Ural geosyncline, whereactive volcanism and hydrothermal activity occurredin the Devonian. The pelitic material was suppliedfrom the land that was located to the northwest [Zay�delson et al., 1990].

Deposits of domanik and mendym horizons in theUpper Devonian take a special place in the section ofthe domanik formation, which is the base of the maingeneration potential in the section of domanikites.

The Procedures of Laboratory Studies

The structure and composition of selected samplesof the domanik horizon rocks was investigated usingvarious methods.

In order to determine the quantitative compositionof the rocks, X�ray diffraction was performed on anUltima�IV device (Rigaku, Japan). The operatingmode was: 40 kW, 40 mA, copper radiation, Ni filter,range of measurements was from 3.6 to 65° 2θ, with astep in the scanning angle equal to 0.02° 2θ, with afixed system of focusing slots. In order to acceleratethe X�ray studies and improve the quality of experi�mental data we used a DTex/Ultra semiconductordetector of the new generation; the scanning speedwas 5°2θ/min.

Diagnosis of the mineral composition was per�formed by comparing the experimental and standardspectra from the PDF�2 database in the PDXL soft�ware package (Rigaku). Quantitative analysis was per�formed by full�profile processing of X�ray pictures ofun�oriented preparations [Pushcharovskii, 2000] inthe RockJock software product [Eberl, 2003].

Lithological study of the rocks was performed on aLeica DM EP optical laboratory microscope and amicroprobe complex based on a Jeol JSM�6480LVraster (scanning) electron microscope with a com�bined system of the X�ray microanalysis. Scanning

electron images were obtained in secondary electrons(surface morphology) [Kalin et al., 2008].

The next phase of the study consisted of tomo�graphic scanning of cylindrical (μKT) samples with adiameter of 3 mm. The study of the samples with thecomputer X�ray microtomography was performedusing a SkyScan�1172 computer microtomograph.The principle of the system is based on obtaining mul�tiple X�ray shadow images of an object from differentangles, which occurs via movement of the object on ahigh�precision table. Based on the shadow images, wereconstructed cross�sectional images of the objectusing the modified algorithm of the Feldkamp conicalradiation, where an image of the internal microstruc�ture and density at the selected height is generated intransmission images. On the X�ray sections of thesample, the dark area corresponds to the lower X�raydensity of the medium while light areas correspond tohigh density [Stock, 2009].

The geochemical characteristics of the materialwere obtained on a Rock Eval�6 pyroliser, which is thelatest modification of a RockEval device. The proce�dure of pyrolysis on the RockEval equipment wasdeveloped at the French Petroleum Institute [Espi�talie, 1984].

After extensive study of the composition and struc�ture of each sample, we found that parameters such asthe mineral composition, the type and maturity of theorganic matter, and the HC composition are identicalfor the majority of the species within the selected col�lection (Table 1).

However, it was found that the textural characteris�tics of the rocks and organic content differ. Taking therevealed features of the structure and composition ofthe collection into account, the experiment wasdivided into two parts: (1) study of the effect of theorganic content on the morphology of the rock in thecourse of thermal exposure and (2) the study of theeffects of textures on primary migration processes atthe same HC content. Furthermore, an additionalexperiment was conducted to study the dynamics ofthe changes in the structure of the pore space in theprocess of the generation of hydrocarbon fluids.

RESULTS

In order to solve the above�mentioned tasks, weperformed a series of experiments to study the porespace in the oil parent rock during hydrocarbon gener�ation, which is based on the experimental works ofemployees of the Department of Geology (MoscowState University) that were performed in 2010 [Korostet al., 2012].

The laboratory experiment was intended to simu�late HC generation in an unbroken rock sample byheating it in a nitrogen atmosphere at a set tempera�ture program and to observe changes in the structure ofthe pore space. Simulation of HC generation was per�formed on a RockEval�6 pyroliser.

448


GILYAZETDINOVA, KOROST

It was found that hydrocarbons that exist in therock in a free state or adsorbed HCs are releasedmainly under the influence of a constant temperatureof 300°C (peak S1). The device then registered HCsthat were obtained because of the cracking of kerogenand heavy resinous�asphaltene fraction, the bitumoid(peak S2) (in the temperature range of 300–650°C,heating rate is 25°C/min) (Figs. 1, 2). The totalorganic�carbon content (Corg) is calculated taking thefact into account that carbon forms 83% of the ele�mental composition of the released HCs.

Observation of the corresponding changes in thestructure of the rock was carried out using a computermicrotomograph. The dark phase that occurs in theX�ray sections of the sample is characterized by X�rayabsorption. The X�ray absorption depends on the den�sity of the mineral and non�mineral components ofthe rock; for example, the X�ray absorption will beminimal for OM due to the low density of the kerogencomponent of the rock. Taking the fact into accountthat the pore space in the studied rocks is minimal (isfilled by OM), the entire compound that correspondsto the intermineral phase of the rock, i.e., the porespace, with minimal X�ray absorption is considered as

OM. Using the computer�tomography data, we calcu�lated the organic content in the bulk of the unbrokensamples, as well as the OM and newly formed pores inthe heated samples. The organic content (porosity)was performed based on computer analysis (division ofX�ray contrast phases in brightness). The phase vol�ume was calculated based on the observed brightnessthat corresponds to the pore space of the rock. In orderto evaluate the transformation of the pore space of thesample, we calculated the volume of the associatedpores. This parameter characterizes the associationdegree of pores in the volume, which is achieved bymathematical analysis. The analysis allows us to cal�culate the number and parameters of each object(pores). Based on the analysis, it is possible to estimatethe volume fraction of the largest cluster, which char�acterizes the highest association of pores in space. Inturn, the association parameter allows us to estimatethe degree of transformation, since in the heating pro�cess the pores, lenses, and interlayers of the rock forma single system.

The experiment was conducted in two stages. Thefirst stage consists of heating cylinders with a diameterof 4 mm to a temperature of 500°C. The main task at

Table 1. Selected characteristics of the samples

The number of the sample OM, % Tmax, °C

catagenesis stage Composition Texture

1 4.59 429, protocatagenesis Siliceous–carbonate Layered

2 12.67 431, mesocatagenesis '' ''

3 10.6 430, proto�, mesocatagenesis Clay–siliceous–carbonate ''

4.1 0.7 424, protocatagenesis Carbonate Spotted

4.2 2.41 420, protocatagenesis Clay–carbonate Layered

4.3 3.44 423, protocatagenesis Siliceous–carbonate Spotted

4.4 5.98 423, protocatagenesis Carbonate Massive

5.1 3.92 427, protocatagenesis Siliceous–carbonate Layered

5.2 1.27 420, protocatagenesis Carbonate–clay Massive

5.3 0.57 433, mesocatagenesis Carbonate ''

100 µm

(a) (b)

100 µm

Fig. 1. The data of TEM�studies on sample 3: (a) initial rock; (b) rock heated to 500°C.



this stage is to analyze the influence of the texture andorganic content on the change in the morphology ofthe rock in the simulation of HC generation.

In the second phase, we analyzed the dynamics ofchanges in the structure of rocks during sequentialheating and its connection with HC generation. As aresult of a series of tests that were carried out on rocksof the domanik horizon, the optimal parameters of therock heating was determined, which were identical tothe parameters of the experiment that was carried outpreviously.

The temperature range of each series of experi�ments had to meet the requirements of the HC gener�ation step by the paternal oil source rock: 100–300°Cis the release of free and adsorbed HCs and water;300–400°C is the initial stage of HC formation byhigh�temperature pyrolysis of organic solids, releaseof chemically bounded water; 400–470°C is the tem�perature range that corresponds to the most intensestage of the formation of hydrocarbons; and 470–510°C is the final stage of HC formation. The maxi�mum heating of the sample during the experiment wasdetermined by the temperature of the beginning of the

active thermal decomposition of carbonates, i.e., infact, by that of the irreversible methamorphization ofthe rock.

The Influence of the Organic Matter Content and Texture Features on the Development

of the Studied Processes

The experiment was performed for five samplesthat satisfied the two previously defined criteria:(1) different contents of OM and (2) equal texture ofthe rock. The rocks were heated to 500°C in one stage.The tomographic data allowed us to analyze thechange in the pore space of the rocks due to their heat�ing (Table 2).

After finishing the first stage of the experiment, itwas found that changes in the structure of the porespace in all samples were different. In three of the fivesamples, the formation of new cracks that were ori�ented on the bedding of the rock was observed. Thesecracks may have formed due to the discharge of newlyformed hydrocarbons. The generation of new HCscaused an increase in pore pressure, which resulted inthe formation of cracks. The layered texture of these

(a) (b)

Fig. 2. X�ray binary sections (black, pore space) and changes in the rock structure according to µKT�plotting of sample 3: (a)initial sample; (b) sample heated to 500°C.

Table 2. The calculated values of connectedness and porosity before and after heating of samples

Number of sample

Calculated connectedness before heating

Calculated connectedness after heating

Calculated porosity before heating

Calculated porosity after heating

1 4.25 62 4.8 7.72 18.2 72.6 8.3 15.43 13.3 94 5.5 19.94.2 8.7 94 5.5 19.94.2 8.7 15 4.2 5.75.1 86 94.3 17.7 20.14.3 34 59.1 9.7 13.8

450



rocks also played an important role. Excessive pressureleading to the formation of cracks can be attributed tothe isolation of interlayers that are associated withcracks (Figs. 1, 2).

At the second stage of the study, samples character�ized by different textures (solid and spotted) wereheated to a temperature of 500°C. Data on the contentof OM and results of computer tomography allowed usto compare rocks that were characterized by differenttextures and rocks that have the same OM content.

It was found that the rate of the conversion of thepore space of the rock depends on the conjugation ofpores, which is also controlled by textural attributes.Layered samples were subjected to large variations dueto isolation of the pore space, while rocks with a spot�ted or massive structure with an equal content of OMwere transformed to a lower degree due to the highdegree of connectedness of pores. The high connect�edness of the pore space that is filled with OM providesintensive migration and rapid unloading of hydrocar�bons; therefore, abnormally high pore pressure(AHPP) does not arise, there is no transformations ofthe rock matrix.

The Dynamics of the Change in the Pore Space in the Process of the Generation of HC Fluids

The following laboratory experiment on the simu�lation of HC generation in the unbroken rock samplewas carried out by consecutive heating in a nitrogen

atmosphere for a predetermined temperature pro�gram; changes in the structure of the pore space weremonitored in order to analyze the dynamics of thesechanges and their relationship with HC generation.

The sample was characterized by high OM content(23.81%) and a low value of Tmax = 410°C. The origi�nal rock had numerous small pores (the pore size was0.02 mm) (Table 3).

After heating the sample to 140°C, no significantchanges in the pore space of the rock were observed.X�ray absorption in the interlayers that were saturatedby OM decreased due to the partial release of free HC,which is seen on the pyrogram as a relatively sharppeak that corresponds to the increase in the number ofreleased HCs (Fig. 2).

At the next stage of heating to 260°C, there werepractically no changes in the morphology of the rock,which probably indicates that the main release of thefree and adsorbed HCs and water proceeded up to140°C (Fig. 3).

Significant changes in the structure of the porespace were observed when heating the rock from 260 to430°C. This temperature range corresponds to themost intense stage of the HC formation. The interlay�ers that were saturated by OM were transformed intopronounced lenticular morphoforms with a length ofup to 1.4 mm and a thickness of 0.09 mm, which areoriented parallel to the bedding (Fig. 4–6). This mor�phology of the rock seems to be associated with a grad�

Table 3. The calculated values of connectedness and porosity, as well as the weight loss after each stage of heating of the rock

Heating, °C Calculated connectedness, % Calculated porosity, % Weight loss, mg

0 97.4 20.6 0140 99.2 31.8 2.855260 99.4 34 0.381430 99.6 50.5 5.562

µm

12

3

1000

2000

3000

4000

0 1000 2000 3000 4000

0 µm 1000 2000 3000 4000

1000

2000

3000

4000

Fig. 3. X�ray density sections of the initial sample: 1, carbonate micrite mass saturated by OM; 2, carbonate biogenic interlayers;3, heavy minerals.



ual increase in interpore pressure during the genera�tion of new portions of hydrocarbon fluids.

During the heating of the rock to 500°C, neitherchanges in the morphology and number of lenticularforms nor significant additional release of hydrocarbonsfrom the sample were found according to RockjEval. Nodestruction of the carbonate material was observed atthis temperature (Fig. 5).

Thus, the experimental results demonstrate therelationship between the HC release stages andchanges in the structure of the sample in the consecu�tive (step by step) heating of the rock to a certain tem�perature.

Certainly, one of the most important issues thatarise in conducting these experiments is the thermalexpansion of the matrix. To evaluate the effect of ther�

1 2

3 4

5

Fig. 4. Changes in the structure of the sample according to µKT�plotting: 1, initial sample; 2, sample heated to 140°C; 3, sampleheated to 260°C; 4, sample heated to 500°C.

452



mal transformation of the matrix on the structure ofthe rock, the following studies were performed.

Plotting was conducted on the rock of the domanikhorizon. The sample was characterized by a relativelylow Corg (1.06%), a generation potential equal to3.92 mg HCs/g of the rock. According to values ofpyrolytic parameters (Tmax) = 442°C), the catagenetictransformation degree of the OM corresponded to themiddle of the “oil window.” Despite the fact that thestudied rock is under the MK katagenesis stage, theOM in this rock is extensively converted [Kozlova, oralreport].

The sample was heated to 500°C in one stage. As aresult, no structural changes in the rock were observed;this fact confirms that OM that was contained in thisrock was strongly transformed and was not able to gen�erate new HCs. In addition, this result clearly demon�strates the absence of thermal expansion of the rockmatrix, at least its result in a significant impact on thetransformation of the rock structure. This indicatesthat the volume expansion of the samples is associatedwith the unloading of the newly formed HCs, whichcaused a critical increase in pore pressure.

CONCLUSIONS

As a result of heating, the morphology of the porespace of all of the rocks that are characterized by sim�ilar characteristics underwent a transformation tosome extent. The morphology of all of the transformedrocks was characterized by the formation of new poresand channels connecting the primary pores. In threeof five samples (in addition to the above�mentionedchanges), the formation of cracks was observed. Thesechanges with the same characteristics of the rocksoccurred because of different textural and morpholog�ical features. Samples 4.2 and 5.1, which had relativelylow values of TOC (total organic carbon) (2.41 and3.92%, respectively), were transformed to a lesserextent as compared to samples 1, 2, and 3 with higherTOC values (4.59, 12.67, and 10.46%, respectively).

Thus, we can conclude that the OM content in therock plays an important role in the transformation ofthe pore space of rocks that are submerged to a depthcorresponding to the temperature of hydrocarbongeneration. The results at this stage of research agreewith the previously obtained data [Lafargue et al.,

1 2 3

0.75 mm

0.75 mm

0.75 mm

Fig. 5. 3D models of phase distribution of the rock heated to 500°C: 1, model of distribution of lenticular forms; 2, model of dis�tribution of the rock matrix; 3, model of lenticular forms combined with that of matrix.

(a) (b)0

2000

4000

µm 2000 4000 6000Z = 0.153 mm

0Z = 0.503 mm

2000 4000 6000

2000

4000

60006000

µm

Fig. 6. X�ray density sections of sample with the transformed OM: (a) initial sample; (b) sample heated to 500°C.



1993; Tisot, 1967; Tiwary et al., 2013; Kobchenkoet al., 2011; Zhao et al., 2012].

The textural features, as well as the OM content inthe rock, play a significant role in the transformationof the pore space. The pore space of rocks with a lay�ered structure, as has been noted above, is transformedinto cracks during heating. This fact is probably due tothe high concentration of OM in interlayers; duringtheir heating the new generation of hydrocarbonsleads to the formation of cracks. This type of disrup�tion occurs under the action of excess pore pressure,which cannot occur in a relatively bonded system ofpores. Cracking requires the isolation of interlayersthat are saturated by OM. The same does not hold truefor rocks with a solid texture. Due to the uniform dis�tribution of OM in the rock, cracks are not formed,since the newly formed portions of hydrocarbon fluidsmigrate into the open pore system.

The second part of the experiment was devoted tothe dynamics of the pore space in the process ofsequential heating of rocks. At the stage of heating ofthe sample to 430°C, there was a maximum yield ofnewly formed hydrocarbons, which is registered in apyrogram as a maximum peak among those that corre�spond to temperature ranges. This supports the hypoth�esis that the maximum hydrocarbon generation pro�ceeds up to 430°C. This observation is in good agree�ment with the data that were reported in [Kobchenkoet al., 2011; Tisot, 1967; Ben Chanaa et al., 1994].

The results of the sample heating with convertedOM allow us to exclude the extension of the rockmatrix as a significant factor that influences the struc�ture of the pore space in the process of the influence oftemperature on the rock.

Our experiment best satisfied the conditions of cat�agenetic OM transformation; however, a number ofassumptions were made during the work. Factors suchas intra�bed pressure, tabular fluids and gases that canalso affect generation and primary�migration pro�cesses of hydrocarbon fluids were not consideredbecause of the lack of equipment that is capable ofgenerating absolutely correct properties of the model.

In this work, we studied the factors that control thechanges in the rock structure in the course of catage�netic OM transformations, as well as the parametersthat affect the primary�migration processes and trans�formation of the pore space in the laboratory simula�tion of the generation of hydrocarbon fluids.

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Translated by V. Avdeeva

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Transformation of the Pore Space during the Simulation of the … · 2016. 1. 21. · MOSCOW UNIVERSITY GEOLOGY BULLETIN Vol. 70 No. 5 2015 TRANSFORMATION OF THE PORE SPACE DURING