Na Zhang, Manchao He, Bo Zhang, Fengchao Qiao, Hailong Sheng, Qinhong Hu. Pore Structure Characteristics and Permeability of Deep Sedimentary Rocks Determined by Mercury Intrusion Porosimetry. Journal of Earth Science, 2016, 27(4): 670-676. doi: 10.1007/s12583-016-0662-z
Citation:
Na Zhang, Manchao He, Bo Zhang, Fengchao Qiao, Hailong Sheng, Qinhong Hu. Pore Structure Characteristics and Permeability of Deep Sedimentary Rocks Determined by Mercury Intrusion Porosimetry. Journal of Earth Science, 2016, 27(4): 670-676. doi: 10.1007/s12583-016-0662-z
Na Zhang, Manchao He, Bo Zhang, Fengchao Qiao, Hailong Sheng, Qinhong Hu. Pore Structure Characteristics and Permeability of Deep Sedimentary Rocks Determined by Mercury Intrusion Porosimetry. Journal of Earth Science, 2016, 27(4): 670-676. doi: 10.1007/s12583-016-0662-z
Citation:
Na Zhang, Manchao He, Bo Zhang, Fengchao Qiao, Hailong Sheng, Qinhong Hu. Pore Structure Characteristics and Permeability of Deep Sedimentary Rocks Determined by Mercury Intrusion Porosimetry. Journal of Earth Science, 2016, 27(4): 670-676. doi: 10.1007/s12583-016-0662-z
Pore structure characteristics of rock are a great concern for researchers and practitioners in rock mechanics and rock engineering fields. In this study, mercury intrusion porosimetry (MIP) was used to measure pore size distribution, as well as several important index parameters of pore structure, for seven common types of deep sedimentary rocks with a total of fifty rock samples. Results show a similar pore size distribution pattern of the rock samples in the same lithological group, but remarkable differences among different lithological groups. Among seven investigated rock types, mudstone has the smallest porosity of 3.37%, while conglomerate has the largest value of 18.8%. It is also found that the porosity of rock types with finer grain size is lower than those with coarser grain size. Meanwhile, a comparison of frequency distribution at ten intervals of pore-throat diameter among seven types of sedimentary rocks reveals that different rock types have different dominant pore-size ranges. Furthermore, permeability of the investigated sedimentary rock samples was derived based on MIP data using reported theoretical equations. Among seven rock types, mudstone has the lowest averaged permeability (3.64×10-6 mD) while conglomerate has the highest one (8.59×10-4 mD). From mudstone to conglomerate, rock permeability increases with an increase of grain size, with only an exception of siltstone which has a relatively larger porosity value. Finally, regression analysis show that there is a good fitting (R2=0.95) between permeability and porosity which could be easily used to derive reliable permeability values of similar kinds of engineering rocks.
Sedimentary rock is the most dominant rock type distributed on the Earth surface and also a typical kind of natural porous media. About 80% of the world total reserves of mineral resources are stored in sedimentary rocks. Thus, pore structure of sedimentary rock plays an important role in many fields of rock mechanics and geotechnical engineering. In addition, lots of critical engineering geological problems or hazards are closely associated with pore structure characteristics (i.e., pore size distribution and porosity) and pore structure related properties (e.g., permeability, strength and durability) of rock.
Pore structure characteristics are of great importance to rock engineering projects, mainly because it can affect the engineering properties of rock in many ways. On one hand, it can have an important effect on the physical-mechanical properties (Di Benedetto et al., 2015) and failure modes of various rocks (Hudyma et al., 2004). For example, Al-Harthi et al. (1999) studied the effect of pores on the engineering properties of Saudi Arabia basalt by using an image analysis technique to estimate the porosity of basalt core samples, and they found that there are good correlations between porosity and mechanical parameters such as compressive strength, modulus of elasticity and Poisson*s ratio. Hudyma et al. (2004) assessed the effect of macroporosity on both the uniaxial compressive strength and failure modes of the lithophysae-rich tuff and plaster analog models, and it was discovered that the compressive strength decreases with an increasing porosity due to lithophysae in tuff and cavities in plaster analog specimens. Meanwhile, it was also noticed that the failure modes transited from spalling through web failure as the percentage of macroporosity within the specimen increased. Sabatakakis et al. (2008) investigated the intrinsic influence of microstructure on the measured strength parameters of intact chemical and clastic sedimentary rocks through a large number of laboratory tests and established the regression equation between total porosity and strength. Török and Vársárrhelyi (2010) suggested that, compared with other petrophysical constituents, porosity had the dominant influence on strength and durability of travertine. Moreover, it is also well known that the mechanical properties of rock vary with water content (Yilmaz, 2010; Erguler and Ulusay, 2009), and the water absorption of rock is greatly affected by pore structure (Zhang et al., 2014, 2012).
On the other hand, pore structure also has a close relationship with permeability and diffusivity of rock and it can directly affect the fluid flow in rock formations. For instance, Rezaee et al. (2006) published a set of relationships between permeability, porosity and pore-throat size for 144 carbonate samples, and these relationships can be used to estimate permeability from porosity and pore-throat radii. Siitari-Kauppi et al. (1997) studied the matrix diffusion of non-sorbing tracers in tonalite from Central Finland and discussed the effect of microscale pore structure on matrix diffusion. Also, Clavaud et al. (2008) analyzed the effect of pore space geometry on permeability anisotropy of three different rocks, and their results showed that for sandstones it is well correlated with the presence of bedding, while for volcanic rocks it is related to the orientation of vesicles or cracks.
Furthermore, pore structure plays an important role in evaluating rock reservoir storage and productivity in oil and gas exploration. Thus, so far extensively specialized research works regarding pore networks and permeability characterization of reservoir rocks have been carried out in the field of oil and gas engineering (Dong et al., 2015; Swanson et al., 2015; Loucks et al., 2012; Ross and Bustin, 2009). Overall, in-depth understanding and quantitative description of the pore structure characteristics have a considerable significance in a wide range of rock engineering fields, including civil, mining, petroleum, geothermal and water conservancy.
However, systematic investigations on engineering sedimentary rocks, especially deep engineering sedimentary rocks, are currently still inadequate. In the present study, pore structure characteristics, such as pore size distribution and porosity, were measured using mercury intrusion porosimetry (MIP) for seven types of deep sedimentary rocks including mudstone, sandy mudstone, siltstone, fine sandstone, medium sandstone, coarse sandstone and conglomerate, with 50 rock samples in total. Permeability of these rocks was also calculated based on MIP data using empirical equations proposed in the literature. Finally, a correlative relationship between rock permeability and porosity was statistically obtained.
1.
MATERIALS AND METHODS
1.1
Collection and Preparation of Rock Samples
The sedimentary rock samples investigated in this study were all collected in the depth interval of 1 050-1 500 m from a deep underground coal mine located in Northeast China. During collection, samples were wrapped with ziplock bags and then sealed immediately with wax after being transported to the ground to maintain their original state. In laboratory, in order to remove moisture in pore spaces, numbered samples were dried in a vacuum drying oven for 2 days at 60 ℃ until their weights had a little change. Before MIP analysis, all dried rock samples were kept in desiccators. Table 1 lists the basic information of seven types of deep sedimentary rock samples.
Table
1.
Sample information of the sedimentary rocks investigated in this study
Sample No.
Lithology
Number of samples
Depth (m)
Geological description
M1-M15
Mudstone
15
1 159.56-1 416.55
Gray, dense, obvious bedding, occasional grey or brown filling
As a widely accepted and well established technique for characterizing pore structure of porous media, MIP has many special features compared with other pore structure characterization methods (Gao and Hu, 2013; Giesche, 2006). Firstly, it can investigate a wide range of pore-throat sizes (normally between 3 nm and ~500 μm). Secondly, it is a relatively time-saving technique. Thirdly, it can provide a comprehensive set of pore characteristics information. In summary, MIP approach not only can directly measure pore-throat size distribution (PSD) and porosity, but also can indirectly evaluate other pore characteristics, such as total pore surface area and median pore diameter. Therefore, in this study the pore structure characteristics of rock samples including PSD, porosity, total pore surface area, median pore diameter, bulk density and apparent density were all obtained by MIP using an AutoPore Ⅳ 9510 porosimeter (Micromeritics Instrument Corporation, Norcross, GA).
The definitions of indirect parameters are briefly introduced as follows. Total pore surface area is the sum of all calculated pore surface areas. Median pore diameter by area is the diameter corresponding to 50% total area on the cumulative pore area versus diameter plot. Bulk density is defined as the mass of the dry bulk sample divided by the bulk volume that includes not only the volume of the solid particles but also the space between the particles. Whereas, apparent density (also called skeletal density) is defined as the mass of the dry bulk sample divided by its apparent volume that is the total sample volume, excluding space between the particles and open pores, but including closed pores.
During MIP tests, both low pressure and high pressure analyses were performed. The highest pressure applied to all the rock samples was approximately 60 000 psia. And the lowest pressure applied to all the rock samples except mudstone was about 0.16 psia. However, for mudstone and sandy mudstone samples it was about 5 psia due to their higher tightness compared to other types of rock samples. Correspondingly, the smallest and largest pore-throat diameters determined for mudstone and sandy mudstone rock samples were about 3 nm and 36 μm, while for the other types of rock samples they were about 3 nm and 1 100 μm. Each rock sample (~5 g; solid) was evacuated to 50 μm Hg for 5 min and the equilibration time was set to be 10 s.
1.3
Permeability Estimation Method Based on MIP Data
Due to the difficulties and high costs related to direct measurement of rock permeability, especially for tight rocks with extremely low permeability, estimation of permeability using measured MIP data is now regarded as an efficient and reliable alternative method (Gao and Hu, 2013). The following equation introduced by Katz and Thompson(1987, 1986) was employed to calculate the permeability
k=1/89(Lmax)2(Lmax/Lc)ϕS(Lmax)
(1)
where k (darcy, D) is the air permeability; Lmax (μm) is the pore-throat diameter at which hydraulic conductance is maximum; Lc (μm) is the characteristic length which is the pore-throat diameter corresponding to the threshold pressure Pt (psia); ϕ is porosity; S(Lmax) represents the fraction of connected pore space at pore width of Lmax which is calculated as (VLmax)/(Vtot). The threshold pressure Pt is determined at the inflection point of the cumulative intrusion curve and the selection of Lmax is dependent on Pt. The step-by-step data processing procedures to determine each parameter in Eq. (1) can be found in the work of Gao and Hu (2013).
2.
RESULTS AND DISCUSSION
2.1
PSD Curves
The PSD curves of these seven types of sedimentary rocks (Fig. 1) are classified into three broader groups (mudstone, sandstone, and conglomerate) according to their lithology. It can be seen from Fig. 1 that all of the three groups have a kind of S-shaped distribution patterns. The PSD patterns of the rock samples in the same lithological group are relatively similar even if slight differences can be found among them. However, the patterns are quite different among distinct groups. Specifically, the front and middle segment of the PSD curve for mudstone is relatively flat and wide with a sharp rise around the pore diameter of 0.05 μm. Unlike mudstone, the PSD curves of sandstone and conglomerate generally have two inflection points which divide the curves into three segments. According to Hartmann and Beaumont (2000), pore sizes are classified as nanopores (< 0.1 μm), micropores (0.1-0.5 μm), mesopores (0.5-2.5 μm), macropores (2.5-10 μm) and megapores (> 10 μm). Therefore, it is suggested that there are predominantly higher percentage of nanopores (pore diameter < 0.05 μm) for mudstone while sandstone and conglomerate apparently have a relatively more proportional of larger-sized pores. Meanwhile, from Fig. 1 it can also be clearly observed that the total pore volumes of the rock samples in different lithological groups are quite different. Moreover, each group has a distinct distribution range of total pore volume. Overall, the ascending order of the average total pore volume for each lithological group is mudstone < < sandstone < conglomerate.
Figure
1.
Pore size distribution of seven types of sedimentary rocks.
The cause of this discrepancy among different lithological groups may be closely linked to their geological origins. Other reasons for different lithological groups having distinct pore size distribution may include the grain size distribution and the shape of the grains of the original particles forming the sedimentary rock, and whether a secondary pore system could have developed for the siltstone.
2.2
Pore Distribution Frequency
In order to analyze the dominant pore-size ranges of different rock types, pore distribution frequencies at ten different intervals of pore-throat diameter were calculated as pore volume percentages and listed in Table 2. The values in Table 2 show that the pore distribution frequencies are quite different for each lithological group. Meanwhile, a comparison of the frequencies among different types of sedimentary rocks reveals that different rock types have different dominant pore-size ranges. Specifically, for mudstone and sandy mudstone, about 80%-95% of the pores are smaller than 10 μm among which about 60%-80% of the pores are smaller than 0.05 μm. For siltstone approximately 66% of the pores distribute in the range of 0.01-0.05 μm. And for the other three types of sandstone and conglomerate, about 30%-40% of the pore-throats are concentrated in the range of 0.01-0.05 μm and about 30%-40% of the pores are larger than 10 μm.
Table
2.
Pore distribution frequency (averages±standard deviation, %) at ten different intervals of pore-throat diameter
Pore-throat diameter (μm)
Mudstone
Sandy mudstone
Siltstone
Fine sandstone
Medium sandstone
Coarse sandstone
Conglomerate
500-1 100
N/Aa
N/A
11.1±5.1
12.6±7.1
16.7±3.3
19.0±10.3
10.7±5.9
100-500
N/A
N/A
12.4±7.2
12.2±6.0
15.9±4.6
14.6±6.4
14.9±5.2
36-100
N/A
N/A
1.2±0.6
1.9±0.6
2.0±0.4
2.0±0.2
1.9±0.5
10-36
19.5±5.7
5.8±2.1
1.0±0.4
1.4±0.5
1.5±0.3
1.7±0.4
2.1±0.6
1-10
8.6±6.4
5.2±4.9
0.5±0.3
1.0±0.3
3.6±5.4
2.0±0.9
5.9±2.9
0.1-1
8.3±12.3
5.6±4.2
1.2±0.7
6.3±2.4
4.9±2.9
7.2±4.3
15.5±5.4
0.05-0.1
3.5±4.6
2.7±2.0
2.6±2.4
3.4±1.3
3.3±1.5
5.0±1.1
12.7±4.6
0.01-0.05
16.1±11.5
43.6±14.1
66.2±9.3
40.2±10.8
31.1±12.1
37.1±8.0
39.8±8.2
0.005-0.01
22.2±11.6
32.9±13.4
8.0±3.6
18.0±2.4
17.2±4.7
9.8±3.6
3.5±1.5
0.003-0.005
21.8±15.1
4.2±5.0
1.3±1.5
2.9±1.7
3.7±1.2
1.5±1.0
0.3±0.3
a N/A. Pore size ranges are not applicable to mudstone and sandy mudstoneone and sandmudstone due to different minimum intrusion pressures chosen for their MIP measurements according to their high tightness.
In summary, for fine grained rock types such as mudstone, sandy mudstone and siltstone, their pore spaces are mainly occupied by nanopores with pore-throats < 0.05 μm while for coarse grained rock types such as conglomerate and sandstone, there are relatively high percentage of pore spaces occupied by large-sized megapores with pore-throats > 10 μm. Finally, what needs to be pointed out is that the different patterns of PSD for different lithological groups presented in Subsection 2.1 can be well explained by the distinct pore distribution frequencies summarized above.
2.3
Porosity and Other Pore-Structure Parameters
The porosity and a few other relative pore structure parameters of the seven types of sedimentary rocks determined by MIP are listed in Table 3. Among different rock types, mudstone has the lowest averaged porosity value of 3.37%, whereas conglomerate has the largest one of 18.79%. Moreover, if we consider these seven lithological types as three major groups, then the porosities for mudstone, sandstone, and conglomerate groups are 3.96%±2.16%, 14.03%±4.09%, and 18.79%±3.63%, respectively, from which we can more clearly see the remarkable differences among different lithological groups. The porosities of different types of sedimentary rocks are further compared in Fig. 2. It can be easily found that from mudstone to conglomerate with an increase in grain size the corresponding porosity also increases notably.
Table
3.
Basic rock and pore structure parameters determined by mercury intrusion porosimetry (MIP)
2.4
Permeability of Different Types of Sedimentary Rocks
Table 4 presents the statistical data of the estimated permeability for seven types of sedimentary rocks investigated in this study. According to the permeability average values listed in Table 4, mudstone has the lowest permeability (3.64℅10-6 mD) while conglomerate has the highest one (8.59℅10-4 mD). A comparison of permeability values (Fig. 3) shows a remarkable difference among seven different rock types. Moreover, it is suggested that from mudstone to conglomerate, rock permeability increases with an increase of grain size, while there is only an exception of siltstone which has a relatively larger porosity (15.2%±4.34%).
Table
4.
Statistics of the estimated permeability for seven different types of sedimentary rocks investigated in this study
The relationship between permeability and porosity of the investigated sedimentary rocks is shown in Fig. 4. As indicated in the figure, with an increase of porosity, permeability increases exponentially. The regression analysis shows that there is a good fitting between them (R2=0.95) with following relationship
k=2×10−6e0.3241ϕ
(2)
Figure
4.
Relationship between permeability and porosity of the deep sedimentary rocks.
where k (mD) represents permeability and ϕ (%) is porosity. The observed empirical relationship between permeability and porosity in this study could be easily used to derive permeability of similar engineering rocks, only based on relatively easy-to-obtain porosity data. It will be a useful and practical reference for engineers working in the related engineering (rock, mining, oil/gas and geothermal) fields.
3.
CONCLUSIONS
As the most common rock type on the Earth surface, sedimentary rocks have attracted continuous attention of the academics and engineers in different engineering fields. This study investigated the pore size distribution and important pore structure parameters of seven common types of deep sedimentary rocks by means of MIP. Moreover, air permeability of these rock types was calculated based on MIP data according to an approach of Katz and Thompson.
The sedimentary rock samples were grouped into three main broader groups of mudstone, sandstone and conglomerate and their overall porosity, pore size distribution and permeability were compared. It was found that overall porosity and permeability increase with grain size from mudstone to conglomerate and different S-shaped pore size distributions for the three main groups. Meanwhile, different dominant pore-size ranges were found for different lithological groups. Furthermore, the relation between porosity and permeability follows an exponential function with a high coefficient of determination.
Results of the present study can contribute to the enrichment of the basic geological database of the sedimentary reservoir rocks and thus will provide vital references for the scientific community.
ACKNOWLEDGMENTS:
This study was supported by the National Natural Science Foundation of China (Nos. 41502264, 51134005), the Specialized Research Fund for the Doctoral Program of Higher Education of China (No. 20130023120016), and the Fundamental Research Funds for the Central Universities of China (No. 2010QL07). The final publication is available at Springer via http://dx.doi.org/10.1007/s12583-016-0662-z.
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Table
2.
Pore distribution frequency (averages±standard deviation, %) at ten different intervals of pore-throat diameter
Pore-throat diameter (μm)
Mudstone
Sandy mudstone
Siltstone
Fine sandstone
Medium sandstone
Coarse sandstone
Conglomerate
500-1 100
N/Aa
N/A
11.1±5.1
12.6±7.1
16.7±3.3
19.0±10.3
10.7±5.9
100-500
N/A
N/A
12.4±7.2
12.2±6.0
15.9±4.6
14.6±6.4
14.9±5.2
36-100
N/A
N/A
1.2±0.6
1.9±0.6
2.0±0.4
2.0±0.2
1.9±0.5
10-36
19.5±5.7
5.8±2.1
1.0±0.4
1.4±0.5
1.5±0.3
1.7±0.4
2.1±0.6
1-10
8.6±6.4
5.2±4.9
0.5±0.3
1.0±0.3
3.6±5.4
2.0±0.9
5.9±2.9
0.1-1
8.3±12.3
5.6±4.2
1.2±0.7
6.3±2.4
4.9±2.9
7.2±4.3
15.5±5.4
0.05-0.1
3.5±4.6
2.7±2.0
2.6±2.4
3.4±1.3
3.3±1.5
5.0±1.1
12.7±4.6
0.01-0.05
16.1±11.5
43.6±14.1
66.2±9.3
40.2±10.8
31.1±12.1
37.1±8.0
39.8±8.2
0.005-0.01
22.2±11.6
32.9±13.4
8.0±3.6
18.0±2.4
17.2±4.7
9.8±3.6
3.5±1.5
0.003-0.005
21.8±15.1
4.2±5.0
1.3±1.5
2.9±1.7
3.7±1.2
1.5±1.0
0.3±0.3
a N/A. Pore size ranges are not applicable to mudstone and sandy mudstoneone and sandmudstone due to different minimum intrusion pressures chosen for their MIP measurements according to their high tightness.
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