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Pore Structure Characterization of Ten Typical Rocks in China Zechen Yan State Key Laboratory of Disaster Prevention and Mitigation of Explosion and Impact, PLA University of Science and Technology, Nanjing, Jiangsu 210007, China Canshou Chen College of Defence Engineering, PLA University of Science and Technology, Nanjing, Jiangsu 210007, China Pengxian Fan 1. State Key Laboratory of Disaster Prevention and Mitigation of Explosion and Impact, PLA University of Science and Technology, Nanjing, Jiangsu 210007, China 2. Collage of Field Engineering, PLA University of Science and Technology,Nanjing, Jiangsu 210007, China Corresponding Author: fan-px@139.com* Mingyang Wang State Key Laboratory of Disaster Prevention and Mitigation of Explosion and Impact, PLA University of Science and Technology, Nanjing, Jiangsu 210007, China; wmyrf@163.com Xiang Fang College of Field Engineering, PLA University of Science and Technology,Nanjing, Jiangsu 210007, China; gygzr@sina.com ABSTRACT The characterization of rock pore structure is of great importance for many engineering fields. In this paper, the test methods for pore structure characterization were reviewed and the mercury intrusion method was recommended. Ten rock samples with different lithology were tested by mercury intrusion method. The results of total porosity, average pore diameter and breakthrough radius were given. The pore size distributions of samples were demonstrated by frequency distribution diagrams and analyzed in detail. According to the test results, igneous rock samples have small effective porosity and wide pore-size distribution range. The volume of meso-pore with size between 10 and 1000 nm accounts for a large proportion of the total pore volume of sedimentary rock. Pore size distribution curves of the tested samples are single peak except sample B2 and B5.The test results imply that the pore structure of rocks with different lithology has little similarity. Relative researches on pore structure of rock and their characteristic method are also discussed. KEYWORDS: rock; pore classification; test methods; pore-size distribution. - 479 - Vol. 20 [2015], Bund. 2 480 INTRODUCTION Rock is a natural porous material, and many engineering problems in rock mechanics and engineering geology are closely related to rock pore structure. For example, the evaluation of rock reservoir productivity in oil and gas exploration, some major disasters such as gas and water inrush in coal mining, and the propagation of stress wave caused by earthquake or explosion in rock and soil medium. As a material with hierarchic structure, the microstructure of rock greatly influences engineering properties like permeability, strength and durability. Recent research (1-4) also reveal that, the stress fluctuation and concentration induced by the meso-structure and internal defects play an important role in the deformation and failure process of rocks. Understanding and quantitatively describing the influence of pore structure on rock properties have a great significance in petroleum geology, mining, civil engineering and water conservancy projects. However, the published data of pore structure of engineer rocks is relatively less in spite of its importance, except for petroleum industry. C. De Las Cuevas5 characterized the pore structure of rock salt from the Lower Salt Unit of the Cardona Saline Fm. (Spain) by using three independent methods: mercury injection porosimetry, saturation in a low viscosity isoparaffin and gas adsorption. He found that the effective porosity obtained by saturation in a low viscosity isoparaffin is significantly less than that obtained by mercury injection porosimetry. V. Cnuddeand et al. (6) studied microstructure of concrete and natural building stones by X-ray computed micro-tomography (micro-CT), water absorption under vacuum and mercury intrusion porosimetry (MIP). Their test results showed that not only the total porosities varied greatly, but also porosities measured by different methods in the certain range of pore diameter were also significantly different due to the material properties and pore structure characteristics. Test results indicate that different test methods may have a significant or even decisive influence on test result. In this paper, we first reviewed the test methods for pore structure characterization of rocks. The advantages, disadvantages and the scope of application of different test methods were analyzed. By mercury intrusion method, we tested 10 rock samples with different lithology to study the pore structure of rocks. Test results were analyzed with the statistics of the distribution of the pore with different size. TEST METHODS FOR CHARACTERIZATION OF ROCK PORE STRUCTURE Pore structure refers to the geometry, size, distribution and interconnected relationship of rock pore, etc. Characterization parameters of pore structure mainly include the porosity, pore-size distribution and characteristics of rock pore. In the past decades, several methods are developed to Vol. 20 [2015], Bund. 2 481 characterize the pore structure of rock or other porous materials. Because different test methods may have a significant or even decisive influence on test result, we first review the test methods. Scanning electron microscope (SEM) Scanning electron microscope (SEM) (7) is a type of electron microscope that produces images of a sample by scanning it with a focused beam of electrons. The electrons interact with atoms in the sample, producing various signals that can be detected and that contain information about the sample's surface topography and composition. An SEM image of mineral has characteristics of stereo image, high resolution and great depth of field, which can analyze the three-dimensional shape and connectivity of pore-throat system, pore throat configuration relationship, the type of clay minerals and their chemical speciation in samples. In recent years, the innovative of electron microscope technology has led to the development of focused ion beam polishing technology (FIB), field emission SEM with higher magnification and transmission electron microscopy, providing tool s to observe small pores. SEM method can qualitative characteristics the pore images of materials and unable to obtain the quantitative data of the pore-size distribution. In addition, SEM needs to process rock samples, which to some extent destroys the internal structure and external morphology of the pores in the rock samples, also causes a distortion of observations. At the same time, because the greater the magnification, the smaller the field of view, it is easy to over generalize the observation and miss important information. Nuclear magnetic resonance (NMR) NMR (Nuclear magnetic resonance)8 technology is a physical phenomenon in which nuclei in a magnetic field absorb and re-emit electromagnetic radiation. It is the response signal of fluid hydrogen nuclei in the rock pore that being measured when the water (oil) saturated rock is given a nuclear magnetic resonance imaging (NMRI) scan. Because the rock usually consists of pores of different sizes, the pin echo trains measured in water (oil) saturated rock by NMR are actually a result of the superposition of variety of transverse relaxation components. After the spin-echo sequence is obtained, transversal relaxation time spectrum can be gotten by using mathematical inversion. According to the principle of NMR, signal with longer relaxation time corresponds to the larger pore space. Meanwhile, the signal strength of water (oil) saturated rock is proportional to the amount of fluid that rock contained. The more fluid that rock contained, the stronger the magnetic resonance signal is. At present, NMR is applied more in normal sedimentary rocks such as sandstone, carbonate rock; other types of rock have more magnetic mineral composition which has a great influence on pore fluid signal. In addition, for rock sample with large pores, due to fluid polarization is not Vol. 20 [2015], Bund. 2 482 complete, NMR method also can cause large error. In principle, this method only measures the open pores in the rock. Open pores refer to those which are connected to the outside. As a result, the porosity is also divided into open porosity and close porosity. Because close pore is not connected to the outside, it is difficult to determine the close porosity. Mercury intrusion porosimetry (MIP) MIP9 method is based on the fact that mercury, as a non-wetting liquid, will enter pore spaces when pressure exceeds capillary pressure. The pore size invaded by the mercury is related to the applied pressure by the Washburn equation: P= − 2γ cos θ r (1) where P is applied pressure; γ is the surface tension of the mercury; θ is the contact angle;ris the pore radius. Because γ is 0.480 N/m for mercury, Eq.1 can be simplified to: r= 750 P (2) where the unit of the pressure is MPa, the unit of the pore radius is nm. It can be seen that each capillary pressure corresponds to a pore radius, and the amount of the mercury invaded under a certain pressure represents the volume of the pore with the corresponding radius. Additional information can be obtained from the mercury ejection curves after reduction of the pressure. According to the Young-Duper equation, work done on mercury by applied pressure should be equal to the work that submerging the powder surface need, then the specific surface area can be determined. The average pore radius can be estimated by the pore volume and specific surface area. The minimum pore diameter that MIP method can test depends on its maximum working pressure. The actual rock mass may have pores of different scales, and open pores are mutually communicated through the throat. When pressure increasing, mercury is pushed from large pore to the throat then into the adjacent pore. Adjacent pore size may be larger than the throat size, but the corresponding injected mercury volume is included in the volume of smaller pore, leading to misjudgment. In order to overcome the shortcomings of the conventional MIP, rate controlled MIP method is developed10. The principle of rate controlled MIP is maintaining a quasi static(准静态) mercury intrusion process at a very low injection speed. The main throat radius is determined by the Vol. 20 [2015], Bund. 2 483 pressure of breaking point, the size of the pore is determined by the injected mercury volume, as a result, size and number of throat can be clearly reflected in the mercury intrusion pressure curve. MIP method has many advantages and becomes the most commonly used method for pore structure characterization. The advantages include: 1) Fast determination speed, usually every 1-2 hours for a sample;2) High measuring pressure, so it is suitable for cores with high, medium or low permeability, and complete capillary pressure curve can be obtained for further analysis;3) Even irregularly shaped rock samples can be tested;4) Measuring range for pore diameter is relatively wide. Meanwhile, the MIP method has two disadvantages:1) mercury is toxic, harmful to the human body; 2) only the features of the open pore can be reflected. Gas adsorption method For the pore range that cannot be measured by MIP, in particular the pores of nanometer, gas adsorption method can be used. The procedure is: use nitrogen (N2) or carbon dioxide (CO2) as adsorbate, gradually increase gas pressure at a constant temperature and measure the amount of the gas that sample adsorbed, in turn gradually reduce the partial pressure and measure the corresponding desorption amount. The pore volume is calculated by the amount of adsorbate at the boiling temperature. Under low temperature and pressure(<-196℃,<0.127MPa) N2 isothermal adsorption can reflect pore-size distribution of 2 ~ 50 nm. CO2 isothermal adsorption method is used to calculate the pore-size distribution of 0.35 ~ 2 nm. Gas adsorption method is an effective means for characterization of pore with size less than 50nm, and the application is restricted by the narrow test range. Micro-CT analysis CT scan method is also known as tomographic imaging method11, and the digital geometry processing is used to generate a three-dimensional image of the inside of the rock core from a large series of two-dimensional radiographic images taken around a single axis of rotation. Through integrating the projection data and iterative arithmetic, section profile of the X-ray attenuation coefficient can be obtained, and this is the foundation of the reconstructing the CT images of core section. CT scanning can provide pore structure, filling distribution, the particle surface structure, and physical property parameters of rock core etc. CT analysis is the only semi-quantitative method that capable of non-destructive imaging the open and close pore inside the rock samples. But CT analysis has its obvious disadvantages. Firstly, the cost of Micro-CT analysis is very high, whose price is about 20 times as high as the MIP;Secondly, the detection range of CT analysis method is limited by the poor resolution. Presently, the best resolution of CT instrument can only reach micron grade, and the maximum horizon is about 1000~2000 times larger than the resolution, which implies that only pores within Vol. 20 [2015], Bund. 2 484 2~3 orders of magnitude can be detected. Thirdly, artificial image processing is needed after CT imaging, and artificial threshold will affect the results to some extent because it is difficult to tell the boundaries between porosity and entities. Fourth, high resolution requires small sample, which is easy to cause the secondary cracks in the process of machining and then cause a deviation in test results. Comparison of pore structure characterize methods In order to select a suitable method, we compare the available methods for rock pore structure characterization. The comparison is listed in Table 1. From Table 1, we can see that the MIP method is the only one which can obtain message of pores with size from nm to hundreds of μm. Table 1: The experimental methods and measurements for testing the porosity Method Test range SEM >1nm NMR >4μm MIP 0.003~400μm Gas adsorption Micro-CT Sample Conditions Solid rock after Advantages Disadvantages High resolution No quantitative data Standard cylinder rock Direct observation and Not suitable for samples with sample display large porosity Core block or Core Quick, wide measuring sheet range conducting treatment Good for measuring the 0.35 ~50nm Rock powder >0.5μm Standard rock sample small pore size Mercury is toxic Narrow measuring range Capable of measuring the High cost close pore complex image processing PORE STRUCTURE CHARACTERIZATION BY MIP METHOD Sample preparation In order to obtain first-hand information and gain an intuitive understanding of pore structure of rock with different lithology, we collected 10 typical types of rock samples and conducted MIP tests in key laboratory of coalbed methane resources and accumulation process, ministry of education, China Mining University. Samples are shown in Figure 1. Vol. 20 [2015], Bund. 2 A1 B1 A2 B2 485 A3 B3 A4 B4 Figure 1: Ten tested rock samples Test results summary The main test results are shown in Table 2. A5 B5 Vol. 20 [2015], Bund. 2 486 Table 2: MIP data of ten studied samples No. Lithology Porosity Average pore Breakthrough radius Density (%) diameter(nm) (μm) (g/cm3) Location A1 basalt 1.7908 28.5 34.4 2.2221 Nanjing A2 granite 1 0.8127 260.8 162.9 2.2676 Nanjing A3 granite 2 0.6686 480.1 75.1 2.1509 Nanjing A4 metamorphic rock 1 1.1222 200.1 144.4 2.1157 Nanjing A5 metamorphic rock 2 1.5921 129.7 37.6 2.1355 Nanjing B1 mudstone 3.1820 20.3 41.3 2.1333 Chongqing B2 sandstone 5.9269 63.2 45.9 2.0729 Chongqing B3 siltstone 1 10.1074 123.3 6.46 1.9222 Nanjing B4 siltstone 2 4.4547 37.6 28.3 2.1017 Nanjing B5 red sandstone 8.9043 38.9 8.34 1.9384 Linyi Remark: Breakthrough radius refers to the radius of the largest throat intruded by mercury in first stage The total porosity (open porosity) of samples in group A (igneous or metamorphic rock) are relatively small, ranges from 0.67% to 1.79%, the average pore diameter and the breakthrough radius are relatively large. The average pore diameters within the group differ considerably, the smallest average pore diameter of basalt is only 28.5 nm, but the average pore size of A3 granite is 480.1 nm, a difference of more than ten times. Five types of tested sedimentary rocks show different regularity. First is the relatively large porosities, the maximum of them exceeds 10%. Second is small average pore size, ranging between 20~125nm. At the same time, breakthrough radii of all the samples are above micron level, among which two kinds of sedimentary rocks (B3 silty sandstone and B5 fine red sandstone) are less than 10μm, six kinds of rock are between 10μm and 100μm, one igneous rocks (A2 granite) and one metamorphic rocks (A4) are larger than 100μm. Pore size distribution In order to investigate the pore size distribution, frequency distribution diagrams were made. The main results are shown in figure 2. The figures give the information about the volume percentages of pores with different sizes and the scale range of the dominant pores. Assume that the total mercury quantity is 100, the height of the histogram represents the proportion of the pore volume within certain pore diameter range. Vol. 20 [2015], Bund. 2 487 Figure 2: Pore-size distribution frequency histogram of ten rock samples Rock sample A1 is black basalt, hard and fine texture, with uniform grains and no visible particles or pores. The initial amount of intruded mercury is large, the pores whose diameters are larger than breakthrough radius account for 15% of total pores. After breaking through the first stage throat, the volumes of pores with diameters between 151~36258nm show a uniform distribution. The dominant pores concentrate between 5~50nm, whose volume accounts for about 50% of the total. Rock sample A2 is cyan granite, hard and fine texture, with visible grains. The initial amount of intruded mercury is large too. The volume of the pores with size ranging from 523 to 25926nm changed little. When pore diameter came to about 500nm, the corresponding proportion of pore volume increased and reached its peaking at the range of 90.7~151nm. Pores with size less than 22.7nm were not detected. Rock sample A3 is pink granite, hard and fine texture, with visible grains. Its effective porosity is least among the ten samples. But its breakthrough radius and average pore diameter are relatively large, reaching at 75.1μm and 480.1 nm respectively, ranking third and first of the ten samples. The dominant pore size concentrate in the range of 303~2119 nm, whose volume accounts for more than 40% of the total. Pores with diameter less than 40.4nm were not detected. Rock sample A4 is a kind of metamorphic rock evolved from granite, hard texture and coarse grains. The sample A4 has a small effective porosity. But the breakthrough radius and average pore diameter are relatively large, reaching at 144.4μm and 200.1 nm respectively, ranking second and third of the ten samples. The dominant pore size concentrate in range of 40.4~2119 nm, whose volume accounts for about 56% of the Vol. 20 [2015], Bund. 2 488 total. The pore-size distribution is widespread and without obvious peak. The smallest detected pore diameter is about 10 nm. Rock sample A5 is a kind of metamorphic rock evolved from sandstone, hard texture and with visible small grains. The dominant pore size concentrates in range of 90.7~1164 nm, whose volume accounts for about 60% of the total. Pores with diameter between 303~523 nm represent the largest volume proportion, at 22%. Size distribution curve has a significant peak. The smallest size of detected pores is about 10 nm. The initial amounts of intruded mercury from A1 to A4 are relatively large. This phenomenon is probably caused by the pockmarks-effect. Pockmarks-effect refers to the increase of the initial amount of intruded mercury caused by mercury (non-wetting phase) pasting to the rough surface of the rock pit. With the increasing pressure, the mercury will intrude into the rock pore after the surface pits are filled. This effect causes interference on test results, but due to lack of sufficient statistical data to quantify the interference, it is difficult to be excluded. Rock sample B1 is a kind of brown mudstone, with small skeleton particles, muddy cement and soft texture. The dominant pore size concentrates in range of 9.1~90.7 nm, whose volume accounts for more than 50% of the total. Pores with the diameter of 22.7~40.4 nm represent the largest volume proportion, at 19%. Rock sample B2 is a kind of bluish gray sandstone, with medium skeleton particles and hard texture. The pore size distribution curve has two significant peaks, located at the range of 303~1164nm and 22.7~151nm. Pores with the diameter of 303~523 nm represent the largest volume proportion, at 20%. Rock sample B3 is a kind of yellow porous sandstone, with very fine skeleton particles and soft texture. The dominant pore size concentrates in range of 303~12960 nm, whose volume accounts for about 70% of the total. The pore size distribution curve has a significant peak in the range of 5065~7544nm. Rock sample B4 is a kind of grey siltstone, with very fine skeleton particles and soft texture. The pore size distribution curve has a significant peak, and the pore distribution is concentrated in the range of 22.7~90.7 nm, whose volume accounts for over 70% of the total. Rock sample B5 is a kind of red sandstone, with very fine skeleton particles and hard texture. The pore size distribution curve has a significant peak in the range of 5065 ~ 7544 nm, but the pore size is widely distributed. Subsection statistics of pore One of the most commonly used classification standards for rock micro-pore is by pore size. According to the classification standard proposed by IUPAC12 (International Union of Pure and Applied Chemistry),rock pore is divided into three categories, they are micro-pore whose pore diameter is less than 2nm, meso-pore whose diameter is between 2~50nm and macro-pore whose diameter is larger than 50nm. Ходот presented a Decimal Classification system13 in 1961, he classified the pore with the diameter less than 10nm as micro-pore, 10 nm~100nm as transition pore, 100nm~1000nm as meso-pore, greater than 1000nm as macro-pore. Vol. 20 [2015], Bund. 2 489 Referring to the classification standards in literature, we regard the pore with diameter less than 10nm as micro-pore, 10~1000 nm as meso-pore, greater than 1000nm as macro-pore. We calculate the proportion of pores with different size of ten rock samples (by volume), the results are listed in table 3. Table 3: Pore volume percentage of ten tested rock samples No. Total volume (ml/g) Volume percentage Micro-pore Meso-pore Macro-pore Micro-pore Meso-pore Macro-pore A1 0.0009 0.0042 0.0030 11.00% 52.00% 37.00% A2 0.0005 0.0012 0.0019 13.89% 33.33% 52.78% A3 0.0000 0.0013 0.0018 0.00% 41.94% 58.06% A4 0.0000 0.0028 0.0025 0.00% 52.83% 47.17% A5 0.0001 0.0056 0.0018 1.33% 74.67% 24.00% B1 0.0027 0.0107 0.0015 18.12% 71.81% 10.07% B2 0.0008 0.0235 0.0043 2.80% 82.17% 15.03% B3 0.0011 0.0205 0.0310 2.09% 38.97% 58.94% B4 0.0030 0.0198 0.0010 12.61% 83.19% 4.20% B5 0.0040 0.0200 0.0219 8.71% 43.57% 47.71% According to Table 3, although igneous rocks (A1, A2, A3) have quiet small effective porosities, they have wide pore-size distributions, pores with the diameter larger than 1μm account a large proportion. The pore conditions of sedimentary rock are related to a variety of factors, such as the skeleton diameter, the deposition conditions etc. In most cases, the meso-pore with diameter of 10 nm~1000 nm account for a large proportion in pore volume. But when the deposition is not sufficient, (such as sample B3 whose texture is soft and not being full compacted), or skeleton particles is relatively large (such as sample B5), the macro-pore account for a larger proportion in pore volume. The pore distribution of metamorphic rock is more complex, not only depending on the rock characteristics before modification, but also being affected by metamorphism process pressure, temperature, and recrystallization conditions. DISCUSSIONS Pore structure of other rocks C. De Las Cuevas5 tested the pore structure in rock salt and found that, there was good agreement between the porosity measured by gas adsorption and mercury injection porosimetry. Gas adsorption confirmed that the results obtained at very high pressures using mercury injection porosimetry are valid. Furthermore, the porosity measured on isoparaffin saturated samples reflects the absence of very large macro-pores, which could not be detected with low pressure Vol. 20 [2015], Bund. 2 490 porosimetry. The pore structure in rock salt is very complex, exhibiting a multiple peaks distribution. Macro-pore, micro-pore and infraporosity were represented by pores varying between 60 and 7 μm, pores with sizes between 800 and 300 nm, and pores of around10nm size respectively. Moreover, macro and micro-pores exhibited a fractal pore-surface structure, whereas infrapores had a non-fractal structure. Among the 10 tested samples presented in this paper, sample B2 and sample B5 demonstrate double peaks distribution, and the pore-size distribution frequency histograms of the other eight samples are single peak curves. The comparison implies that the pore structure of rocks with different lithology has little similarity and one should confirm the rationality when using the method of analogy. V. Cnuddeand et al6 studied microstructure of concrete and natural building stones (quartz sandstone and bioclastic limestone). They found that, in most cases, the MIP systematically generates higher total porosity values. The main reasons for these different results can be explained by the different measurable pore-size range. Test range of MIP basically covers all of the pore size inside specimens. The water absorption determines pores larger than 100 nm, while micro-CT visualizes pores larger than 10μm. The specific difference depends on the specific pore size distribution. Surprisingly, the HPC (high performance concrete) breaks the rule. Its porosity measured by water absorption was larger than that measured by MIP. Analysis showed that, not only the total porosity varied greatly, but also the porosity in the overlapping pore-size range are significantly influenced by material properties and pore structure characteristics. For artificial material like HPC, porosity with the pore size ranging from 10 to 60μm measured by MIP is much less than that measured by water absorption. It is speculated that there are many closed pores and pores with size greater than 60μm in casting type manmade material, resulting in MIP failed to measure the complete data. Similar deviations happen to porous rock with many close pores, such as volcanic gas reservoir and volcano bubbles rock14. Discussion on Micro-CT analysis Micro-CT is widely used method for pore structure characterization after mercury intrusion porosimetry. JuYang15 et al. (2008) studied pore scale and space distribution characteristics of red sandstone with porosity between 22.9% and 23.8% using CT scanning method. They reconstructed the three-dimensional porous structural model of sandstone. Since the limit of device resolution, they studied the pore with the diameter no less than 50μm. Li Jiansheng16 et al. (2010) scanned clay rock in coal stratum non-destructively by micro-CT. They came to a conclusion that with the increase of the pore diameter, the porosity of clay rock in coal stratum is reduced by the negative exponent rule. However, the study based on Micro-CT analysis remains some arguable aspects. According to the theoretical basis of CT scan, CT image is the reflection of the attenuation of radiation passed through the sample. It is impossible to distinguish pores and base material directly. When Vol. 20 [2015], Bund. 2 491 processing the obtained image, the selection of gray threshold determines the test results of pore structure directly. Ju Yang et al15. (2008) compared the porosity calculated by CT image that processed by different thresholds with the porosity obtained by helium porosity analyzer, and chose the thresholds which made two porosities equal for binary processing. The process confuses two important concepts. First, the porosity calculated by CT image that processed by different thresholds is the total porosity (including open and close pores), but the porosity obtained by helium porosity analyzer is the effective porosity. The thresholds which make two porosities equal cannot represent the actual pore boundary. Second, the resolution of the CT scan can only identify the porosity of the micron magnitude, and many test data show that the volume of the rock pore with the diameter above micron level only accounts for a small part of the total pore volume. Based on the above understanding, pore data obtain by Micro-CT should be considered with care. Relationship between pore structure and engineering properties The engineering properties of rocks are influenced by the pore structures. Many experiments have been conducted to investigate the intrinsic relationship between the meso structure and macro properties. A. A. Al-Harthiet al17 (1999) investigated the influence of the porosity on the engineering properties of vesicular basalt in Saudi Arabia, and established a statistical quantitative relation. N. Hudyma et al18 (2004) reported that the compressive strength and elastic modulus of lithophysae-rich Topopah Spring tuff specimens decrease as the porosity increase. Yang Yongming et al19 (2010) reconstructed the three-dimensional porous structural models of sandstone and numerically studied the relation between the pore distribution characters parameters and the failure process of Brazil disk. The results indicated that porosity affected the failure states of disk models greatly. Lin Zhihong et al. 20 (2010) experimental studied the influences of physical indices and microstructure parameters on strength properties of red stone from Western Hunan, and their results indicated that the UCS showed a negative exponential relationship with porosity. Ju Yang et al. 21 (2010) established 3D finite element models of rocks with varied porosities and investigated the dynamic behaviour of porous rock samples by numerical experimentation. The results showed that the dominant deformations are the failure of matrix around pores and coalescence of existing micro cracks and the energy dissipation rate increased linearly with the increasing of porosity for a constant impact velocity. The existing investigations provide us a preliminary understanding on the relation of micro structure and macro properties of engineering rock. However, the studies are statistical or numerical, and the mechanism of the influence of pore structure is still behind the scenes. Zhou Xiaoping et al22,23 established a non-Euclidean model for the analysis of failure process of deep Vol. 20 [2015], Bund. 2 492 rock mass, with an emphasis on the density and the length of microcracks. But they did not give the describing method or measureable index of rock. More and more researchers realize the importance to connect the macro properties with the micro structure of rocks. In view of the above mentioned facts, the investigative work on the relation between pore structure and engineering properties should be enhanced. CONCLUSIONS Rock is a kind of natural porous material. The pore structure characteristics of rock are very important in many engineering fields. In this paper, the test methods for pore structure characterization were reviewed and the application scopes of the methods are presented. Ten rock samples with different lithology are tested by mercury intrusion method. The results of total porosity, average pore diameter and breakthrough radius are given, and the pore size distributions of samples are demonstrated by frequency distribution diagrams and detailed analyzed. Test results indicate that the igneous rock samples have small effective porosities and wide pore-size distributions. Compare to igneous rock samples, sedimentary and metamorphic rock samples showed lager discreteness. Pore size distribution curves of the tested samples are single peak except sample B2 and B5. The test results imply that the pore structure of rocks with different lithology has little similarity. Relative researches on pore structure of rock and its characteristic method are also discussed. ACKNOWLEDGEMENT The authors would like to acknowledge the financial support from the National Key Basic Research Program of China (Grant: 2013CB036005), and the National Natural Science Funds of China (Grant: 51304219). The authors also thank the financial support of State Key Laboratory for GeoMechanics and Deep Underground Engineering, China University of Mining & Technology (Grant: SKLGDUEK1305) and China Postdoctoral Science Foundation, which collectively funded this project. REFERENCES 1. A. V. Dyskin (1999) “On the role of stress fluctuations in brittle fracture,” International Journal of Fracture., vol.100, pp.29–53. 2. A. V. Dyskin, Vanvliet M., and Vanmier J. (2001) “Size effect in tensile strength caused by stress fluctuations,” International Journal of Fracture., vol.108, pp.43–61. Vol. 20 [2015], Bund. 2 493 3. Wang Mingyang, Fan Pengxian and Li Wenpei (2010) “The mechanism of splitting and unloading failure of rock,” Chinese Journal of Rock Mechanics and Engineering., vol.29, pp.234–241. 4. Fan Pengxian, Wang Mingyang and Qian Qihu (2010) “Time Effect and Main Influence Factors of Unloading Splitting of Deep–Seated Rock with Non uniformities,” Chinese Journal of Rock Mechanics and Engineering., vol.29, pp.1389– 1396. 5. C. De Las Cuevas (1997) “Pore structure characterization in rock salt,” Engineering Geology., vol. 47, pp.17–30. 6. V. Cnudde, A. Cwirzen, B. Masschaele and P.J.S. Jacobs (2009) “Porosity and microstructure characterization of building stones and concretes,” Engineering Geology., vol.103, pp.76–83. 7. C. O. Wells and C. D. Joy (2006) “The early history and future of the SEM,” Surface and Interface Analysis., vol.38, pp.12–13. 8. R. F. Sigal and E. Odusina (2011) “Laboratory NMR measurements on methane saturated Barnett Shale samples,” Petrophysics., vol.52, pp.32–49. 9. R. Voka, C. Gallé, M. Dubois and P. Lovera (2000) “Mercury intrusion porosimetry and hierarchical structure of cement pastes: theory and experiment,” Cement and Concrete Research., vol.30, pp.521–527. 10. H. H. Yuan and B. F. Swanson (1989) “Resolving pore space characteristics by rate controlled porosimetry,” SPE Formation Evaluation., vol.4, pp.17–24. 11. J. Coenen, E. Tchouparova and X. Jing (2004) “Measurement parameters and resolution aspects of micro X–ray tomography for advanced core analysis,” Proc. Int. Conf. on ‘Society of Core Analysts’, Abu Dhabi, U.A.E, pp.256–261. 12. IUPAC (International Union of Pure and Applied Chemistry) (1994) “Subcommittee on Characterization of Porous Solids Recommendations for the characterization of porous solids (Technical Report),” Pure and Applied Chemistry., vol.66, pp.1739– 1758. 13. Zhao Zhigen and Jiang Xinsheng (2000) “Discussion about the Classification of Pore in Coal,” Reporting Of Standardization., vol.21, pp.23–24. 14. Yang Zhengming, Guo Hekun, Jiang Hanqiao, Liu Li and Zhang Yujuan (2009) “Characteristic parameters of microcosmic pore configuration in volcanic gas reservoir,” Journal of Liaoning Technical University (Natural Science)., vol.28, pp.286–289. Vol. 20 [2015], Bund. 2 494 15. Ju Yang, Yang Yongming and Song Zhenduo (2008) “A statistical model for porous structure of rocks,” Science in China., vol.51, pp.2040–2058. 16. Li Jiansheng, Wang Dong and Kang Tianhe (2010) “Algorithmic study on rock pore structure based on micro-CT experiment,” Chinese Journal of Geotechnical Engineering., vol.32, pp.1703–1708. 17. A. A. Al-Harthi, R. M. Al-Amri and W. M. Shehata (1999) “The porosity and engineering properties of vesicular basalt in Saudi Arabia,” Engineering Geology., vol.54, pp.313–320. 18. N. Hudyma, B. B. Avar and M. Karakouzian (2004) “Compressive strength and failure modes of lithophysae-rich Topopah Spring tuff specimens and analog models containing cavities,” Engineering Geology., vol.73, pp.179–190. 19. Yang Yongming,Ju Yang,Liu Hongbin and Wang Huijie (2009) “Influence of porous structure properties on mechanical performances of rock,” Chinese Journal of Rock Mechanics and Engineering., vol.28, pp.2031–2038. 20. Lin Zhihong, Xiang Wei and Zhang Yunming (2010) “Experimental research on influences of physical indices and microstructure parameters on strength properties of red stone from western hunan,” Chinese Journal of Rock Mechanics and Engineering., vol.29, pp.124–133. 21. Ju Yang, Wang Huijie, Yang Yongming, Hu Qinang and Peng Ruidong (2010) “Numerical simulation of mechanisms of deformation, failure and energy dissipation in porous rock media subjected to wave stresses,” Science China., vol.53, pp.1098– 1113. 22. Zhou Xiaoping (2011) “Zonal disintegration of deep crack-weakened rock masses: A non-Euclidean model,” Theoretical and Applied Fracture Mechanics., vol.55, pp.227-236. 23. Zhou Xiaoping and Qian Qihu (2013) “Non-Euclidean Model of Failure of Deep Rock Masses Under Incompatible Deformation,” Chinese Journal of Rock Mechanics and Engineering. Vol.32, pp.767-774. © 2015 ejge