Effects of composition and pore structure on the reservoir gas capacity of Carboniferous shale from Qaidam Basin,China

Shale adsorption and breakthrough pressure are important indicators of shale gas development and key factors in evaluating the reservoir capacities of shales. In this study, geochemical tests, pore-structure tests, methane adsorption tests, and breakthrough-pressure tests were conducted on shales from the Carboniferous Hurleg Formation in eastern Qaidam Basin. The effects of the shale compositions and pore structures on the adsorption and breakthrough pressures were studied, and the reservoir capacities of the shales were evaluated by analyzing the shale adsorptions and sealing effects. The results indicate that the organic carbon content was only one of factors in affecting the adsorption capacity of the shale samples while the effect of the clay minerals was limited. Based on the positive correlation between the adsorption capacity and specific surface area of the shale, the specific surface area of the micropores can be used as an indicator to determine the adsorption capacity of shale. The micro-fracturing of brittle minerals, such as quartz, create a primary path for shale gas breakthrough, whereas the expansion of clay minerals with water greatly increases the breakthrough pressure in the shale samples. Methane adsorption tests showed that maximum methane adsorption for shale samples Z045 and S039 WAS 0.107 and 0.09655 mmol/g, respectively. The breakthrough pressure was 39.36 MPa for sample S039, maintained for 13 days throughout the experiment; however, no breakthrough was observed in sample Z045 when subjected to an injected pressure of 40 MPa for 26 days. This indicates that sample Z045, corresponding to a depth of 846.24 m, exhibited higher adsorption capacity and a better reservoir-sealing effect than sample S039 (498.4 m depth). This study provides useful information for future studies of Qaidam Basin shale gas exploration and development and for evaluation of shale quality.     

Pore structure of Cambrian shales from the Sichuan Basin in China and implications to gas storage

The microstructure of black siliceous shale from the lower Cambrian Niutitang Formation, Sichuan Basin in China was investigated by the combination of field emission scanning electron microscope (FE-SEM) and argon ion beam milling. The nanometer-to micrometer-scale pore systems of shales are an important control on gas storage and fluid migration. In this paper, the organic porosity in shale samples within oil and gas window has been investigated, and the formation mechanism and diagenetic evolution of nanopores have been researched.FE-SEM reveals five pore types that are classified as follows: organic nanopores, pores in clay minerals, nanopores of framework minerals, intragranular pores in microfossils, and microfractures. Numerous organic nanopores are observed in shales in the gas window, whereas microfractures can be seen within the organic matter of shales in the oil window. Microfractures in oil window shales could be attributed to pressure buildup in the organic matter when incompressible liquid hydrocarbon are generated, and the orientation of microfractures is probably parallel to the bedding and strength anisotropy of the formation. Pores in clay minerals are always associated with the framework of clay flakes, and develop around rigid mineral grains because the pressure shadows of mineral grains protect pores from collapse, and the increasing of silt content would lead to an increase in pressure shadows and improve porosity. Nanopores of rock framework are probably related to dissolution by acidic fluids from hydrocarbon generation, and the dissolution-related pores promote permeability of shales. Porosity in the low-TOC, low-thermal-maturity shales contrast greatly with those of high-TOC, high-thermal-maturity shales. While the high-TOC shales contain abundant organic microporosity, the inorganic pores can contribute a lot to the porosity of the low-TOC shales.     

Effect of pore structure on shale oil accumulation in the lower third member of the Shahejie formation,Zhanhua Sag,eastern China: Evidence from gas adsorption and nuclear magnetic resonance

As shale oil occurs primarily in micro–nano pores and fractures, research about the effect of pore structure on shale oil accumulation has great significance for shale oil exploration and development. The effect of pore structure on shale oil accumulation in the lower third member of the Shahejie formation (Es₃^l), Zhanhua Sag, eastern China was investigated using gas adsorption, soxhlet extraction, nuclear magnetic resonance (NMR) analysis, and field emission scanning electron microscope (FE-SEM) observation. The results indicated that the samples contained a larger amount of ink-bottle-shaped and slit-shaped pores after extraction than before extraction. The pore volume and specific surface area of the samples were approximately 2.5 times larger after extraction than before extraction. Residual hydrocarbon occurred primarily in the free-state form in pores with diameters of 10–1000 nm, which can provide sufficient pore volume for free hydrocarbon accumulation. Therefore, pores with diameters of 10–1000 nm were regarded as “oil-enriched pores”, which are effective pores for shale oil exploration, whereas pores with diameters smaller than 10 nm were regarded as “oil-ineffective pores”. Samples with only well-developed small pores with diameters smaller than 1000 nm showed high oil saturation, whereas samples with both small pores and also relatively large pores and micro-fractures presented low oil saturation. As the minimum pore size allowing fluid expulsion is 1000 nm, pores with diameters greater than 1000 nm were considered as “oil-percolated pores”. Large pores and micro-fractures are generally interconnected and may even form a complex fracture mesh, which greatly improves the permeability of shale reservoirs and is beneficial to fluid discharge.     

Investigation on the pore structure and multifractal characteristics of tight oil reservoirs using NMR measurements: Permian Lucaogou Formation in Jimusaer Sag,Junggar Basin

Pore structure is a critical parameter to estimate the reservoir quality and evaluate the resource potential. However, the pore structure and heterogeneity of the unconventional tight oil reservoirs of Permian Lucaogou Formation of Jimusaer Sag, Junggar Basin are not studied well. In this paper, the multifractal analysis based on the NMR T₂ distributions was applied to investigate the pore structure and heterogeneity. The reservoir quality index (RQI) and flow zone indicator (FZI) were calculated using porosity and permeability. Two parameters T₃₅ and T₅₀ were newly defined as relaxation times corresponding to the 35% and 50% saturation on the T₂ reverse accumulative curve, respectively. The results showed that the RQI, and FZI values were extremely low, and that the NMR T₂ distributions of water saturated samples had much short relaxation components with no or little long relaxation components, indicating a complex and poor microscopic pore structure of tight oil rocks. The typical multifractal characteristics, such as the large values of singularity strength range (Δα), revealed that the pore structures of samples were strongly heterogeneous. It was also found that the clay contents have an obvious influence on the multifractal parameters, and the FZI and new defined T₃₅ are two good indicators for heterogeneity of pore structure. In addition, the feasibility and applicability of calculating the multifractal parameters from NMR and other well logs were discussed.     

Nano-scale pore structure and fractal dimension of organic-rich Wufeng-Longmaxi shale from Jiaoshiba area,Sichuan Basin: Investigations using FE-SEM,gas adsorption and helium pycnometry

Much attention have been recently paid to the upper Ordovician Wufeng shale (O₃w) and lower Silurian Longmaxi shale (S₁l) in the Jiaoshiba area of Sichuan Basin, which is now the largest producing shale gas field in China. Field emission scanning electron microscopy (FE-SEM), low pressure gas (N₂ and CO₂) adsorption, helium pycnometry, X-ray diffraction and geochemical analyses were performed to investigate the pore structure and fractal dimension of the pores in O₃w-S₁l shale formation in the Jiaoshiba area. FE-SEM images show that organic matter (OM) pores are dominant in the organic-rich samples and these pores are often irregular, bubble-like, elliptical and faveolate in shape, while in organic-poor samples, limited and isolated interparticle (interP), intraparticle (intraP) and OM pores are observed. Reversed S-shaped isotherms obtained from nitrogen adsorption are type Ⅱ, and hysteresis loops indicate that the shape of micropore in the samples is slit-or plate-like. BET surface areas and total pore volume vary from 12.2 to 27.1 m²/g and from 1.8 × 10⁻² to 2.9 × 10⁻² cm³/g, with an average of 19.5 m²/g and 2.3 × 10⁻² cm³/g, respectively. Adsorption volume from both N₂ and CO₂ adsorption increases with respect to TOC contents. Porosities obtained from helium porosimetry are comparable with these from gas (CO₂ and N₂) adsorption in O₃w-S₁l shale. However, porosity determined by quantitative FE-SEM analysis is much smaller, which is mainly related to limited resolution and the small areas of investigation.Based on the Frenkel-Halsey-Hill (FHH) model of low-pressure N₂ adsorption, fractal dimensions of the pores varied from 2.737 to 2.823. Relationships between pore structure parameters and TOC content, mineral composition and fractal dimension reveal that the fractal dimension is mainly associated with micropores. Samples with higher TOC content, higher quartz content and lower clay content tend to contain more heterogeneous micropores, resulting in higher fractal dimensions and more complicated pore structure in shales. Therefore, fractal dimension is an effective parameter to reflect the complexity of pore structure and the degree of micropore development in O₃w-S₁l shale.     

Characterization of shale pore system: A case study of Paleogene Xin'gouzui Formation in the Jianghan basin,China

The pore size classification (micropore <2 nm, mesopore 2–50 nm and macropore >50 nm) of IUPAC (1972) has been commonly used in chemical products and shale gas reservoirs; however, it may be insufficient for shale oil reservoirs. To establish a suitable pore size classification for shale oil reservoirs, the open pore systems of 142 Chinese shales (from Jianghan basin) were studied using mercury intrusion capillary pressure analyses. A quantitative evaluation method for I-micropores (0–25 nm in diameter), II-micropores (25–100 nm), mesopores (100–1000 nm) and macropores (>1000 nm) within shales was established from mercury intrusion curves. This method was verified using fractal geometry theory and argon-ion milling scanning electron microscopy images. Based on the combination of pore size distribution with permeability and average pore radius, six types (I-VI) shale open pore systems were analyzed. Moreover, six types open pore systems were graded as good, medium and poor reservoirs. The controlling factors of pore systems were also investigated according to shale compositions and scanning electron microscopy images. The results show that good reservoirs are composed of shales with type I, II and III pore systems characterized by dominant mesopores (mean 68.12 vol %), a few macropores (mean 7.20 vol %), large porosity (mean 16.83%), an average permeability of 0.823 mD and an average pore radius (r_a) of 88 nm. Type IV pore system shales are medium reservoirs, which have a low oil reservoir potential due to the developed II-micropores (mean 57.67 vol %) and a few of mesopores (mean 20.19 vol %). Poor reservoirs (composed of type V and VI pore systems) are inadequate reservoirs for shale oil due to the high percentage of I-micropores (mean 69.16 vol %), which is unfavorable for the flow of oil in shale. Pore size is controlled by shale compositions (including minerals and organic matter), and arrangement and morphology of mineral particles, resulting in the developments of shale pore systems. High content of siliceous mineral and dolomite with regular morphology are advantage for the development of macro- and mesopores, while high content of clay minerals results in a high content of micropores.     

Heterogeneous nanoporosity of the Silurian Longmaxi Formation shale gas reservoir in the Sichuan Basin using the QEMSCAN,FIB-SEM,and nano-CT methods

Nanoporosity of a shale gas reservoir provides essential information on the gas accumulation space and controls the gas reserves. The characteristics of heterogeneous nanoporosity of four shale samples are analyzed by combining quantitative evaluation of minerals by scanning electronic microscopy (QEMSCAN), focused ion beam-scanning electron microscopy (FIB-SEM), and nano-CT. The representative elementary area (REA) is proposed by QEMSCAN to detect the imaging area that can represent the overall contents of minerals and organic matter. Combined with the statistics of pores in minerals and organic matter by FIB-SEM, the quantitative nanoporosity is obtained. The nano-CT is used to compare the total nanoporosity that was obtained by FIB-SEM. The results show that shale has distinct characteristics in nanoporosities due to the variation in organic matter and mineral content. The major pore sizes of the organic matter and clay minerals are smaller than 400 nanometers (nm), and the pore sizes of feldspar and pyrite are mainly 200–600 nm. The pore sizes for pores developed in quartz and carbonate minerals range from a few nanometers to 1000 nm. Furthermore, pores smaller than 400 nm mainly provide the total nanoporosity. The nanoporosities in the organic matter are approximately 17%–21%. Since the organic matter content (0.54%–6.98%) is low, the organic matter contributes approximately 5%–33% of the total nanoporosity in shale. Conversely, the nanoporosities in quartz and clay are generally lower than 3%. Since the mineral content (93.02%–99.46%) is obviously higher than the organic matter content, the minerals contribute approximately 67%–95% of the total nanoporosity in shale.     

Pore structure of the graptolite-derived OM in the Longmaxi Shale,southeastern Upper Yangtze Region,China

The Lower Silurian Longmaxi Shale in the southeastern Upper Yangtze Region, which has been the main target for shale gas exploration and production in China, is black marine organic-rich shale and rich in graptolites. Graptolites, usually only periderms preserved in shales, are important organic component of the Longmaxi Shale. However, the pore structure of graptolite periderms and its contribution to gas storage has not yet been studied before. A combination of optical microscopy for identification and “mark” of graptolite and scanning electron microscope (SEM) for pore observations were conducted for the Longamxi Shale samples. Results show that pores are anisotropic developed in the Longmaxi graptolite periderms and greatly associated with their fine structure. Micrometer-sized fractures and spindle-shaped pores between cortical fibrils in the cortical bandage are greatly developed at section parallel to the bedding, while they are rare at section perpendicular to the bedding. Besides, numerous sapropel detritus rich in nanometer-sized pores are discretely distributed in the shale. Though graptolite periderms are low porosity from SEM image analysis, microfractures and elongated pores along the graptolite periderm wall may still make the graptolite an interconnected system. Together with the discrete porous sapropel detritus in shale, these graptolite-derived Organic Matter (OM) may form an interconnected organic pore system in the shale. The difference of pore development observed in graptolite periderms and sapropel detritus also give us new insight for the organic pore heterogeneity study. The OM composition, their fine structure and orientation in the rock may be important factors controlling OM pore development. The combination of identifying OM type under optical microscopy and pores observation under SEM for may be an effective method to study the OM pore development especially in shale that contain more OM.     

BIB-SEM characterization of pore space morphology and distribution in postmature to overmature samples from the Haynesville and Bossier Shales

Four Haynesville Shale and four Bossier Shale samples were investigated using a combination of Scanning Electron Microscopy (SEM) and Broad Ion Beam (BIB) polishing. This approach enables the microstructure and porosity to be studied down to the mesopore size (<50 nm) in representative areas at the scale of the BIB cross-sections. The samples vary in mineralogy, grain size and TOC and the maturity ranges from 2.42 to 2.58 VR_r in the Haynesville Shale to 1.79–2.26 VR_r in the Bossier Shale. This variety within the samples enabled us to study controls on the porosity distribution in these shales. Visible pores exist as intraparticle pores mainly in carbonate grains and pyrite framboids and as interparticle pores, mainly in the clay-rich matrix. Pores in organic matter show a characteristic porosity with respect to the type of organic matter, which mainly consists of mixtures of amorphous organic matter and minerals, organic laminae and discrete macerals. A clear positive trend of organic-matter porosity with maturity was found. Pore sizes are power law distributed in the range of 4.4 μm to at least 36 nm in equivalent diameter. The differences in power law exponents suggest that a more grain supported, coarse-grained matrix may prevent pores from mechanical compaction. Porosities measured in the BIB cross-sections were significantly lower in comparison to porosities obtained by Mercury Intrusion Porosimetry (MIP). This difference is mainly attributed to the different resolution achieved with BIB-SEM and MIP and type of pore network. Extrapolation of pore size distributions (PSDs) enables the BIB-SEM porosity to be estimated down to the resolution of the MIP and thus to upscale microstructural observation at the confined space of the BIB-SEM method to bulk porosity measurement. These inferred porosities are in good agreement with the MIP determined porosities, which underpins the assumption that pores segmented in BIB-SEM mosaics are representative of the MIP methodology.     

Evaluation of Eocene source rock for potential shale oil and gas generation in north Cambay Basin,India

Source rock potential of 108 representative samples from 3 m intervals over a 324 m thick shale section of middle Eocene age from the north Cambay Basin, India have been studied. Variation in total organic carbon (TOC) and its relationship with loss on ignition (LOI) have been used for initial screening. Screened samples were subjected to Rock-Eval pyrolysis and organic petrography. A TOC log indicated wide variation with streaks of elevated TOC. A 30 m thick organic-rich interval starting at 1954 m depth, displayed properties consistent with a possible shale oil or gas reservoir. TOC (wt%) values of the selected samples were found to vary from 0.68% to 3.62%, with an average value of 2.2. The modified van Krevelen diagram as well as HI vs. T_max plot indicate prevalence of Type II to Type III kerogen. T_max measurements ranged from 425 °C to 439 °C, indicating immature to early mature stage, which was confirmed by the mean vitrinite reflectance values (%R_o of 0.63, 0.65 and 0.67 at 1988 m, 1954 m, and 1963 m, respectively). Quantification of hydrocarbon generation, migration and retention characteristics of the 30 m source rock interval suggests 85% expulsion of hydrocarbon. Oil in place (OIP) resource of the 30 m source rock was estimated to be 3.23 MMbbls per 640 acres. The Oil saturation index (OSI) crossover log showed, from a geochemical perspective, moderate risk for producing the estimated reserve along with well location for tapping the identified resource.     

Geochemical characteristics of gases from the largest tight sand gas field (Sulige) and shale gas field (Fuling) in China

This study performed a detailed geochemical analyses of the components, stable carbon isotopes of alkane gas and CO₂, stable hydrogen isotopes of alkane gas and helium isotopes of reproducing gas from the largest tight gas field (Sulige) and shale gas (Fuling) field in China. The comparative study shows that tight gas from the Sulige gas field in the Ordos Basin is of coal-derived origin, which is characterized by a positive carbon and hydrogen isotopic distribution pattern (δ¹³C₁ > δ¹³C₂ > δ¹³C₃ > δ¹³C₄; δ²H₁ > δ²H₂ > δ²H₃), i.e., the carbon and hydrogen isotopes increase with increasing carbon numbers. Carbon dioxide from this field are of biogenic origin and the helium is crust-derived. Shale gas from the Fuling shale gas field belongs to oil-derived gas which has complete carbon and hydrogen isotopic reversal of secondary alteration origin (δ¹³C₁ < δ¹³C₂ < δ¹³C₃; δ²H₁ < δ²H₂ < δ²H₃), i.e., the carbon and hydrogen isotopes decrease with increasing carbon numbers. Such complete isotopic reversal distribution pattern is due to the secondary alteration like oil or gas cracking, diffusion and so on under high temperature. In that case, positive carbon or hydrogen isotopic distribution pattern will change into complete isotopic reversal as the temperature increases. Carbon dioxide is of abiogenic origin resulting from the thermal metamorphism of carbonates and helium is crust-derived.     

Geochemistry,reservoir characterization and hydrocarbon generation potential of lacustrine shales: A case of YQ-1 well in the Yuqia Coalfield,northern Qaidam Basin,NW China

Ever since a breakthrough of marine shales in China, lacustrine shales have been attracting by the policy makers and scientists. Organic-rich shales of the Middle Jurassic strata are widely distributed in the Yuqia Coalfield of northern Qaidam Basin. In this paper, a total of 42 shale samples with a burial depth ranging from 475.5 m to 658.5 m were collected from the Shimengou Formation in the YQ-1 shale gas borehole of the study area, including 16 samples from the Lower Member and 26 samples from the Upper Member. Geochemistry, reservoir characteristics and hydrocarbon generation potential of the lacustrine shales in YQ-1 well were preliminarily investigated using the experiments of vitrinite reflectance measurement, maceral identification, mineralogical composition, carbon stable isotope, low-temperature nitrogen adsorption, methane isothermal adsorption and rock eval pyrolysis. The results show that the Shimengou shales have rich organic carbon (averaged 3.83%), which belong to a low thermal maturity stage with a mean vitrinite reflectance (R_o) of 0.49% and an average pyrolytic temperature of the generated maximum remaining hydrocarbon (T_max) of 432.8 °C. Relative to marine shales, the lacustrine shales show low brittleness index (averaged 34.9) but high clay contents (averaged 55.1%), high total porosities (averaged 13.71%) and great Langmuir volumes (averaged 4.73 cm⁻³ g). Unlike the marine and marine-transitional shales, the quartz contents and brittleness index (BI) values of the lacustrine shales first decrease then increase with the rising TOC contents. The kerogens from the Upper Member shales are dominant by the oil-prone types, whereas the kerogens from the Lower Member shales by the gas-prone types. The sedimentary environment of the shales influences the TOC contents, thus has a close connection with the hydrocarbon potential, mineralogical composition, kerogen types and pore structure. Additionally, in terms of the hydrocarbon generation potential, the Upper Member shales are regarded as very good and excellent rocks whereas the Lower Member shales mainly as poor and fair rocks. In overall, the shales in the top of the Upper Member can be explored for shale oil due to the higher free hydrocarbon amount (S₁), whereas the shales in the Lower Member and the Upper Member, with the depths greater than 1000 m, can be suggested to explore shale gas.     

Cause of shale gas geochemical anomalies and mechanisms for gas enrichment and depletion in high-maturity shales

This article reviews the abnormal characteristics of shale gases (natural gases produced from organic-rich shales) and discusses the cause of the anomalies and mechanisms for gas enrichment and depletion in high-maturity organic-rich shales. The reported shale gas geochemical anomalies include rollover of iso-alkane/normal alkane ratios, rollover of ethane and propane isotopic compositions, abnormally light ethane and propane δ¹³C values as well as isotope reversals among methane, ethane and propane. These anomalies reflect the complex histories of gas generation and associated isotopic fractionation as well as in-situ “mixing and accumulation” of gases generated from different precursors at different thermal maturities. A model was proposed to explain the observed geochemical anomalies. Gas generation from kerogen cracking at relatively low thermal maturity accounted for the increase of iso-alkane/normal alkane ratios and ethane and propane δ¹³C values (normal trend). Simultaneous cracking of kerogen, retained oil and wet gas and associated isotopic fractionation at higher maturity caused decreasing iso-alkane/normal alkane ratios, lighter ethane and propane δ¹³C and corresponding conversion of carbon isotopic distribution patterns from normal through partial reversal to complete reversal. Relatively low oil expulsion efficiency at peak oil generation, low expulsion efficiency at peak gas generation and little gas loss during post-generation evolution are necessary for organic-rich shales to display the observed geochemical anomalies. High organic matter richness, high thermal maturity (high degrees of kerogen-gas and oil-gas conversions) and late-stage (the stage of peak gas generation and post-generation evolution) closed system accounted for gas enrichment in shales. Loss of free gases during post-generation evolution may result in gas depletion or even undersaturation (total gas content lower than the gas sorption capacity) in high-maturity organic-rich shales.     

BTEX anomalies used as indicators of submarine oil and gas reservoirs

It is a conventional method for petroleum prospecting to generally use paraffin hydrocarbon as basic indexes of oil and gas. This conventional geochemical technology, however, shows some limits in the prospecting as paraffin is vulnerable to influences from human and biologic activities. Consequently, BTEX (short for benzene, toluene, ethyl benzene and xylem, which are direct biomarkers) among aromatic hydrocarbon series has been taken into account for the oil and gas prediction. Domestic and foreign study results demonstrate that BTEX is hardly disturbed and can well indicate oil and gas reservoirs. Based on measured data from a South China Sea area, the present authors have used self-developed visual assessment software for petroleum prospecting has been used to process data, strip background anomalies, and outline significant BTEX anomalies. By comparison with stratigraphic profiles of the target area, it is confirmed that BTEX is a good indication of marine oil and gas during the petroleum prospecting.     

BTEX异常对海域油气藏指示作用的研究

常规的油气化探方法一般是应用烷烃类作为油气勘探的基本指标,但是烷烃类易受人类活动和生物活动的干扰,使常规的化探技术在油气勘探中一直受到限制。人们开始考虑采用直接的生物标记化合物来预测油气藏,如芳烃系列中的苯系化合物苯(benzene)、甲苯(toluene)、乙苯(ethylbenzene)、二甲苯(xylem),简称BTEX。国内外研究表明,BTEX基本不受人类活动和生物活动的干扰,对油气藏具有良好的指示作用。依据南海某区的实测资料,采用自主研发的油气化探可视化评价软件进行数据处理,剥离背景异常,圈出有效的BTEX异常,并与靶区地层剖面进行了对比,结果证实了BTEX对海域油气藏具有良好的指示作用。     

2D and 3D nanopore characterization of gas shale in Longmaxi formation based on FIB-SEM

Studying complex pore structures is the key to understanding the mechanism of shale gas accumulation. FIB-SEM (focused ion beam-scanning electron microscope) is the mainstream and effective instrument for imaging nanopores in gas shales. Based on this technology, 2D and 3D characteristics of shale samples from Lower Silurian Longmaxi formation in southern Sichuan Basin were investigated. 2D experimental results show that the pores in shale are nanometer-sized, and the structure of those nanopores can be classified into three types: organic pores, inorganic pores and micro fractures. Among the three types, organic pores are dominantly developed in the OM (organic matter) with three patterns such as continuous distributed OM, OM between clay minerals and OM between pyrite particles, and the size of organic pores range from 5 nm to 200 nm.Inveresly, inorganic pores and micro fractures are less developed in the Longmaxi shales. 3D digital rocks were reconstructed and segmented by 600 continuous images by FIB cutting and SEM imaging simultaneously. The pore size distribution and porosity can be calculated by this 3D digital core, showing that its average value is 32 nm and porosity is 3.62%.The 3D digital porosity is higher than its helium porosity, which can be regarded as one important parameter for evaluation of shale gas reserves. The 2D and 3D characterized results suggest that the nanometer-sized pores in organic matter take up the fundamental storage space for the Longmaxi shale. These characteristics have contributed to the preservation of shale gas in this complex tectonic area.     

The impact of composition on pore throat size and permeability in high maturity shales: Middle and Upper Devonian Horn River Group,northeastern British Columbia,Canada

Shale reservoirs of the Middle and Upper Devonian Horn River Group provide an opportunity to study the influence of rock composition on permeability and pore throat size distribution in high maturity formations. Sedimentological, geochemical and petrophysical analyses reveal relationships between rock composition, pore throat size and matrix permeability.In our sample set, measured matrix permeability ranges between 1.69 and 42.81 nanodarcies and increases with increasing porosity. Total organic carbon (TOC) content positively correlates to permeability and exerts a stronger control on permeability than inorganic composition. A positive correlation between silica content and permeability, and abundant interparticle pores between quartz crystals, suggests that quartz may be another factor enhancing the permeability. Pore throat size distributions are strongly related to TOC content. In organic rich samples, the dominant pore throat size is less than 10 nm, whereas in organic lean samples, pore throat size distribution is dominantly greater than 20 nm. SEM images suggest that in organic rich samples, organic matter pores are the dominant pore type, whereas in quartz rich samples, the dominant type is interparticle pores between quartz grains. In clay rich and carbonate rich samples, the dominant pore type is intraparticle pores, which are fewer and smaller in size.High permeability shales are associated with specific depositional facies. Massive and pyritic mudstones, rich in TOC and quartz, have comparatively high permeability. Laminated mudstone, bioturbated mudstone and carbonate facies, which are relatively enriched in clay or carbonate, have fairly low permeability.     

Nanoscale pore structure and fractal characteristics of a marine-continental transitional shale: A case study from the lower Permian Shanxi Shale in the southeastern Ordos Basin,China

Shale samples collected from seven wells in the southeastern Ordos Basin were tested to investigate quantitatively the pore structure and fractal characteristics of the Lower Permian Shanxi Shale, which was deposited in a marine-continental transitional (hereinafter referred to as the transitional) environment. Low-pressure nitrogen adsorption data show that the Shanxi Shale exhibits considerably much lower surface area (SA) and pore volume (PV) in the range of 0.6–1.3 m²/g and 0.25–0.9 ml/100 g, respectively. Type III kerogen abundant in the transitional Shanxi Shale were observed to be poorly developed in the organic pores in spite of being highly mature, which resulted in a small contribution of organic matter (OM) to the SA and PV. Instead, I/S (illite-smectite mixed clay) together with illite jointly contributed mostly to the SA and PV as a result of the large amount of inter-layer pores associated with them, which were evident in broad-ion-beam (BIB) imaging and statistical analysis. Additionally, the Shanxi Shale has fractal geometries of both pore surface and pore structure, with the pore surface fractal dimension (D1) ranging from 2.16 to 2.42 and the pore structure fractal dimension (D2) ranging from 2.49 to 2.68, respectively. The D1 values denote a pore surface irregularity increase with an increase in I/S and illite content attributed to their more irregular pore surface compared with other mineralogical compositions and OM. The fractal dimension D2 characterizing the pore structure complexity is closely related to the pore arrangement and connectivity, and I/S and illite decrease the D2 when their contents increase due to the incremental ordering degree and connectivity of I/S- or illite-hosted pores. Meanwhile, other shale constituents (including kaolinite, chlorite, and OM) that possess few pores can significantly increase the pore structure complexity by way of pore-blocking.     

Laboratory characterization of the porosity and permeability of gas shales using the crushed shale method: Insights from experiments and numerical modelling

Gas production from shale resource plays has transformed the USA energy market. Despite the knowledge gained from the analysis of large amounts of shale core, appraisal of shale gas resource plays requires a large number of wells to be drilled and tested. Ideally, core analysis results would provide an indication of both the gas filled porosity and permeability of shale resource plays, which could then be used to reduce the number of wells needed during appraisal. A combination of laboratory experiments, numerical modelling and a round-robin test have been conducted to assess the validity of the crushed shale method (CSM), which has been widely used in industry to assess the porosity and permeability of shale. The results suggest that the CSM can provide reasonably precise estimates of porosity measured at ambient stress if a standard sample cleaning method is adopted; although a reliable method to correct these values to subsurface conditions needs to be developed. The CSM does not, however, appear to provide useful information on shale permeability. A round-robin test shows that differences of up to four orders of magnitude in permeability were provided by different laboratories when analysing the same sample. These huge differences seem to occur due to a combination of errors in calculating permeabilities from pressure transients, differences in the way that permeability is calculated as well as uncertainties regarding the effective size of crushed shale particles. However, even if standardized, the CSM may not be particularly useful for characterizing the flow capacity of shale because it is insensitive to the presence of high permeability zones that would control flow in the subsurface.     

Pore characterization of organic-rich Lower Cambrian shales in Qiannan Depression of Guizhou Province,Southwestern China

Nine organic-rich shale samples of Lower Cambrian black shales were collected from a recently drilled well in the Qiannan Depression, Guizhou Province where they are widely distributed with shallower burial depth than in Sichuan Basin, and their geochemistry and pore characterization were investigated. The results show that the Lower Cambrian shales in Qiannan Depression are organic rich with TOC content ranging from 2.81% to 12.9%, thermally overmature with equivalent vitrinite reflectance values in the range of 2.92–3.25%, and clay contents are high and range from 32.4% to 53.2%. The samples have a total helium porosity ranging from 2.46% to 4.13% and total surface area in the range of 9.08–37.19 m²/g. The estimated porosity in organic matters (defined as the ratio of organic pores to the volume of total organic matters) based on the plot of TOC vs helium porosity is about 10% for the Lower Cambrian shales in Qiannan Depression and is far lower than that of the Lower Silurian shales (36%) in and around Sichan Basin. This indicates that either the organic pores in the Lower Cambrian shale samples have been more severely compacted than or they did not develop organic pores as abundantly as the Lower Silurian shales. Our studies also reveal that the micropore volumes determined by Dubinin–Radushkevich (DR) equation is usually overestimated and this overestimation is closely related to the non-micropore surface area of shales (i.e. the surface area of meso- and macro-pores). However, the modified BET equation can remove this overestimation and be conveniently used to evaluate the micropore volumes/surface area and the non-micropore surface areas of micropore-rich shales.