Study on the Full-Range Pore Size Distribution and the Movable Oil

Jul 7, 2019 - The pore size distribution (PSD) and fluid mobility parameters are vital parameters for predicting rock properties and the reservoir qua...
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A study on the full-range pore size distribution and the movable oil distribution in glutenite Weichao Tian, Shuangfang Lu, Wenbiao Huang, Shuping Wang, Yang Gao, Weiming Wang, Jinbu Li, Jianpeng Xu, and Zhuochen Zhan Energy Fuels, Just Accepted Manuscript • DOI: 10.1021/acs.energyfuels.9b00999 • Publication Date (Web): 07 Jul 2019 Downloaded from pubs.acs.org on July 16, 2019

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A study on the full-range pore size distribution and

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the movable oil distribution in glutenite

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Weichao Tian1,2,3, Shuangfang Lu1,2*, Wenbiao Huang1,2, Shuping Wang4, Yang Gao5, Weiming

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Wang1,2, Jinbu Li1,2, Jianpeng Xu1,2, Zhuochen Zhan1,2

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1Key

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Shandong 266580, China

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2School

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266580, China

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3Department

Laboratory of Deep Oil and Gas, China University of Petroleum (East China), Qingdao,

of Geosciences, China University of Petroleum (East China), Qingdao, Shandong

of Geology & Geophysics, Texas A&M University, College Station, Texas 77843,

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USA

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4Oil

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266580, China

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5Exploration

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Karamay, Xinjiang 834000, China

Industry Training Center, China University of Petroleum (East China), Qingdao, Shandong

and Development Research Institute, Xinjiang Oilfield Branch of PetroChina,

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ABSTRACT

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The pore size distribution (PSD) and fluid mobility parameters are vital parameters for predicting

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rock properties and the reservoir quality classification. Due to the characteristics of strong

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heterogeneity, complex pore-throat structure and wide PSD of glutenite, it is more difficult to

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acquire the full-range PSD and fluid occurrence states of glutenite. This paper investigates the full-

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range PSD, the distribution and the controlling factors of the movable oil in glutenite based on

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various experiments. X-ray diffraction (XRD), casting thin sections, scanning electron microscopy

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(SEM), low-temperature nitrogen adsorption (LTNA), high-pressure mercury intrusion (HPMI),

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and nuclear magnetic resonance (NMR)-centrifugation experiments were conducted on 18

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glutenite samples from the Mahu Sag, Junggar Basin, China. A new method for characterizing the

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full-range PSD of glutenite was proposed by integrating LTNA and NMR-centrifugation

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experiments, and the full-range PSD is in good agreement with the casting thin sections and SEM

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images. Moreover, in terms of the distribution patterns of the T2 spectra under the n-dodecane

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saturation condition, the glutenite samples are divided into four categories (i.e., type- I, type- II,

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type- III and type- IV). From type- I to type- IV, both the pore size and the movable oil saturation

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of glutenite samples show a gradually decreasing trend. In addition, the movable oil mainly occurs

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in the pore-throat configurations of type- A, type- B and type- C in glutenite. The development of

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the different types of pore-throat configurations is controlled jointly by the sedimentary

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compositions and mineral compositions. For higher quartz clastic and feldspar mineral contents,

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and lower calcite and clay mineral contents, glutenite is more developed in type- A, type- B and

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type- C pore-throat configurations. The above findings will provide intellectual support for

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identifying high quality glutenite reservoirs and improving the productivity of glutenite oil

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reservoirs.

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Keywords: glutenite, full-range pore structure, movable oil, controlling factors, NMR-

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centrifugation

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1. INTRODUCTION

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Glutenite is extensively developed in the Junggar Basin. In recent years, a one billion ton super-

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large glutenite oil reservoir was discovered in the Permian and Triassic strata of the Mahu Sag,

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which has become a new base to increase in the reservoir volume and yield of the Xingjiang

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oilfield.1,2 However, the glutenite reservoir has the characteristics of strong heterogeneity, a

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complex pore-throat structure and a wide pore size distribution (PSD),

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prominent risk factors in petroleum exploration. The key to reducing the exploration risks of

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glutenite reservoirs is to find high-quality reservoirs. The quality of a reservoir depends on its

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storage capacity and fluid flow capacity (i.e., fluid mobility), which are essentially controlled by

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microscopic pore-throat structures (e.g., PSD, and throat size distribution). Therefore, quantitative

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analysis of the full-range pore structure and the distribution of the movable oil in glutenite are

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urgently needed.

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which have become

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The nuclear magnetic resonance (NMR) technique is a quick and nondestructive technique that

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can obtain information on the rock physical properties and fluid occurrence states through the

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NMR T2 spectrum of a core saturated with hydrogen fluid, such as the porosity, permeability, PSD,

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and percentage of movable fluids.5–10 However, to characterize the full-range PSD, the key is to

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determine the conversion coefficient (C) between T2 and the pore size. Scholars in China and

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abroad have conducted studies on this topic and proposed many methods to determine the C value,

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such as the empirical method, the T2 cutoff method, and the similarity method. The C value

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acquired by the empirical method is only applicable to a specific area, and for the same area, rocks

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with large differences in the iron-bearing mineral content will have relatively large differences in

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C values.11 The T2 cutoff method is only applicable to reservoirs with good pore connectivity, and

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the applicability to low-permeability/tight reservoirs is poor.12 The similarity method is currently

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the most commonly used method to determine the C value for low-permeability/tight reservoirs.

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The similarity method determines the C value by comparing the NMR T2 spectra with the PSDs

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obtained from other experiments (e.g., high-pressure mercury intrusion (HPMI), rate-controlled

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porosimetry, and the image method). For instance, many scholars determined the C value by

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means of HPMI.9,13–18 However, HPMI characterizes smaller pores only by increasing the injection

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pressure, and an excessively high injection pressure could cause matrix compression, particle

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damage, and opening of closed pores.19,20 Furthermore, HPMI only obtains the sizes of throat and

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the volumes of controlled pores but cannot acquire the size distributions of the intergranular pores,

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intergranular dissolution pores, and moldic pores developed in glutenite. Xiao et al.21,22 proposed

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a method that combined rate-controlled porosimetry and NMR to characterize the full-range PSD.

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However, the glutenite in the study area has a relatively low permeability, and the mercury

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injection saturation is often lower than 50%. Thus, this method is also not appropriate to study the

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PSD of glutenite. In addition, scholars determine the C value by contrasting the NMR T2 spectrum

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and the PSD derived from the image method.23,24 However, glutenite has a coarse grain size and

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strong heterogeneity; thus, the PSD obtained by the image method is not representative. However,

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similar to NMR experiments, low-temperature nitrogen adsorption (LTNA) experiments can

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comprehensively characterize the size distributions of pores and throats, and the experiments

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characterize the minimum pore size depending on the set minimum relative pressure. Moreover,

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the minimum pore characterized by an NMR experiment is related to the molecular size of the

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saturated fluid and the NMR parameter TE value. Therefore, when we properly select the saturated

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fluids and set the NMR parameters, the PSDs obtained by LTNA and the NMR T2 spectrum will

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have a very good similarity in the range of T2c and irreducible fluids occurs in pores with T299.999%) as the adsorbate and gradually increased and reduced the relative pressure

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(0.0090.45. The shape of the

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hysteresis loop in the adsorption/desorption isotherm reflects the pore morphology of the porous

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medium. Referring to the International Union of Pure and Applied Chemistry (IUPAC) for the

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classification of hysteresis loops,34 we can divide the hysteresis loops of the glutenite samples into

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four types (Figure 4): sample 1# has a typical H3-type hysteresis loop. Its hysteresis loop is the

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smallest, which reflects that the pores are open-slit pores. The hysteresis of sample 8# is close to

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the H3-type hysteresis loop, and the hysteresis loop is relatively small, which indicates that the

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pores are mainly slit pores. The hysteresis loop of sample 11# is a typical H2-type hysteresis loop,

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and the hysteresis loop is the largest, which reflects that the pores are ink-bottle-shaped pores with

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thin necks and broad bodies. The loop of sample 5# is close to the H2-type hysteresis loop, and

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the hysteresis loop is relatively larger, which indicates that the pores are mainly ink-bottle-shaped

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pores. A statistical analysis found that the hysteresis loops for the glutenite samples are mainly

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H3-type and transition between H2 and H3 types, while the H2-type hysteresis loop is not

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common.

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The SSA of the glutenite is distributed in the range of 2.298-12.780 m2/g with a mean of 4.524

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m2/g. The pore volume (VLTNA) varies from 0.0058 ml/g to 0.02462 ml/g with an average of

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0.01313 ml/g. Thus, the porosity of LTNA can be determined by equation ΦLTNA=VLTNA×ρrock and

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ranges from 1.44% to 5.30%. Through analysis of the correlations among the various mineral

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constituents in glutenite and SSAs and pore volumes (Figure 5), we can draw the following

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understanding. The SSA has a good correlation with the clay minerals (especially chlorite) content,

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but the correlations with the other minerals are not notable. The VLTNA and quartz and clay minerals

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(especially chlorite) contents exhibit relatively good correlations, but the correlations with the

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other minerals are poor. The analysis above indicates that the pores characterized by the LTNA

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experiment are mainly intercrystalline pores in clay and some intragranular dissolution pores in

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quartz. Moreover, a large number of nanoscale intercrystalline pores in clay and intragranular

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dissolution pores in quartz can be observed under SEM (Figures 3c and e-h).

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The BJH model and DFT model are the two most widely used methods at present to calculate

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the PSD of the porous medium by LTNA. From Figure 6, it can be seen that the glutenite samples

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appear to have an apparent peak at ≈4 nm in the PSDs derived from the BJH model using the

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desorption branch. However, the peak does not occur in the PSDs calculated by the BJH and DFT

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models using the adsorption branch, indicating that it is an artificial peak. Previous studies have

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shown that artificial peaks are mainly caused by the tensile strength effect (TSE).28,35 The TSE

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occurs as a result of the development of ink-bottle-shaped pores in the glutenite samples. The

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higher the proportion of ink-bottle-shaped pores is, the more distinct the artificial peak is, which

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can be verified in samples 1# and 11#. From the previous analysis, it can be seen that the ink-

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bottle-shaped pores of sample 11# are more developed than those of sample 1#. Moreover, the

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artificial peak of sample 11# is more distinct than that of sample 1# (Figure 6). Therefore, we adopt

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the adsorption branch data to calculate the PSDs. The dV-PSDs (dV representing incremental pore

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volume) obtained by the BJH and DFT models have relatively large differences in both shape and

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amplitude, which is mainly due to the large difference in the number of data collection points when

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the two models calculate the PSD. This difference is lessened to a certain extent for the

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dV/dlog(w)-PSD (w representing pore width), which implies that the use of dV/dlog(w) weakens

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the influence of the number of data collection points to a certain extent. Because of the influence

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of the number of data collection points on the calculation of the PSD and the number of data

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collection points is greater when the DFT model is used to calculate the PSD, in the following, we

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adopt the PSD calculated by the DFT model to calibrate the NMR T2 spectrum.

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The PSDs for glutenite calculated by the DFT model are shown in Figure 7. The dV-PSD is

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characterized by a left half peak or single-peak, and the peak position is distributed in the range

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>0.02 μm, implying that the pore volume is mainly contributed by pores >0.02 μm.

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3.4. NMR T2 distribution.

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The T2 spectra under the dry sample condition, So and Soir were measured in the NMR

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experiment. The dry sample condition is obtained after oil washing and drying at 110°C, and the

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information revealed by the T2 spectrum is mainly the surface-bound water of the rock particles

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and the hydroxyl water that is tightly bound between clay sheets.36,37 The T2 spectra analyzed at So

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and Soir below are all obtained by subtracting the dry sample T2 spectrum, that is, the influences of

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the surface-bound water of the rock particles and the tightly bound hydroxyl water between clay

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sheets are eliminated.

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3.4.1 NMR T2 distribution at So. The T2 spectra at So are measured for all of the glutenite samples,

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which are shown as solid lines in Figure 8. The T2 spectra at So usually show three peaks, namely,

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P1 in the range of 0.1-1.5 ms, P2 in the range of 3-30 ms, and P3 in the range of 50-1000 ms. P1

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and P3 are present in all samples, but the amplitude of P3 varies greatly in the different samples.

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However, certain samples do not have P2 (Figure 8b), or in certain samples, P2 and P1 combine

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to form a peak (P1+P2) (Figure 8c).

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The morphological characteristics of the T2 spectra of the glutenite samples are controlled by

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their pore-throat structures. According to the morphological characteristics of the T2 spectrum at

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So, we can divide all the glutenite samples into four types. The T2 spectra of type- I samples have

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three continuous peaks (P1, P2, and P3). The amplitude of P1 is higher than those of P2 and P3,

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and the amplitude of P3 is close to that of P2, indicating that this type of sample has developed

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three types of pores with large differences in size. A large number of large-sized intergranular

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pores and intergranular dissolved pores can be seen in the casting thin section (Figures 2a and b),

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and the areal porosity is above 4%. In addition, micro/submicroscale intragranular dissolution

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pores and nanoscale intercrystalline pores in clay can also be observed in the SEM image (Figures

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3a and b). The T2 spectra of type- II samples have distinct P1 and P3 peaks, with the P3 peak

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slightly left-shifted compared to that of the type- I sample, and the peak position is near 100 ms,

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implying that these samples mainly have two types of pores with a relatively large difference in

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size. The casting thin sections display many large dissolution pores with an areal porosity between

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3 and 6% (Figures 2c and d). The SEM images show a large number of nanoscale intercrystalline

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pores in clay (Figures 3c and d). The T2 spectra of the type- III samples have distinct P1 and P2

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(Figure 8c, samples 7# and 9#) or P1+P2 peaks (Figures 8c, sample 8#), and the amplitude of P3

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is extremely low, which indicates that large-sized pores are not developed and mainly two types

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of pores are developed with minor differences in size. The casting thin sections and SEM images

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show that this type of sample mainly has intragranular dissolution pores and nanoscale

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intercrystalline pores in clay, and only a small number of intergranular pores or intergranular

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dissolution pores were observed (Figures 2e and f, and 3e and f); the microscale areal porosity is

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lower than 2%. The T2 spectra of the type- IV samples have a high-amplitude P1 peak, but the

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amplitudes of both the P2 and P3 peaks are very low, which implies that such samples only have

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nanoscale pores. The casting thin sections and SEM images show that this type of sample mainly

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has nanoscale intercrystalline pores in clay and intragranular dissolution pores, and microscale

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intragranular dissolution pores are occasionally observed in rock fragments with an areal porosity

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0.44 μm is the best. When the throat size increases or decreases, R2 declines.

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The above analyses show that the volume of movable oil is mainly contributed by the pore volume

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controlled by throats >0.44 μm.

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In summary, it can be concluded that the distribution of the movable oil are microscopically

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related to the type of pore-throat configuration in the glutenite. Figure 14 shows the five main

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pore-throat configurations for glutenite. Type A is the configuration of large pores (>6 μm) and

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large throats (>0.44 μm), in which oil has the highest mobility. Taking sample 1# as an example,

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the throats are mainly distributed above 0.44 μm, and the oil in the pores >6 μm is almost 100%

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movable (Figure 15a). Type B represents the configuration of large pores (>6 μm) and small throats

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(6 μm is relatively low (Figure 15f).

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Type C represents the configuration of relatively small pores (0.44

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μm), and the oil mobility inside type C pores is also relatively high. For example, the throats of

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sample 1# are mainly distributed above 0.44 μm, and almost all of the oil in pores larger than 0.5

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μm is movable (Figure 15a). Type D reflects the configuration of small pores (type D>type E.

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Macroscopically, the mineral composition and rock structure control the characteristics of the

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pore-throat structure and further determine the mobility of oil.41–43 The casting thin section

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observations show that the higher the quartz clastic content is, the lower the matrix and plastic

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rock fragment contents are, and the stronger the compaction resistance of a rock is, the larger the

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sizes of the throats and primary pores preserved in the glutenite are(Figure 2). Smo shows a weak

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positive correlation with the quartz mineral content (Figure 16a), mainly because the quartz

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mineral content measured by XRD contained both the quartz clastics and quartz minerals in the

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rock fragments. Therefore, the type A pore-throat configuration will have a higher proportion only

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when the quartz clastic content is high. The Smo and feldspar mineral content exhibit distinct

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positive correlations. A high feldspar content will increase the compaction resistance of rocks and

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contribute to the occurrence of dissolution, which is further favorable for the development of type

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A, type B and type C pore-throat configurations. Smo has a negative correlation with the calcite

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mineral content. Calcite mainly occurs in the form of cement (Figures 2e and g), which leads to

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substantial reductions in the pore and throat sizes and leads to glutenite having a more developed

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type D pore-throat configuration. Smo has a certain negative correlation with the clay mineral

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content (especially chlorite, chlorite/smectite mixed layer and smectite). Clay minerals are often

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filled between particles in the form of cements or argillaceous matrix, forming type D and type E

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pore-throat configurations, which cause an extremely low Smo. Therefore, macroscopically, Smo

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notably increases as the quartz clastic content (non-quartz mineral content) and feldspar content

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increase and rapidly declines as the calcite and clay mineral contents increase.

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5. CONCLUSIONS

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Eighteen glutenite samples from the Baikouquan Formation and lower Wuerhe Formation in the

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Mahu Sag on the NW margin of the Junggar Basin, were collected to characterize the full-range

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PSDs and quantitatively study the distribution and controlling factors of the movable oil in

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glutenite. The main conclusions of this paper are as follows: (1) The observations of casting thin

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sections and SEM images indicated that the glutenite in the study area mainly had primary

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intergranular pores, intergranular dissolution pores, moldic pores, intragranular dissolution pores,

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and intercrystalline pores in clay. (2) The pores characterized by the T2 spectrum at Soir and LTNA

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are mainly intercrystalline pores in clay, and the pores exhibit an extremely good similarity in

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morphology and magnitude. By comparing the T2 spectrum at Soir and DFT PSD, a novel method

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of calculating the full-range PSD was proposed. According to the morphological characteristics of

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the T2 spectra at So, the glutenite samples can be divided into four types (i.e., type- I, type- II, type-

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III and type- IV). From type- I to type- IV, the proportion of micron-sized pores gradually

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decreases, which is consistent with the change in the areal porosity derived from the casting thin

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sections. (3) The Smo of the 18 glutenite samples is distributed in the range of 14.23-51.25%. The

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mobility of the oil in glutenite depends on the pore-throat configuration. The higher the proportions

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of type A, type B, and type C pore-throat configurations are, the better the mobility of oil in the

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glutenite. When glutenite has high quartz clastic and feldspar mineral contents and low calcite and

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clay mineral contents, glutenite exhibits more type A, type B and type C pore-throat

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configurations. Otherwise, the type D and type E pore-throat configurations are more developed

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in glutenite.

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AUTHOR INFORMATION

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Corresponding Author

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* S., Lu. E-mail: [email protected]

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Author Contributions

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Weichao Tian performed the NMR experiments and wrote the main manuscript. Shuangfang

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Lu defined the statement of problem and provided the main idea. Wenbiao Huang and Yang Gao

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provided assistance with data interpretation. Shuping Wang and Jinbu Li processed the data and

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plotted the figures. Weiming Wang supported the experimental funding. Jianpeng Xu and

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Zhuochen Zhan performed the LTNA experiments. All authors reviewed the manuscript.

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Notes

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The authors declare no competing financial interest.

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ACKNOWLEDGMENT

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This study was financially supported by the National Natural Science Foundation (41672125),

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the National Science and Technology Major Project (2017ZX05070-001), and the Fundamental

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Research Funds for the Central Universities (18CX06033A). The first author would like to

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acknowledge the China Scholarship Council (CSC) for the financial support of his living expenses

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at the Texas A&M University as a visiting Ph.D. student.

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Zhi, D.; Tang, Y.; Zheng, M.; Guo, W.; Wu, T.; Zou, Z. Discovery, Distribution and Exploration Practice of Large Oil Provinces of Above⁃source Conglomerate in Mahu Sag. Xingjiang Pet. Geol. 2018, 39 (1), 1–8.

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Fan q. Study on Pore Structure of Tight Glutenite Reservoir, Southwest Petroleum University, 2016.

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FIGURES

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Figure 1. Location of the study area and lithological profile of typical wells.

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Figure 2. Main pore types of glutenite in casting thin sections (Q, quartz; F, feldspar; R, rock

3

fragment; C, carbonate cementation; red arrow, primary intergranular pore/intergranular

4

dissolution pore; yellow arrow, intragranular dissolution pore; and black arrow, moldic pore).

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1 2

Figure 3. Main types of pores observed under SEM and their characteristics. a. Intragranular

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pores in quartz; b. intragranular dissolution pores in feldspar and clay minerals filled between the

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particles; c. intercrystalline pores in clay and intragranular dissolution pores in quartz; d.

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intragranular dissolution pores in feldspar, which are partially filled by flaky clay minerals; e.

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intragranular dissolution pores in feldspar filled with clay minerals; f. intercrystalline pores in

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clay, and clay minerals fully filling the intergranular pores; g. intragranular dissolved pores in

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feldspar and intercrystalline pores in clay (both are at the nanometer scale); and h. intragranular

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dissolution pores in quartz.

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Figure 4. N2 adsorption/desorption isotherms of the glutenite samples.

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1 2

Figure 5. Correlations between the pore volume and SSA obtained from LTNA and the mineral

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compositions of the glutenite samples

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Figure 6. Comparison of the PSDs calculated by the BJH model and DFT model using the

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adsorption and desorption branches of the LTNA experiments.

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1 2

Figure 7. PSDs calculated by the DFT model of the glutenite samples.

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Figure 8. NMR T2 spectra at So and at Soir for the glutenite samples.

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1 2

Figure 9. T2c calculated by the NMR T2 spectra at So and Soir of sample 1#.

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Figure 10. Comparison of the PSDs calculated by the DFT model and NMR T2 spectra at Soir in

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the glutenite samples.

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1 2

Figure 11. The full-range PSDs of all glutenite samples.

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Figure 12. Occurrence characteristics of the movable oil in the different types of glutenite

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reservoirs.

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1 2

Figure 13. The relationship between the movable oil volume and the cumulative mercury

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volume controlled by throats larger than a certain throat.

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Figure 14. Schematic diagram of the five main types of pore-throat configurations developed in

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glutenite.

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1 2

Figure 15. Relationships between the distribution of movable oil, the full-range PSD and pore-

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throat distributions in the typical glutenite samples.

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Figure 16. Relationship between the movable oil saturation and mineral composition in the

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glutenite samples.

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TABLES

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Table 1. Lithology and Main Mineral Contents of the Glutenite Samples Sample No.

Lithology

Formation

Q /%

F /%

C /%

CM /%

K /%

I /%

Ch /%

S /%

Chlorite/smectite mixed layer /%

Gravel-bearing Baikouquan 53.2 40 0 6.8 1.088 2.244 2.448 0 0.544 sandstone 2 M139 Conglomerate Baikouquan 38.4 46.3 5.1 10.3 0.412 4.635 2.575 2.678 0 Gravel-bearing 3 M601 Baikouquan 41.9 45.3 1.3 11.4 2.280 1.368 4.446 0 2.166 sandstone 4 M603 Sandstone Baikouquan 45.5 45.6 0.7 8.2 0.656 6.068 0.984 0 0.328 5 M603 Glutenite Baikouquan 38.5 47.3 0 14.3 3.146 3.432 5.148 0 1.144 6 M136 Glutenite Baikouquan 51.6 32 4.6 11.7 0.234 9.126 1.521 0 0.819 7 X723 Conglomerate Baikouquan 49.7 41.3 3.6 5.4 0.432 1.890 1.998 0 0.810 8 X723 Conglomerate Baikouquan 40.9 47.5 6.9 4.7 1.598 1.175 1.269 0.658 0 9 M211 Glutenite Wuerhe 49.8 35 0.3 14.9 1.937 0 3.725 9.238 0 10 M604 Conglomerate Baikouquan 44.7 41.8 1.7 11.8 2.124 1.534 4.838 0 2.006 11 M152 Sandstone Baikouquan 25.0 37.3 34.1 3.5 1.295 0 1.225 0 0 12 M154 Conglomerate Baikouquan 48.1 41.4 0.5 10.0 1.300 2.900 4.100 0 1.400 Gravel-bearing 13 M154 Baikouquan 31.9 32.3 30.1 4.4 0.748 0.836 1.980 0 0.616 sandstone 14 M154 Conglomerate Baikouquan 62.3 18.7 0 19.1 1.719 4.775 6.685 2.101 3.820 Gravel-bearing 15 M136 Baikouquan 46.3 43.7 0 10.0 0.600 2.300 3.400 1.300 2.400 sandstone 16 M139 Glutenite Baikouquan 35.7 52.8 3.3 8.2 0.328 4.346 2.706 0.082 0.574 17 X723 Conglomerate Baikouquan 44.2 41.9 4.3 9.6 1.152 2.976 3.648 0 1.344 18 M218 Sandstone Wuerhe 44.0 28.6 0 25.2 0.756 2.268 10.584 11.592 0 Note: Q is quartz, F is feldspar, C is calcite, CM is clay mineral, K is kaolinite, I is illite, Ch is chlorite, and S is smectite. 1

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Well

Page 44 of 45

M139

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Table 2. Petro-physical Properties and Key Parameters for the NMR and LTNA Experiments of

2

the Glutenite Samples

Physical properties Sample no.

LTNA

Porosity Permeability

NMR

Pore SSA /m2·g-1

T2c /ms

Smo /%

C /μm·s-1

0.02462

4.3057

0.438

51.25

112.01

1.81

0.01044

2.2982

3.747

43.73

74.43

14.50

6.48

0.01288

3.8639

2.225

41.89

75.00

4

11.08

3.21

0.01167

4.7043

2.201

42.69

31.48

5

6.74

3.50

0.00865

5.8424

5.718

40.30

39.56

6

13.86

5.89

0.01452

2.8191

1.861

40.06

94.72

7

9.30

13.48

0.01121

2.6432

9.739

30.83

36.28

8

8.34

2.50

0.01188

4.4123

7.401

29.20

42.68

9

10.47

3.93

0.01010

5.7785

12.993

18.09

106.91

10

8.89

4.66

0.01568

7.0315

2.161

27.23

48.32

11

3.74

1.67

0.00580

3.0151

2.501

20.15

40.09

12

11.29

4.63

0.01498

3.2803

1.551

32.80

88.34

13

6.56

6.17

0.00975

3.6834

1.068

20.03

67.25

14

7.21

6.98

0.01261

4.3501

7.370

18.81

33.57

15

11.17

8.71

0.01510

5.0969

2.518

28.45

57.52

16

12.48

4.64

0.01309

2.9006

0.951

41.78

103.36

17

8.22

0.92

0.01662

4.6173

1.620

21.66

67.47

18

11.92

5.84

0.01919

12.7804

3.157

14.23

125.81

/%

/mD

1

20.30

12.73

2

9.60

3

volume /ml·g-1

3

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