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Natural Gas Geoscience ›› 2020, Vol. 31 ›› Issue (9): 1271-1284.doi: 10.11764/j.issn.1672-1926.2020.04.021

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The effect of particle size on low pressure gas adsorption experiments for high-maturity shale

Teng-fei LI1(),Hui TIAN1(),Xian-ming XIAO2,Peng CHENG1,Xing WANG1,3,Yao-wen WU1,3,Zi-jin WU1,3   

  1. 1.Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China
    2.China University of Geosciences, Beijing 100083, China
    3.University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2020-02-25 Revised:2020-04-26 Online:2020-09-10 Published:2020-09-04
  • Contact: Hui TIAN E-mail:litengfei@gig.ac.cn;tianhui@gig.ac.cn

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Abstract:

To evaluate the effect of particle size on the determination of shale physical parameters and explore the suitable particle size range for such analysis, three samples with different TOC content from the Lower Cambrian Niutitang Formation in southeast Chongqing area were investigated. Combined with low pressure N2/CO2 adsorption experiments, organic petrology, laser Raman spectroscopy and XRD mineralogical results, the influence of crushing and sieving on the measurement of mineral composition, specific surface area and pore size distribution were discussed. The results are as follows:(1) Pores within organic matter and intergranular of clay minerals are the main types in shale samples, and the development of organic pores are heterogeneous;(2) The procedure of sieving can cause irregular differentiation to mineral composition of shale samples;(3) The results of low pressure N2 adsorption experiment indicate that when the particle size is less than 0.425 mm(>40 Mesh), smaller particle size can increase the specific surface area and obviously affect pore volume of mesopores and macropores; However, when the particle size is greater than 2 mm(<10 Mesh), further increase in particle size will significantly increase the experimental time; (4) Particle size has no distinct impact on the micropores in shales. Combining the experimental reliability and time efficiency as well as the heterogeneous nature of shale samples, particle sizes between 10-40 Mesh are recommended for the experimental analysis of shale physical parameters.

Key words: Shale gas, Particle size, Mineral composition, Low pressure N2 and CO2 adsorptionFoundation items:The China National Science Fund for Distinguished Young Scholars (Grant No. 41925014), The Joint Fund of National Natural Science Foundation of China (Grant No. U1810201).

CLC Number: 

  • TE122.2

Fig.1

Schematic diagram of sampling location（modified from Ref.[39]）"

Table 1

Basic geochemical characteristics of shale samples"

样品 编号层位eqRO/%TOC/%粒径 /目矿物组成/%
石英长石伊利石黄铁矿
JG-2-1?1n3.234.001~557.212.930-
JG-2-25~1044.611.244.2-
JG-2-310~2048.912.138.9-
JG-2-420~4049.811.239-
JG-2-540~6050.81039.2-
JG-2-660~8053.711.734.6-
JG-2-780~1004411.744.3-
JG-2-8<10050.110.939-
JG-8-2?1n3.169.025~10669.724.3-
JG-8-310~2062.69.626.21.6
JG-8-420~406010.929.1-
JG-8-540~6064.512.622.8-
JG-8-660~80649.526.5-
JG-8-780~100678.224.8-
JG-8-8<10059.110.230.7-
JG-11-1?1n3.337.371~5----
JG-11-25~10----
JG-11-310~20----
JG-11-420~40----
JG-11-540~60----
JG-11-660~80----
JG-11-780~100----
JG-11-8<100----

Fig.2

Raman spectrum of bitumen in shale samples"

Fig.3

Field emission scanning electron microscope (FE-SEM) images of shale samples"

Fig.4

Mineral composition of JG-2 and JG-8 series samples"

Fig.5

Low pressure N2 adsorption and desorption isotherms for samples with particle size between 20-40 mesh and the relationship between TOC and specific surface area"

Fig.6

Local low pressure N2 adsorption isotherms of samples with different particle sizes"

Table 2

Parameters of low pressure N2 adsorption experiment results"

样品编号TOC/%单点吸附总孔体积 /(cm3 /100 g)吸附实验时间 /hBET 比表面积 /（m2/g）
JG-2-14.003.1723.436.28
JG-2-23.2117.326.11
JG-2-33.2812.976.13
JG-2-43.3412.186.20
JG-2-53.6612.536.71
JG-2-63.8112.607.08
JG-2-73.9212.607.18
JG-2-84.3013.188.05
JG-8-29.023.1853.5328.85
JG-8-33.2438.1328.45
JG-8-43.4138.8329.02
JG-8-53.5638.2229.48
JG-8-63.9037.0330.51
JG-8-74.1436.0531.86
JG-8-84.9135.4832.70
JG-11-17.372.09113.1524.37
JG-11-22.2368.3324.70
JG-11-32.3345.9224.28
JG-11-42.4542.1724.57
JG-11-52.5539.8324.43
JG-11-62.8339.3725.21
JG-11-73.0339.4025.27
JG-11-83.8738.3826.43

Fig.7

Plots showing the relationships between particle size and BET specific surface area"

Fig.8

Plots showing the relationships between particle size and single point adsorption total pore volume of pores"

Fig.9

Pore volume distribution with pore size derived from the N2 adsorption branch of isotherms using BJH model"

Fig.10

The completion time of low pressure N2 adsorption experiment for shale samples with different particle sizes"

Fig.11

Low pressure CO2 adsorption isotherms for shale samples with different particle sizes"

Fig.12

Plots showing micropore volume derived from the CO2 adsorption isotherms for shale samples with different particle sizes"

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