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1 JAMSTEC Rep. Res. Dev., Volume 2, March 215, 41 5 doi: /jamstecr.2.XX hatakedak@mwj.co.jp 41

2 Experimental examination for electrical resistivity measurement using the alternative current impedance method doi: /jamstecr.2.XX Experimental examination for electrical resistivity measurement using the alternative current impedance method Kentaro Hatakeda 1, Weiren Lin 2, Tadanori Goto 3, Takehiro Hirose 2, Wataru Tanikawa 2, Yohei Hamada 2, and Osamu Tadai 1 Laboratory experiment of electrical resistivity measurement using an alternative current (AC) impedance method is important to interpret the electrical survey and logging data, and to understand the electrical properties of rocks and sediments. This study investigated the accuracy and applicability of the AC impedance method by measuring resistors of known resistance (Experiment 1), electrolyte solutions of known resistivity (Experiment 2), and rocks and deep-sea core samples (Experiment 3). We confirmed that the accuracy of the measurement system was the same as that provided by manufacture in the Experiment 1. Two-electrode method was used for the Experiment 2, and the results showed that resistivity and phase angle increased with lowering of frequency and decreasing of the sample resistivity. The resistivity data was more accurate when the phase angle was close to zero. In the Experiment 3, we examined the way to prevent overestimation and underestimation of resistivity by drying and wetting of the sample surface, respectively, and wrapping a sample with parafilm was the most effective. In addition, we measured the samples of various porosity using two- and four-electrode methods. Four-electrode method had an advantage that is applicable to wide range of frequency (1 2 to 1 5 Hz) because of its less influence of electrode polarization at low frequency, but reliable data ware also obtained using two-electrode method by measuring highly resistive samples or measuring with high frequency. Our data showed both twoand four-electrode methods were applicable to samples of various porosity (.3 to 67%). Keywords : Electrical resistivity, alternative current impedance, two-electrode method, four-electrode method Received 6 October 214 ; Revised 11 December 214 ; Accepted 11 December Marine Works Japan Ltd. 2 Kochi Institute for Core Sample Research, Japan Agency for Marine-Earth Science and Technology (JAMSTEC) 3 Department of Civil and Earth Resources Engineering, Graduate School of Engineering, Kyoto University Corresponding author: Kentaro Hatakeda Marine Works Japan Ltd. Monobe-otsu 2, Nankoku, Kochi , JAPAN Tel hatakedak@mwj.co.jp Copyright by Japan Agency for Marine-Earth Science and Technology 42 JAMSTEC Rep. Res. Dev., Volume 2, March 215, 41 5

K. Hatakeda et al. Archie 1942 Patnode and Wyllie 195 Boyce 1968 Bussian 1983 1994 1996 1996 Roberts and Lin 1997 2 Kahraman and Alber 26 Roberts and Lin 1997 Henry et al.

3 K. Hatakeda et al. Archie 1942 Patnode and Wyllie 195 Boyce 1968 Bussian Roberts and Lin Kahraman and Alber 26 Roberts and Lin 1997 Henry et al. 23 Kahraman and Alber 26 Expedition 322 Scientists 21 1kHz Collet and Katsube 1973 Klein and Santamarina Collet, Börner and Schön Agilent LCR 4263B 4 BNC Fig.1 1Hz 1kHz 1mΩ 1MΩ Z Fig Z = R + jx = Z θ (1) R = Z cos θ (2) X = Z sin θ (3) Z = R 2 + X 2 (4) θ = tan 1 (X/R) (5) Fig. 1. Resistivity measurement system (Agilent 4263B) 1. Agilent 4263B JAMSTEC Rep. Res. Dev., Volume 2, March 215,

Experimental examination for electrical resistivity measurement using the alternative current impedance method R Xj Z θ R LCR Z θ 6 ρ ρ = Z cos θ S/L (6) S L 1Ω 51.

4 Experimental examination for electrical resistivity measurement using the alternative current impedance method R Xj Z θ R LCR Z θ 6 ρ ρ = Z cos θ S/L (6) S L 1Ω 51.1Ω 1Ω 2Ω 1kΩ 9kΩ 5kΩ 1MΩ 1Hz 12Hz 1kHz 1kHz 1kHz KCl NaCl 1Hz 1kHz KCl NaCl Table1 KCl JIS K13:28 NaCl Carmichael 1982 Imaginary X Fig.3 JIS K ρ T = ρ t (1 α/1 (T t)) (7) ρ T T C ρ t t C α %/ C 2%/ C Table Theoretical resistivity of each solution NaCl Resistivity at 2 C concentration (Ω m) 35 g/l g/l g/l 1.73 KCl Resistivity at 25 C concentration (Ω m) 1 mol/l.9.1 mol/l mol/l 7.97 Z R Real Fig. 2. Principle of impedance 2. Fig. 3. Sample holder for solution JAMSTEC Rep. Res. Dev., Volume 2, March 215, 41 5

5 K. Hatakeda et al Table235 g/l NaCl Aji granite Belfast gabbro Rajasthan sandstone Berea sandstone 48 IODP Exp. 343 Wedge sediments Gray mudstone 24 Table 2. Samples used in this study. Deep-sea cores recovered from Hole C19E, IODP Exp. 343 (Wedge sediments: 1R-1, cm, 177 mbsf, and Gray mudstone: 5R-1, cm, 697 mbsf) were included (Lin et al., 214) 2. IODP Exp. 343 Hole C19E Wedge sediments 1R-1, cm, 177 mbsf Gray mudstone 5R-1, cm, 697 mbsf Lin et al. 214 Sample Diameter Length Grain density Porosity (mm) (mm) (g/cm 3 ) (%) Belfast gabbro Aji granite Rajasthan sandstone Berea sandstone Gray mudstone Wedge sediments g/L NaCl 1 Fig.4A 1994 Fig.4B 35 g/l NaCl 4 3kg 1 12Hz 1 Ω 5 kω.1% 1MΩ.2% Table3.1% 1Ω 1MΩ Electrode (A) 3 kg Sample Rubber plate Filter paper Rubber plate (B) 3 kg Sample Potential electrode Current electrode Fig. 4. Sample assemblies for (A) two-electrode and (B) fourelectrode methods 4. A B Table Result of the resistor measurement (n=1) n=1 Frequency 1 Ω 51.1 Ω 1 Ω 2 Ω Impedance Phase Impedance Phase Impedance Phase Impedance Phase (Ω) ( ) (Ω) ( ) (Ω) ( ) (Ω) ( ) 1 khz khz khz Hz Hz Frequency 1kΩ 9kΩ 5 kω 1 kω Impedance Phase Impedance Phase Impedance Phase Impedance Phase (kω) ( ) (kω) ( ) (kω) ( ) (kω) ( ) 1kHz khz khz Hz Hz JAMSTEC Rep. Res. Dev., Volume 2, March 215,

6 Experimental examination for electrical resistivity measurement using the alternative current impedance method KCl NaCl 1 Table4 Emmert et al., 211 Schwan 1966 Table 4. Frequency dependence of impedance and phase angle for KCl and NaCl solutions (n=1) 4. KCl NaCl n=1 KCl 1 mol/l.1 mol/l.1 mol/l Impedance Phase Impedance Phase Impedance Phase Frequency (Ω) ( ) (Ω) ( ) (Ω) ( ) 1 khz khz khz Hz NaCl 35 g/l 17.5 g/l 3.5 g/l Impedance Phase Impedance Phase Impedance Phase Frequency (Ω) ( ) (Ω) ( ) (Ω) ( ) 1 khz khz khz Hz Difference from the theoretical value (%) y = -.464x R² = Phase angle ( ) Fig. 5. Difference between the measured (1 khz) and theoretical resistivity compared with phase angle 5. 1kHz % Collet and Katsube 1973 Kalvøy et al. 211 Emmert et al. 211 Henry et al. 23 Kahraman and Alber 26 KCl NaCl Table1 1kHz 1 mol/l KCl mol/l KCl 6% 35 g/l NaCl % 17.5 g/l NaCl %.1 mol/l KCl.4 1.8% 3.5 g/l NaCl.5 1.5%.1 mol/l KCl.2 1.2% Fig.5, 6 1% ±1% Berea sandstone Rajasthan sandstone Aji granite 1 % 3 5A Table5B asu sisti ity y =.996x +.8 R² = 1. KCl solution NaCl solution o ti al sisti ity Fig. 6. Relation between the measured (1 khz) and theoretical resistivity 6. 1 khz 46 JAMSTEC Rep. Res. Dev., Volume 2, March 215, 41 5

7 K. Hatakeda et al. 1kHz 1kHz % 1994 Fig.7 1 > 1% Berea sandstone Rajasthan sandstone Gray mudstone Wedge sediments E+2 1.E+3 1.E+4 1.E E+2 1.E+3 1.E+4 1.E E E+2 1.E+3 1.E+4 1.E E+2 1.E+3 1.E+4 1.E E+2 1.E+3 1.E+4 1.E E+2 1.E+3 1.E+4 1.E Fig Table Comparison of frequency dependence of resistivity and phase angle between two electrode and four electrode methods Comparison of (A) water loss and (B) resistivity in the different sample surface conditions A 1 B Wrap (A) Water loss (%) (B) Resistivity (Ω m) Parafilm Closed container None Wrap Parafilm Closed container None ( min) None (1 min) Berea Sandstone Rajasthan sandstone Aji granite JAMSTEC Rep. Res. Dev., Volume 2, March 215,

8 Experimental examination for electrical resistivity measurement using the alternative current impedance method 2 KCl NaCl 1kHz < 1% 1Hz 1kHz 1kHz 1kHz Collet and Katsube 1973 Kahman and Alber 26 1kHz Hz Börner and Schön 1995 Fig.8 1 khz 1 khz ϕ ρ 8 r 2 =.97 ρ =.613 ϕ 1.12 (8) 1Ω 1MΩ.1% KCl NaCl Belfast gabbro Aji granite Rajasthan sandstone Berea sandstone ray dstone edge sedi ents Archie 1942 Boyce 1968 Bussian 1983 Worthington 1993 Kahman and Alber 26 Formation Factor Fractional porosity Fig. 8. Relation between resistivity and fractional porosity JAMSTEC Rep. Res. Dev., Volume 2, March 215, 41 5

9 K. Hatakeda et al. 1kHz % Archie, G.E. (1942), The electrical resistivity log as an aid in determining some reservoir characteristics, Petroleum Transactions of AIME, 146, Börner, F.D., and Schön, J. H. (1995), Low frequency complex conductivity measurements of microcrack properties, Surveys in Geophysics, 16, Boyce, R.E. (1968), Electrical resistivity of modern marine sediments from the Bering Sea, J. Geophys. Res., 73, Collet, L.S. (1959), Laboratory investigation of overvoltage, in Overvoltage research and geophysical applications, Ed. Wait, J.R, Pergamon Press, 5 6. Collett, L.S., and Katsube, T.J. (1973), Electrical parameters of rocks in developing geophysical techniques, Geophys, 38, Bussian, A..E. (1983), Electrical conductance in a porous medium, Geophysics, 48, Carmichael, R.S. (1982), Handbook of Physical Property of Rocks, CRC Press, Boca Raton, vol. 1. Emmert, S., Wolf, M., Gulich, R., Krohns, S., Kastner, S., Lunkenheimer, P., and Loidl, A. (211), Electrode polarization effects in broadband dielectric spectroscopy, The European Physical Journal B, 83, Expedition 322 Scientists (21), Methods, in Proc. IODP, 322, Eds. Saito, S., Underwood, M.B. et al., Tokyo, doi:1.224/iodp.proc , 652, Henry, P., Jouniaux, L., Screaton, E.J., Hunze, S., and Saffer, D.M. (23), Anisotropy of electric conductivity record of initial strain at the toe of the Nankai accretionary wedge, J. Geophys. Res., 18, , doi:1.129/22jb2287 Kahraman, S., and Alber, M. (26), Predicting the physicomechanical properties of rocks from electrical impedance spectroscopy measurements, Int. J. Rock Mech. Min. Sci., 43, Kalvøy, H., Johnsen, G.K., Martinsen, Ø.G., Grimnes, S. (211), New method for separation of electrode polarization impedance from measured tissue impedance, Open Biomed. Eng. J., 5, Klein, K., and Santamarina, J.C. (1997), Methods for broadband dielectric permittivity measurements (soil-water mixtures, 5 Hz to 1.3 GHz), Geotech. Test. J., 2, Lin, W., Fulton, P.M., Harris, R.N., Tadai, O., Matsubayashi, O., Tanikawa, W., Kinoshita, M., (214), Thermal conductivities, thermal diffusivities, and volumetric heat capacities of core samples obtained from the Japan Trench Fast Drilling Project (JFAST), Earth, Planets and Space, 66,. doi:1.1186/ , 56, , 27, K13 14pp. 213 K Patnode, G.E., and Wyllie, M.R.J. (195), The presence of conductive solids in reservoir rocks as a factor in electric log interpretation, Trans. A.I.M.E., 189, Roberts, J.J., and Lin, W. (1997), Electrical properties of partially saturated Topopah Spring tuff: Water distribution as a function of saturation, Water Resour. Res., 33, Schwan, H.P. (1966), Alternating current electrode polarization, Biophysik, 3, JAMSTEC Rep. Res. Dev., Volume 2, March 215,

10 Experimental examination for electrical resistivity measurement using the alternative current impedance method Worthington, P.F. (1993), The uses and abuses of the Archie equations, 1: The formation factor-porosity relationship, J. Appl. Geophys., 3, JAMSTEC Rep. Res. Dev., Volume 2, March 215, 41 5

Accuracy check of grading of XCT Report Accuracy check of grading and calibration of CT value on the micro-focus XCT system Tetsuro Hirono Masahiro Ni

JAMSTEC Rep. Res. Dev., Volume 8, November 2008, 29 36 X CTm/pixel X CT X CT. -. mol/l KI KI CT CT X CT CT ; - - +- -- hirono@ess.sci.osaka-u.ac.jp Accuracy check of grading of XCT Report Accuracy check