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Quantification of shale volume from borehole logs calibrated

by SEM analysis: A case study

Article  in  First Break · December 2010

DOI: 10.3997/1365-2397.2010027

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 40

How Log Interpreter Uses

SEM Data for Clay Volume Calculation
Mohammadhossein Mohammadlou and Mai Britt Mørk
Norwegian University of Science and Technology, NTNU, Trondheim,
Norway

1. Introduction
Guggenheim and Martin (1995), define the clay as a naturally occurring aluminum silicate
composed dominantly of fine-grained minerals. Several other definitions and classifications
based on the grain size, pore size, sedimentation, lattice, and other properties can be found
in the literature. The attention here is, however, not related to these definitions instead it is
about “how to calculate reservoir clay volume using Scanning Electron Microscope (SEM)
data“.
The rock that predominantly contains clay minerals is by definition called Shale. Shales are
mostly fine-grained clastic sedimentary rocks composed of clays and fragments of other
minerals i.e., carbonates and siliciclastics. Most of the clay minerals contain variable
amounts of water trapped in the mineral structure (Wiki definition). Clay volume is one of
the key parameters used to correct porosity and water saturation for the effects of clay
bound water in petrophysical evaluation (Crain, 2000).
A problematic aspect of evaluating hydrocarbon bearing reservoirs is to accurately model
the effects of clay and shale components on reservoir properties. Clay minerals and other
sedimentary materials as detrital shale components in the form of shale lamina, structural
clasts and dispersed shale matrix can be deposited in the sedimentary rocks. Clay minerals
are also commonly present as diagenetic clays, including pore-filling clays, pore-lining clays
and pore-bridging clays (Wilson and Pittman 1977).
Accurate quantification of the clay content, distribution and clay type in the reservoir rock
using core and wireline log data is rather complicated by a number of factors including: rock
heterogeneity, mud filtrate invasion and fluid contamination, alteration of clay
microstructure and wettability by mud invasion. On the other hand, a number of geological
and petrophysical methods have been developed to run the clay volume calculation.
Traditionally, a log interpreter i.e., petrophysicist, uses wireline log data including clay
indicator logs of gamma rays and spectral gamma rays in combination with other porosity
and resistivity logs to estimate reservoir clay volume. Integrated analyses of these logs
together with geological information are generally used for clay volume calculation. Clay
volume in homogeneous reservoir rocks can be estimated by conventional methods
however, a mixture of clay minerals, quartz, and calcite notably complicates the
interpretation of wireline log data. Rock heterogeneity influences the resistivity logs and

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820 Scanning Electron Microscopy

thereby water saturation as well. The focus here, however, is to discuss the use of SEM data
in combination with wireline logs to calculate reservoir clay volume.

2. Conventional shale volume calculation

Generally, porosity logging tools (neutron, density and sonic) display higher porosity
measurements in clay-rich rocks, whereas much of the porosity is neither effective for
hydrocarbon accumulation nor for hydrocarbons transmission through the rock. The shale
porosity has to be removed from the total porosity to obtain effective reservoir porosity. The
clay correction is therefore an essential step to carry out before estimating reservoir porosity
and saturation. Figure 1 displays the gamma-ray, spectral gamma-ray, and calculated clay
volume from these logs for a reservoir in the offshore Norwegian Barents Sea. Presence of
siliciclastic fines and diagenetic minerals (e.g. dolomite) within carbonate breccias has
resulted in a heterogeneous carbonate reservoir in the prospect area. Interactive
Petrophysics (IP) software was used for wireline log interpretation and petrophysical
analysis of the well.
Carbonate rocks, depending on the diagenesis and sedimentary environment, are generally
uranium-rich compared to siliciclastic rocks (Luczaj and Goldstein, 2000). A large amount of
uranium may precipitate during and after carbonate rock deposition. The process of
uranium precipitation is more abundant in the dolomitic sediments. The easy solution to
distinguish the uranium-rich from non-uranium rocks is to compare the two most well
known logs of natural gamma ray spectrometry (NGS) against natural gamma ray log (GR).
Natural gamma-ray (NGS) spectrometry allows estimation of the elemental concentrations
of potassium (K), uranium (U), and thorium (Th), which can be used to interpret sediment
composition, clay volume, and diagenesis.
Comparison of these logs in Figure 1 shows uranium-rich carbonate rocks in zones 2 and 3
compared to the more silica-rich intervals of zone 5. The higher uranium content originates
from uranium-rich organic matter in the reservoir rock. To calculate the shale volume of the
reservoir, the spectral gamma-ray log is used. It is also used to verify the calculated shale
volume from the gamma-ray log. In Figure 2, track numbers 4, 5, and 6 show the results of
the clay volumes for all reservoir sections in this well. The results are shown for potassium,
thorium and corrected gamma-ray logs respectively. The shale and clean (sand) lines are
drawn on the potassium, thorium, and corrected gamma-ray logs to estimate the bounding
values for zero and 100% shale volume. The bounding values to the corrected gamma-ray
response are assumed to be 25 API for zero shale volume and 85 API for 100% shale volume.
(Crain Petrophysical Handbook). According to the results in figure 2, discrepancy of the
results is considerable. The higher uncertainty in clay volume calculation impacts more
effectively the reservoir porosity and saturation estimation afterward.

3. NMR log application for shale volume calculation

The NMR log T2 distribution and its characteristics are dependent on the fluid content and
pore properties of the formation, and independent of mineral composition. It is by default
used for pore size distribution, capillary bound water and free fluid estimation. Basically,
modern NMR tools determine the fluid content in the pore space near the wellbore in the
order of few inches into the formation. They measure the total rock porosity regardless of
the pore fluid type (Dunn et al., 1998). The two T2 distributions, one from the fully polarized

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How Log Interpreter Uses SEM Data for Clay Volume Calculation 821

echo train and one from the partially polarized echo train, are merged together to build a T2
distribution from 0.3 ms to over 3000 ms for estimating the total porosity. In other words,
the sum of the volume fractions occupied by water, oil, and gas will be the total NMR
porosity. Traditional NMR tools miss the very fast T2 decay times; however, in modern tools
the T2 spectra include all types and sizes of pores and cracks (Coates et al., 1999).

Fig. 1. Well log data, reservoir zonation and lithology.

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822 Scanning Electron Microscopy

Fig. 2. Shale volume calculation from different methods: track-4 shale volume from
potassium log; track-5 shale volume from thorium log; track-6 shale volume from uranium-
corrected gamma-ray; track-7 shale volume from NMR log.

The NMR T2 distribution displays a distinct peak at small relaxation times, proving the
existence of clay minerals in the logged intervals. To categorize the contribution to porosity
from clay, a T2 cut-off value for clay-bound water is applied to the T2 distribution over the
reservoir section. Morriss et al. (1997) proposed a T2 clay-bound water cut-off of 3 ms by
studying 45 siliciclastic reservoirs. In a supplementary study by Prammer et al. (1996)
different T2 cut-off values were found for particular clay types at shorter decay times.
Knowing the clay type and implementing an appropriate T2 cut-off value, more accurate

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How Log Interpreter Uses SEM Data for Clay Volume Calculation 823

determination of clay-bound water volume is possible.The clay-bound water T2 cut-off and

clay type/shale volume estimation are important parameters in reservoir characterization.
The shale volume estimation is more complicated when the rock is composed of a mixture
of clay minerals and tiny fragments of other minerals. Greater amounts of fragments of non-
clay minerals increase the uncertainty of obtaining an accurate clay bound T2 cut-off value
for clay-bound water (Chitale et al., 1999). Although estimation of the T2 cut-off has been
discussed by many authors, there is still uncertainty in the optimum choice for the value.
With reference to the work of Matteson et al. (2000), the standard relaxation time of 3.3 ms is
used, which is appropriate where the clay type is not kaolinite.
The calculated shale volumes from gamma-ray, spectral gamma-ray (thorium and
potassium only), and NMR logs (Figure 7, track 4,5,6 and 7)) show that the calculated
volumes are not identical from these methods. Depending upon the chosen gamma-ray and
spectral gamma-ray values for the clean and shaly rock samples, the results for the shale
volume can differ significantly with different methods. The results from the spectral
gamma-ray log in tracks 4 and 5 are in good agreement within the whole reservoir section
except in zone 5. The uranium-corrected gamma-ray log, however, shows shale-free
reservoir except in zone 5 and parts of zones 2 and 4. To estimate shale volume from the
NMR log, representative clayey intervals (100% clay volume) and the amount of clay-bound
water in those intervals estimated from the NMR log are classified as references for
particular clay types in the well. The amount of clay-bound water estimated from the NMR
log response at any other point in the well is compared to that in the selected reference clay
in order to estimate the shale volume at that point. There may be errors in this estimate if the
selected reference clay was inappropriate. The estimated shale volume from the NMR log is
significantly less than that from the gamma-ray log indicators (track 6, Figure 2), presum-
ably due to the errors in conversion of clay-bound water to the shale volume.
A clear response to the presence of clay in the T2 distribution is seen right at the top of
Figure 2 in zone 1, the top seal of marine claystones. However, assuming that the top shale
seal is totally composed of clay minerals, the NMR estimated shale volume is also not
accurate within this interval. Selection of too low a T2 cut-off for clay-bound water or too
rapid a decay of the clay-bound water could explain the errors. In addition to the clays,
viscose hydrocarbons (tar) relax at much shorter relaxation times than the clay-bound water
T2 cut-offs. The NMR log interpretation can be more complicated where both clay and tar-
mats are present in the reservoir rock. Retrieved fluid samples from the wireline formation
tester and recovered hydrocarbons from core material obtained from the studied well have
not shown any tar in this reservoir. Overall, zones 4 and 5 of the reservoir show
uncorrelated results compared to the rest of the well. Assuming a formation rich in
potassium minerals coupled with high gamma-ray response, the rock type could be either
shale, a mixture of shale and other potassium-bearing rocks, or other rock types rich in
radioactive minerals.
To identify the clay minerals and potassium sources of zones 1 and 5, the thorium–
potassium reference cross-plot of Schlumberger (1985) and corresponding cross-plot of the
well data are shown in Figure 3. According to these plots, potassium sources in zone 5 are
glauconitic or feldspathic sandstone together with illite and mica, whereas the clay minerals
of zone 1 are mixed-layer clay and/or illite. The result gives valuable information about the
source of the clays but it could not provide a volumetric response for the shale volume of

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824 Scanning Electron Microscopy

the rock. Further calibration of the logs and petrographical analysis of the rock samples are
necessary to quantify the reservoir shale volume.

Fig. 3. (a) Schlumberger reference crossplot of thorium/potassium; and (b) corresponding

crossplots for zones 1 and 5 to identify the clay types.

4. Scanning electron microscope (SEM) analyses

To identify the rock mineralogy and quantify the mineral volume fractions, SEM analysis
was carried out on the selected reservoir samples. Because of inconsistencies in the amount

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How Log Interpreter Uses SEM Data for Clay Volume Calculation 825

of calculated shale volume in zone 5 (Figure 7), most of the samples are chosen from this
zone. Backscattered electron imaging of polished thin sections is used to map mineral
distributions in a grey scale with intensity related to the average atomic number of the
minerals (Reed, 2005). Mineral identification was supplemented by energy dispersive
spectroscopy analysis, and X-ray mapping of element distributions was done to further
identify and quantify the mineral distributions. A backscattered electron image of a sample
of sandy carbonate rock in zone 5 is shown in Figure 4a. To estimate the proportion of one
particular mineral, the image is processed and one component, e.g., potassium feldspar, is
characterized (Figure 4b). The energy dispersive spectrum of potassium feldspars (black in
Figure 4b) is shown in Figure 4c. The proportion of elements (K, Si, Al, and O) in this figure
verify that the selected grains are potassium feldspar. Energy dispersive spectroscopy is
used to recognize every selected mineral in a thin section sample by its elemental
composition, but X-ray mapping of the section provides a map of each element.

Fig. 4. Details of scanning electron microscope imaging of one sample from zone 5. (a)
Backscattered electron image. (b) Processed image for the characterization of potassium
feldspar, showing up as black. (c) Energy dispersive spectrum of a selected clay mineral to
identify it.

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826 Scanning Electron Microscopy

The X-ray elemental mapping of the selected thin section in Figure 4 also confirms the
abundance of potassium feldspar in this section, but not clays. Figure 5 shows the elemental
map of Na, O, K, C, S, Si, Mg, Ca, Ti, Al, and Fe for the selected sample in Figure 4. The
volume fraction of potassium feldspar from this analysis is calculated as 16–23 %. The map
of feldspar content in other thin sections in zone 5 shows that the potassium volume
increases toward the bottom of the formation. A lesser amount of illite/mica is estimated in
comparison with the estimated volume from the conventional method. The clay types and
volume estimations from SEM analysis are also consistent with the Schlumberger crossplot.
The results show that the clay minerals of the sample from zone 5 are illite and mica with a
volume fraction of 15–21 % (Figure 6).

Fig. 5. The backscattered electron image of the thin sample section in Figure 4 with details of
elemental mapping for Na, O, K, C, S, Si, Mg, Ca, Ti, Al, and Fe.

A few thin sections cannot be representative of the whole reservoir section because they
have been selected from a heterogeneous interval. However, SEM analysis together with the
NMR and spectral gamma-ray logs facilitates shale volume calculation. SEM data provide
shale volume and clay types at the selected depths which can be correlated with the spectral
gamma-ray log to extract the shale and potassium feldspar volume at those depths.
Comparison of these results with the NMR-estimated shale volumes shows that the NMR
log underestimates the shale volume. In contrast, the spectral gamma-ray log overestimates
the shale volume.
The potassium readings on the spectral gamma-ray log in zone 5 and part of zone 2 come
from a mixture of clay minerals and potassium feldspar. As discussed by Ellis and Singer
(2008) with reference to the gamma-ray response in shaly rocks, the correlation between clay
minerals and thorium is largest, because of the potassium association with other
components of the shale, such as feldspars. They also established an empirical equation for

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How Log Interpreter Uses SEM Data for Clay Volume Calculation 827

the total gamma-ray response based on the three radioactive components of the spectral
gamma-ray signal, however potassium-rich shaly sand could be inaccurately interpreted as
shale by this equation. Therefore, the contribution of potassium feldspar has to be removed
from the spectral gamma-ray log to estimate an accurate shale volume in the selected
samples. Using Ellis and Singer’s (2008) approximation and estimated potassium values
from the SEM samples, the corrected gamma-ray log values were calibrated for selected
samples and subsequent shale volumes. The new potassium-corrected log was then used
with the thorium log to estimate a revised shale volume in zone 5. Figure 7 shows the
calculated shale volumes from all the above-mentioned methods. The calculated clay
volumes using potassium, thorium, and uranium-corrected gamma-ray (CGR) and the
integration of SEM, CGR and NMR logs are shown in Figure 7 from tracks 4 to 7,
respectively. In track 7, the final corrected shale volume has been plotted for the whole
interval.

Fig. 6. Backscattered electron image of the sample section in zone 5 showing illite, mica, and
feldspar.

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828 Scanning Electron Microscopy

Fig. 7. Shale volume calculation by using HCGR, thorium-potassium ratio, thorium, and
integration of SEM, thorium, and potassium.

5. Summary
Although the gamma-ray log has traditionally been used for the analysis of shaly
formations, the shale volume estimation from this measurement is, to a greater or lesser
extent, inaccurate. The GR log responds to the natural-gamma radiation from the formation.

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How Log Interpreter Uses SEM Data for Clay Volume Calculation 829

The spectral gamma-ray log works on the same principle, except that the gamma rays are
assigned to three different energy bins, showing the concentrations of K, U, and Th in the
formation. Generally, carbonate rocks show higher uranium measurements on the spectral
gamma-ray log because of the presence of organic matter. Uranium is, therefore, removed
prior to the use in clay volume calculation.The sources of potassium also have to be
distinguished because potassium is present in shaly and non-shaly rocks. In this study, the
NMR log is used as an easy tool to check the reliability of the shale volume calculation from
gamma-ray and spectral gamma-ray logs. Inconsistency between the shale volumes
estimated from these methods is significant in the lowermost reservoir section. To solve the
problem, SEM analysis was done to identify the mineralogy and mineral volume fractions.
Backscattered electron images and X-ray mapping of selected samples show a noticeable
contribution of potassium feldspar in zone 5. The potassium feldspar content of the rock
influences both the gamma-ray and spectral gamma-ray logs and thus the shale volume
calculation. The spectral gamma-ray log of potassium was therefore corrected on the basis of
SEM information. Subsequently, the SEM information was used as a reference point for the
calibration of the spectral gamma-ray log to estimate the shale volume. The uniformity of
the spectral gamma-ray logs within zone 5 used for calibration over the entire zone 5. The
NMR log was also used to verify the calculation to some extent. The volume of potassium
feldspar was then removed from the total potassium reading in the spectral gamma-ray log
to obtain the actual shale volume of the rock. The results show a considerable reduction in
the estimated shale volume of the reservoir rock. Overestimation of shale volume has a
direct impact on the reservoir evaluation by causing underestimation of the effective
porosity and, consequently, hydrocarbon volume.

6. Acknowledgements
Authors thank Norwegian University of Science and Technology and Statoil for support and
access to petrophysical data, and Stephen Lippard for his advice on the manuscript.

7. Nomenclature
Name Description (unit)
BS Bit size (inch)
CBW Clay-bound water (decimal fraction)
Depth Depth from rotary table (m)
Dt Sonic transit time (μs/ft-1)
HCAL Caliper log (inch)
HCGR Compensated gamma-ray (API)
HCGR_SHALE Shale volume from HCGR log (decimal fraction)
HFK Spectral gamma-ray log potassium (%)
HTHO Spectral gamma-ray log thorium (ppm)
HTHO_SHALE Shale volume from thorium log (decimal fraction)
HURA Spectral gamma-ray log uranium (ppm)
NMR_SHALE Shale volume from NMR log (decimal fraction)
nmrT2cutoff T2 cut-off (ms)
NPHIC Neutron log (corrected) (decimal fraction)

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830 Scanning Electron Microscopy

PHIE Effective porosity (decimal fraction)

PHIT Total porosity (decimal fraction)
RHOC Density log (corrected) (g cm-3)
Vanhydrite Anhydrite volume (decimal fraction)
VDol Dolomite volume (decimal fraction)
VLime Limestone volume (decimal fraction)
VSand Sandstone volume (decimal fraction)
VWL Wey clay volume (decimal fraction)

8. References
Chitale, D.V. Day, P. I. and Coates, G. R. [1999] Petrophysical implications of laboratory
NMR and petrographical investigation on a shaly sand core. SPE Annual Technical
Conference and Exhibition, Houston, Texas.
Coates, G.R. Xiao, L. and Prammer, M.G. [1999] NMR logging principles and applications.
Halliburton Energy Services Publication H02308, USA, 253 pp.
Darling, T. [2005] Well logging and formation evaluation. Gulf professional publishing,
Oxford OX2 8DP, UK, 302 pp.
Dunn, K. J. Bergman, D. J. LaTorraca, G. A. Stonard, S. W. and Crowe, M. B. [1998] A
method for inverting NMR data sets with different signal to noise ratios. 39th
Annual Logging Symposium of SPWLA, Keystone, USA.
Ellis, D, V. and Singer, J. M. [2008] Well logging for earth scientists. Springer, 2nd edition
Netherlands, 698 pp.
Guggenheim, S. and Martin RT [1995] Definition of clay minerals. Joint report of the AIPEA
nomenclature and CMS nomenclature committees. Clays Clay Miner 43:255-256.
Luczaj, J. A. and Goldstein R. H. [2000] Diagenesis of the lower Permian Krider Member,
southwest Kansas, U.S.A.: Fluid-inclusion, U-Pb, and fission-track evidence for reflux
dolomitization during latest Permian time. Journal of Sedimentary Research, 70, 762-
773.
Matteson, A. Tomanic, J.P. Herron, M.M. Allen, D.F. and Kenyon, W.E. [2000] NMR
relaxation of clay/brine mixtures. SPE Reservoir Eval. & Eng. 3 (5), 408-413.
Mohammadlou, M., Mork M. B., Langeland, H., [2010] Quantification of shale volume from
borehole logs calibrated by SEM analysis: a case study. First break, 28, 21-29.
Reed, S. J. B. [2005] Electron microscope analysis and scanning electron microscopy in
geology. Cambridge University Press, UK, 2nd Edition, 232 pp.
Ruppel, S. C. [1992] Styles of deposition and diagenesis in Leonardian carbonate reservoirs
in West Texas. Annual exhibition and technical conference, SPE 24691.
Schlumberger [1985] Log interpretation charts. Schlumberger, New York, USA, 207 pp.
Schlumberger [1989] Schlumberger log principles and applications. Schlumberger, Wireline
& Testing, Texas, USA, 230 pp.
Straley, C. et al. [1994] Core Analysis by Low Field NMR. SCA-9404 presented at the 1994
Intl. Symposium of the Soc. of Core Analysts, Stavanger, Norway.
Prammer, M.G. et al. [1996] Measurements of clay-bound water and total porosity by
magnetic resonance. The Log Analyst. 37(6), 61.
Tiab, D. and Donaldson E. C. [2004] Petrophysics, theory and practice of measuring
reservoir rock and fluid transport properties. Gulf professional publishing, 2nd
edition, Oxford OX2 8DP, UK, 926 pp.

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 Scanning Electron Microscopy
Edited by Dr. Viacheslav Kazmiruk

ISBN 978-953-51-0092-8
Hard cover, 830 pages
Publisher InTech
Published online 09, March, 2012
Published in print edition March, 2012

Today, an individual would be hard-pressed to find any science field that does not employ methods and
instruments based on the use of fine focused electron and ion beams. Well instrumented and supplemented
with advanced methods and techniques, SEMs provide possibilities not only of surface imaging but quantitative
measurement of object topologies, local electrophysical characteristics of semiconductor structures and
performing elemental analysis. Moreover, a fine focused e-beam is widely used for the creation of micro and
nanostructures. The book's approach covers both theoretical and practical issues related to scanning electron
microscopy. The book has 41 chapters, divided into six sections: Instrumentation, Methodology, Biology,
Medicine, Material Science, Nanostructured Materials for Electronic Industry, Thin Films, Membranes,
Ceramic, Geoscience, and Mineralogy. Each chapter, written by different authors, is a complete work which
presupposes that readers have some background knowledge on the subject.

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Volume Calculation, Scanning Electron Microscopy, Dr. Viacheslav Kazmiruk (Ed.), ISBN: 978-953-51-0092-8,
InTech, Available from: http://www.intechopen.com/books/scanning-electron-microscopy/how-log-interpreter-
uses-sem-data-to-estimate-a-reservoir-clay-volume-

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