Journal of Petroleum Science and Engineering 198 (2021) 108242

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Journal of Petroleum Science and Engineering

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Evaluating drilling fluid infiltration in porous media – Comparing NMR,

gravimetric, and X-ray CT scan methods
Badr S. Bageri a, Abdulrauf R. Adebayo b, *, Jaber Al Jaberi a, Shirish Patil a, Rahul B. Salin b
a
Department of Petroleum Engineering, King Fahd University of Petroleum & Minerals, Saudi Arabia
b
Center for Integrative Petroleum Research, King Fahd University of Petroleum & Minerals, Saudi Arabia

A R T I C L E I N F O A B S T R A C T

Keywords: The infiltration of drilling fluids into underground rocks during drilling can cause adverse effects such as un­
Filter cake derground fluid loss, formation damage, and borehole collapse. An effective filter cake formed by the drilling
Drilling fluid fluid on the borehole wall can minimize such adverse effects to a degree that is dependent on the characteristics
Mud
of the drilling fluid. For this reason, drilling fluids are routinely screened in the laboratory based on the sealing
CT scan
NMR
properties of their filter cakes. However, there appear not to be a universally adopted method for characterizing
Porosity filter cakes. This study utilizes a nuclear magnetic resonance (NMR) approach to characterize filter cakes and
then compares the result with some existing methods. Fluid loss tests were conducted to form filter cakes over
four consolidated sandstone and carbonate rock samples. NMR measurements were conducted pre and post filter
cake deposition. NMR measurements of filter cake porosity and infiltrated solids were compared with those from
conventional methods such as gravimetric and X-ray computer tomography (CT) measurements. The results
obtained from the three methods show significantly different values. To resolve this, cross correlations plots were
made between measurements obtained from the three methods and the measured cake thickness. NMR measured
porosity and infiltrated solids showed an excellent correlation with the measured cake thickness compared to the
other two methods. However, the porosity values from NMR is significantly lower than the values obtained from
the other methods. Through sensitivity analyses, we provide reasons why values from other methods are high
and not as representative as the NMR method. We also gave a detailed explanation why NMR method is more
accurate and useful compared to the other methods.

1. Introduction
Filter cake plays an important role in stabilizing boreholes during
drilling boreholes for water or oil and gas. During drilling operations,
drilling fluid (a mixture of clay and additives) is circulated downhole to
serve multiple purposes such as lubricating the drill bits, clean out
drilled cuttings, mechanical support for the wells, and suppress reservoir
fluid from gushing into the well (Afolabi, 2018; Caenn and Chillingar,
1996; Mao et al., 2020). To suppress reservoir fluids, the drilling fluid
(sometimes simply referred to as mud or drilling mud) is often circulated
at a bottom-hole pressure greater than the reservoir pressure. This
process is called overbalanced drilling. In such a drilling process, the
bottom-hole mud pressure forces some drilling mud particles and liquid
into the near wellbore rock matrix. A controlled penetration of the mud
particles around the wall of the well helps to build a filter cake layer
around the wellbore, which serves to prevent further penetration of mud
particles and liquid into the reservoir (Agwu and Akpabio, 2018; Barry
et al., 2015; Zhong et al., 2019). For the drilling mud to build an
effective filter cake, additives must be carefully selected that will cause
the drilling mud to form a thin and yet stable filter cake that will provide
highly efficient sealing properties on the wall of the well (Bageri et al.,
2015, 2016). Filter cake will not form without filtration loss (losing the
liquid component of the mud into the well). Once the filter cake is
formed, it will control further fluid loss. A wide range of drilling chal­
lenges particularly in high-pressure high temperature wells can be
avoided or minimized with appropriate mud additives (Mahmoud et al.,
2020).
The adverse impact of fluid loss into and reaction with the near
wellbore area can be extreme Zhong et al. (2019). Moreover, losing the
liquid component of the mud into the well comes at a high drilling cost
(Sherwood and Meeten, 1997). All these call for a concerted research
effort towards improving the filtration properties of drilling fluids. It is

* Corresponding author.
E-mail address: abdulrauf@kfupm.edu.sa (A.R. Adebayo).

https://doi.org/10.1016/j.petrol.2020.108242
Received 27 August 2020; Received in revised form 3 December 2020; Accepted 8 December 2020
Available online 13 December 2020
0920-4105/© 2020 Elsevier B.V. All rights reserved.
B.S. Bageri et al.
desired that the filter cake formed during drilling be thin and stable and
that they should minimize solid and liquid loss into the underground
rocks. Many articles in the literature present the effects of various pa­
rameters on filter cake structure and properties such as the drilling fluid
rheological properties, drilled cuttings content and rock properties
(Bageri et al., 2016; M. Mahmoud et al., 2017a,b). The amount of clay in
the drilling mud also plays a significant role in improving its rheological
properties (Bageri et al., 2019; Vipulanandan and Mohammed, 2020).
New additives are being introduced in drilling fluids to improve their
sealing properties and minimize filtration loss. Such additives include
Nano-silica, ferric oxide nanoparticles, magnesium aluminum silicate
nanoparticles, Nano-clay, cellulose nanoparticles, perlite, copper oxi­
de/polyacrylamide nanocomposite, and others (Bageri et al., 2020;
Rafati et al., 2018; Hong et al. 2020).
1.1. Limitations of laboratory tests
It is also imperative that the performances of additives in drilling
fluid be accurately determined. Such performance evaluation must be
carried out at conditions that best represents downhole well conditions
using different techniques and procedures. To obtain a representative
sample of the filter cake that may be formed during drilling, a filtration
loss test is required. The common method of studying infiltration process
is using high-pressure high-temperature filter press based on recom­
mended standards set by the American Petroleum Institute (API) (Bageri
et al., 2013b). The test involves measuring the rate and amount of fluid
displaced from a porous medium upon which the filter cake is deposited,
under a specific pressure, temperature, and time (usually 30 min). In this
method, a sand column, or a consolidated rock sample pre-saturated
with water is placed inside a vertical column of glass or stainless-steel
cylinder. The drilling fluid to be tested is then poured into the cell and
a loading pressure is applied against the fluid such that the drilling fluid
is infiltrated into the sand column or rock sample under applied pres­
sure. A filter cake is formed on top of the sample. The sealing properties
of a drilling mud can be evaluated in terms of the thickness, porosity,
and permeability of the filter cake it forms, and the volume of solids that
the filter cake allowed to invade the sample. The conventional practice
of measuring mud cake thickness in the laboratory is to remove the
mudcake from the filtration cell and after washing, measure its thickness
by a caliper or a ruler. This procedure requires excessive handling of the
fragile filter cake, which can disfigure the cake and introduce additional
measurement artefacts (Adebayo et al., 2020). Some researchers (Bageri
et al., 2013a; Yao et al., 2014) studied the composition, structure, and
morphology of the formed filter cake using different investigative tools
such as scanning electron microscopy (SEM), energy dispersive X-ray
spectroscopy (EDS), and x-ray diffraction (XRD) analysis. Computed
tomography (CT) scan approach was also used to classify the texture of
the external and internal layer of the filter cake in addition to determine
the porosity of the filter cake and rock sample (Elkatatny et al., 2013;
Mahmoud et al., 2017a,b). Mercury porosimeter method was also used
to characterize filter cake porosity and pore volume distribution (Bageri
et al., 2013b). A direct measurement of the wet and dry filter cake can
give a direct value of the filter cake porosity and an indirect indication of
its permeability and solid invasions (Bageri et al., 2013b). These re­
ported methods require that the filter cake be removed from the filtra­
tion cell, and after washing, measure its properties. All these lead to
excessive handling of the fragile cake, which can disfigure the cake and
introduce additional measurement artefacts.
Recently, nuclear magnetic resonance (NMR) methods have been
shown to be a promising tool in evaluating formation damage (Al-Yaseri
et al., 2015; Al Jaberi et al., 2020; Wu et al., 2019), filtration properties
of drilling fluids and filter cake (Adebayo et al., 2020). NMR have been
used to evaluate porosity and pore size distribution of rock samples
before and after mud solid invasion (Adebayo et al., 2020; Adebayo and
Bageri, 2019). The major advantage of using NMR technique for filter
cake analysis is that the filter cake can be investigated with minimal
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Journal of Petroleum Science and Engineering 198 (2021) 108242
handling and processing. Furthermore, any developed methodology
using NMR has the possibility to be applied in real boreholes since NMR
logging tools already exist. Although, the NMR technique is promising,
but no work has been carried out to validate or compare it with other
conventional methods. This study investigates the use of NMR technique
to evaluate filter cake porosity and the amount of infiltrated solids in
rock samples. NMR measured porosity and infiltrated mud solids were
obtained and compared with some other known methods such as
gravimetric and CT scan method.
2. Experimental methods
2.1. Drilling fluid and rock samples
Water based drilling fluids commonly consists of bentonite clay (gel)
with additives such as barium sulfate (barite), calcium carbonate (chalk)
or hematite. In this study, a high-density water-based barite drilling
fluid was used with the composition shown in Table 1 (Bageri et al.,
2020). The drilling fluid was prepared to have a density of 18 pounds per
gallon (ppg) so as to ensure solid invasion in the rock samples wherein
the NMR method and other techniques are used to quantify solid inva­
sion and filter cake properties.
Rock samples comprising of 2-inch-long and 1.5-inch diameter
outcrop sandstone and carbonate rock samples were used in this study as
the filtration media in the fluid loss test. The properties of the core
samples are summarized in Table 2. The selected samples have a wide
range of permeability (0.23mD - 211mD) so as to obtain a variety of mud
cake and infiltration profiles.
2.2. Fluid loss test apparatus
A high-pressure high-temperature (HPHT) fluid loss cell was built to
accommodate a 2-inch-long and 1.5-inch diameter rock (Adebayo and
Bageri, 2019). The test was conducted to generate filter cake on top of
the rock samples, with a procedure that mimics field scale drilling fluid
invasion. A differential pressure of 300 psi was applied to form the filter
cake, where the inlet pressure and outlet backpressure were regulated at
a constant value at 500 psi and 200 psi, respectively. The test was carried
out at 150 ◦ F. The mud filtration volume was monitored during the test
and the deposited filter cake thickness was measured at the end of the
test. The fluid loss test was repeated with different rock samples, listed in
Table 2, and the same composition of barite water-based drilling fluid
shown in Table 1.
2.3. Low-field NMR equipment
A low magnetic field (2 MHz) NMR spectroscopy system (Geospec
2.1 rock analyzer from Oxford instrument) was used to evaluate for­
mation damage by comparing the pore size distribution of the rock
samples before and after filter cake deposition. The volume and particle
size distribution of the filter cake were also determined using the same
method. In NMR relaxometry, T2 relaxation is a measure of the time it
takes a hydrogen molecule (or proton) to relax back to its natural
Table 1
The composition of barite water-based drilling fluid.
Name Unit Description
Water bbl. 0.691
Bentonite lb. 4
XC-polymer lb. 0.5
KCl lb. 20.0
KOH lb. 0.5
NaCl lb. 66
Barite lb. 352.0
CaCO3 medium lb. 5.0
Sodium sulfite lb. 0.25–0.30
B.S. Bageri et al. Journal of Petroleum Science and Engineering 198 (2021) 108242

Table 2 temperature of 100 0C. The dried sample was imaged again using the
Properties of the rock samples. X-ray CT scanner in order to understand and quantify the solid invasion.
Sample ID Mineralogy Porosity (%) Permeability mD
2.5. Test procedures
Sample 1 Sandstone 11.5 211
Sample 2 Sandstone 13.46 0.23
Sample 3 Carbonate 8.19 1.66 The filter cake porosity at the end of the fluid loss test and the profile
Sample 4 Carbonate 10.15 4.33 of invaded solids were measured using three methods namely:

1. Gravimetric (weight) method

direction of precession after it was excited by a magnetic field in a di­
2. X-ray CT scan method
rection transverse (perpendicular) to the magnetic field. T2 relaxation is
3. NMR relaxometry method
measured in milli seconds (ms) and it is related to surface to volume
ratio of the pores and the surface relaxivity (ρ) of the rock minerals
In Fig. 1, we gave a simplified illustration of the steps involved for
lining the pore surface according to equations (1) and (2). T2 measure­
the three methods. Fig. 2 shows the images of the actual formed filter
ments are conducted in NMR equipment using a special pulse sequence
cake using the fluid loss tests. The properties of the formed filter cake
called CPMG named after the inventors, (Adebayo and Bageri, 2019;
such as thickness, cake porosity and the concentration of infiltrated
Carr and Purcell, 1954). T2 measurements were obtained using the
solids utilizes the three methods.
CPMG pulse sequence with optimized scanning parameters as follows:
Tau (inter echo spacing) value of 0.1 milli seconds; signal to noise ratio
2.5.1. Gravimetric method
of 200; recycle delay of 11,250 milli seconds. NMR T2 measurements is
The gravimetric method for filter cake porosity (∅c ) as presented in
related to the pore size distribution of the rock according to Equations
the literature (Bageri et al., 2013b; Dewan and Chenevert, 2001) is
(1) and (2).
summarized in the following steps:
1 S
= ρ (1)
T2 V i. Measure the dry weight of the rock (core) sample (dwcore).
ii. Saturate the core sample with water and measure its saturated
1 2
= ρ( ) (2) weight (swcore).
T2 r iii. Measure the total saturated weight of the core sample and the
filter cake immediately after the fluid loss test (WFC + swcore).
Where T2 is the relaxation time (ms) of the hydrogen molecules in a
The net wet weight of the deposited filter cake (WFC) layer is,
given pore of a porous material, ρ is the pore surface relaxivity (μm/s), S
WFC = (WFC + swcore) - (swcore).
is the surface area of the pore (μm2), V is the volume of the pore (μm3),
and r is the pore radius (μm). Since, NMR T2 distribution has a one to one
correspondence with the pore size distribution of a porous medium, the
T2 profile can be considered a representation of the pore size distribution
of the porous medium (Howard and Kenyon, 1992; Kleinberg, 1996;
Allen et al., 2000).

2.4. X-ray CT scanner

The internal structure of each rock sample at pre- and post-drilling

fluid invasion was also examined using cross-sectional digital imaging
obtained over the full length of each sample with an x-ray medical CT-
scanner model TSX-032A. Each sample was scanned at 1 mm slice
thickness and 1 mm slice interval using a power of 20 kV and 300 mA
(Bageri et al., 2020). At the end of the fluid loss and NMR test, the filter Fig. 2. Filter cakes after fluid loss test.
cake was wiped off the samples and dried in an oven for at least 6 h at a

Fig. 1. Illustration of the different methods and stages of measurements to derive filter cake porosity.

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B.S. Bageri et al. Journal of Petroleum Science and Engineering 198 (2021) 108242

iv. Dry the filter cake at 100 ◦ C for at least 3 h in order to evaporate
the water (Bageri et al., 2016).
v. Take the combined dry weight of the filter cake and the core
sample (DFC + dwcore). The net dry weight of the filter cake
(DFC) can be calculated as, DFC = (DFC + dwcore) - (dwcore).
an indication of the quantity of the invaded solids.
2.5.2. CT scan method
Like the gravimetric method, the steps for the CT method as present
by Elkatatny et al. (2013) for filter cake porosity measurement are:

The filter cake porosity can be calculated directly based on the ratio
of its pore volume to its bulk volume using the following equation:
Vp
∅c = , (3)
Vb
Where: Vp and Vb are the pore and bulk volume of the filter cake
respectively. The difference between the wet and dry weight of the filter
cake can be used to estimate the pore volume of the filter cake (Equation
(4)), while the bulk volume of the filter cake can be calculated using
equation (5) and assuming that the filter cake has uniform thickness and
diameter (Bageri et al., 2013b).
FCnww − FCndw
Vp = , (4)
ρf
π of solid invasion. The CTdry of the filter cakes could not be performed in
Vb = (D)FC (h)FC , (5)
4
Where: FCnww is the net wet weight of the filter cake, FCndw is the net dry
weight of the filter cake, ρf is the density of the filtration fluid and
(D)FC and (h)FC are the filter cake diameter and thickness respectively.
It is however quite challenging to obtain accurate dimensions and
weights of the filter cake alone. This is because the filter cake does not
have a perfect shape, after drying as can be seen in Fig. 3. In addition,
removing it from the surface of the rock sample and drying can further
complicate matters as some of the filter cake can be lost during removal
and the shape further disfigured such that you do not have a consistent
thickness and diameter. Furthermore, macro or micro cracks are created
on the filter cake during drying. An alternative method of porosity
measurement by gravimetric method is presented by Dewan and Che­
nevert (2001). This method does not require the dimensions of the filter
cake and uses the cake grain density instead as follows:
α
∅c = ρ , (6)
α + ρgf
i. Scan the filter cake layer immediately after the fluid loss test.
Record the CT number of the wet filter cake (CTwet).
ii. Dry the filter cake to evaporate the water and then scan the filter
cake layer to get the dry CT number of the filter cake layer
(CTdry)
iii. The filter cake porosity is therefore given as:
CTwet − CTdry
∅c = (8)
CTwater − CTair
Where: CTwater and CTair are the CT number of water and air respec­
tively. The CT scan of the rock sample can be performed at an interval of
1 mm along the sample length and filtration direction. The higher the
concertation of the invaded solids the higher the CT number (Bageri
et al., 2015). Accordingly, the profile of the CT scan can reveal the depth
this study due to system breakdown in the middle of the experiments.
However, various CT values of the rock samples were obtained, which
allowed us to study and quantify infiltrated solids.
2.5.3. NMR method
The following steps were followed to obtain NMR porosity of filter
cake and other filtration loss properties.
i. Saturate the core sample with the brine (3%KCl) and then run
NMR scan on the initial rock sample before loading it in the fluid
loss test. This measurement serves as the baseline NMR mea­
surement representing only the fluid in the rock sample. This
measurement is labelled as NMR1.

Where: ρf and ρg are the density of the filtration fluid and the mud cake
grains respectively, and α is measured using the relation:
FCnww
α= − 1 (7)
FCndw
We refer to the two gravimetric methods as gravimetric method – 1
(equation (3)) and gravimetric method – 2 (equation (6)). The difference
between the weight of the dry core before and after the loss test can give

Fig. 3. Filter cakes and samples after drying. Fig. 4. Low field NMR setup.

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B.S. Bageri et al. Journal of Petroleum Science and Engineering 198 (2021) 108242

ii. Scan the rock sample in the NMR scanner, along with the filter
cake on top, as illustrated in Fig. 4. In this stage, the NMR T2
measurements represent three elements (Rock + Filter cake +
solid invasion), labelled as NMR2. The infiltrated solids reduce
the NMR signals because they displaced the water that earlier
contributed to the signals in the baseline measurements above.
iii. Carefully remove the filter cake and scan the rock sample to get
the NMR profile for only the rock with invaded solids, labelled
NMR3.
iv. The porosity of the filter cake can be estimated as:
a. Filter cake porosity = NMR2 – NMR3
v. Reduction in rock porosity after the filtration process = NMR1 – Fig. 6. Filter cake porosity and solids invasion measured by gravi­
NMR3. This reduction in porosity includes all of the possible metric method.
factors that may cause the change of rock porosity, such as solid
invasion (porosity loss), rock-fluid dissolution (porosity in­ weight of the rock sample in stage 1 and stage 5 of Fig. 1.
crease), and/or particle migration (porosity increase).
3.2.2. CT scan method
3. Results and discussions The profiles of CT number for the rock samples pre and post mud
invasion are shown in Fig. 7 and Fig. 8. As seen in both figures, the re­
This section presents the results of the filter cakes’ porosity and the gions close to the filtrate invasion points exhibit higher CT number after
concentrations of the solids that infiltrated the rock sample upon which solid invasion (damage) relative to the pre-damage values. This obser­
they were deposited. The filter cake thickness was the only direct vation is consistent for all the four samples. The change in the rock
measurements made, and as such, was used to validate the different density (CT number) is due to solid deposition in these regions. The
methods by cross correlating the cakes’ thickness with their porosity dotted line is an average of the CT number at the filter cake deposition
values obtained from the three methods. The solid concentrations were regions.
also correlated with cake thickness. In sandstone samples (Fig. 7), the concentration of the invaded solids
decreased at distances away from the point of mud invasion until a
3.1. Filter cake thickness distance where the pre- and post- CT profiles cross over. After the
crossover, the CT number of the rock after filtrate invasion became
Fig. 2 shows the images of the formed filter cake on top of the lower than before filtrate invasion. The reason for this could be that the
different core samples at the end of the fluid loss tests. The thickness of filtrates that invaded the rock sample interacted with the rock clay
the filter cake was directly measured using a Vernier caliper (with a minerals such that it dissolved and dislodged some of the clay minerals
resolution of 0.01 mm). The filter cake thicknesses were obtained by from the rock sample (particle dissolution and migration) and thus
subtracting the actual length of the sample from the total length of the slightly decrease the rock density (or CT number). This trend is observed
sample with the filter cake on it. Fig. 5 compares the thickness of the four in both sandstone samples. The question that comes to mind is whether
filter cakes deposited on the four samples. particle dissolution and migration only occurs after the cross over or not
and whether mud particle invasion stops at the distance where the CT
numbers cross over or goes beyond. For the results of the sandstone
3.2. Filtration properties
samples, it can be said that clay dissolution and migration likely
occurred throughout the entire sample length. However, mud particle
In this section, we present the porosity of the filter cakes and the solid
invasion dominates clay dissolution and migration around the rock entry
invasion profile as evaluated by each of the aforementioned methods-
region (before cross over) while clay dissolution and migration domi­
gravimetric, CT scan and NMR methods.
nated mud solid invasion after the cross over region. However, in the
carbonate samples, a different trend was observed as shown in Fig. 8.
3.2.1. Gravimetric method
There was no clear crossover after the region of solid invasion. The post
The grain density of the mud cake was measured as 3.89 g/cc using a
damage CT number apparently remains higher throughout the entire
gas pycnometer. The measured filter cake properties using the gravi­
metric method are presented in Fig. 6. The blue bars represent the
measured filter cake porosity (%.) while the orange bars represent the
concentration of the solids (grams) that invaded the rock samples. The
concentration of invaded solid was estimated from the difference in the

Fig. 7. CT number profile for the sandstone core samples (sample 1 & 2) pre
Fig. 5. Filter cake thickness. and post damage.

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B.S. Bageri et al. Journal of Petroleum Science and Engineering 198 (2021) 108242

Table 4
Cumulative pore sizes (porosity) NMR analysis for the core samples pre and post
to the fluid loss test.
Stage 2 Stage 3 Stage 4 Estimated Solid
Concentration

NMR1 NMR2 NMR3 (NMR2- (NMR1-

NMR3) NMR3)

Rock before (Rock + FC) Rock after Filter Invaded

solids’ after solids’ solids’ cake solids
invasion invasion invasion

NMR Porosity values (%)

Sample 11.43 11.05 9.13 1.92 2.30

1
Sample 14.53 11.41 10.63 0.78 3.90
2
Sample 9.88 10.21 8.80 1.41 1.08
3
Fig. 8. CT number profile for the carbonate core samples (sample 3 & 4) pre
Sample 10.85 10.53 10.08 0.45 0.77
and post damage.
4

Total T2 relaxation time of the volume occupied (pu.ms)

length of the samples. Though the distance near the fluid entry region
showed distinct difference between the pre and post CT numbers sug­ Sample 113110.00 109820.31 90708.74 19111.57 22401.27
1
gesting that mud particle invasion is more significant in the fluid entry
Sample 144979.60 113965.56 106175.54 7790.02 38804.07
region than beyond. The remnant of the invaded solids transported from 2
this region throughout the sample length could be responsible for the Sample 94805.51 98723.58 84637.01 14086.58 10168.50
higher CT numbers. Interestingly, the difference in the CT numbers at 3
Sample 104395.03 102259.41 97698.55 4560.86 6696.48
axial distances beyond the fluid entry region is more pronounced in
4
sample-4 than sample-3. The post CT number is distinctly higher than
the pre-CT number because sample-4 is more permeable than sample-3,
which allows the mud particles to invade deeper through the entire The difference between these two curves represents the porosity occu­
sample length. Furthermore, clay is not present in carbonate rocks and pied by the solids that invaded the rock samples. The amount or con­
as such there is no dissolution and migration that can cause a lower CT centration of invaded solids can be expressed in terms of the difference
number in this region as observed in the sandstones (Fig. 7). The average in the areas under the two curves. The difference in area is shown for
CT number for the entire rock sample and the interval close to the area of each sample in Table 4. The unit of this area is derived from direct
filter cake deposition (0.5 inch) is shown in Table 3. The concentration multiplication of the two axes (pu.ms), which can be understood as an
of invaded solids in the core samples can be obtained by taking the equivalent total water signals obtainable from those pores occupied by
difference between the average of CT numbers post- and pre-invasion as the invaded solids. In parts (b) of the figures, the green curves represent
shown in Table 3. We could not conduct CT scan on the dry filter cakes the cumulative porosity of the rock samples (with filter cake sitting on
for technical reasons. As such, filter cake porosity with CT scan was not them; NMR2, stage 3 of Fig. 1). The red curves in this part represent the
estimated. cumulative porosity of the rock samples after the filter cakes were
removed from their top. The difference in the porosities for these two
3.2.3. NMR method curves in part (b) is the filter cake porosity also shown in Table 4.
As indicated in Fig. 1, NMR measurements were performed at three Similarly, the difference in the area under the two curves in part (b) is
different stages namely NMR1, NMR2 and NMR3 as explained in section believed to indirectly provides quantitative estimation of the amount of
2.5.3. Table 4 shows each sample NMR porosities at the different stages. filter cake on each rock sample. The unit of estimated area under these
The columns, as labelled, represent the NMR measurements at the curves is also (pu.ms). This unit is a quantitative illustration of the filter
different stages for the four rock samples. Figs. 9–12 show how the filter cake volume and concentration of the invaded solids, which can be
cake porosity and concentration of invaded solids were extracted for conceptualized as the equivalent water signal coming from the volume
each of the samples. The horizontal axis is the T2 relaxation time, which occupied by the mud particles (filter cake or invaded solids). In the next
has a linear relationship with pore sizes, while the vertical axes repre­ section, comparison is made between the filter cake porosity, filter cake
sent the cumulative porosity of these pores. The blue curves in part (a) of thickness, and invaded solid profile for the three methods. The advan­
these figures represent the cumulative porosity of the rock samples tages and limitations of each method is also highlighted.
before infiltration (NMR1, stage 2 of Fig. 1). The red curves in part (a) of
the figures represent the rock sample after infiltration (NMR3, after the 3.2.4. Comparison between gravity, CT scan, and NMR methods
filter cake was removed from the top of the rock sample, i.e. stage 4).
3.2.4.1. Filter cake porosity. In this section, comparison is made be­
tween filter cake porosity and concentration of invaded solids as
Table 3 measured by the three methods. For filter cake porosity, it is possible to
Average CT number for the core samples pre and post to the fluid loss test. compare the porosity values from each method since the porosity unit is
Average CT Number for Entire Average CT Number for 0.5 in the same for all the methods compares the porosity values from NMR
rock sample section contacted with the filter and gravimetric methods.
cake
As observed from Fig. 13, there is disparity in the values of porosity
Pre Post (Post – Pre) Pre Post (Post – Pre) from the different methods in all the samples. The source of the differ­
Sample 1 1763.0 1761.8 1.2 1757.3 1762.6 5.3 ence between these methods can be attributed to different possible
Sample 2 1876.0 1872.5 3.5 1876.1 1877.8 1.7 sources of errors in the gravimetric methods. The gravimetric method is
Sample 3 2272.4 2272.5 0.1 2256.4 2261.6 5.2 largely dependent on the filter cake weight (dry and wet weights), the
Sample 4 2462.1 2469.4 7.3 2435.2 2447.1 11.9

6
B.S. Bageri et al.
Fig. 9. NMR cumulative pore sizes (porosity) Analysis for Sample (1): showing (a) Rock before and after invasion, (b) Rock with the filter cake after invasion
compared with rock after invasion without filter cake.
Fig. 10. NMR cumulative pore sizes (porosity) Analysis for Sample (2): showing (a) Rock before and after invasion, (b) Rock with the filter cake after invasion
compared with rock after invasion without filter cake.
cake dimensions, and cake grain density. Gravimetric method requires
measurements of other independent parameters whose accuracy
significantly affect the estimated cake porosity. The gravimetric method
– 1 assumes that the filter cake diameter is equal to the inner diameter of
the fluid loss cell or the diameter of the rock sample. It also assumes a
uniform cake thickness. However, the formed filter cakes most often are
not homogenous in dimension as earlier observed in Fig. 3. In gravi­
metric method – 2, the cake grain density is introduced to avoid cake
dimension. However, error in the measurements of the grain density can
also affect the porosity value. It is therefore important to investigate the
sensitivity of the independent parameters (weights, dimensions, and
cake density). Hence, we carried out a sensitivity analysis to investigate
how each of these parameters affect our porosity measurements. Error in
gravimetric method is likely due to loss in cake materials during
handling, transporting, and drying. The sensitivity of the measured
weights of cake was evaluated by introducing an error in the dry weight
of the cake in a range of 0.01–0.1 g. Many weight measurements in the
laboratory are often within this error margin. Fig. 14 shows the corre­
sponding filter cake porosity by both gravimetric methods for every
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Journal of Petroleum Science and Engineering 198 (2021) 108242
0.01g error in the filter cake dry weight. This analysis was conducted on
one sample (sample 1). The cake porosity at an error of 0.00g is the
measured value that is reported in this study. The percentage change in
porosity due to the error in measured weight of the cake is shown in
Fig. 15. It is important to note from the figure that, an error as small as
±0.05g and ±0.1g for a cake of 7.79g, caused a 71% and 142% change
respectively in the cake porosity using gravimetric method – 1. The
change in porosity for gravimetric method – 2 is 68% and 136% for a
weight error of ±0.05g and ±0.1g for the same cake. In Fig. 16, we
investigated the significance of this error on cake thickness by plotting
the corresponding change in cake porosity for the four different filter
cakes produced in our experiments. Remember that the four filter cakes
have different thickness as previously illustrated in Fig. 5. As expected,
the effect of the error on cake porosity decreased when the cake thick­
ness increased above a certain value.
Similarly, we introduced an error in the bulk volume in the range of
0.01–0.1 cm3 for a filter cake of 3.55 cm3 bulk volume and evaluated the
corresponding change in the filter cake porosity using sample 1 as a case
study. As shown in Fig. 17, the change in the cake porosity due to errors
B.S. Bageri et al. Journal of Petroleum Science and Engineering 198 (2021) 108242

Fig. 11. NMR cumulative pore sizes (porosity) Analysis for Sample (3): showing (a) Rock before and after invasion, (b) Rock with the filter cake after invasion
compared with rock after invasion without filter cake.

Fig. 12. NMR cumulative pore sizes (porosity) Analysis for Sample (4): showing (a) Rock before and after invasion, (b) Rock with the filter cake after invasion
compared with rock after invasion without filter cake.

Fig. 14. Sensitivity of filter cake porosity on weight error.

Fig. 13. Comparison of mud cake porosity between Gravimetric and
NMR methods.
in bulk volume is not as significant as that due to weight error. For every
±0.025 cm3 error in bulk volume there is a corresponding 1% change in
the cake porosity. This is quite insignificant compared to the weight
error, where a weight error of ±0.05g caused a 71% change in the cake
porosity. For the gravimetric method – 2, we evaluated change in the
cake porosity due to error in grain density measurement. We varied the
grain density of the cake by a range of 0.01–0.1 g/cc. As seen in Fig. 18,

8
B.S. Bageri et al.
Fig. 15. Percentage change in filter cake porosity due to weight error.
Fig. 16. Effect of cake thickness and weight error on filter cake porosity.
Fig. 17. Sensitivity of cake porosity on error in cake volume: gravimetric
method – 1.
Fig. 18. Sensitivity of cake porosity on error in cake grain density: gravimetric
method – 2.
9
Journal of Petroleum Science and Engineering 198 (2021) 108242
an error in cake density has the least effect in the porosity values as an
error of ±1 g/cc caused 3% change in the cake porosity.
It is obvious from the results above that gravimetric methods are
prone to various artefacts coming from drying, handling, and trans­
porting of the fragile filter cake. They are also dependent on other
measured parameters such as cake dimensions and cake grain density.
Another way of checking the reliability of the measured porosity values
is to correlate them with the cake thickness. In Fig. 19, we correlated the
mud cake porosity value from each method with their thickness, which
was measured physically with a digital caliper. Scientifically, mud cake
porosity scales linearly with mud cake thickness. Hence, a good coeffi­
cient of correlation between the two parameters is a way of checking the
reliability of their measurements. As observed from the linear correla­
tion, porosity measurements from NMR method has the best correlation
coefficient (R2 = 0.97) followed by gravimetric method – 1, which has
R2 of 0.61. Gravimetric method – 2 produced a poor fit with R2 value of
0.34. It is worth mentioning that NMR method only depends on the
signal coming from the water in the pores of the filter cake to estimate
the cake porosity value. As earlier discussed, a well-calibrated NMR
system converts NMR T2 signal to volume (cm3) through a calibration
factor that relates NMR signal to a known volume of water in a standard
bottle of known porosity. The measured pore volume of cake is con­
verted to porosity by dividing the pore volume by the cake bulk volume.
Hence, NMR porosity values can also be said to be dependent on the cake
thickness. Fortunately, the sensitivity analysis in Fig. 17 shows that error
in cake volume has no significant effect on the cake porosity. Although
porosity from CT method was not concluded in this study, but it is
obvious that cracks created by the drying process will yield porosity
values higher than the actual filter cake porosity. The heating process at
high temperature, which goes for several hours, may also affect the
structure of the clay particles in the filter cake. Overall, the process of
measuring filter cake porosity using gravimetric and CT scan method is
quite time consuming and requires excessive handling of the samples
filter cake.
3.2.4.2. Solid invasion. For solid invasion profile, each of the three
methods quantifies solid invasion using different parameters such as
weight of infiltrated solids (gravimetric method), CT number of infil­
trated solids (CT scan method), and porosity (pu.ms) of the pores
invaded by solids (NMR method). The gravimetric method is the most
direct measurements of the infiltrated solids since it is based purely on
weight difference before and after solid infiltration into the rock sam­
ples. As such, the weight of the infiltrated solids is cross correlated with
the quantities determined by CT scan and NMR methods (Figs. 20 and
21). In the NMR methods, the T2 values of the pores filled with infil­
trated particles is represented by the difference in the area under the T2
curves for pre- and post-infiltration of solids (Figs. 9–12). The area is
plotted on the vertical axis against the corresponding weights of the
solids as measured from weight difference. As seen from Fig. 20, the
NMR measurements show a good correlation with the gravimetric
method, when the outlier is excluded from the fit. The CT measurements
Fig. 19. Cross plot of filter cake porosity and thickness.
B.S. Bageri et al.
Fig. 20. Cross-plot of quantity of infiltrated solids - NMR versus gravi­
metric method.
Fig. 21. Cross-plot of quantity of infiltrated solids – CT scan versus gravi­
metric method.
of solids in the rock samples were also correlated with the gravimetric
measurements as shown in Fig. 21, with a correlation of coefficient that
is not as good as that with NMR measurements. Another measurement
obtained from the NMR method is the cake concentration (pu.ms). It is
important to mention here that NMR measurements presented in this
paper give the net total pore profile, wherein net pore enlargement and
pore plugging can be deduced. However, it is also possible to use NMR
technique to measure axial distribution of mud solid invasion, clay/
matrix dissolution and migration in each rock in the same way as the CT
scan profile. The use of spatial NMR or such scenario is presented in
Bageri et al. (2019).
Fig. 22 shows the correlation between the NMR values of filter cake
concentration (pu.ms) versus direct measurements of cake thickness. A
good correlation exists between the two measurements. This correlation
is a useful tool for measuring filter cake thickness from NMR experi­
ments. The coefficient of regression is high (R2 = 0.97) based on four
data points, a more robust linear equation is needed to have a general
relation between NMR measurements and actual filter cake thickness.
4. Conclusions
The sealing and infiltration properties of slurries such as drilling
fluids in representative rock samples were probed with NMR relaxom­
etry, gravimetric, and x-ray CT scan methods. Two gravimetric methods
were evaluated namely, the one based on weight and dimensions of the
cake (we refer in this paper to as gravimetric method – 1), and the one
based on density and weight of the cake (we refer to as gravimetric
method – 2). The NMR method is new and the porosity values obtained
with it were compared with those obtained from the others, which are
often reported in the literature. We showed that with NMR approach, a
filter cake porosity, its thickness, and its pore size distribution can be
evaluated in the lab without vigorous sample handling and transport, as
is the case in the conventional gravimetric and CT scan methods. The
10
Journal of Petroleum Science and Engineering 198 (2021) 108242
Fig. 22. Cross-plot of NMR filter cake concentration versus measured
cake thickness.
porosity values obtained from NMR is quite low when compared with
those obtained from the gravimetric methods. A sensitivity analysis of
the independent parameters required to estimate the gravimetric po­
rosities showed that a weight error of ±0.05g and ±0.1g in a 7.79g filter
cake caused a change in the cake porosity by as high as 71% and 142%
respectively. The effect of error, in filter cake density and dimensions, on
cake porosity is relatively insignificant. A cross correlation between the
porosity values from the three methods and the measured cake thickness
showed that the NMR porosity values is more reliable. NMR method
showed a high correlation of coefficient (R2 = 0.97), while gravimetric
method – 1 and gravimetric method – 2 showed R2 values of 0.61 and
0.33 respectively. Several factors can be attributed to the poor correla­
tion or accuracy of the gravimetric methods, the most paramount being
the excessive sample handling, drying, and movement during both
gravimetric and CT scan measurements. These activities can introduce
error in the weight measurements. The NMR method on the other hand
has a minimal sample handling, movement, and does not require drying
the cake. The invasion profiles of the solid particles into the rock sam­
ples were also quantified and compared between NMR, CT scan and
gravimetric methods. Overall, NMR method correlated best with the
measured solid weights, compared to the CT scan method. Another
advantage of the NMR method is that it offers additional cake and
infiltration information such as concentration of filter cake (cake vol­
ume), pore size distribution of the filter cake and the pore sizes occupied
by the invading solids. All these measurements can also be obtained in a
timely manner and in a single NMR experiment.
Credit author statement
Badr Bageri: Conceptualization, Methodology, Investigation, Writing
– original draft, Data curation. Abdulrauf Adebayo: Conceptualization,
Methodology, Supervision, writing- Original draft, reviewing. Jaber Al
Jaberi: Methodology, Formal analysis, reviewing. Shirish Patil: Formal
analysis, reviewing and Resources. Rahul Salin: Methodology and data
curation.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgement
The authors are grateful to the College of Petroleum Engineering and
Geosciences at King Fahd University Petroleum & minerals for the
research support.
B.S. Bageri et al.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.petrol.2020.108242.
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