PETROLEUM EXPLORATION AND DEVELOPMENT

Volume 44, Issue 3, June 2017

Online English edition of the Chinese language journal

Cite this article as: PETROL. EXPLOR. DEVELOP., 2017, 44(3): 477–486. RESEARCH PAPER

Extending thermal stability of calcium carbonate pills

using sepiolite drilling fluid
ETTEHADI Ali1, 2, *, ALTUN Gursat1
1. Department of Petroleum and Natural Gas Engineering, Istanbul Technical University, Maslak 80626, Istanbul, Turkey;
2. Department of Petroleum and Natural Gas Engineering, Izmir Katip Çelebi University, Balatcik-Cigli 35620, Izmir, Turkey

Abstract: The aim is to investigate the plugging ability of sepiolite clay water base drilling fluids over a wide range of high permeable
zones at high temperature and high pressure conditions. The special emphasis of this study is to extend the usage of loss preventer mate-
rial (LPM) as a component of fresh water sepiolite base mud that has never been investigated for this purpose before. The rheology and
loss tests at 27204 C and 2070 or 6895 kPa revealed that the sepiolite drilling mud shows good rheology and high solid suspension ca-
pability at all temperatures except 149 C, and low loss circulation at high temperature and high pressure. The Permeability Plugging Ap-
paratus (PPA) experiment, in which the 1090 µm permeable ceramic plate was simulated as formation, showed that the sepiolite drilling
mud without CaCO3 can not plug the pores, while the sepiolite drilling mud with CaCO3 can plug the pores quickly and keep the CaCO3
particles suspended even at high temperature (up to 193 C). The PPA experiment results were proved by the analysis using SEM and
ideal packing theory.

Key words: sepiolite drilling mud; loss circulation; plugging performance; thermal stability; calcium carbonate particle; HTHP drilling

Introduction magnesium silicate clay mineral of fibrous texture. Altun et al

Lost circulation, one of the most common drilling problems,
would increase drilling costs and drilling risks, and cause
other issues. Statistics show USD $2 to 4 billion each year is
spent on plugging drilling fluid and materials around the
world[1]. The circulation loss problem constitutes important
portion of total NPT. According to US Department of Energy,
on average 10% to 20% of the drilling cost in high tempera-
ture high pressure (HTHP) wells was spent on mud loss con-
trol[1]. For water base mud systems, high temperature causes
clay particles to flocculate, and thus unacceptable high viscos-
ity, water loss and excessive thick filter cake, and possibly
more rapid mud loss. Moreover, high pressure differential
between the mud hydrostatic and formation pore pressure
make the loss circulation risk increase. Lost circulation can
cause formation damage and production reduction, which
could be serious in complex formation conditions. Lost con-
trol materials (LCMs) can effectively plug unconsolidated and
fractured formations, and play an important role in stopping
lost circulation. Moreover, stable and economic drilling fluid
under high temperature and pressure is needed to extend the
usage of LPMs. Commonly used Water-base drilling fluids
have poorer stability at temperatures above 121 C (250 F);
and synthetic-base muds are high in cost[2]. Sepiolite is a
found through experiment[36] that sepiolite drilling fluid could
keep good rheology under high temperature. Adding calcium
carbonate into bentonite drilling fluid as LCM is very com-
mon now, but there are few studies on adding it into sepiolite
drilling fluid as LCM. In this study, the plugging ability of the
sepiolite base drilling fluids with and without CaCO3 pills
have been tested in lab to find out if the sepiolite mud can
enhance the thermal stability of CaCO3, and thus prevent lost
circulation effectively.
1. Experiment method and materials
1.1. Preparation of mud
The sepiolite clay used in this study is a raw clay sample
(commercial product known as Turk Taciri Bej (TTB)) bought
from AEM Company (AEM, 2015) near Sivrihisar-Eskisehir
district of Turkey. The raw sepiolite clay sample was sieved to
<200 mesh (<74 µm) after grinding with no physical or
chemical treatment. X-ray Fluorescence Spectrometry (XRF)
was used to perform elemental analysis of the sepiolite clay.
The test conditions of measuring the sample purity and char-
acterizing crystalline materials of sepiolite clay are defined in
reference [3]. The formulas of sepiolite base drilling fluids are
given in Table 1, in which there are some technical additives:

Received date: 17 Aug. 2016; Revised date: 28 Feb. 2017.

* Corresponding author. E-mail: ali.ettehadi@ikc.edu.tr
Copyright © 2017, Research Institute of Petroleum Exploration and Development, PetroChina. Published by Elsevier BV. All rights reserved.
 ETTEHADI Ali et al. / Petroleum Exploration and Development, 2017, 44(3): 477–486
Table 1. Formulas of sepiolite base mud systems
3
Quantity (kg/m )
Materials
Base mud Base mud with CaCO3
Sepiolite 57 57
Soda Ash 0.286 0.286
Polymer-1 11.43 11.43
Polymer-2 14.28 14.28
Calcium Carbonate None 57
pH was controlled by the sodium carbonate (soda ash,
Na2CO3, product of Karakaya ); an anionic acrylic copolymer
(polymer-1, product of Halliburton) was added as a thinner to
ensure the thermal rheological stability; and a vinyl am-
ide/vinyl sulfonate copolymer (polymer-2, product of Halli-
burton) was used as a filtration control agent.
Couette type viscometer (Fann Model 35SA/SR-12) was
used to measure rheological properties such as apparent vis-
cosity, plastic viscosity (PV), yield point (YP), and gel
strength (GS). HTHP filter press (Fann 500 ml HTHP filter
press) was used to test the static filtration properties of the
samples at elevated temperatures. The pore plugging appara-
tus (PPA) made by Fann Instruments (No. 206846), was em-
ployed to investigate plugging ability and fluid loss of the
sepiolite mud through porous media under upward pressure,
because PPA can simulate the gravity effect on impermeable
mud cake buildup under wellbore conditions. In the PPA, fluid
loss can be measured with ceramic discs 6.35 cm (2.5 inches)
in diameter and 0.635 cm (0.25 inch) thick. The prepared mud
samples were tested with ceramic discs with pore diameters of
10, 20, 35, 60, and 90 micron (corresponding to 2, 5, 10, 20,
100 Darcy of air permeability) at differential pressures of
2070 kPa and 6895 kPa (300 and 1000 psi) and temperatures
from 27 °C to 204 °C (400°F). CaCO3 pills in the technical
grade were added to the base mud as LPM. Particle size dis-
tribution of CaCO3 was measured using ethanol as dispersant
(Fig. 1). The test results show the CaCO3 particles are wide in
size distribution, and thus can provide effective pore sealing.
Standard procedures (API RP 13B-1, 2004) were followed
throughout the experimental study[7]. First, fresh water-base
un-weighted sepiolite (TTB clay) base drilling fluid was pre-
pared according to the formulas given in Table 1. Then the
Fig. 1. Particle size distribution of CaCO3.
 478 
sample was aged for 16 hours under heating condition. The
mud sample was heated to 27 °C and 49 °C by heat jacket
respectively, and then its rheological and HTHP filtration
properties were measured. After that, plugging performance of
the base mud sample without CaCO3 was measured using PPA
apparatus. Second, 57 kg/m3 (20 lbm/bbl) CaCO3 was added
to the base mud system as LCM. Similarly, after hydrothermal
treatment in an aging cell, the rheological properties of this
mixture were measured. Finally, the plugging performance of
this mixture was tested by PPA experiment.
1.2. Evaluation of PPA test results
Based on the results of PPA experiments, spurt loss, total
fluid loss, and static filtration rate were calculated to qualita-
tively analyze the plugging performance of the mud samples.
The calculation equation of spurt loss[8] is:
V0  2 V7.5  V30  V7.5   (1)
The total fluid loss is calculated by the following equa-
tion[8]:
Vtotal  2V30 (2)
Static filtration rate is the ratio of fluid loss to the square
root of elapsed time, its calculation equation[8] is:
2 V30  V7.5 
v (3)
2.739
Plugging index Ip indicating plugging efficiency of drilling
fluid was introduced to evaluate the plugging performance at
different temperatures, and it is calculated by Eq. 4:
V   27   V30  t 
I p  30 (4)
V30  27 
The data collected after 5 minutes into the experiment was
used in the calculation, evaluation and plotting to minimize
the error.
1.3. Scanning electron microscopy (SEM) analysis
Plugging effectiveness of the fresh water sepiolite base mud
was evaluated also using scanning electronic microscopy
(SEM). The surface morphology of the new and used ceramic
discs was observed by using a Quanta FEG 250 Microscope
equipped with EDAX ZAF quantifier. After a light coating
with gold, samples were observed with an FEI Quanta
FEG-250 field emission environmental SEM (FE-ESEM) at
magnifications ranging from 3500 to 3200,000 to determine
the range of pore sizes present in each porous disc. Five rep-
resentative areas (approximately 1 cm2) in each pore discs
were tagged for observation in order to acquire more accurate
pore sizes. In order to find out plugging ability of the prepared
mud samples with and without CaCO3, the pore discs were
characterized using image analysis software, ImageJ, to cal-
culate the pore area before and after plugging test. First, the
SEM images in JPEG format were converted to binary images,
then, the binary images were analyzed with the ImageJ soft-
ware to get a statistic table including the number of pores,
percentage pore area, and analysis of the size of individual
pores. In the computation of average pore diameter with
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ImageJ, it was assumed all the pores were circular, and the
ceramic discs did not have secondary porosity. Using the his-
tograms and the assumptions mentioned above, outliers were
removed and the actual mean diameters were calculated.
1.4. Ideal packing theory
Ideal Packing Theory (IPT) is a graphical approach to de-
termine the optimum particle-size distribution of bridging
material or LCM for the given formation characteristics[9].
First, according to the formation information, the optimum
target size distribution of the bridging agent is calculated.
Zhang et al[10] proposed a method for determining the optimum
target line, in which the most representative pore size was se-
lected from thin section SEM analysis (i.e. D90), then a straight
line was plotted by connecting the origin of Cartesian coordi-
nate (with square root of particle diameter as x-coordinate and
cumulative probability as y-coordinate) to the D90 point; and this
straight line is the optimum particle size distribution line. The
optimum particle size distribution line obtained based on for-
mation information and the particle size distribution line of
the plugging material are plotted on the same graph to esti-
mate the plugging effect of the plugging material.
2. The results and discussion
2.1. Rheological and filtration properties of the sepiolite
base mud samples
Rheological properties of unweighted sepiolite drilling
fluid without CaCO3 at 27 °C and 49 °C were measured (Ta-
ble 2).
It can be seen from the table that with the rise of tempera-
ture, the YP of the sepiolite fluid system decreases before
149 °C and then increases with the further increase in tem-
perature, this behavior is a clear sign of the initiation of ther-
mal activation of sepiolite clays at 149 °C[11]. Gel strength (GS)
shows the similar variation pattern. Therefore, special atten-
tion must be paid to the rheological properties of the fluid
system at high temperature to ensure its solid suspending and
hole cleaning abilities. Solid suspension of drilling fluid is
vital for plugging pores and throats and preventing loss circu-
lation, therefore, the pumping rate can be slightly increased at
high temperature to prevent possible borehole cleaning issue.
It can be seen from Table 2 that the sepiolite drilling fluid has
higher yield point even at high temperatures (for example,
204 °C), indicating the drilling fluid has good hole cleaning
capacity even at lower pump rate. Moreover, the lower flow
rate leads to less erosion to the mud cake, consequently, less
filtration loss and less formation damage.
Photographic frames of sepiolite drilling fluid with CaCO3
at different aging temperatures are shown in Fig. 2. It can be
seen from the figure the sepiolite mud is a homogeneous
mixture except 149 °C (300 °F); while at 149 °C CaCO3 par-
ticles settle down and clearly separate from the mud phase due
to the low gel strength, indicating the insufficient solid sus-
pension ability.

Table 2. Rheological and filtration properties of sepiolite base mud without CaCO3
Plastic viscos- Yield Shear stress at HTHP water
Aging Gel strength/Pa
ity/(Pa·s) point/Pa 600 r/min/Pa loss/mL
tempera-
27 C 49 C
ture/C 27 C 49 C 27 C 49 C 27 C 49 C 7.5 min 30 min
10 s 1 min 10 min 10 s 1 min 10 min
27 0.025 0.017 11.50 8.14 2.874 5.269 10.538 2.395 3.832 8.143 37.75 26.02 1.1 3.0
37 0.026 0.017 9.10 6.71 1.916 4.790 10.059 1.437 3.832 7.664 36.22 24.49 1.2 3.2
65 0.026 0.016 8.62 6.71 2.395 4.311 9.580 1.437 3.353 7.185 35.71 23.47 1.6 3.7
93 0.021 0.015 8.14 6.23 1.916 3.353 7.185 1.437 2.395 4.790 30.10 21.94 3.0 5.5
121 0.016 0.013 6.71 5.75 1.437 3.832 8.143 1.437 2.395 7.664 23.47 19.39 5.1 10.0
149 0.014 0.010 4.79 3.83 0.958 1.437 2.395 0.958 1.437 1.916 19.39 14.28 6.4 14.5
177 0.013 0.011 6.23 4.31 1.437 1.916 7.185 1.437 1.916 6.227 19.90 15.81 7.7 16.0
204 0.016 0.011 7.19 6.71 2.874 3.353 4.790 1.916 2.395 4.311 24.00 18.36 11.5 25.0

Fig. 2. Sepiolite base mud at different aging temperatures.

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HTHP water losses of the sepiolite drilling fluid samples

listed in Table 2 are desirable in terms of field usage even at
high temperatures. The water loss increases slightly from 3.2
ml/30 min at 37 °C to 16 ml/30 min at 177 °C. In comparison,
the water loss of bentonite base mud specified in API standard
is 15 ml/30 min at ambient condition[7]. The fluid loss of se-
piolite mud sample at 204 °C is slightly higher (25 ml/30 min)
than at lower temperatures, due to the polymer degradation at
temperatures above 177 °C.

2.2. PPA test results

Firstly, the plugging ability of sepiolite base mud without

CaCO3 was tested with ceramic discs with pore sizes of 10, 20,
and 35 micron at 2070 kPa (300 psi) and ceramic discs with
10, 20, 60, and 90 micron pore sizes at 6895 kPa (1000 psi)
Fig. 4. PPA test results with 20 μm pore size ceramic disc.
respectively. The test results are shown in Figs. 3-7, in which
the black dashed lines indicate data points before the 5th min-
ute, to minimize error, these data points weren’t used in the
evaluation. The evaluations of the test results are shown in
Tables 3 and 4.
For the sepiolite drilling fluid without CaCO3, the spurt loss
and total fluid loss tested with ceramic discs of different pore
sizes at 2070 kPa are very high (Table 3), and the PPA tests
with ceramic discs of 60 and 90 micron pore sizes at 6895 kPa
totally failed due to the excessive spurt loss (Table 4). It

Fig. 5. PPA test results with 35 μm pore size ceramic disc (2 070
kPa).

Fig. 6. PPA test results with 60 μm pore size ceramic disc (6 895
kPa).

can be seen from Fig. 8a too that the sepiolite base mud with-
out CaCO3 can’t form mud cake, and thus can’t plug the pores
of formation. The fibrous structure of sepiolite clay might be
the main reason that drilling fluid can’t plug formation pores
and is high in fluid loss.
The sepiolite drilling fluid with CaCO3 added has much
better plugging capacity, and much lower spurt loss and total
fluid loss (Tables 3 and 4). PPA tests results for mud samples
Fig. 3. PPA test results with ceramic disc of 10 μm pore size. containing CaCO3 are also depicted in Figs. 3-7. The plugging
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drilling fluid (Fig. 2). That is to say that the PPA test results at
149 C confirm the results obtained from rheological tests.
However, the HTHP filtration test results show the drilling
fluid has not very high fluid loss at 149 °C (Table 2), incon-
sistent with the PPA test results. Since both of the apparatus
basically measure the fluid loss at static condition, the differ-
ence could be due to the applied pressure direction. Moreover,
this may also related to the effectiveness of the additives at
around 149 °C. It can be seen from Tables 3 and 4 that in-
crease of pressure has positive effect on the plugging of
pores. At the same temperature (no more than 193 °C), the
plugging index obtained through PPA tests at 6895 kPa is
Fig. 7. PPA test results with 90 μm pore size ceramic disc (6 895
higher, indicating earlier initiation of internal plugging than at
kPa).
2070 kPa.
indexes of the drilling fluid tested with 10 μm, 20 μm and 35 PPA test results also show the drilling fluid has not enough
μm pore size ceramic discs at 27 C and 2070 kPa were 90.6%, plugging capacity at temperature above 193 °C (except in 20
95.6% and 94.5% (Table 3). Another sign that the sepiolite micron disc). The total fluid loss tested with 10 μm, 20 μm, 35
drilling fluid with CaCO3 can effectively plug pores is the μm pore size discs at 2070 kPa differential pressure and
formation of mud cake (Fig. 8b). 204 °C are 88.0 mL,126.4 mL and 220.0 mL respectively
In the test with 10 μm pore size ceramic disc (Fig. 3), the (Table 3), while the total fluid loss measured with 10 μm, 60
total fluid loss increases with the rise of temperature on the μm and 90 μm pore size discs at 204 °C and differential
whole, but abnormality occurred at 149 °C (Tables 3 and 4). pressure of 6895 kPa, are 262, 261.2, and 319 ml (Table 4).
The PPA tests with 20 µm, 35 µm, 60 µm, and 90 µm pore Observation of the mud cake mass on 35 µm pore size
sizes discs at 149 °C totally failed, with all drilling fluid lost, ceramic disc at different temperatures reveals the same
therefore, there is no corresponding data in Tables 3 and 4. conclusions (Fig. 9). Although the test is not completely same
This is related to the changes in the rheological properties of with the formation of mud cake in borehole, Fig. 9 shows the
the fluid system at 149 °C (Table 2), at this temperature, cal- mud cake has poor filtration properties at 204 °C. In addition,
cium carbonate particles settle down and precipitated from the Table 3 shows the ceramic disc with 20 micron pore size has
Table 3. Related parameters calculated using PPA test results with different pore sizes ceramic discs at 2070 kPa
Static filtration
Tempera- Plugging index/% Spurt loss/mL Total fluid loss/mL
rate/(mL·min1/2)
ture/C
10 μm 20 μm 35 μm 10 μm 20 μm 35 μm 10 μm 20 μm 35 μm 10 μm 20 μm 35 μm
1.6 0 2.6 10.0 14.0 19.0 2 3 3
27 90.6 95.6 94.5
(86.0) (209.0) (308.8) (106.0) (317.0) (348.0) (4) (20) (7)
65 80.0 92.4 90.7 3.2 5.2 0.8 21.2 24.0 32.4 3 3 6
93 75.1 91.8 89.7 1.2 7.6 0 26.4 26.0 36.0 5 3 7
149 51.5 / / 2.2 / / 51.4 / / 9 / /
177 58.1 87.7 86.1 2.0 5.0 0 44.4 39.0 48.2 8 6 9
193 37.7 80.0 77.5 0 0 0 66.0 63.4 78.4 12 12 15
204 17.0 60.1 36.8 0 6.4 10.4 88.0 126.4 220.0 17 22 38
Note: The figures in the brackets are results of sepiolite drilling fluid without CaCO3, “/”indicates total failure of test due to excessive spurt loss

Table 4. Related parameters calculated using PPA test results with different pore sizes ceramic discs at 6895 kPa
Plugging index/% Spurt loss/mL Total fluid loss/mL Static filtration rate/(mL·min1/2)
Tempera-
10 20 60 90 10 20 60 90 10 20 60 90 10 20 60 90
ture/C
μm μm μm μm μm μm μm μm μm μm μm μm μm μm μm μm
0 0.8 29.8 19.6 36.0 50.6 4 6 4
27 93.0 — 93.5 90.8 — — —
(220) (/) (/) (280.0) (/) (/) (11) (/) (/)
65 90.9 — 91.1 89.3 0 — 1.6 32.6 25.6 — 48.8 58.6 5 — 9 5
93 88.2 — 89.8 87.1 1 — 3.2 38.0 33.0 — 56.0 70.8 6 — 10 6
149 77.7 — / / 0 — / / 62.4 — / / 10 — / /
177 80.5 88.0 86.5 80.9 0 3 1.2 50.8 54.6 65.8 74.0 104.8 10 11 14 10
193 54.6 78.9 74.9 76.4 0 4 0 25.4 127.2 116.0 138.0 129.8 24 20 24 19
204 6.4 — 52.5 41.9 54 — 25.6 33.6 262.0 — 261.2 319.6 38 — 52 52
Note: The figures in the brackets are results of sepiolite drilling fluid without CaCO3, “/”indicates total failure of test due to excessive spurt loss;
and“—”indicates the experiment under the corresponding conditions was not conducted
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Fig. 8. Mud cake formed on 20 µm disc at 27 °C: a) base mud b)
sample with CaCO3.
Fig. 9. Mud cake formed in PPA tests on 35 µm discs at a) 27 °C
b) 193 °C c) 204 °C.
the highest plugging index at the same temperature and 2070
kPa, even at 204 °C, the plugging index reaches 60.1%.
2.3. Results of Scanning Electronic Microscope analysis
(SEM)
It can be seen from Fig. 10 that the most common pore di-
ameters of new ceramic discs with nominal pore sizes of 10
μm, 20 μm, 35 μm, 60 μm, 90 μm are 10 μm, 19 μm, 35 μm,
58 μm and 90 μm, almost the same as the nominal pore sizes.
The SEM images of ceramic disc in PPA test and the im-
ages after processed by ImageJ software are shown in Figs. 11
and 12. Due to the limited space of the paper, for the sepiolite
drilling fluid with CaCO3, only the images of 20 μm pore size
ceramic disc are given. Five areas on the SEM image of each
ceramic disc were selected randomly to calculate the pore area
percentage, and the results are shown in Tables 5 and 6.
In the PPA test of sepiolite drilling fluid without CaCO3 at
27 C, the used ceramic discs had similar pore area percentage
with new ceramic discs (Tables 5 and 6), which indicates the
Fig. 10. Frequency distribution of pore sizes of ceramic discs used in the PPA test.
 482 
sepiolite drilling fluid without CaCO3 can’t plug pores even at
ambient temperature.
In the PPA test of sepiolite drilling fluid with CaCO3, with
the rise of temperature, the pore area of used ceramic discs
increased before 149 °C, and then decreased after 149 °C (Ta-
bles 5 and 6). This could be related to rheological characteris-
tic of the sepiolite fluid system. Except the discs tested at 149
°C, discs used in other temperatures had much lower pore area
than new ceramic discs (Tables 5 and 6), indicating the sepio-
lite drilling fluid with CaCO3 has good solid suspension ca-
pacity, and can plug pores effectively. In addition, the sepio-
lite drilling fluid has good plugging effect at temperatures
higher than 149 °C, indicating its good thermal stability.
It can also be seen from Tables 5 and 6 that the sepiolite
drilling fluid has the best plugging effect for 20 µm pore size
ceramic disc, and the difference of pore areas of this disc be-
fore and after test is the largest; while the plugging effect of
the 10 µm pore size ceramic disc is the poorest. This is con-
sistent with the result of PPA test.
2.4. Validation of PPA test results using Ideal Packing
Theory
PPA results obtained in the previous section of the study
have been verified and evaluated with Ideal Packing Theory
(IPT) to get a deeper understanding on plugging ability of the
sepiolite fluid system. As ceramic discs of five pore sizes
were used in the PPA test simulating permeable formations,
five optimum particle distribution target lines using the se-
lected discs information were plotted based on “worst-case”
(Fig. 13), and the particle distribution of CaCO3 was plotted
on the same graph. The D90 obtained from the SEM analysis
was selected as the most representative pore size. According
to results shown in Fig. 10, the D90 of ceramic discs with
nominal pore sizes of 10 µm, 20 µm, 35 µm, 60 µm, and 90
µm are 32 µm, 65 µm, 143 µm, 180 µm, and 250 µm, respec-
tively. To reach ideal packing, the particle size distribution
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Fig. 11. SEM images of ceramic discs and pore area analysis (sepiolite mud without CaCO3) (a—i: 27 C and 2070 kPa; j—o：27 C and
6 895 kPa).

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Table 5. Pore area percentage of ceramic discs in the PPA test of sepiolite drilling fluid with CaCO3 at 2 070 kPa
Pore area percentage/%
Ceramic disc No. of the
New ceramic Used ceramic disc
pore size/μm observed area
disc 27 C 65 C 93 C 149 C 177 C 193 C 204 C
1 31.47 13.12(30.64) 17.53 17.66 27.52 13.89 13.72 13.06
2 33.23 13.56(32.81) 17.86 16.92 26.59 13.56 13.62 12.75
3 30.92 12.98(29.65) 16.54 18.02 26.98 14.52 12.48 12.82
10
4 30.05 12.35(29.32) 16.35 18.32 27.46 14.12 14.23 13.95
5 30.70 13.65(29.43) 17.98 17.95 28.24 13.42 14.02 13.04
Average 31.27 13.13(30.37) 17.25 17.77 27.36 13.90 13.61 13.12
1 28.78 7.94(28.19) 7.38 8.95 27.20 7.35 6.54 5.85
2 28.13 6.26(27.85) 7.02 9.57 26.58 6.35 5.80 5.35
3 29.67 6.52(27.67) 8.94 8.64 26.84 7.45 6.34 6.20
20
4 29.14 6.87(28.56) 6.98 9.24 27.68 6.52 5.75 5.42
5 29.52 7.06(28.94) 7.64 7.02 28.04 6.46 5.98 5.22
Average 29.05 6.93(28.24) 7.59 8.68 27.27 6.83 6.08 5.61
1 28.47 10.55(26.26) 11.54 12.82 27.54 10.55 10.27 8.93
2 29.51 11.35(28.25) 10.98 11.46 28.96 10.63 10.60 9.75
3 28.50 10.04(27.63) 10.53 10.67 27.44 10.24 11.02 10.04
35
4 29.42 9.85(27.90) 12.02 10.98 25.96 11.64 10.32 9.54
5 28.52 9.76(28.85) 10.42 11.92 26.82 11.86 10.06 9.62
Average 28.88 10.31(27.78) 11.10 11.57 27.34 10.98 10.45 9.58
Note: Figures in brackets are the results of sepiolite without CaCO3

Table 6. Pore area percentage of ceramic discs in the PPA test of sepiolite drilling fluid with CaCO3 at 6 895 kPa
Pore area percentage/%
Ceramic disc No. of the ob-
New ceramic Used ceramic disc
pore size/μm served area
disc 27 °C 65 °C 93 °C 149 °C 177 °C 193 °C 204 °C
1 31.47 10.66(26.26) 15.40 15.04 25.64 11.74 11.19 10.54
2 33.23 10.98(28.25) 15.98 16.89 26.89 12.04 10.85 10.06
3 30.92 11.34(27.63) 16.52 16.24 26.34 11.65 10.94 11.04
10
4 30.05 9.89(27.90) 14.34 16.64 25.98 12.52 11.96 11.85
5 30.70 9.64(28.85) 15.02 17.08 27.52 11.08 11.06 10.34
Average 31.27 10.50(27.78) 15.45 16.38 26.47 11.81 11.20 10.77
1 28.78 — — — — 6.10 5.81 —
2 28.13 — — — — 6.52 5.24 —
3 29.67 — — — — 5.85 5.98 —
20
4 29.14 — — — — 5.24 6.12 —
5 29.52 — — — — 6.84 6.34 —
Average 29.05 — — — — 6.11 5.90 —
1 29.14 9.75(28.54) 10.16 10.47 28.96 9.89 9.45 8.98
2 29.03 10.02(28.02) 11.20 11.50 27.56 10.20 9.24 9.43
3 28.32 9.64(29.34) 10.52 11.34 28.34 9.75 8.86 9.02
60
4 27.48 9.52(27.64) 9.82 10.02 27.64 9.56 9.62 8.76
5 29.00 9.95(26.96) 9.75 10.18 27.89 9.42 9.52 8.92
Average 28.59 9.78(28.10) 10.29 10.70 28.08 9.76 9.34 9.02
1 31.56 10.02(30.58) 11.22 12.50 30.25 10.12 9.54 9.03
2 33.00 9.58(29.64) 11.95 12.95 30.14 11.52 10.25 10.02
3 31.23 10.64(30.96) 12.32 11.82 29.53 11.62 10.52 9.98
90
4 31.51 10.92(29.34) 11.02 12.36 29.64 11.02 9.85 9.56
5 29.10 11.04(29.86) 10.86 13.02 30.02 10.94 10.24 10.24
Average 31.28 10.44(30.08) 11.47 12.53 29.92 11.04 10.08 9.77
Note: Figures in brackets are the results of sepiolite without CaCO3; “—”indicates no corresponding experiment was conducted

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Fig. 12. SEM images and pore area analysis (sepiolite mud with CaCO3) of 20 µm disc (at 2070 kPa).

sepiolite mud has fairly good rheological properties, low fluid

Fig. 13. Ideal particle size distribution of discs and particle size
distribution of CaCO3.
line of the bridging material should approximate the slope of
the formation target line and remain slightly below it. It can
be seen from Fig. 13, the target line of 20 µm ceramic disc
and the available bridging agent (CaCO3) distribution line are
the closest, therefore, validating the results of PPA test.
loss and strong solid suspension capacity at high temperature.
PPA tests show the sepiolite mud without calcium carbonate
can’t plug formation pores at any temperature, pressure and
pore size. In contrast, the sepiolite mud containing CaCO3 has
inadequate plugging ability only at 149 C (300 F) due to the
anomaly in its rheological behavior; but can effectively plug
pores in relatively short time and is low in filtration loss at
other testing temperatures. In the PPA test, plugging effect on
20 micron disc is the best, and this observation has been col-
laborated by IPT approach and SEM analysis. By considering
the results of rheology and PPT experiments, SEM analysis
and IPT, it can be inferred that the usage of sepiolite mud
validates the extension of the usage of CaCO3 as a loss circu-
lation material up to 193°C (380°F) with a highly acceptable
rheological and fluid loss properties.
In conclusion, sepiolite drilling fluid with CaCO3 has good
plugging capacity and thermal stability at high temperatures,
and is a good option for high temperature high pressure wells
with circulation loss.

3. Conclusions Acknowledgement
Rheological properties of the sepiolite mud decrease with We would like to thank ITU-BAP (The Scientific Research
the rise of temperature and to the minimum at 149 C, and Projects Coordination Unit of Istanbul Technical University)
then increases with the further increase of temperature. The for supporting and allowing us to publish the findings of this
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 ETTEHADI Ali et al. / Petroleum Exploration and Development, 2017, 44(3): 477–486

study. [3] ALTUN G, OSGOUEI A E. Investigation and remediation of

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