Copyright 2001, Society of Petroleum Engineers Inc.

This paper was prepared for presentation at the 2001 SPE International Symposium on Oilfield
Chemistry held in Houston, Texas, 1316 February 2001.
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Abstract
A simple and robust indentation test has been found to be
useful in evaluating shale additive performance, providing
results that correlate strongly with those of the much more
time-intensive high pressure hollow cylinder tests. This
method has been used to evaluate shale inhibitors and many
other common drilling fluids additives. Experiments have been
carried out with carefully prepared samples of Pierre 2 Shale
aged in different formulations. A ranking of shale strength
versus mud formulation has been constructed for the following
water based fluid additives: glycols (soluble and with Cloud
Point), salts (organic and inorganic), gypsum, and polymers
(Xanthan Gum, cationic, polyanionic cellulose). Based on the
X-ray diffraction pattern analysis of aged shale samples a
shape factor has been proposed to identify effective additives.
Introduction
During drilling shale is exposed to mechanical stresses and
drilling fluid interactions that can cause wellbore instability or
reduce overall process efficiency. In order to understand
which are the relevant parameters responsible for shale
behaviour, identify their relative importance and choose the
right laboratory experiments and conditions to test them, it is
important to make a distinction between wellbore walls and
cuttings
1
. The cuttings suffer a stress release at the moment of
their formation and, depending on the clean up efficiency in
the wellbore, their contact with the drilling fluid can last from
a few hours to days. On the other side, the wellbore walls
generally maintain their rock integrity and the stress release is
less with respect to the cuttings, but exposure to the drilling
fluid can be quite long and could even cause wellbore failure.
In both cases, the effect of the drilling fluids is related to
additives interaction with the rock matrix and pressure
propagation from the mud to the rock. This happens even
when additives to prevent mud filtrate invasion (silicates
2,3
and
oil in water emulsions
3
) or balance/reduce the formation pore
pressure by "osmosis"
2,3,4,5,6,7
are used.
In previous papers
3,4
pressure propagation from the mud to
the formation and ways to prevent it have been addressed from
the point of view of wellbore stabilization. In this work, the
interaction between shale and drilling fluids over a long time
scale has been investigated in order to identify shale strength
variations for wellbore stability and cuttings dispersion.
Several commercial shale additives have been ranked by
indentation test and X-Ray Diffraction analysis. Both these
approaches give a clear indication of the pronounced impact
that the drilling fluid additives have on shale structure and
behaviour. Particularly X-Ray diffraction analysis of
morphological alterations induced by additives in the smectitic
clay fraction of the rock has furnished a useful basis to
develop a criterion for a quick additives performance
evaluation.
Experimental
Materials
Shale. A fully-saturated outcrop shale (Pierre 2 Shale)
from South Dakota (U.S.A.), with activity very close to 1, has
been used; the mineralogical composition, physical properties
and pore water composition are reported in Tables 1A-D. The
reconstituted pore fluid used in the experiments was a 2.5
g/litre sodium chloride solution.
Drilling fluids additives. A combination of commercial
additives has been selected to prepare drilling fluids with
simplified compositions: potassium and sodium salts
(chloride, nitrate, carbonate, and acetate), three polyglycols
with Cloud Point (CP A, CP B and CP C), three soluble
polyglycols (SG A, SG B, SG C), an inhibitive cationic
polymer, a low molecular weight poly-anionic cellulose, a
viscosifying polymer (Xanthan Gum), and a Gypsum mud.
Salts have been used at a concentration of 0.67 mole/litre
(corresponding to 5% w/w concentrations of potassium
chloride). As a reference, two paraffinic oils with different
viscosity have been selected.
A few tests have been conducted with more complex
drilling fluid formulations. These are listed in Table 2: Z is a
dispersant, P a filtrate reducer, E a lubricant, S an asphalt, K a
salt, H a glycol, A and Si, inorganic additives.
SPE 65001
Water-Based Muds and Shale Interactions
S. Carminati, SPE, L. Del Gaudio and G. Del Piero, EniTecnologie S.p.A., and M. Brignoli, SPE, ENI-Agip Division
2 S. CARMINATI, L. DEL GAUDIO, G. DEL PIERO, M. BRIGNOLI SPE 65001
Methods
Hollow Cylinder Test (HCT). This method has been
developed to characterise the shale mechanical behaviour. Fig.
1 shows the experimental set-up. A hollow shale sample
(external diameter 25.4 mm, internal diameter 10 mm, length
15 mm) is hosted in a high pressure (P
max
=300bar), high
temperature (T
max
=120C) tri-axial cell. The confining
pressure is applied on the hollow rock sample through a rubber
sleeve, the axial pressure through a stainless steel head, the
pore pressure (externally to the sample) and the mud pressure
(internally to the sample) through independent reservoirs by
two high pressure pumps (High Performance Liquid
Chromatography). Pressures have been recorded by
piezoelectric transducers.
Test procedure: experiments are conducted according to
the following steps:
1. Shale aging: the hollow shale sample is left in different
formulations for 8 days at 80C.
2. Shale consolidation: equilibration for two days at room
temperature, with confining pressure at 200 bar, pore and
drilling fluid reservoirs at 100 bar. The pore fluid
reservoir is filled with simulated pore water (2.5g/litre
sodium chloride), and the mud circuit with a paraffinic
oil.
3. Drilling fluid evaluation: after consolidation the mud
pressure is decreased step by step (5 bar every 5 minutes).
Pressures are continuously recorded. The experiment ends
when the shale sample breaks.
Indentation test. This test gives an index of the rock
hardness
8,9
. Small cubic pieces of Pierre 2 Shale, with
precisely oriented bedding plane, are aged at 80C for 12 days
in different drilling fluids. After aging, they are embedded
with their bedding plane in a horizontal position in acrylic
resin to form a disk and then grounded to uncover the upper
surface of the shale. Each cutting is indented to a maximum
penetration of 0.3 mm at a speed of 0.01 mm/s (Fig. 2). The
slope of the initial linear portion of the loading curve gives the
rock hardness (indentation index).
X-Ray Diffraction. XRD powder patterns have been
collected using a Siemens D500TT diffractometer, CuK
radiation (=1.5418 ) and the step-scan acquisition method.
The 2 range of collection was 270 with step = 0.03 and
acquisition time chosen between 12 and 24 per step. Sample
have been analyzed after grinding (random XRD powder
pattern) and after the conventional extraction and treatment of
the clay fraction (oriented, glycolated and calcined sample).
The crystalline phases have been identified by means of
search-match method using the Siemens Diffrac AT software
and the JCPD database. Quantitative analysis has been
performed with the SYROQUANT package (vers. 2). Some
structural data were taken from the ICSD (Inorganic Crystal
Structure Database). Accurate d spacing () and integrated
intensities (a.u.) have been obtained applying the "full profile
fitting" method by means of the Siemens FIT software.
Results and Discussion
The main objectives of this activity are the study of the
interactions between shale and drilling fluids, and their
consequences on wellbore stability and cuttings dispersion,
and the research of a method that can help in quickly
classifying the additive performance.
Hollow Cylinder and Indentation Tests
Wellbore stability analysis is a very complex matter, making it
difficult to find methods that can be used to quickly rank many
additives in a representative way. The most reliable tests are
the ones that simulate high pressure and high temperature
downhole conditions, with the top simulators that can afford
drilling with real mud circulation and wellbore stability
analysis
6
. The drawback is that they are very expensive and
time consuming. In our experiments downhole conditions for
additive performance evaluation have been reproduced with a
hollow cylinder apparatus. These tests have been then
correlated with the simpler and robust indentation test.
Fig. 3 presents typical experimental results from hollow
cylinder tests: confining and axial pressures are kept constant,
mud pressure has been decreased step by step (5 bar every 5
minutes), and the pore pressure has been allowed to freely
change. Curve A is for a sample that is able to totally sustain
the confining and axial load without collapsing for any mud
pressure (from 200 bar to 0 bar). Curve B shows the recorded
mud pressure when wellbore collapse is approaching; a strong
signal of this is the mud pressure increase due to the effect of
the collapsing sample.
In Table 3 are reported the experimental results of hollow
cylinder tests on shale samples aged in different solutions with
glycols and potassium salts. The solutions that increased the
shale strength are the mixture between KCl and glycols
(soluble and with Cloud Point); the samples aged in these
solutions were able to keep the whole confining and axial
pressures with zero mud pressure without breaking. On the
contrary both the sample aged in the KCl solution and glycol
(with Cloud Point) solution failed respectively at 45 and 60
bar, showing a relative better effect for the KCl.
These results have been compared with those from
indentation tests. Traditionally this test gives an indication of
the material hardness, and a correlation with the uniaxial
compressive strength has been found for more consolidated
and brittle rocks
10
that present a fragile failure under loading.
Soft shale behaves quite differently: they rarely break under
loading, and present variations on the curve slope. Fig. 4
shows some typical results in a sort of "elastoplastic"
behaviour; the curves start with a certain slope (hardness) and
reach a maximum load (the maximum in the applied force)
before the elastic unloading. To be noticed that the harder
shale (Curve I) has the lower maximum load, and such a
behaviour in the case of competent rocks is strictly related to a
better wellbore stability.
Table 3 shows the comparison between indentation and
hollow cylinder tests for a Pierre 2 Shale. Having such a
characteristic shape, two parameters have been reported for
SPE 65001 WATER-BASED MUDS AND SHALE INTERACTIONS 3
indentation curves: hardness (a standard parameter defined as
the slope of the initial part of the curve), and the maximum
load previously mentioned (a non-standard parameter to define
the peak of the curve). Contrary to expectations, from these
results the maximum load shows a better correlation with
shale stability rather than the standard hardness. Actually a
sample with high hardness and medium load, like the one aged
in KCl, does not show a good wellbore stability, while the
samples with medium hardness and high maximum load (like
the samples aged in the glycol/KCl solutions) show a very
good stability. This fact agrees with the idea that KCl induces
a fragile hardening of the shale sample, and seems to be
reflected by a high hardness with a low maximum load. This
correlation opens a perspective to rank additive performance
on shale strength by indentation rather than hollow cylinder
test.
Based on this idea many other indentation tests have been
performed on shale samples aged in different solutions. Six
different glycols (three soluble and three with Cloud Point)
have been analyzed, and compared with other commercial
additives that are normally employed in water based drilling
fluids: organic and inorganic salts, low molecular weight
cationic and anionic polymers, high molecular weight
polymers (Xanthan Gum), and a gypsum mud. Figs. 5-9
present the maximum load from indentation tests normalized
with respect to the value obtained before aging. The following
overall distinctions can be made for the additives tested: (1)
The low molecular weight polyanionic cellulose and a soluble
glycol decrease the shale maximum load down to the value of
the shale sample aged in pure water. (2) There is a family of
additives that do not alter the maximum load (sodium salts,
glycols, and their combinations, Xanthan Gum, gypsum mud
and the paraffinic oils). (3) A family that improves the shale
performance from two to four times the maximum load of the
virgin shale (potassium salts, potassium salts with glycols,
cationic polymer, Xanthan Gum and the low molecular weight
polyanionic cellulose); among them one of the glycols with
Cloud Point is particularly effective, even at low concentration
(2% w/w) if used in combination with potassium carbonate
(3% w/w).
According to the standard practice in shale additive
evaluation
13
, this ranking is expected to be valid for cuttings
dispersion as well.
X-Ray diffraction
This technique has been used to study the additives
mechanism of action. Additives can modify the clay interlayer
spacing, and from the extent of this modification a few
speculations of their performance have been drawn. This kind
of analysis has been performed on the shale samples after
aging in the same solutions where cuttings for indentation test
have been aged. No clear correlation were found between the
interlayer spacing (random, oriented and glycolated) and the
maximum load from indentation tests (Fig. 10): the same
interlayer spacing can be associated with either high or low
normalized maximum load values.
Studying in detail the XRD pattern, in addition to the
differences of the interlayer spacing, the smectite in the
glycolated samples shows differences in shape, intensity and
broadening in dependence on the additive used (Fig. 11).
These differences can be appreciated from the 002 intensities,
scaled on the same weight of sample, and the f.w.h.m. (full
width at half maximum). Nevertheless, in order to compare the
samples using a single number (a sort of figure of merit), the
intensities and f.w.h.m. were combined according to the
equation: S=I(002)/[f.w.h.m. *1000]. In practice, the shape
factor S is a sort of peak height in an arbitrary scale which
depends on peak intensity and "broadness". Representing on
the same graph both the shape factor S and the maximum load
(Fig. 12), turns out that the aged Pierre 2 Shale samples with
high maximum load are in the region with S less than 2, while
the shale samples with low maximum load are in the region
with S above 2.
After the analysis of the effects of simple mixtures on X-
Ray Diffraction patterns in relation with shale mechanical
behaviour, a few test have been run with complex
formulations. Table 2 shows formulations and results. It turns
out that glycols with potassium chloride, cationic polymers
and silicates are the additives that most improve shale
strength, and the shape factor S is less than 2.
An explanation of the physical meaning of the shape factor
S is related to order and concentration of the smectite layers in
the shale matrix. For a given smectite content, high S value
means an ordered stacking of layers, while low S value (less
than 2) means a disordered stacking of layers. That is, shale
strengthening is favored by a disordered shale structure.
Among the additives that proved to be effective there are the
glycols with Cloud Point. In principle this kind of glycol
should phase separate and act by blocking pores. On the
contrary, as demonstrated by the increased interlayer spacing
(d random) in Table 2, they penetrate into the pores of the
shale and interact with the smectite platelets. Another
important aspect that can be pointed out is the close value in
interlayer spacing (d random) found for glycols with KCl and
cationic polymers suggesting that the best performance can be
reached if an optimum value around 14.5 is observed.
This procedure has been proved to be effective for an
outcrop shale with a high smectitic content. If this criteria to
classify additives performance is valid for any kind of shale
there is the strong advantage that the experimental procedure
is applicable when all the other techniques fail: particularly,
small pieces of shale samples can be used without any
problem (XRD sample must be ground before analysis and
does not require large pieces of shale) or desaturated shale can
be aged in different solutions.
This criteria can open a new way in additives evaluation
for shale strengthening both for wellbore stabilization and
cuttings dispersion.
4 S. CARMINATI, L. DEL GAUDIO, G. DEL PIERO, M. BRIGNOLI SPE 65001
Conclusions
A correlation between hollow cylinder and indentation tests
has been found to characterize the mechanical behaviour of
shale for wellbore stability and cuttings dispersion predictions.
Many additives have been ranked and good shale
hardening has been found for silicates, cationic polymers and
for combinations of glycols and potassium salts, even at low
concentrations (2-3% w/w).
An original shape factor from X-Ray diffraction patterns
has been introduced in our analysis that proved to be effective
in discriminating between additives performance on Pierre 2
Shale strength (high smectitic content).
Acknowledgements
We thank ENI-Agip Division for its support and permission to
publish this paper. A particular acknowledgement goes to Mr.
A. Omini (EniTecnologie S.p.A.), and M. Rossi (ENI-Agip
Division) for their invaluable contributions in running hollow
cylinder tests.
References
1. Van Oort, E,: "Physico-Chemical Stabilization of Shales", paper
SPE 37263 presented at the 1997 SPE International Symposium
on Oilfield Chemistry, Houston, Texas, 18-21 February.
2. van Oort, E.: A Novel Technique for the Investigation of
Drilling Fluid Induced Borehole Instability in Shales, paper
SPE/ISRM 28064 presented at the 1994 SPE/ISRM Conference
on Rock Mechanics in Petroleum Engineering (Eurock 94),
Delft, The Netherlands, Aug. 29-31.
3. Carminati, S., Del Gaudio, L., and Brignoli, M.: "Shale
Stabilization by Pressure Propagation Prevention", paper SPE
63053 presented at the 2000 SPE Annual Technical Conference
and Exhibition, Dallas, Texas, 1-4 October 2000.
4. Carminati, S., Del Gaudio, L., Zausa, F. and Brignoli, M.: "How
do Anions in Water-Based Muds Affect Shale Stability?", paper
SPE 50712 presented at 1999 SPE International Symposium on
Oilfield Chemistry, Houston, Texas, 1619 February 1999.
5. Mody, F.K. and Hale, A.H.: A Borehole Stability Model to
Couple the Mechanics and Chemistry of Drilling Fluid Shale
Interaction, paper SPE/IADC 25728 presented at the 1993
SPE/IADC Drilling Conference, Amsterdam, The Netherlands,
Feb. 23-25.
6. Simpson, J.P., Walker, T.O., and Aslakson, J.K.: "Studies
Dispel Myths, Give Guidance on Formulation of Drilling Fluids
for Shale Stability", paper IADC/SPE 39376 presented at the
1998 SPE/IADC Drilling Conference, Dallas, Texas, 3-6 March.
7. Bol, G.M., Wong, S-W, Davidson, C.J. and Woodland, D.C.:
Borehole Stability in Shales, SPE Drilling & Completion,
(June 1994), 87-94.
8. Szwedzicki, T.: Indentation Hardness Testing of Rock,
Technical Note on the Int. J. Rock Mech. Min. Sci. & Geomech.
Abstr. (1998), 35, 825-829.
9. Zausa, F. and Santarelli, F.J.: A New Method to Determine
Rock Strength from an Index Test on Fragments of Very Small
Dimension, paper presented at the 1995 ISRM International
Congress on Rock Mechanics, Tokyo, September.
10. Zausa, F., Civolani, L., Brignoli, M., and Santarelli, F.: "Real
Time Wellbore Stability Analysis at the Rig Site"; paper SPE
37670 presented at the 1997 SPE/IADC Drilling Conference,
Amsterdam, The Netherlands, 4-6 March.
11. Horsrud, P., Holt, R.M., Sonstebo, E.F. and Bostrom, B.: Time
Dependent Borehole Stability: Laboratory Studies and
Numerical Simulations of Different Mechanism in Shale, paper
SPE/ISRM 28060 presented at the 1994 SPE/ISRM Conference
on Rock Mechanics in Petroleum Engineering (Eurock 94),
Delft, The Netherlands, Aug. 29-31.
12. Marsala A., Brignoli M., Del Gaudio L., Carminati, S.: "Water
Based Drilling Fluid Evaluation: Acoustic on Cuttings Reveals
Geomechanical Modifications Induced on Shale Formations", to
be presented at the 2001 Offshore Mediterranean Conference,
Ravenna, Italy, March 28-30.
13. Reid, P.I., Harrington, P.M. and Minton, R.C.: "Shale Tests
Help Develop Inhibitive Water-Based Muds"; Ocean Industry,
October 1991, pp. 19-24.
SI Metric Coversion Factors
ft x 3.048 E-01 = m
in. x 2.54 E+02 = m
ft
2
x 9.290 304 E-02 = m
2
psi x 6.894 757 E-03 = MPa
bar x 1.0 E+01 = MPa
lbf x 4.448222 E+00 = N
lbf/100ft
2
x 4.788 026 E-01 = Pa
TABLE 1A- Pierre 2 Shale:
mineralogical composition
Mineralogy % w/w
Quartz 25
Feldspar 4
Dolomite 2
Pyrite 1
Siderite 1
Calcite 3
Total Clay 64
TABLE 1B- Pierre 2 Shale:
clay fraction
% w/w
Kaolinite 5
Chlorite 1
Illite 30
Smectite 50
Mixed-Layer 14
TABLE 1C- Pierre 2 Shale:
physical properties
Bulk Density 1.98g/cc
Grain Density 2.56g/cc
Porosity 33 %v/v
Moisture Content 20% w/w
Cation Exchange Capacity 35meq/100g
Indentation Index (cuttings in
resin disk)
140N/mm
Permeability to Simulated Pore
Water
(Confining Pressure: 200bar,
Pore Pressure:100bar)
50-100nDarcy
SPE 65001 WATER-BASED MUDS AND SHALE INTERACTIONS 5
TABLE 1D- Pierre 2 Shale:
pore water composition
(collected by squeezing)
Ion Concentration (mg/litre)
chloride 1139
calcium 7
magnesium 4
sodium 1097
potassium 6
TABLE 2. Relation between maximum load and XRD results
for cuttings aged in different solutions
Fluid
composition
Normalized
maximum
load
d ()
random
d ()
oriented
d ()
glycolated
Shape
factor
S
Virgin shale 1.0 13.5 13.9 17.1 5.9
Water 0.8 14.8 15 17.3 7.6
Cationic 2.3 14.3 14.4 17 1.2
CP A, KCl 4.4 14.6 14.6 16.4 0.6
CP A 1.1 15.3 14.8 17.7 3.1
CP B, KCl 4.1 14.8 14.4 18 0.9
CP B 1.0 16.3 14.9 17.6 4.3
CP C, KCl 4.1 14.4 14.5 16.9 0.8
CP C 1.0 15.2 15.4 17.7 2.3
SG A, KCl 3.2 14 14.2 16.1 0.8
SG A 1.0 14.1 14.2 17.4 6.5
SG B, KCl 3.0 14.2 14.3 14.6 1.4
SG B 0.9 14.4 17.1 17.3 2.7
SG C, KCl 3.5 13.5 14.3 14.3 0.4
SG C 1.3 13.9 13.9 17.2 3.5
ZPE 0.9 14.5 14.4 17.4 7
S 0.8 11.7 12.1 17.3 6
SZEK 2.3 12.3 14.3 18.1 0.8
Si 2.1 11.6 12.2 18.1 1.4
SiZK 3.3 12.3 13.9 16 0.6
HE 0.7 12.8 13.7 17.4 5.3
HSiSPEK 3.9 12.7 13.8 15.7 0.4
HSiSZPK 4.3 13.9 14 15.6 0.4
A 1.0 12.7 12.7 17.1 8.6
AHPE 1.0 13.3 12.9 17.1 6.9
AHSZE 1.2 13.3 12.8 17.1 7.6
AHSiSZEK 3.7 13.6 14 15.5 0.5
TABLE 3. Comparison between indentation (hardness and
maximum load) and hollow cylinder test (Pmud) on Pierre 2
Shale samples aged at 80C for 12 days. The lower the mud
pressure at collapse the more stable is the hole.
Additives in
solution
Hardness
(N/mm)
Maximum
load
(g)
Pmud at
collapse
(bar)
KCl 0.67 M 229 2913 45
CP B 5% w/w 68 1509 60
CP B 5% w/w, KCl 0.67 M 192 5389 0
SG A 5% w/w, KCl 0.67 M 192 4096 0
Figure 1. View of the hollow cylinder cell with control on confining
pressure, axial pressure, pore pressure and mud pressure.
Figure 2. View of the cuttings embedded (after aging) in a resin
disk with the needle used for indentation tests.
P
axial
Pump
P
mud
Mud circuit
P
pore
P
conf
6 S. CARMINATI, L. DEL GAUDIO, G. DEL PIERO, M. BRIGNOLI SPE 65001
Figure 3. Hollow cylinder test results on Pierre 2 Shale aged for 8 days at 80C in a glycol solution with Cloud Point (5% w/w) and potassium
chloride at 5% w/w (Curve A) and a solution with the same glycol alone (Curve B). The first sample (Curve A) is able to bear the load even with
0 mud pressure, while the second one breaks at the mud pressure around 60 bar.
Figure 4. Curves from indentation tests on cuttings aged at 80C for 12 days in a potassium chloride water solution (concentration 0.67
mole/L) alone (Curve I) and in combination with a glycol with Cloud Point, CP, (Curve II). The maximum load is the peak value of the force
required to penetrate the cuttings at a fixed depth. Hardness is the slope of the curve (N/mm).
0
0.2
0.4
0.6
0.8
1
1.2
0 0.2 0.4 0.6 0.8 1 1.2
Normalized depth
N
o
r
m
a
l
i
z
e
d

f
o
r
c
e
CP B, KCl KCl
0
20
40
60
80
100
120
140
160
180
0 20 40 60 80 100 120 140 160 180 200
Time (minutes)
M
u
d

p
r
e
s
s
u
r
e

(
b
a
r
)
CP B, KCl CP B
Curve A
Curve B
Maximum
load
Hardness
Curve II
Curve I
SPE 65001 WATER-BASED MUDS AND SHALE INTERACTIONS 7
Figure 5. Normalized maximum load from indentation tests. Cuttings have been aged at 80C for 12 days in water, in two different paraffinic
oils, sodium and potassium salts water solutions (concentration 0.67 mole/L referred to the cation). Native Pierre 2 Shale hardness has been
taken for comparison.
Figure 6. Normalized maximum load from indentation tests. Cuttings have been aged at 80C for 12 days in different solutions of soluble
glycols (SG) at a concentration of 5% w/w, mixed with potassium and sodium salts (concentration 0.67 mole/L referred to the cation).
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
SG A SG A, NaCl SG A, Na2CO3 SG A, KCl SG A, KNO3 SG A, K2CO3 SG A,
CH3COOK
N
o
r
m
a
l
i
z
e
d

m
a
x
i
m
u
m

l
o
a
d
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
Shale H2O OIL A OIL B NaCl Na2CO3 K2CO3 CH3COOK KNO3 KCl
N
o
r
m
a
l
i
z
e
d

m
a
x
i
m
u
m

l
o
a
d
8 S. CARMINATI, L. DEL GAUDIO, G. DEL PIERO, M. BRIGNOLI SPE 65001
Figure 7. Normalized maximum load from indentation tests. Cuttings have been aged at 80C for 12 days in different solutions of glycols with
Cloud Point (CP) at a concentration of 5% w/w, mixed with potassium and sodium salts (concentration 0.67 mole/L referred to the cation).
Figure 8. Normalized maximum load from indentation tests. Cuttings have been aged at 80C for 12 days in different water solutions.
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
Xanthan Xanthan, KCl Xanthan, KCl,
SG A
Cationic Cationic,
CH3COOK
Cationic, KCl CP A 2% w/w CP A 2% w/w,
K2CO3 3%
w/w
Gypsum mud Pac-LV Pac-LV, KCl
N
o
r
m
a
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d

m
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x
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m

l
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d
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
CP B CP B, NaCl CP B, Na2CO3 CP B, KCl CP B, KNO3 CP B, K2CO3 CP B,
CH3COOK
N
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m
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d

m
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m

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d
SPE 65001 WATER-BASED MUDS AND SHALE INTERACTIONS 9
Figure 9. Normalized maximum load from indentation tests. Cuttings have been aged at 80C for 12 days in water, in different solutions of
glycols with Cloud Point (CP) and soluble glycols (SG) at a concentration of 5% w/w, and mixture with potassium chloride (concentration 0.67
mole/L). Native Pierre 2 Shale hardness has been taken for comparison.
Figure 10. Interlayer spacing (random, oriented and glycolated) from XRD against normalized maximum load from indentation tests of
cuttings aged in different solutions (Table 2).
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
Shale Water CP A,
KCl
CP A CP B,
KCl
CP B CP C,
KCl
CP C SG A,
KCl
SG A SG B,
KCl
SG B SG C,
KCl
SG C
N
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m
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d

m
a
x
i
m
u
m

l
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10
11
12
13
14
15
16
17
18
19
20
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0
Normalized maximum load
I
n
t
e
r
l
a
y
e
r

s
p
a
c
i
n
g

(
A
n
g
s
t
r
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m
)
d () random d () oriented d () glycolated
10 S. CARMINATI, L. DEL GAUDIO, G. DEL PIERO, M. BRIGNOLI SPE 65001

5 10 15 20
2-theta ()
I (a.u.)
A
B
Figure 11. XRD patterns (glycolated) on cuttings aged at 80C for 12 days in different solutions without KCl (A) and with KCl (B). The shape
factor S has been computed as the ratio between the intensity peak high (I 002) after background subtraction and the full width at half
maximum (f.w.h.m.) multiplied for 1000 [S=I(002)/(f.w.h.m.*1000)].
Figure 12. Shape factor S from XRD patterns against normalized maximum load from indentation tests on virgin shale and cuttings aged in 26
different solutions prepared with commercial additives for water based drilling fluids (Table 2). The formulations that increase the shale
strength have the shape factor S less than 2.
0
1
2
3
4
5
6
7
8
9
10
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0
Normalized maximum load
S
h
a
p
e

f
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t
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