Journal of Petroleum Science and Engineering 205 (2021) 108909

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Journal of Petroleum Science and Engineering

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Experimental investigation of deterioration in mechanical properties of

oil-based mud (OBM) contaminated API cement slurries & correlations for
ultrasonic cement analysis
Nachiket Arbad a, Fernando Rincon a, Catalin Teodoriu a, *, Mahmood Amani b
a
The University of Oklahoma, USA
b
Texas A&M, Qatar

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

Keywords: Well construction, well abandonment and restoration of well integrity are the reasons at a broad level why
Oil-based mud (OBM) cementing jobs are performed. During well construction phase, the primary objective of cementing job is to
Contamination replace the drilling mud in the annulus with pure cement. Intermixing of the drilling mud and the cement slurry
API Cement
produces unpumpable mixture, especially in the case of OBM. As literature review suggests the displacement
Ultrasonic pulse velocity (UPV)
efficiency of spacers and pre-flushes used to displace the drilling mud is not 100%, cement slurries are
contaminated with drilling mud left behind the casing. Recently, several research groups have performed studies
to understand the strength development phenomenon of OBM contaminated cement slurries, but they failed to
document properly the experimental procedures used and correlations for the strength development of OBM
contaminated cement slurries.
The primary aim of this study was to develop a standard laboratory experimental procedure for understanding
the strength development of OBM contaminated cement slurries and develop correlations for future references.
This extensive study was carried out on API Class C cement samples cured at room temperature and elevated
temperature. Destructive as well as non-destructive tests were performed on the contaminated as well as un­
contaminated cement samples to measure the uniaxial compressive strength (UCS) and the ultrasonic pulse
velocity (UPV) respectively. Results obtained from these tests showed deterioration in the strength of cement
samples as the OBM contamination increases. Correlations for early strength development of OBM contaminated
cement slurries were developed using the test results. These correlations developed would help the operators in
better estimation of the strength developed by the OBM contaminated cement slurries. In other words, better
estimation of weight on cement (WOC) time using the more accurate strength development correlations.

1. Introduction
The basic purpose of casing cementation is to provide the necessary
structural assistance to casings & liners along with other purposes like
zonal isolation and corrosion inhibition. The primary cementing oper­
ations aims to replace the drilling mud present behind the casing with
pure cement slurry. Displacing drilling mud with cement slurry causes
contamination of the cement slurry with drilling mud and forms
unpumpable mixture. Such contamination also hinders the cement hy­
dration process and affects the mechanical and rheological properties of
the cement slurry. Spacers are pumped to avoid intermixing of cement
slurry and drilling mud. Flushes or pre-flushes are pumped ahead of
spacers and cement slurry to improve the mud displacement efficiency
and reduce the contamination of cement slurry with drilling mud
(Bourgoyne et al., 1984; IADC, 2000; Rabia, 2002).
In 1973, laboratory testing of compatibility between the several
OBM mixtures, spacer systems and cement slurries were performed and
best combinations were successfully used in field (Morris et al., 1973).
The reduction in compressive strength of the cement slurry (cured for
24 h at 380 ◦ F) due to contamination with 10% OBM and 10% spacer
was 57% and 0.2% respectively. Similarly, at 50% OBM contamination
the strength reduction was 98% and for 50% spacer contamination the
reduction was 93%. Clearly OBM contamination proved to be more
harmful as compared to spacer contamination. In another study (Harder

* Corresponding author.
E-mail address: cteodoriu@ou.edu (C. Teodoriu).

https://doi.org/10.1016/j.petrol.2021.108909
Received 25 August 2020; Received in revised form 29 April 2021; Accepted 30 April 2021
Available online 11 May 2021
0920-4105/© 2021 Published by Elsevier B.V.
N. Arbad et al. Journal of Petroleum Science and Engineering 205 (2021) 108909

Table 1 200 ◦ F) due to contamination with 10% and 40% OBM was 24% and
Cement compositions. 79% respectively. Similarly, with the addition of 2% ENP surfactants
Parameter/Cement Density Total Mc Mw MOBM reduction in strength was 23% for 10% OBM contamination and 57% for
Composition (kg/l) Volume (gms) (gms) (gms) 40% OBM contamination (Harder et al., 1992).
(ml) Findings from the previous study motivated Harder et al. (1993) to
Class C 1.776 600 683 382.48 – perform another study which analysed the reduction in the strength of
Class C + 0.6% ≈1.771 ≈605 683 382.48 ≈6 OBM contaminated cement slurries with respect to 4 different types of
OBM OBM prepared in laboratory with combinations of two base oils (mineral
Class C + 2.2% 683 382.48
oil and diesel oil) and two primary emulsifier (alkanolamide and stan­
≈1.757 ≈620 ≈24
OBM
dard fatty acid). The objective of this study was to understand and
optimize the OBM chemistry with respect to the cementing operation.
et al., 1992) it was found that the plugging operations in OBM needed The reduction in the cement strength was less when mineral oil was used
minimum of two to three attempts due to incompetent kick-off plug. as base oil compared to diesel oil. Similarly, greater strength was
Deterioration in strength of kick-off plug was caused due to OBM observed when alkanolamide was primary emulsifier as compared to
contamination of cement slurries. Depending upon the OBM contami­ standard fatty acid (Harder et al., 1993).
nation the WOC time to achieve the desired compressive strength varied Literature review reveals the advantages of using OBM for a partic­
greatly. In other words, increasing OBM contamination increased the ular field over water based mud eliminating several drilling problems
WOC time and/or the number of kick-off plug attempts. Addition of 1% associated with it and the challenges associated with cementing opera­
ethoxylated nonyl phenols (ENP) surfactants to the cement slurries tions in the presence of OBM. Case studies show the added benefits of
increased the compressive strength and greatly reduced the WOC time. using OBM instead of WBM solved several critical drilling challenges
Plugging operations in OBM were successful in their first attempt for a (Chambers et al., 2000; Emadi et al., 2015; Fleming et al., 2019; Fossum
three well program saving the cost involved for extra plugging attempts et al., 2007; Harold et al., 2015; Kabanov et al., 2014; Sheer et al., 2019;
because of addition of 1% ENP surfactants to cement slurries. The Sinha et al., 2017). As the usage of OBM gained popularity, researchers
reduction in compressive strength of the cement slurry (cured for 24 h at reexamined the mud-cement interaction to improve their understanding

Fig. 1. Cement sample dimension measurements.

Fig. 2. Dimensional analysis of cement samples.

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N. Arbad et al. Journal of Petroleum Science and Engineering 205 (2021) 108909

about the strength development of OBM contaminated cement slurries

Fig. 3. Test mark compressive strength test machine.
(Aughenbaugh et al., 2014; Katende et al., 2020; Li et al., 2015, 2016,
2016; Salehi et al., 2016; Soares et al., 2017; Vipulanandan et al., 2014).
Compatibility of the drilling fluid, spacer and cement slurry de­
termines the success of the project. Several studies were performed to
understand the drilling mud-spacer-cement compatibility (Rueda et al.,
2003) (Berg et al., 2002) (Guillot et al., 2007) (Shadravan et al., 2015)
(Shadravan et al., 2017) (Singh et al., 2017; Davison et al., 2001,
Nagarajan et al., 2010, Patel et al., 1999). In the present decade, several
research groups studied the OBM contamination of cement slurries and
the implications to the UCS development using various methods to un­
derstand the hydration phenomenon (Aughenbaugh et al., 2014; Li
et al., 2015, 2016, 2016; Olteanu and Teodoriu, 2020; Romanowski
et al., 2018; Soares et al., 2017; Vipulanandan et al., 2014). A compre­
hensive review of these studies reveals the lack of standardisation in the

Fig. 4. Avg. UCS vs Curing Time for Samples cured at 25 ◦ C.

Fig. 5. Avg. UPV vs Curing Time for Samples cured at 25 ◦ C.

Fig. 6. Avg. UCS vs Curing Time for samples cured at 75 ◦ C.

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N. Arbad et al. Journal of Petroleum Science and Engineering 205 (2021) 108909

Fig. 7. Avg. UPV vs Curing Time for samples cured at 75 ◦ C.

construction in particularly in Germany.

Table 2 Given the fact of OBM still being used and the need of lubricants in
Reduction in Avg. UCS of OBM contaminated samples cured at 25 ◦ C. water base muds are still common today, the cement contamination with
Class C @25 ◦ C 1 Day 3 Days 7 Days small amount of OBM needs in depth investigation. When OBM muds are
0% OBM 0 0 0 used, the proper design of a cement spacer should remove the most of
0.6% OBM 5% 31% 7% the OBM from the well, however given the fact that no spacer has a
2.2% OBM 16% 26% 22% 100% removal efficiency, it is expected that a small amount of OBM will
remain, especially at the surface of the casing and formation. During
cement pumping, this small amount of OBM will inevitably contaminate
Table 3
the cement and thus the need of the present study. As it will be shown
Reduction in Avg. UCS of OBM contaminated samples cured at 75 ◦ C. later, this study is trying to evaluate the short- and long-term cement
properties. Teodoriu and Olteanu (2020) have shown that the existence
Class C @75 ◦ C 0.17 0.25 0.33 1 Day 3 Days 7 Days
Day Day Day
of OBM contamination in cement it is not noticeable through ultrasonic
evaluation in early stages of cement hydration, leading to the impression
0% OBM 0 0 0 0 0 0
that the cement properties will remain undisturbed for long term curing
0.6% OBM 16% 1% − 6% 35% 38% 40%
2.2% OBM 30% 36% 27% 52% 52% 55% time. The present study is so far the only study comparing room tem­
perature and elevated temperature cement samples with and without
contamination for both short and long term, with major focus on UCS
experiments performed and inadequate experimental information pub­ and relationship to UPV. The results will provide an accurate data set for
lished makes it difficult to compare the results of different research future reference works on cement contamination.
group (Arbad and Teodoriu, 2020). Following sections will describe the methodology used for per­
When water base drilling muds are in use, small quantities of oil base forming experiments and discuss the results in detail.
products are used to improve lubrication properties. They will be
however found in small amounts during cementing process. 2. Materials and methods
Class C cements are generally used in shallow wells as well as in
underground storage applications, especially when drilling through salt. This section lists the materials used in the laboratory experiments
We have found that in Middle East class C cement is the most reported with their detailed specifications, sample preparation methods and de­
cement class in use. Also, we have found that class C cement was very tails of the equipment’s used in the study.
common in the eastern Europe, and lately it is used in cavern well

Fig. 8. Strength development for samples cured at 25 ◦ C.

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N. Arbad et al.
Fig. 9. Strength development for samples cured at 75 ◦ C.
Fig. 10. UCS vs UPV for Samples cured at 25 ◦ C.
2.1. Mold preparation
3-gang parallel stainless steel 2” cube molds supporting ASTM C109,
AASHTO T71 and AASHTO T106 standards were used for preparing the
cement samples. These cubes were lightly greased with dope to ensure
the easy removal of cement samples from the molds.
2.2. Sample preparation
This study was extensively carried out on API Class C cement for the
reasons presented in the introduction. The samples were prepared
following the API RP 10B-2: Recommended Practice for Testing Well
Cements. OBM which acts as a contaminant in this study was obtained
from a local operator in Oklahoma. Composition of 8.4 ppg OBM was as
follows: Diesel oil (73%), Water (19.6%) and Solids (7.4%). Petro-Mul
was used as the primary emulsifier in combination with Petro-wet as
the secondary emulsifier (Bri-Chem Supply LTD - Product Datasheet, n.d.
Bri-Chem Supply LTD,).
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Journal of Petroleum Science and Engineering 205 (2021) 108909
In this research study, three Class C cement compositions were tested
as follows:
• Class C cement – Density of 1.776 kg/l (also called as the API
Cement)
• Class C cement + 0.6% OBM (8.4 ppg) – Density of 1.771 kg/l
• Class C cement + 2.2% OBM (8.4 ppg) – Density of 1.757 kg/l
The cement was used as neat cement; hence no other additives have
been used. Neat cement experiments are always used as reference data
for any other experiments to understand the effect of additives or
contaminants.
Distilled water was used for sample preparation. The reason of using
distilled water, is given by the fact that tap water available in our lab­
oratory does not have constant properties, especially total dissolved
solid content, and thus, for good reference data all our cement samples
are mixed using distilled water. Saleh et al. (2018) have shown that the
water quality will affect the cement properties, especially short term
N. Arbad et al. Journal of Petroleum Science and Engineering 205 (2021) 108909

Fig. 11. UCS vs UPV for samples cured at 75 ◦ C.

data. API cement acts as a reference point to understand the behaviour

Table 4
of OBM contaminated cement samples. Table 1 shows the detailed
Correlations between UCS, UPV & Curing time.
cement compositions tested in this study.
Correlations Class C @25 ◦ C

UCS (MPa) & Curing time t (day)
0% OBM UCS = 9.4396*ln(t)+ 9.761
0.6% OBM UCS = 8.1913*ln(t)+ 8.037
2.2% OBM UCS = 6.8148*ln(t)+ 7.9785
Correlations Class C @75 ◦ C
UCS (MPa) & Curing time t (day)
0% OBM UCS = 5.1721*ln(t)+ 21.199
0.6% OBM UCS = 2.1971*ln(t)+ 14.294
2.2% OBM UCS = 1.8537*ln(t)+ 10.539
UCS (MPa) & UPV (m/sec)
UCS = 0.0773*e^(0.002*UPV)
UCS = 0.2247*e^(0.0016*UPV)
UCS = 0.8655*e^(0.001*UPV)
UCS (MPa) & UPV (m/sec)
UCS = 0.0773*e^(0.002*UPV)
UCS = 0.3574*e^(0.0015*UPV)
UCS = 0.1683*e^(0.0017*UPV)
2.3. Mixing procedure
Digital weighing scales were used to accurately measure the weight
of cement, water, and OBM. Cement slurries were mixed using the
OFITE - Model 20 Constant Speed Blender which conforms to API
Specifications (OFITE, 2018). Functionality of the blender was tested
prior to mixing all cement slurries. 382.48 g of distilled water was
poured in the mixing cup and 683 g of Class C cement was taken in a
container. According to API Specifications, the cement must be added to
mixing cup with distilled water within first 15 s when the motor of the
blender runs at constant rotational speed of 4000 RPM. As soon as the
cement is added cover the mixing cup with lid and after 15 s the motor of

Fig. 12. Comparison of strength development of 0% OBM contaminated samples at 25 ◦ C and 75 ◦ C.

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N. Arbad et al. Journal of Petroleum Science and Engineering 205 (2021) 108909

Fig. 13. Comparison of strength development of 0.6% OBM contaminated samples at 25 ◦ C and 75 ◦ C.

Fig. 14. Comparison of strength development of 2.2% OBM contaminated samples at 25 ◦ C and 75 ◦ C.

the blender will run at constant rotational speed of 12,000 RPM for next Precision™ Thermo Scientific water baths were used to cure the
35 s. samples at elevated temperatures.
Small modification was made to prepare the OBM Contaminated
cement samples. Specific OBM contamination was mixed with distilled
2.5. Samples dimensions
water prior to testing the functionality of the blender mixer.
Cement samples were carefully removed from the molds once they
2.4. Curing process
were cured. Digital calliper was used to measure the length and width of
the prepared cement samples. Three readings each of length and width
Cement slurry prepared following the API specification was poured
were taken as shown in Fig. 1.
into the lightly greased molds with constant speed till they were half
Average of the three readings were taken to get accurate measure­
filled. To remove the trapped air bubbles (if any), the molds were gently
ments (Romanowski et al., 2018). The target size of the prepared sam­
tapped followed by pouring the remaining slurries till it reaches the top
ples was approximately 50.8 mm or 2′′ in length, respectively width.
of the molds. Then, the molds cured at two different curing conditions
Dimensions of all the samples were with ±3% of the API recommended
for 4 h, 6 h, 8 h, 1 day, 3 day and 7 day –
value i.e. 2”. Average length and width of all samples is plotted in Fig. 2
showing majority of the samples dimension close to 2” or 50.8 mm.
• 25 ◦ C & atmospheric pressure
More than 100 samples have been used for the data shown in this
• 75 ◦ C & atmospheric pressure
paper. Additional 12 nonconform samples have been excluded from this
analysis since they were showing unexpected results, i.e. wrong

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N. Arbad et al.
dimensions or UCS.
2.6. UCS & UPV determination
Destructive as well as non-destructive tests were performed on the
accepted cement samples to measure the UCS and UPV values. Non-
destructive tests were performed using the Proceq™ Ultrasonic device
which has accuracy of ±2%. PosiTector™ Ultrasonic couplant was
applied to both the transducers to measure the UPV values. Every time
prior to measuring the UPV values the system was calibrated using the
calibration rod.
Destructive tests were performed using the Test Mark Compressive
Strength test machine after the UPV values were measured. Cement
samples were placed between the plates as shown in Fig. 3. Dimensions
of the cement samples were entered using the digital screen and load is
applied uniaxially on the cement samples. The device calculates the UCS
with accuracy of ±0.5% and displays it directly on the screen.
3. Results
Samples were prepared and cured based on the procedure described
above. Each data point presented in this paper is based on a minimum
three cubes tested for each curing temperature and time. If data varia­
tion was too large additional samples were prepared and new average
data point was generated. This procedure is also recommended by API
and ASTm standards. This section presents the results obtained from
destructive as well as non-destructive tests performed on the cement
samples. For simplicity, the values presented in this section are average
values of all the samples tested for a specific curing condition. Fig. 4
shows the destructive test results of strength development for samples
cured at room temperature.
For shorter curing time of 4hrs, 6 h & 8 h at room temperature the
cubes did not develop enough strength for the tests to be performed on
them. Conversely, it was possible to get results for shorter curing time of
4hr, 6hrs and 8 h at elevated temperature of 75 ◦ C. Fig. 5 shows the UPV
results for samples cured at 25 ◦ C.
Fig. 6 shows the average results of strength development for cement
samples cured at 75 ◦ C and Fig. 10 shows the non-destructive test (UPV)
results for samples cured at 75 ◦ C.
4. Discussions
The deterioration in the strength of cement samples is less or negli­
gible for shorter curing time as seen in Figs. 5 and 7. The effect of OBM
contamination on the strength is seen when the curing time is longer.
Most of studies performed by other research groups focused higher OBM
contaminations (5%, 10%, 25%, 50%) and shorter curing time ranging
from 1 to 3 days ((Harder et al., 1992) (Aughenbaugh et al., 2014) (Li
et al., 2016) (Soares et al., 2017)), however all studies have clearly
documented the decrease of UCS with the increase of contamination.
Tables 2 and 3 shows the percentage reduction in the strength of
OBM (0.6% and 2.2% OBM) contaminated cement samples cured at
room temperature and elevated temperature, respectively. The average
UCS value for samples cured at 25 ◦ C for 1 day with 0% OBM contam­
ination is 8.82 MPa while with 0.6% OBM contamination is 8.34 MPa
(Fig. 5). The percent reduction with 0.6% OBM contamination is
calculated by subtracting its UCS value from 0% OBM contamination
UCS value and then dividing it with 0% OBM contamination value.
Similar calculations were performed for 2.2% OBM contamination, and
the values are tabulated below.
At higher temperature, the UCS degradation of OBM contaminated
cement samples is much higher as compared to reduction in strength of
OBM contaminated cement samples at room temperature.
The reduction in the strength of cement samples is more than 50% for
2.2% OBM contamination cured at 75 ◦ C for one day. The reduction in
strength for 5% OBM contaminated Class C cement cured at ≈77 ◦ C for 1
8
Journal of Petroleum Science and Engineering 205 (2021) 108909
day was approximately 21% (Aughenbaugh et al., 2014). The differ­
ences in results may be due the type of OBM used in the experiment,
experimental procedures, and/or the equipment’s used in the studies i.e.
use of compression strength test machine instead of Ultrasonic Cement
Analyser.
Figs. 8 and 9 shows the strength development for all the samples
tested at 25 ◦ C and 75 ◦ C, respectively. The UCS values obtained from
destructive tests were plotted on y axis against the respective curing
time on x axis. Preliminary curve fitting and regression analysis were
performed to develop the correlations for strength development of
samples tested.
The reason for performing both destructive and non-destructive tests
was to get accurate data and develop correlations between UCS and
UPV. Prior to performing the destructive tests, the UPV values for all
samples were measured. Figs. 10 and 11 shows the UCS variation with
respect to UPV for samples cured at 25 ◦ C & 75 ◦ C, respectively.
Regression analysis were performed to develop correlations between
UCS & UPV. As expected, a little amount of contaminant (0.6%) does not
change the UPV response of the cement. However, also as expected and
presented by other papers (Teodoriu and Olteanu, 2020) the increase of
the OBD contamination over 2% shows a clear different relationship
between UCS and UPV, see Fig. 10.
At elevated temperatures (75 ◦ C) the contaminant effect on the UPV
response is also visible at lower concentrations. This is mainly because of
a faster UCS increase as a result of faster hydration process induced by
the elevated temperature. As shown in Fig. 11, three independent curves
can be noticed which represent the neat cement, 0.6% OBD contami­
nation and 2.2% OBD contamination respectively.
The correlations developed in this study are tabulated in Table 4.
Note the units for UCS is MPa, for UPV it is in m/sec and curing time t is
in days.
The correlation for UCS & UPV for 0% OBM contamination is same
for both 25 ◦ C & 75 ◦ C but the correlation for UCS & curing time is
different.
Fig. 12 through 14 shows the UCS comparison of the samples at 25 ◦ C
and 75 ◦ C versus curing time. As expected when neat cement is
compared the UCS at elevated temperature shows a higher value
compared with the samples at 25 ◦ C, see Fig. 12. However, when the
contaminated samples are compared, a different behavior is noticed.
The short term curing measured UCS data are as expected higher than
the samples at 25 ◦ C however, after 3 days for 0.6% contaminated
samples and about 1.5 days for 2.2% contaminated samples the
measured UCS is lower than the same UCS obtained at room tempera­
ture. This behaviour is very important for any well integrity applica­
tions, especially when long term behaviour is necessary. We assume that
this trend is because of the faster hydration process that takes place at
elevated temperature, which consumes the immediately available
water, while the contaminant will impede new water to move through
the cement to continue the hydration.
5. Conclusions
This paper shows the experimental intensive testing of cement class C
contaminated with small amount of oil base mud. Unlike previous
studies, this paper focuses on OBM contamination between 0 and 2.2%
OBM by weight of cement.
Our experiments revealed that OBM will affect specifically the long-
term mechanical properties of the cement rather than commonly
measured for 8 h and 24 h UCS. Tha data shows a decrease of 55% of
contaminated cement UCS cured for 7 days at 75 ◦ C. On contrary, at
room temperature the UCS loss is rather moderate with 20% for the
highest contamination level.
The main contribution of this paper is the newly developed UCS vs.
UPV correlations that show an alteration of the UPV response with the
increase amount of OBM contamination.
The paper shows for the first time that ultrasonic response highly
N. Arbad et al.
differs when contaminants are present. In particularly we have noticed
that the elevated temperature UCS vs. UPV curve are intersecting, with a
much flatter curve for elevated temperature samples. These observations
have a critical impact on the current ultrasonic cement analyser results
and the data reported. These findings are showing the importance of
ultrasonic calibration curves for each cement additive or contaminant.
Author contributions
All authors have read and agreed to the published version of the
manuscript. Conceptualization: CT, NA; Methodology: CT, NA; Formal
analysis, NA, CT, MA; Experimental work: NA, FR, CT; Writing—original
draft preparation, NA, CT; Writing-review and editing, CT; Editing
reviewer comments: NA, CT, MA; Supervision of experiments: CT Proj­
ect Acquisition MA, CT.
Funding
This publication was made possible by an NPRP award [NPRP 11S-
1126-170029] from Qatar National Research Fund (a member of The
Qatar Foundation). The statements made herein are solely the re­
sponsibility of the authors.
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.
Acknowledgments
We would like to thank to Central Plains Cement Company for their
support with cement materials. Many thanks to the Well Integrity Lab­
oratory at OU for granting access to the cement data base.
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