SPE-180319-MS

Cementing Design and Placement Methods to Optimize Seal Integrity and

Lower Cost for Deepwater Wells Drilled With Non-Aqueous Drilling Fluid

Paul Sonnier and Larry Watters, CSI Technologies; Dennis Clapper, Baker Hughes; Bill Head, RPSEA; George
Scherer, Robert Prod'homme, Myoungsung Choi, and Zhidong Zhang, Princeton University

Copyright 2016, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Deepwater Drilling & Completions Conference held in Galveston, Texas, USA, 14-15 September 2016.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
of the paper have not been reviewed by the Society of Petroleum Engineers and are subject to correction by the author(s). The material does not necessarily reflect
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consent of the Society of Petroleum Engineers is prohibited. Permission to reproduce in print is restricted to an abstract of not more than 300 words; illustrations may
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Abstract
The challenges of both primary and remedial cementing in Non-Aqueous Drilling Fluid (NAF) are well
known in the deepwater industry. NAFs allow for stable drilling in high pressure high temperature (HPHT)
and ultra-deepwater environments. However, mud properties that were beneficial for drilling become
detrimental to completions. Fluid incompatibilities resulting from contamination, residue, fluid swapping
and other fluid interactions can result in reduced compressive strength, channeling, downhole gelation and a
poor cement bond. Incompatibility and incomplete hole cleaning can result in safety and environmental risks
including job failure, future operational issues and loss of zonal isolation. Commercially available products
are available to assist with mud displacement, however, there is a need for a fundamental characterization
of mud-cement interactions on a chemical level to improve the knowledge of related technical risks and the
technology required for risk reduction and long-term well integrity.
The objectives of this project are to develop fundamental knowledge of mud-cement compatibility issues
related specifically to deepwater cementing, to quantify risks associated with cementing in NAF and to
develop best practices and derive recommendations in order to reduce the recognized risks.

Introduction
For temperature, pressure, and lithology encountered in drilling today's deepwater wells, optimized rate of
penetration and hole stability are achieved with NAF. However, NAF properties that were beneficial for
drilling become detrimental to completions. Operators drilling deepwater wells in the Gulf of Mexico focus
significant effort on designing spacer fluid systems to mitigate detrimental NAF consequences, but design
criteria do not all directly correlate to optimized cement seal performance. Spacer's required functions are
multiple and interdependent: separate the cement from NAF, sweep NAF from the well, be rheologically
compatible with NAF and cement, do not negatively affect cement performance properties when intermixed,
and leave well surfaces water wet for cement bond. Spacer systems may be over-designed to optimize one
function resulting in increased material and design cost. Alternatively, spacer fluid designs may focus on
one or two performance characteristics while discounting others which can increase risk of seal integrity.
2 SPE-180319-MS

NAF-Portland cement interactions during cementing can induce fluid gelation resulting in incomplete
NAF displacement from the annulus, degrade cement mechanical properties, and disrupt cement bond to
the pipe and bore hole1. This can in turn result in safety and environmental risks including job failure,
future operational issues and loss of zonal isolation. Commercial fluid spacer products are available to
assist with NAF displacement2, 3. Fundamental functions required of commercial spacers are well defined
and understood4. This understanding however, is not always applied uniformly in daily operations which
lack standard evaluation tests to quantify cementing fluid interactions. Escalating NAF use, evolving
NAF chemistry, and increasingly harsh application conditions point toward the need for fundamental
characterization of NAF-cement interactions on a chemical level to improve the knowledge of related
technical risks and the technology required for risk reduction and long-term well integrity.
In 2014, RPSEA commissioned a study of deepwater cementing in NAF to develop fundamental
knowledge of mud-cement compatibility issues, to quantify risks associated with this operation, and to
develop best practice recommendations to streamline design and execution while decreasing risk. The
authors presented results of Phase 1 earlier5. This paper presents methods of designing spacers and cements
for deepwater wells developed from that study with analysis of their utility and potential benefits when
applied to field conditions.
The objectives of this project were to develop fundamental knowledge of NAF-cement interactions
related specifically to deepwater cementing, to quantify risks associated with cementing in NAF, and to
develop best practices and derive recommendations in order to reduce the recognized risks. This study
analyzed the relationship between temperature, pressure, cement bond, degree of NAF removal, wettability,
and its effect on zonal isolation in complex well architecture. An Industry Advisory Group (IAG) composed
of operator and service company engineers directly involved in all aspects of drilling and cementing
deepwater wells collaborated in the investigation providing realistic conditions, design parameters, and
current operational practices. Fluids under laboratory investigation included typical commercially available
designs of cement slurries, NAF, and spacers with a focus on micro-particulate fluids and other new
technologies.
Phase 1 achievements included better understanding of important NAF-spacer-cement interactions and
methods to evaluate them in the laboratory. Specific knowledge included:

• Current lab tests of wettability are imprecise, subject to procedural errors, and difficult to relate
to cement performance.
• Current lab tests of spacer effectiveness in NAF do not address the fluids effect on bond to well
surfaces.
• Effects of gelation of intermixed fluids on cement displacement efficiency and placement pressure
may not be as critical as currently believed.
• Performance and mechanical properties of intermixed cement-spacer fluids is not sufficiently
examined in current design procedures.
Focus of Phase 2 work was directed by the investigators and the IAG after review of Phase 1 results.
Primary investigative areas carried into Phase 2 include:

• Confirmation of wettability measurement correlated to bond strength, surface roughness, and

adhesion of cement to steel. Methods for HTHP measurement are evaluated.
• Correlation of wettability and bonding to seal durability considering effects of wettability and NAF
or spacer contamination.
• Field study of NAF, spacer, and cement intermixing vs that predicted by numerical simulation.

• Results from a "shadow study" of field cementing application results compared to new testing
protocols.
SPE-180319-MS 3

Results from the work thus far indicate that lab testing methods quantifying spacer effectiveness
with cement bond strength show promise for evaluation of spacer effectiveness. Adhesion testing, seal
durability testing, and contaminated cement performance properties reveal that maximum spacer or cement
contamination that still yields effective well seal is lower than traditional industry models indicate. The field
mixing study indicates that fluid interfaces exiting the annulus are less distinct with more contamination
than expected.
Planned benefits of the project included more meaningful and focused design method for cement and
spacers used in deepwater wells drilled with NAF. Ultimately, the goals of an improved design method are
to require less engineering and testing time and to result in improved cement placement and bonding. Long-
term well integrity should improve and environmental and safety issues, such as leaks from the formation
and Sustained Casing Pressure (SCP), should be mitigated. The enhanced integrity of the cement should
not only save operators from costly remedial work and additional rig time, but also increase productivity
as well as reduce environmental and safety risks. Results presented herein support that project is on track
to achieve the stated goals.

Experimental Results and Discussion

Various design methods were investigated in this project. The methods included current industry
recommended procedures such as visual wettability, compatibility, and SSST tests. Additional techniques
were evaluated to better quantify effects of NAF-cement interaction and its effect on cement bonding.
Improvements were made in developing quantitative results that could be correlated to real world results.
New testing methods were designed to focus fluid interaction improvements to measureable performance
governing cement seal effectiveness and well integrity. The quantifiable performance parameters relate to
proper displacement of NAF from the well. Proper displacement of NAF entails thoroughly supplanting
NAF from the well by cementing fluids without detrimental fluid incompatibility or increased pump pressure
and leaving well surfaces contacted by cement suitably water wet for cement bonding. Results of this basic
evaluation are presented and discussed below. Summaries of each new test procedure appear in the appendix
of this paper. Complete, detailed procedures and full results of all testing performed during this research
will be released by RPSEA upon completion of the project.
Test conditions were at three different temperatures, 80°F, 140°F and 255°F. Testing at 80°F and 140°F
were performed under atmospheric conditions while the testing performed at 255°F was performed under
pressure. The Appendix gives the details for the various fluids and testing methods performed.

Wettability
The term wettability is defined as the degree to which a surface can be water-wet. In wells that are drilled
with NAF, the surfaces of the formation and casing are oil-wet. The oil-wet environment is not conducive
to bonding for the cement system. The cement system is better able to bond to a surface that is water-wet.
A quantitative method to measure the wettability of a surface is by the use of a goniometer. A goniometer
measures contact angle of a droplet of water on a surface. Contact angle of the droplet is relatable to the
surface affinity for the water. High contact angle (beaded droplet) indicates oil wet surface while lower
contact angle indicates water-wetting. Figures 1 and 2 show effects on contact angle from oil-wet to water-
wet.
4 SPE-180319-MS

Figure 1—Oil-Wet Surface

Figure 2—Water-Wet Surface

Phase 1 results confirmed that goniometer testing could yield meaningful wettability information for
NAF-spacer-cement fluid trains if solids were removed from the fluids. Presence of solids can produce
interference that renders data meaningless. However, chemical interactions of these cementing fluids on
steel can be quantified using solids-free fluids. Further, laboratory methods to expose the steel coupon to
fluids under realistic shear, time interval, and temperature were developed. Various fluids were tested on
metal coupons and measured for the contact angles after each treatment.
Table 1 demonstrates the capability of the goniometer to provide quantifiable measurements for assessing
wettability. By varying the concentrations of the surfactants from 0.25 gal/bbl to 2.0 gal/bbl a change in
contact angle can be seen to follow a trend from higher to lower in the spacers tested. The varying results
from spacer to spacer also show that low contact angles can be achieved with different amounts of surfactant.
Many times in the industry when incompatibilities occur one option is to either change the surfactant or
increase its loading. By having a measurement of the contact angle there can now be a more quanitifiable
result to base the decision on increasing or changing surfactants to achieve a more wettable and compatible
surface. A question that can now be raised is what is considered an acceptable contact angle for wettability.
One way to provide an answer is to relate the contact angle to bonding.
SPE-180319-MS 5

Table 1—Contact Angle vs Surfactant concentration

Contact Angle (degrees) @

NAF-Spacer combination at 80°F Surfactant concentration (vol gal/bbl)

0.25 0.50 1.0 2.0

NAF B-Spacer F 30 5 5 5

NAF B-Spacer G 75 80 60 5

NAF B-Spacer I 45 35 0 0

NAF C-Spacer F 10 10 5 10

NAF C-Spacer G 25 5 5 0

NAF C-Spacer I 10 10 5 5

Phase 2 testing focused on wettability measurement at elevated temperatures. The steel coupon exposure
method was modified to accommodate heated fluids using a stirred fluid loss cell. The exposure method,
summarized in the Appendix, involved:
1. attaching a steel coupon to the cell paddle,
2. filling the cell with heated, solids-free NAF,
3. rotating the paddle for 10 min contact time,
4. removing the paddle and re-immersing in solids-free spacer,
5. repeating the circulation with solids-free cement fluid,
6. measuring contact angle via the goniometer after exposure to spacer and cement.
Table 2 has a summary of contact angles after application of each fluid for a series of NAF-Spacer-cement
trains used for laboratory comparison. As can be seen the contact angle that the NAF supplied was usually
between 80°-85°. Treatments of spacers and cement gave varying results. It is believed that the lower the
contact angle, the better for bonding. Since there is now a quantifiable way to measure wettability the next
step is to investigate its relationship to bonding. Determining the ranges of contact angle needed to provide
sufficient bonding areas would benefit the industry. There would now be a quantifiable method to determine
if the fluid trains are sufficient to provide a competent seal.

Table 2—Contact Angles vs Shear Bond

Train Components Angle Angle after Shear

Temp.
NAF Spacer Cement after NAF Spacer Bond (psi)

80°F Yes None 100% 80° - 15

Yes C + 2 gal/bbl Surfactant 100% 85° 70° 30

Yes G + 2 gal/bbl Surfactant 100% 80° 10° 75

Yes E/F + 2 gal/bbl Surfactant 100% 80° 10° 75

None None 100% - - 85

255°F None None 100% 80° - 230

Yes None 100% 80° - 220

Yes I + 2 gal/bbl Surfactant 100% 80° 15° 155

Yes B 100% 80° 55° 155

Yes G + 0.25 gal/bbl Surfactant 100% 85° 20° 180

Yes G + 0.5 gal/bbl Surfactant 100% 85° 10° 220

Yes G + 1.0 gal/bbl Surfactant 100% 80° 10° 300

6 SPE-180319-MS

Train Components Angle Angle after Shear

Temp.
NAF Spacer Cement after NAF Spacer Bond (psi)

Yes G + 2.0 gal/bbl Surfactant 100% 80° 10° 350

Yes E/F + 0.25 gal/bbl Surfactant 100% 80° 15° 275

Yes E/F + 0.5 gal/bbl Surfactant 100% 85° 15° 260

Yes E/F + 1.0 gal/bbl Surfactant 100% 85° 15° 240

Yes E/F + 2.0 gal/bbl Surfactant 100% 80° 10° 270

Shear bond testing was performed on the same metal coupons as those used in the wettability study. After
exposing the coupons to combinations of NAF, spacers, and cement (whole, solids-laden fluids rather than
solids' free), the coupons were cemented in place as seen in Figure 3. After curing at appropriate temperature
and pressure, coupons were pulled from the set cement to measure the magnitude of bonding. Table 2 shows
this relationship between contact angles and bonding.

Figure 3—Shear Bond Apparatus

These high-temperature results when compared with low-temperature from Phase 15, also presented in
Table 2, do not follow clear trends of wettability vs shear bond. Low-temperature data display a strong
positive correlation between reduced contact angle after spacer and magnitude of shear bond. The high-
temperature data do not follow this correlation. Spacer I appeared to water-wet very well but shear bond
from this fluid train was the same as for the spacer B fluid train which exhibited significantly higher
contact angles. One possible explanation for this is increased cleaning and scouring effectiveness of cement
fluid at elevated temperature. Additionally, higher temperature would induce fluid viscosities making film
depositions thinner and easier to remove. Whatever the reason, these results call into question the validity
of wettability as a design tool for spacer effectiveness as application temperature increases. This question
is being addressed in continued Phase 2 study.

Adhesion versus Surface Condition

Spacers may contain viscosifiers, weighting material, surfactants, solvents, mutual solvents, etc. The
components can all simultaneously influence the performance and the ultimate success of spacers6. To
investigate the efficiency of drilling fluid removal by spacers, we can measure the amount of residual mud
SPE-180319-MS 7

on the surface of the casing7. Since the ultimate purpose of cementing is to provide a good bond, the goal
is to directly measure the adhesion and bond strength between the hardened cement and steel.
In concrete technologies, pull-out tests are commonly used to study bond strength between rebar and
concrete8. However, circular steel coins were used in the previous studies7 due to the ease of measuring
the surface condition, but the coin is not a good geometry for a pull-out test. Thus, for this investigation,
a modified Brazilian disk which can secure both cement cylinders and steel coins9 was adapted as a
sample holder. Another reason for choosing the Brazilian disk is that the ultimate goal of this study is to
quantify the interfacial fracture toughness properties between cement and steel. In this study, the effect of
surface corrosion on wettability was investigated. Overall, three types of surface conditions were compared:
polished, sandblasted and rusted.
Specimen preparation for the shear bond strength test was similar to Phase 1 studies10 which measured the
residual NAF thickness on the surface of steel pipes (see Figure 4). The procedure attempts to simulate the
shear rates used in the oilfield cementing operation. The 10-min contact time is generally used in the field.

Figure 4—Experimental procedure for preparing specimen

Prior to the test, coins were washed by detergent to remove any trace of organics. Isopropanol was then
used to further clean the coin. The plastic tube was greased to reduce the bonding between cement and the
inner wall of the tube. This can minimize the risk that shrinkage of cement during hydration will pull cement
away from the coins. After two cement flushings, the cement was drained until only a layer of cement paste
about ½ inch thick was left in the tube. Above the cement slurry, water was added to keep the material wet,
which can reduce the chemical shrinkage and drying shrinkage effects.
After a two-day aging period, the specimen is ready for the shear bond strength test. A sample holder was
built to secure the specimen (see Figure 5). In principle, the load angle (angle between the interface and the
loading direction) can be adjusted from 0° to 25°, which corresponds to pure mode I and pure mode II crack
opening9. For this project all testing was performed at load angle θ = 22°, which includes both mode I and II.
8 SPE-180319-MS

Figure 5—Fabricated Brazilian Disk

Figure 6—Schematic drawing of Shear Bond strength test

When compressing the assembly, the applied force is resolved into two directions, shear and compression.
Shear force tends to break the assembly, while compressive force pushes the materials into contact and
resists shear. The shear bond strength is formulated as

(1)

When the load angle θ=22°, about 93% of load force is applied in the shear direction. A typical sample
fracture curve is displayed in Figure 7.

Figure 7—Typical load-deflection curve

Table 3 lists results from the adhesion study as well as a comparison to the shear bond testing. The main
observations are:

• Cement bond is highest when bonding to clean steel without previous contact to other fluids. This
implys that the NAF/spacers retained on the steel surface reduce bond strength.
• Spacer B generally produced higher shear bond strength than Spacer G. The contamination by
Spacer G can retard setting of cement11.
SPE-180319-MS 9

• Rusted coins generally produce higher shear bond strength than polished or sandblasted coins.
This may be due to differences in the chemical properties of rust and steel, as it has been found
that rust can improve the wettability of steel12. Alternatively, this result may simply indicate better
mechanical interlocking between cement and the rough surface of the rust. However, variability of
the results suggests broader study is required to explain the effects of rusted surfaces on cement
bond.

Table 3—Shear Bond strength vs Adhesion results

Test Adhesion Adhesion

Fluid Train Shear Bond (psi) Adhesion Rusty (psi)
Temperature (°F) Polished (psi) Sandblasted (psi)

Cement 80 85 75 100 220

NAF-Spacer G-Cement 80 30 25 50 55

NAF-Spacer B-Cement 80 65 55 50 40

NAF-Cement 80 15 35 30 40

Cement 140 Not measured 150 215 220

NAF-Spacer G-Cement 140 Not measured 15 20 35

NAF-Spacer B-Cement 140 Not measured 90 95 50

Compatibility
Compatibility of NAF, spacer, and cement slurry is evaluated via two main attributes: gelation of fluid
mixtures and detrimental effects on cement performance properties.
Determining if a fluid train is rheologically compatible is performed in the laboratory by mixing ratios of
the fluids and measuring the resulting rheology as well as looking for visual signs of incompatibility such
as gelation, flocculation, and clabbering. If a resulting mixture is unmixable or looks to be too viscous to
pump, the fluids are considered incompatible. If the fluid mixtures look homogenous and remain at or below
the more viscous of the two fluids, then the fluids are considered compatible. A range of fluid mixtures in
between compatible and incompatible is commonly encountered in both the laboratory and the field. These
mixtures are not fully compatible, but remain well below the criteria for calling them incompatible.
The effects of contamination by the NAF or the spacer are shown in Table 4 with the reporting of
compressive strengths over time. The baseline cement was contaminated with various amounts of NAF
or spacer by % volume. Results show significant delays in initial set and reduced compressive strength
development with as little as 10% by volume contamination. Interestingly, contamination affects from
spacers can be more severe than those from NAF. Spacer G delayed strength development past the 48 hour
mark.

Table 4—Contaminated compressive strengths at 140°F

Composition 50 psi 500 psi 24 hours 48 hours

100% Cement 3:39 4:16 3800 3950

90% Cement:10% NAF 14:47 16:40 1390 2295

85% Cement:15% NAF 15:41 18:02 1040 1715

90% Cement:10% Spacer B 16:56 18:46 1210 2480

85% Cement:15% Spacer B 19:22 21:41 765 1920

90% Cement:10% Spacer G Not set Not set Not set Not set

85% Cement:15% Spacer G Not set Not set Not set Not set
10 SPE-180319-MS

Contamination effects on shear bond results were performed with the cement, NAF and spacers at 140°F
as seen in Table 5. The baseline value for the cement was 200 psi with no application of NAF or spacer on
the coupons before cementing in place for 48 hours. All other fluid trains showed a decrease in shear bond.
The question remains as to how severe this lowering of bond strength would be to the ability of the cement
to provide sufficient well integrity. This will be further discussed in the Annular Seal section.

Table 5—140°F Shear Bonds

NAF Spacer Cement Shear Bond (psi)

None None 100% 200

Yes B 100% 75

Yes B 90%Cement:10%NAF 40

Yes B 85%Cement:15%NAF 30

Yes B 90%Cement:10%Spacer B 70

Yes B 85%Cement:15%Spacer B 60

Yes G + 2.0 gal/bbl Surf 100% 40

Yes G + 2.0 gal/bbl Surf 90%Cement:10%Spacer G 0

Yes G + 2.0 gal/bbl Surf 85%Cement:15%Spacer G 0

During performing simulations with predictive software the placement efficiencies did not vary much
when using compatible, slightly incompatible, to moderately incompatible, or completely incompatible fluid
trains. These results raised questions regarding focus of fluid compatibility testing. Significant effort is
invested in designing fluid trains with acceptable compatibility and rheological hierarchy. However, effects
of contamination on cement seal performance are not usually evaluated.
These results prompted the investigation in Phase II to verify the results of the numerical simulator
with actual field results. Part of that verification included measurement of fluid train intermixing
during cementing wells drilled with NAF. Several proprietary numerical placement simulators advertised
calculation of intermixing extent13, but no generally-available industry simulators claimed to address
intermixing. Field measurement of intermixing would quantify the potential for cement performance
damage. This intermixing measurement entailed collecting return samples from a well during cement
placement and analyzing fluids to determine extent of intermixing at fluid interfaces. Since it is not practical
to collect samples of returned fluids from a deepwater well, land wells drilled with NAF were chosen for
the study.

Field Calibration of Numerical Placement Simulator

A simplified field study collecting and analyzing return samples from cementing jobs was performed on
land wells drilled with NAF. Land well operations were chosen to allow easy collection of returns. The
subject wells were of interest because the operator routinely brings lead cement to surface. Thus, the extent
of intermixing of NAF with spacer and spacer with cement could be assessed through the sampling.
Results from one of the wells are presented below. The hole size was 9-7/8 inches drilled to 6400 ft with
7-inch casing. Fluid volumes and final fluid locations are presented in Table 6. Fluid compatibility testing
revealed that the spacer was rheologically compatible with both NAF and cement. A slight viscosity increase
of the 50:50 NAF:spacer mixture was noted, but the service company deemed the fluids were compatible.
SPE-180319-MS 11

Table 6—Fluid volumes and final position for simulator verification test

Density Location of
Fluid Volume pumped (bbl)
(lb/gal) leading Edge (ft)

NAF 10.2

Spacer 10.6 40 Surface

Lead Cement 11.8 210 Surface

Tail Cement 16.2 265 234

Displacement Fluid 8.5 223 6320

For the example well described here, the 7-inch production casing was cemented in the 9-5/8-inch
hole. Drilling fluid was 10.2 lb/gal NAF, followed by 40 bbl of 10.6 lb/gal water based spacer containing
surfactants. This was followed by an 11.8 lb/gal lead cement. The majority lead cement was circulated to
surface. Return samples were taken approximately every minute beginning 120 minutes into placement
continuing until the placement was complete. Samples were returned to the lab for analysis to quantify
amounts and compositions of fluid present in each sample. Samples that remained fluid were evaluated
via standard retort procedure14 to determine relative volumes of oil, water, and solids. All samples were
analyzed using FTIR spectroscopy to quantify ratios of cement, NAF, and spacer.
Figure 8 tracks fluid front position of each fluid in the cementing train as calculated from a commercially
available placement simulator. Note that this simulator does not consider or calculate fluid intermixing, so
sharp fluid interfaces are expected.

Figure 8—Fluid front positions over time

Table 7 lists time and composition of representative fluid samples taken during the placement correlated
with modeled results of fluid reaching the surface.
12 SPE-180319-MS

Table 7—Predicted vs actual fluid returns composition (vol%)

Time (min) Volume Pumped (bbl) %NAF %Spacer %Cement Predicted return

128 455 100 0 0 NAF

133 495 98 2 0 NAF

138 520 98 2 0 First Spacer

148 575 96 4 0 First Lead Cement

149 607 68 32 0 Lead Cement

163 620 68 32 0 Lead Cement

166 631 56 40 4 Lead Cement

173 661 7.5 60 33.5 Lead Cement

181 690 0 0 100 Lead Cement

Results of this investigation indicate that fluid intermixing between NAF and spacer is significant.
Mixture volumes extend for several hundred linear feet. The total volume of spacer extends over 140 bbl
of return fluid. No samples of unadulterated spacer were taken. This degree of intermixing is greater than
that expected. Most notable is the fact that no individual spacer fluid was detected but was intermixed and
emulsified into the NAF over a large volume of returns. Coincidentally, spacer returns appeared at the exact
time predicted by the simulator. However, the long delay of cement detection in returns indicates that some
spacer overran NAF and intermixed with it. Thus the spacer actually arrived early. Most likely explanation
for cement returns appearing later than predicted is increased hole volume due to washout.
The emulsion of spacer into the NAF was extremely stable. No phase separation occurred in any of
the mixtures, and normal methods of breaking the emulsion in the lab were unsuccessful. Ultimately,
the emulsions were broken using the API retort, an extremely aggressive technique for separating stable
emulsions. NAF:spacer emulsion stability was confirmed by an SSST test run after samples were collected.
Additions of over 60 vol% of spacer to the NAF produced no conductivity reading increase.
It is tempting to interpret these results as general indication that significant spacer intermixing occurs
on all wells drilled with NAF. The lack of pure spacer indicates that this spacer did not provide separation
as designed. Results of SSST indicate the fluids formed a stable emulsion as evidenced in the subsequent
difficulty in separating the samples. Similar intermixing occurred between spacer and cement. In this
operation, the operator and service company counted on the large excess lead cement volume for additional
hole cleaning and surface preparation. Outcome of this cement application were successful. However, the
result warns that specific design effort is required to ensure that spacer actually separates NAF and cement.
Focus on rheology and wettability can overshadow the potential hazards of contamination.

Correlation of Seal Durability using Annular Seal Testing

Annular seal testing involved the use of a testing fixture that simulates cement providing a barrier between a
formation and casing as seen in Figure 9. This test method was developed as a means of laboratory evaluation
and prediction of seal performance in field conditions15. For the current investigation, the fixture surfaces
were exposed to different fluid trains before allowing the cement to harden in place. Gas is then applied to
the cemented annulus while the inner casing is cycled with pressure to induce failure of the cement sealant.
The modified test protocol, detailed in the Appendix, simulated flow of the fluid train through the annulus
prior to cement placement. Each fluid, NAF, spacer, and cement, was placed in the annular space and agitated
at a shear rate of 100 sec-1 for 10 minutes. After agitation, the fluid was drained and replaced with the next.
After cement exposure, the cement slurry was drained, and the annulus was refilled with fresh cement. The
test fixture was then cured and annular seal was evaluated as in past investigations. Failure in this test is
noted by gas flow through the cemented annulus. This failure is not correlatable to one specific cement
SPE-180319-MS 13

performance property. Instead the results have been empirically correlated to a group of cement performance
properties, formation and pipe mechanical properties, and dimensions to produce a scaling relationship
applicable to field conditions.

Figure 9—Annular Seal Apparatus

Table 8 is a summary of testing the different fluid trains for annular seal evaluation. The results of testing
various fluid trains reveal several interesting trends. Cement seal was maximized with no previous fluid
contact to the test fixture. Spacer E/F and Spacer G with appropriate surfactant concentrations produced
results similar to the no-previous-fluid base line. Surfactant concentration for both Spacers E/F and G
demonstrated an optimum. The surfactant package concentration vs. performance trend observed in shear
bond testing held for the annular seal results.

Table 8—Annular Seal Results

Fluid Train Components

Energy to Failure (lb-in)
Train No. NAF Spacer Cement

1 None None 100% >1.068E+07

2 Yes None 100% Immediate Failure

3 Yes B 100% 6.378E+05

4 Yes G + 0.25 gal/bbl Surf. 100% Immediate Failure

5 Yes G + 0.5 gal/bbl Surf. 100% >1.068E+07

6 Yes G + 1.0 gal/bbl Surf. 100% 6.540E+06

7 Yes G + 2.0 gal/bbl Surf. 100% 7.652E+06

8 Yes E/F + 0.25 gal/bbl Surf. 100% 7.583E+05

9 Yes E/F + 0.5 gal/bbl Surf. 100% 7.513E+05

10 Yes E/F + 1.0 gal/bbl Surf. 100% 9.780E+02

11 Yes E/F + 2.0 gal/bbl Surf. 100% 1.095E+06

14 SPE-180319-MS

Table 9 presents results of annular seal testing with fluid trains simulating contamination of cement
with either NAF or spacer. These results indicate significant cement seal performance degradation when
contamination is included. The results are supported by shear bond data.

Table 9—Annular Seal vs Shear Bond

Train Components Energy to Failure Shear

Fluid Train No.
NAF Spacer Cement (lb-in) Bond (psi)

13 Yes B 90% Cement:10% Mud B 7.197E+05 40

15 Yes B 90% Cement:10% Spacer B 8.865E+05 70

17 Yes G + 2 gal/bbl Surf. 90% Cement:10% Spacer G Immediate Failure 0

64 None None 90% Cement:10% Mud B Immediate Failure -

66 None None 90% Cement:10% Spacer B >1.068E+07 -

69 None None 90% Cement:10% Spacer G Immediate Failure -

Overview and Future Effort

Collective results presented in this paper emphasize several elements of spacer design for NAF application.
First, all aspects of fluid performance and chemistry require balanced design to increase cement seal
integrity. Fluid separation, must be ensured. Wettability and its effect on seal integrity must be quantified
along with effects of rheological compatibility and mechanical property degradation from contamination.
A balanced, quantifiable design method incorporating all these facets will deliver a fluid train with highest
chance of placing an effective, durable cement seal.
This paper reports a "screen capture" summary of an enormous collection of data and analyses. The
work is ongoing and will be completed in September 2016. Public access to the final report presenting and
analyzing all the data will follow shortly. The results of this study will certainly identify topics requiring
additional investigation. A few of those topics supported by the summarized information presented here are:

• Temperature effects of wettability vs bond

• Contamination effects of spacers on cement performance

• Degree of intermixing during field operations

• Laboratory quantification of spacer's separation effectiveness

Conclusions
1. Wettability measurements using a goniometer to measure effects of solids-free fluids on steel coupons
is a viable method for design of fluids for cementing wells drilled with NAF.
2. Laboratory shear bond method that accounts for fluid train contact and temperature as described here
correlates well with wettability. This shear bond measurement is relatable to surface wettability, bond
strength, adhesion, and seal effectiveness.
3. Both the laboratory wettability measurement and the shear bond methods evaluated in this study
provide realistic material surface, controlled fluid train contact time, representative shear rate, and
yield results correlatable to seal effectiveness.
4. Novel adhesion measurement used in this study demonstrated effect of surface condition and
roughness on cement adhesion. Rusty pipe improves adhesion and bond strength.
5. Residual fluid film of fluids preceding cement slurry may affect cement adhesion bond. Effect may
be due to physical presence of film or chemical impedance of cement strength.
SPE-180319-MS 15

6. Cement slurry contamination by spacer fluid can reduce cement strength development. This
compatibility parameter is equally important to fluid design as rheological compatibility.
7. Quantitative field anecdotal evidence indicates that intermixing of NAF, Spacer, and cement in
the annulus may be more substantial than generally believed. This indicated intermixing reinforces
concern over degradation of cement properties from contamination.
8. Surfactant concentration optimization may be required to optimize wettability as well as minimize
contamination effects.
9. Cementing fluid design methodology employing wettability and compatibility/contamination
evaluations developed during this study has potential to improve cement seal performance.

Acknowledgements
We would like to acknowledge the support provided by RPSEA.

Nomenclature
bwow = By Weight of Water
ft3/sk = Cubic Feet per Sack
gal/bbl = Gallon per Barrel
gal/sk = Gallon per Sack
HPHT = High Pressure High Temperature
IAG = Industry Advisory Group
lb/bbl = Pound per Barrel
lb/gal = Pound per Gallon
MPa = Megapascal
NAF = Non-Aqueous Fluid
OBM = Oil Based Mud
psi = Pounds per Square Inch
RPSEA = Research Partnership to Secure Energy for America
SBM = Synthetic Based Mud
SCP = Sustained Casing Pressure
SSST = Spacer Surfactant Sensitivity Test

References
1. Harder, C., Carpenter, R., Wilson, W., Freeman, E., and Payne, H.: "Surfactant/Cement Blends
Improve Plugging Operations in Oil-Base Muds." Web. SPE-23928-MS Prepared for presentation
at the SPE/IADC Drilling Conference, New Orleans, Louisiana, February 18–21, 1992.
2. Maserati, G., and Daturi, E.: "Nano-emulsions as Cement Spacer Improve the Cleaning of Casing
Bore During Cementing Operations." SPE-133033-MS. Web. Prepared for presentation at the
SPE Annual Technical Conference and Exhibition, 19–22, Florence, Italy, September 2010.
3. Carrasquilla, J., Guillot, D.J., Ali S. A., and Nguyen, C.: "Microemulsion Technology for
Synthetic-Based Mud Removal in Well Cementing Operations." SPE-156313-MS. Web. Prepared
for presentation at the SPE Deepwater Drilling and Completions Conference, 20–21, Galveston,
Texas, USA, June 2012.
4. McClure, J., Khalfallah, I., Taoutaou, S., Bermea, J., Kefi, S.: "New Cement Spacer Chemistry
Enhances Removal of Nonaqueous Drilling Fluid." JPT article pp. 32–35 October 2014.
5. Sonnier, P., Watters, L., Head, B., Clapper, D., Choi, M., Zhang, Z.: "Fundamental Understanding
of Non-Aqueous Drilling Fluids Leads to Optimizing Seal Integrity while Reducing Design
16 SPE-180319-MS

Time and Cost." AADE-16-FTCE-34. Prepared for presentation at the AADE Fluids Technical
Conference and Exhibition, Houston, Texas, April 12–13, 2016.
6. Christian, C.D., Ellis, D.R., Brege, J.J., Quintero, L. and Clark, D.E., 2009, April. The
development of an effective water-wetting cement spacer for the displacement of non-aqueous
fluids (NAF). In AADE Technical Conference and Exhibition (pp. 1–5).
7. Zhang, Z., Scherer G.W., and Prud'Homme R.K., 2016. Effect of surface roughness on the
thickness of residual oil-based mud on the steel casing. In draft.
8. Castel, A. and Foster, S.J., 2015. Bond strength between blended slag and Class F fly ash
geopolymer concrete with steel reinforcement. Cement and Concrete Research, 72, pp.48–53.
9. Wang, J. S., and Suo, Z. 1990. Experimental determination of interfacial toughness curves using
Brazil-Nut-Sandwiches. Acta Materialia. Vol. 38, No. 7, pp. 1279–1290.
10. Choi, M., Scherer, G.W., and Prud'homme, R.K., 2016. Novel methodology to evaluate
displacement efficiency of drilling mud using fluorescence in primary cementing. In draft.
11. Zhang, Z., Scherer G.W., and Prud'Homme R.K., 2016. Properties of cement slurries
contaminated by spacers in oil-field cementing. In draft.
12. Lu, W. and Chung, D.D.L., 1998. Effect of rust on the wettability of steel by water. Cement and
Concrete Research, 28(4), pp.477–480.
13. Chen, Z., Chaudhary, S., Shine, J.: "Intermixing of Cementing Fluids: Understanding Mud
Displacement and Cement Placement." IADC/SPE 167922 Prepared for presentation at the
IADC/SPE Drilling Conference and Exhibition, Fort Worth, Texas, March 4–6, 2014.
14. API RP 13B-2, "Recommended Practice for Field Testing of Oil-based Drilling Fluids, Fifth
edition." Standard by the American Petroleum Institute, April 1, 2014.
15. Bassett, J., Watters, J., Combs, K., Nikolaou, M.: "Lowering Drilling Cost, Improving
Operational Safety, and Reducing Environmental Impact through Zonal Isolation Improvements
for Horizontal Wells Drilled in the Marcellus Shale." SPE-168847-MS Prepared for the
Unconventional Resources Technology Conference, Denver, Colorado, August 12–14, 2014.
SPE-180319-MS 17

Appendix

Fluid Designs
3
Cement: 16.4 lb/gal Cement Design with 1.07 ft /sk yield, 4.12 gal/sk Water, 4.39 gal/sk Total Mixing Fluid

Blend Cement Sack Weight (lb) % of Total Sack Weight

Cement - Class H 94 100

Material Description Concentration Units

Antifoam 0.02 gal/sk

Dispersant 0.03 gal/sk

Fluid Loss 0.1 gal/sk

Retarder 0.12 gal/sk

KCl 3 %bwow

14.5 lb/gal Spacer B Design

Material Description Concentration Units

Barite 313.00 lb/bbl

Spacer Blend B 37.50 lb/bbl

Deionized Water 31.00 gal/bbl

14.5 lb/gal Spacer C Design

Material Description Concentration Units

Barite 281.00 lb/bbl

Spacer Blend C 69.00 lb/bbl

Surfactant 0.25 to 2.00 gal/bbl

Deionized Water 29.00 gal/bbl

14.5 lb/gal Spacer E Design

Material Description Concentration Units

Barite 393.00 lb/bbl

Solvent 30.60 gal/bbl

14.5 lb/gal Spacer F Design

Material Description Concentration Units

Barite 339.00 lb/bbl

Spacer Blend F 2.00 lb/bbl

Surfactant 0.25 to 2.00 gal/bbl

Deionized Water 30.50 gal/bbl

18 SPE-180319-MS

14.5 lb/gal Spacer G Design

Material Description Concentration Units

Microemulsion na na

14.5 lb/gal Spacer I Design

Material Description Concentration Units

Barite 332.00 lb/bbl

Spacer Blend D 11.00 lb/bbl

Surfactant 0.25 to 2.00 gal/bbl

Deionized Water 30.50 gal/bbl

12.7 lb/gal NAF A

9.5 lb/gal NAF B

11.9 lb/gal NAF C

Test Procedures
Goniometer Test Procedure
Before the test, the sample coupons should be cleaned to remove any potential contaminants and ensure the
consistency of test results. Prepare the coupon using the following steps:
1. Wash the coupon with DI water.
2. Wipe the coupon with lint free non-abrasive wipes or towels to remove the residual water droplets.
3. Rinse the coupon thoroughly with isopropanol (Purity>98%).
4. Dry the coupon with clean/dry compressed air. Make sure there is no alcohol or water left on the
coupon. If any moisture is present, the goniometer may give incorrect readings.
Verify the water reservoir has enough water for the test. If the water level is low, refill the reservoir with
DI water using 1 mL syringe and needle. Plug the goniometer to the computer with a USB cable. The cable
powers the instrument and allows control of the instrument with software. Start the program. Display the live
video image in the "Live Image Screen" to monitor the movement of the droplet. Calibrate the instrument
in accordance with calibration procedure. In the options tab, set the error count to 10. In the static tab, right
click the measure button and set the count to 20 images in 0.5 min. Change the option on the bottom to
"Auto: Pump volume 4μl drop arrow down, delay 3s". Place the goniometer on top of the prepared sample
coupon, and then click "measure". The program will automatically start measuring the contact angle of each
droplet. After the test, unplug the goniometer and store the instrument in the box.
Due to the instrument limitation and surface conditions, the contact angle testing may have a range of
variation. Following steps are adopted to limit the variability of the results.
5. For each test, take 5 drops of water per coupon to make sure the result is not impacted by individual
testing spot.
6. Take 10 images per droplet, measure the contact angles and calculate the average.
For testing with the Base Oil, Base Oil Wash, Base Oil + Emulsifiers and Surfactant Washes use the
following steps.
SPE-180319-MS 19

1. After measurement of the Baseline is complete place the coupon in a container with the next fluid
treatment.
2. Agitate gently for 10 minutes by hand
3. Remove the coupon and dry with the compressed air
4. Measure the contact angles with the goniometer
5. Repeat these steps with the surfactant wash

Shear Bond Test Procedure

Apparatus preparation (See Figure 11)
1. Prepare 3 pieces of 2" diameter, 2" tall steel pipe.
2. Place one metal coupon next to each pipe and grind down to make the coupon 0.25" taller than the pipe.
3. Prepare 6 rubber gaskets that can hold 1 metal coupon in the middle and fit in the pipe.
4. Prepare 2 rubber holders that can hold 3 metal coupons and be assembled to a table top mixer.
Performing the test
5. Clean the coupons with DI water and isopropanol, as described in the goniometer section.
6. Assemble 3 pieces of coupon to a table top mixer with the rubber holder, soak the coupons in oil/mud
and mix for 10 minutes at low rpm. Place the ground side of the coupon down. See Figure 10.
7. Replace oil/mud with spacer. Repeat step 6.
8. Replace spacer with cement slurry. Repeat step 6.
9. Place the coupon (ground side down) through the bottom gasket.
10. Place the gasket and coupon inside the pipe.
11. Pour cement slurry into the pipe until nearly full.
12. Place the top gasket on top of the coupon and slide down until it is just inside the pipe.
13. Cure the cement slurry in water bath for 48 hours at 150°F.
14. Remove the top and bottom gaskets. Measure the shear bond strength between cement and coupon.

Figure 10—Coupon with grounded end

20 SPE-180319-MS

Figure 11—Shear Bond setup side view

Figure 12—Coupons in holder

Wettability Test Procedure

1. Equipment and materials required
a. Contact angle goniometer
b. Stirred Fluid Loss Apparatus Exposure
c. 2 each metal coupons (see specifications below)
d. 1 each clamp for attachment of coupons to paddle (see specification)
e. 1 each timer (mm:ss)
f. Non-aqueous drilling fluid (NAF) base oil to be tested
g. Aqueous pre-flush or spacer to be tested
h. Deionized or distilled water
i. Isopropyl alcohol (98% or greater purity), also known as isopropanol, IPA
j. Proper PPE, including goggles, face shield, or safety glasses with lab coat and gloves suitable
for handling NAF and/or isopropyl alcohol, and a well-ventilated work area or air hood.
SPE-180319-MS 21

2. Fluid Preparation
a. Prepare the NAF and the spacer according to the instructions of the suppliers.
3. Stainless steel coupon preparation
a. Coupon specifications
i.Approximate dimensions: 75mm x 15 mm x 1 mm with centered 3.25 mm mounting
hole or as needed for suitability with selected goniometer. Made of 316 stainless steel
with surface polished to 32 (+/- 4) RMS (Root Mean Square, micro-inch) finish.
b. Cleaning and preparation
i.Wash the coupon with DI water.
ii.
Wipe the coupon with lint-free non-abrasive wipes or towels to remove any residual
water droplets.
iii. Rinse the coupon thoroughly with isopropanol (Purity>98%).
iv. Dry the coupon with clean/dry compressed nitrogen. Make sure there is no alcohol or
water left on the coupon. (Note: If any moisture is present, the goniometer may give
incorrect readings.)
4. Fluid exposure procedure
a. Preparations
i.Before exposure to test fluids in testing apparatus, measure and record the contact angle
of coupons exposed to surfactant fluid in atmospheric conditions. (Follow instructions
on 5.b.)
b. Procedure
i. Subject the clean coupons to the surfactant wash for 10 minutes
ii. Dry coupons with nitrogen
iii. Measure and record the contact angles as per instructions in 5.b.
iv. Subject the coupons to the Base Oil of the NAF for 10 minutes
v. Attach the coupons to the clamp mounted on the paddle for the stirred fluid loss
apparatus.

Figure 13—Coupon mounted on paddle of example stirring fluid loss apparatus

22 SPE-180319-MS

vi. Assemble the cell according to the manufacturer's procedure and fill the cell with the
volume of surfactant wash specified by the manufacturer for wettability testing.
vii. Install the paddle end onto the cell.

Figure 14—Coupons mounted on paddle being inserted

into example stirring fluid loss apparatus pressure cell

viii. Install the cell into the stirred fluid loss apparatus. Ensure that the coupons are not
immersed in the spacer during installation (see Figure 15).

Figure 15—Loading cell from bottom of apparatus

SPE-180319-MS 23

ix.
Apply 6.9 MPa (1000 psi) to the cell.
x.Heat the spacer to BHCT or other desired test temperature.
xi.
After reaching test temperature, invert the cell so that the coupons are immersed in the
spacer.
xii. Stir at 150 RPM for a time consistent with the anticipated spacer exposure time in the
well. If this time is unknown, stir for 10 minutes.
xiii. Turn the motor off.
xiv. Invert the cell so that the coupons are no longer immersed in the spacer.
xv. Cool the cell to a safe handling temperature [<88°C (190°F)].
xvi. Release the pressure.
xvii. Remove the cell, being careful not to invert it, keeping the paddle end up so that the
coupons are not re-immersed in the spacer fluid.
xviii. Remove the paddle end.
xix. Remove the coupons without touching the surfaces to be tested and test for contact angle
according to the procedure described in clause 5.
5. Determination of surface wetting condition
a. Preparation of coupon after exposure
i.
Wearing gloves, carefully remove the coupons from the paddle, holding them by the
edges to avoid touching the test surface.
ii. Dry off the coupons using nitrogen.
iii. Measure and record the contact angle using the procedure described in clause 5.
b. Measurement of contact angle
i. Goniometer Calibration
1. Check that the contact angle instrument is connected to the computer.
2. Start the contact angle measurement program.
3. A live video image should appear in the Live Image Screen.
4. Load the coupon in the goniometer according to the manufacturer's instructions
for the selected equipment and calibrate the goniometer according to the
manufacturer's instructions.
ii. Determination of contact angle on coupon surface
1. Measure the contact angle of at least 5 separate water drops on the coupon
surface. Using either static or dynamic mode procedure, take between 5 to 10
readings within the first 15 to 20 seconds for each droplet and report the individual
measurements as well as the arithmetic average of contact angle. (Note: Discard
readings if (1) the volume of the droplet is reduced by 20% (evaporation on
surface) and/or (2) the software registers zero or out of the range in the sequence
of contact angle measurements.)
2. The general procedure of the contact angle measurement is:
a. Verify the water reservoir has enough water for the test. If the water level is
low, refill the reservoir with DI water using 1 mL syringe and needle.
b. Plug the goniometer to the computer with a USB cable. The cable powers
the instrument and allows control of the instrument with software.
c. Start the program. Display the live video image in the "Live Image Screen"
to monitor the movement of the droplet.
24 SPE-180319-MS

d. Calibrate the instrument in accordance with calibration procedure.

e. In the options tab, set the error count to 10.
f. In the static tab, right click the measure button and set the count to 10 images
in 0.5 min. Change the option on the bottom to "Auto: Pump volume 4μl
drop arrow down, delay 3s".
g. Place the goniometer on top of the prepared sample coupon, and then
click "measure". The program will automatically start measuring the contact
angle of each droplet.
h. After the test, unplug the goniometer and store the instrument in the box.
i. Due to the instrument limitation and surface conditions, the contact angle
testing may have a range of variation. Following steps are adopted to limit
the variability of the results.
j. For each test, take 5 drops of water per coupon to make sure the result is not
impacted by individual testing spot.
k. Take 10 images per droplet, measure the contact angles and calculate the
average.
6. Results and Interpretation
a. Report
i. Specifics of the base oil composition.
ii. Specifics of the surfactant wash.
iii. Test conditions (temperature, rpm, exposure times, etc.).
iv. Visual observations of the coupons' surfaces.
v. The contact angles of the surfactant treated coupon and the two coupons treated with
base oil and the surfactant wash.
b. Interpretation
If the two coupons give significantly different contact angles after exposure to the drilling fluid and spacer
(greater than 10 degrees difference), repeat the test or increase the surfactant concentration and repeat the
test.

Annular Seal Test Procedure

The Annular Seal Tests were developed in order to measure the ability of cement to maintain an annular seal
in a simulated small-scale wellbore. Apparatus stresses the cement by internal pipe pressure application-
and-release cycles. Seal failure is detected as gas flow through the cemented annulus. Once the cement is
fully cured 15 psi gas pressure is applied to the cement seal and monitored for flow if the cement seal fails.
The inner pipe is cycled 25 times from 0 psi to 1000 psi, then the pressure is increased by 1000 psi and
cycled for 25 times. This ramping is continued until the pressure reaches 10,000 psi. If no failure after the
25 cycles at 10,000 psi, the gas pressure is increased to 30 psi and continued cycling at 10000 psi until
failure. Steel was used as the outer casing.