SPE 95816
Long-Term High-Temperature Laboratory Cement Data Aid in the Selection of
Optimized Cements
S.S. Jennings, SPE, Saudi Aramco
Copyright 2005, Society of Petroleum Engineers
This paper was prepared for presentation at the 2005 SPE Annual Technical Conference and
Exhibition held in Dallas, Texas, U.S.A., 9 – 12 October 2005.
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Abstract
Cements placed in gas wells for Saudi Arabia drilling
operations were evaluated for physical properties. Three
intermediate casing cement compositions were tested. The
cement systems tested were: 1) bentonite extended, 2)
standard density class G and 3) optimized particle packing
lightweight system containing hollow ceramic spheres. These
tests were requested because of concerns that the cements that
were currently being used were not durable in the long term.
Khuff and pre-Khuff gas wells in Saudi Arabia have high
production rate potential therefore the curing test temperature
of 300 oF and test pressures of 3000 psi were applied to the
samples. The samples were cured for one year.
The tests performed were API compressive strength tests,
permeability, shrinkage or expansion, Young’s Modulus,
Poisson ratio, rheology and settling. Data for 24 hour, 7 days,
1, 2, 3, 6, 9 and 12 months test periods are presented for all
cements.
Certain cements, for which there are no previously published
shrinkage data, have been identified. New technology in
cement laboratory testing identified undesirable properties in
certain cements. Using this new lab technology, some cements
exhibited undesirable short and long-term physical properties.
Data representing various cement slurry designs and
corresponding physical properties results are included in this
paper.
Introduction
Certain cements at high temperature can have undesirable
physical properties due to exposure to pressure and high
temperature. The undesirable properties can occur in both the
liquid cement and the hardened cement. Gas wells and cement
behind the casings in Saudi Arabia are exposed to harsh
environments. High flow rates, high pressure and high
temperature all contribute to the deterioration of the long-term
durability of the cement.
The preferred method for cementing this intermediate casing
at approximately 9,000 feet is to utilize a hydraulically
operated DV tool with inflation packer. When the DV tool
operates effectively, high quality 118 pcf cement is placed
around the wellbore and in between the previous casing to
surface. Problems with DV tool reliability steered us to the
investigation of searching for lightweight cement that would
save rig time and provide long-term durability.
The cement required by drilling operations was identified as a
lead 75 pcf cement followed by a 118 pcf tail cement. We
chose to use a specially designed cement blend containing
Hollow Ceramic Spheres for the 75 pcf lead cement. Foam
cement was not tested because foam cement testing is
operationally more difficult to perform and laboratory testing
of foam cements with retained high pressure requires lab
equipment that is not available to us. Foam cement or other
lightweight systems were considered for use on these
intermediate casing cement operations but were not tested as
part of this work.
Discussion
Hollow Ceramic Spheres (HCS) have been used in cement
slurries to reduce density for many years.1-5 Long-term testing
for high temperature exposure on these cements has now been
completed in order to determine their durability at 300 0F.
Previous literature shows positive results for physical
properties for cements with HCS. The results reported were
for relatively short-term testing.
The successful primary cementing of a well cannot be
determined immediately after the cement job is completed.
Many cement jobs have been successfully displaced and poor
quality cement was left in the annulus. Drilling and workover
engineering requested the R&D Center to perform some long-
term durability tests on HCS lightweight cement. Also
2 SPE 95816
requested for testing were the standard 101 pcf bentonite
extended cement and 118 pcf normal density cements that are
currently being used in our Khuff/pre-Khuff gas wells. Both
systems contained 35% (by weight of cement) silica flour.
R&D scientists raised concern over HCS blends’ durability
due to the uncertainty of non-cement type materials in the
blend and the possible lack of sufficient temperature stabilized
cement binding type material. Test conditions set by drilling
and workover engineering were to test the cement for one year
at 300 0F and 3,000 psi curing pressure.
After discussion with Drilling and Workover Engineering
representatives the following tests were performed (table 1):
Table 1
Physical Properties Test Duration (test periods)
Compressive Strength API Crush 1, 7 days, 1,2,3,6,9 and
12 months
Permeability to gas 1, 7 days, 1,2,3,6,9 and
12 months
Shrinkage or Expansion Short term
Young’s Modulus 1, 7 days, 1,2,3,6,9 and
12 months
Poisson Ratio 1, 7 days, 1,2,3,6,9 and
12 months
Rheology Short term
Settling Short term
Durable cement for long-term oil and gas well applications has
not been fully defined. This is mainly due the complexity of
cement chemistry. Water to cement ratio, silica to cement ratio
and exposure temperatures change the physical properties of
set cement in various parts of the hole. Durable cement cured
at 300 0F and 3,000 psi for this application was set with the
following criteria:
• No or very little compressive strength
retrogression after two months.
• No increase in permeability.
• Minimal shrinkage (less than 2.0%)
• Constant or lowering Young’s Modulus with
aging.
• Increasing or constant Poisson ratio with
extended curing.
Testing for this work required the use of three HP/HT curing
chambers. The three curing chambers were run at 217 0F and
3000 psi for ten days then heated to 300 0F and 3000 psi non-
stop for one year. Due to the size and number of samples only
one specimen was used for each test. All cements were mixed
from the same batch/consignment number.
Cement formulations used for long term testing are shown
below:
• 71 PCF - HCS blend + 0.15% bwob (FLA)+ 0.06 gps
(dispersant)+ 0.025 gps (retarder) + 0.15% bwob
(anti-settling) + 2 pt/10 bbls (non-foamer) @ 8.80
gps total mixing fluid
• 101 PCF – Class G (HSR) + 1.9 % bwoc Bentonite
(prehydrated) + 35% bwoc (silica flour) + 0.60%
bwoc (FLA) + 0.05 gps (dispersant) + 0.025 gps
(retarder) + 2 pt/10 bbls (non-foamer) @ 11.47 gps
total mixing fluid
• 118 PCF – Class G (HSR) + 35% bwoc (silica flour)
+ 0.60% bwoc (FLA) + 0.10 gps (dispersant) + 0.03
gps (retarder) + 1 pt/10 bbls (non-foamer) @ 6.26 gps
total mixing fluid
Cementing Service Company provided a pre-blended sample
and a special mixing and pressure conditioning procedure for
HCS cement blend. The components of the sample were not
revealed to R&D Center scientists. The mixing and pressure
conditioning procedures were performed prior to performing
any test. Standard API6 testing and conditioning could not be
applied to test HCS blends for two reasons. First, some of the
hollow spheres break in the blender at high RPMs. Second,
pressure applied when simulating down-hole hydrostatic and
pump pressure breaks or cracks the hollow spheres. When
these hollow spheres fail or crack the density increases. This
simultaneously produces an initial volume decrease. A typical
71 pcf HCS blend should have an initial down-hole density of
75-81 pcf after the 10 minute conditioning time at a curing
pressure of 4200 psi for a 9,000 feet casing job. The variance
in slurry density is due to the inconsistency in crush strength
from batch to batch of hollow ceramic spheres.
The uncertainty of the components in the HCS blend and the
resistance of the service company to provide the individual
components, led to our investigation of how the HCS blend
would react with respect to long-term high-temperature
durability.
Compressive Strength
Samples of all three cements were prepared and API
compressive strength cubes were made. The samples were
prepared and placed in a HT/HP curing chamber at 217 0F and
3000 psi for ten days. One day and one week samples were
removed and the cubes were crushed according to API
specifications. After 10 days the temperature in the curing
chamber cells was raised to 300 0F, simulating the cement
heating due to the well flowing.
The early compressive strength of all three cement systems
fell into expected values. The compressive strength data of
HCS blend has shown that the submitted sample had
unacceptable compressive strength retrogression. The highest
recorded compressive strength was 2,858 psi at seven days.
The compressive strength after one year of curing has reduced
to 532 psi (fig. 1).
SPE 95816 3

Long Term API Crush Strengths Long Term Permeability

@ 300 0F, 3,000 psi @ 300 0F, 3,000 psi
9000 1.6

Permeability to gas (mD)

API Comp. Strength (psi)

1.2

6000
HCS 72 pcf
HCS 72 pcf 0.8
Bentonite 101pcf
Bentonite 101pcf
118 pcf Cement
Cement 118 pcf
3000 0.4

0
0 0 100 200 300 400
0 100 200 300 400 Time (days)
Time (days)
Fig. 3 – Long-term permeability of the samples tested show that
Fig. 1 – API crush strengths of all three systems are shown the 118 pcf cement is superior to either of the lightweight
above. The compressive strength of HCS blend has continuously cements. The long-term increase in the permeability of 101 pcf
declined from its peak strength of 2,858 psi in seven days to 532 bentonite cement and HCS blend was observed.
psi in one year.
Young’s Modulus
Compressive Strength Data Young’s Modulus for all three cements was declining the first
The following figures are data generated from the compressive six months. Young’s Modulus data for 72 pcf HCS blend
strength tester. The graph illustrates the programmed load and generally showed a decreasing trend. The Young’s Modulus
the maximum load versus time. Compressive strength (API for 101 pcf cement increased from 6 month to one year test
Crush) data for HCS blend for one year is shown below (fig. period. One year data for the 118 pcf cement shows a slight
2). decline in Young’s Modulus (fig. 4).
Compressive Strength API Crush of LiteCrete 72 Long Term Young's Modulus
pcf cured one year @ 300 0F / 3,000 psi @ 300 0F, 3,000 psi
1.0E+07
Young's Modulus (psi

3000
2500
Load (lbs)

2000 1.0E+06
1500 HCS 72 pcf
1000 Bentonite 101pcf
500 118 pcf Cement
1.0E+05
0
0:00:00 0:00:09 0:00:17 0:00:26 0:00:35 0:00:43
Time (sec) 1.0E+04
0 100 200 300 400
Load - Prog (Lbf) Load - Maximum (Lbf)
Time (days)
Fig. 2 - Compressive load to failure data for 72 pcf HCS blend Fig. 4 – Long-term Young’s Modulus data of all three systems are
cement for an API cement specimen that was cured at 300 deg F shown above.
and 3,000 psi for 1 year. Surface area for this sample was 3.902
sq. in.
Poisson Ratio
Permeability Poisson Ratio of HCS blend was initially considered good.
Samples were cured in the same curing chamber, at the same After the sample was cured for 9 months the Poisson Ratio
time, with the compressive strength samples. The samples decreased to an unacceptable limit having brittle
were given to the Petrophysics lab for gas permeability characteristics. The one year sample was similar. The 101 and
measurements. The initial permeability of HCS blend was 0.1 118 pcf cement also showed declining Poisson Ratio, the
mD. After the one-year curing period the permeability was values were considerably higher than the HCS blend (fig. 5).
0.77 mD. The initial permeability of the 101 pcf cement was Typical Poisson Ratio for concrete is 0.19.
0.60 mD and for one year the permeability was 1.07 mD. The
118 pcf cement had a initial permeability of 0.02 mD and a
one year permeability of 0.01 mD (fig. 3).
4 SPE 95816
Long Term Poisson Ratio @ 300 0F, 3,000 psi
0.50
0.38
Poisson Ratio
0.25
0.13
0.00
0 100 200 300
Time (days)
Fig. 5 - Poisson Ratio of HCS blend after nine months indicates
that the cement became extremely brittle which is not
characteristic for durable cement.
Shrinkage and Expansion
New Technology
Evaluating the performance of all three cements tested, we
used a new technology, Cement Expansion and Shrinkage
Tester (CEST) 7 (fig. 6). The sample curing cell uses a water
cushion between a floating piston attached to a LVDT and a
rubber diaphragm. Water is not allowed to come in contact
with the test cement. An API report states, “If fluid entry is
not allowed to enter the cement matrix, inner shrinkage leads
to inner pore pressure reduction.” The cement matrix will have
a tendency to collapse, leading to bulk shrinkage.8
Fig. 6 – The CEST shown above in horizontal orientation, test the
real time shrinkage or expansion of cement cured at temperatures
0 1000
up to 400 F and pressures up to 10,000 psi.
The cell is the same diameter as the standard size Ultrasonic
Cement Analyzer (UCA). (fig. 7)
HCS 72 pcf
Bentonite 101pcf
118 pcf cement
400 Fig. 7 – The CEST cell has the same outside diameter as the
standard UCA cells.
Shrinkage and Expansion Data
Corrected displacement shown on the charts is the
subtraction of the expansion that occurs after the cement has
reached the curing temperature, usually in four hours.
Shrinkage (negative expansion) was noted in all samples
tested. Initial expansion, which is due to the heating of water,
is subtracted out.
The 101 and 118 pcf cement shrunk approximately 2%,
which falls in line with most published literature9 (figs. 8-9).
The 71 pcf HCS blend cement continued to shrink well after
the cement set. Two tests were performed. The first test was
performed to determine the shrinkage at room temperature and
100 psi pressure. Results show shrinkage of approximately
2.7% in 24 days (fig. 10). The next test was performed at
formation temperatures and pressures. The total shrinkage of
the cement was approximately 17% under pressurized
conditions for 44 hours. The shrinkage is accelerated by the
reaction of cement with the silica based spheres in conjunction
with heat. The sample was removed from the test cell
(pressure released) and physical measurements were made on
the bulk shrinkage of the HCS blend and 10.1% shrinkage in
44 hours was observed. The basic observation here is that the
majority of the shrinkage occurred after the cement had set
(fig. 11). It should be noted that no additional water was
allowed to contact the cement system. The most common high
pressure testing vessels allow water to come in contact with
the set cement. This is the case with most samples placed in
the HP/HT curing chamber.
Shrinkage of 101 PCF Cement @ 190 deg F
4000 0
Press. (psi) Temp (deg F)
3000
Corr. Displ. (%)
-1
2000
-2
0 -3
0 3 6 9 12 15 18
Time (hrs)
Temperature (°F) Pressure (psi) Displacement
Fig. 8 – Shrinkage of 101 pcf cement was similar to published
data for these types of cements.
SPE 95816 5

Shrinkage of 118 PCF Cement @ 190 deg F Shrinkage of 71 PCF HGS 5000, 190 0F, 3,700 psi
4000 1 4000 10

3000

Corr. Displ. (%)

3000 0

Corr. Displ. (%)

Pressure (psi)/
Temp (deg F)
0
Pressure (psi)/
Temp (deg F)

2000 -1 2000

-10
1000 -2 1000

0 -3 0 -20
0.0 3.0 6.0 9.0 12. 15.
0 3 6 9 12 15 18
Time (hrs) Time (hrs)
Temperature (°F) Pressure (psi) Displacement (%) Temperature (°F) Pressure (psi) Displacement (%)

Fig. 9 - Shrinkage of 118 pcf cement was similar to published data Fig. 12 - A request was made from drilling to also test the HGS.
for these types of cements. Similar to HCS, high shrinkage was observed. The majority of
shrinkage occurred after the cement was set.
Shrinkage of 72 pcf HCS - 100 psi / 74 deg F
120 1
The high shrinkage of the cements with both hollow
ceramic and glass spheres is due to the additional breaking of
0
spheres after heat and pressure are applied. Shrinkage was also
Temp (deg F)

observed if the test pressure was reduced from 3,700 psi to

Corr. Displ. (%)

80
Press. (psi)/

-1
100 psi with the temperature constant at 210 0F. It is also
postulated that many hollow spheres in the blend have been
40
-2
cracked during the initial mixing and pressurization. When
cement is placed in the well, continued hydrostatic pressure or
0 -3
formation pore pressure along with temperature cause more
0
spheres to fail. This leads to additional void spaces in the
Time - total curing time 572 hours cement matrix. These void spaces in the cement matrix
Temperature (°F) Pressure (psi) Displacement (%) produce a reduction in cement pore pressure, which is ideal for
Fig. 10 HCS cement blend was tested for a total of 572 hours at bulk shrinkage.
room temperature and 100 psi test pressure in the horizontal During the slurry preparation, special care was taken to
position. Continuous shrinkage was noted throughout the test remove the released air from the broken spheres that occurred
period.
during the initial pressurization. This was accomplished by
placing a vacuum on the sample after the initial pressurization.
Shrinkage of 72 pcf HCS, Well A-2, 190 0F The samples were then placed in the CEST with pressurization
4000 10 and increasing temperature curing to simulate well conditions.
The graphs above show that the additional shrinkage occurred
3000 after the cement had reached the final curing temperature. The
Temp (deg F)

Corr. Displ. (%)

Press. (psi) /

2000
1000
0 -20
0 11
Time (hrs)
Temperature (°F)
Fig. 11 – Temperature and time were the main parameters that
contributed to the shrinkage of this 72 pcf HCS cement blend.
This data led to the investigation of Hollow Glass Spheres
(HGS) that were rated for 5,000 psi for use in in lightweight
cements. The service company’s HCS blend testing
procedures were used for testing the HGS. Similar shrinkage
occurred as compared to the HCS blend (fig. 12).
0
apparatus used to test the shrinkage does not allow additional
water to come in contact with the cement. Normal lab
-10 procedures allow for additional water to enter the cement
while being cured in a hydraulically pressurized curing
chamber.
22 33 44
Corrected displacement, for the purposes of this work, is
determined at the time when the cement has been heated to
Pressure (psi) Displacement (%)
final curing temperature. At this point in the curing time, the
displacement is corrected to zero displacement. This was
chosen because the expansion of water has reached a
maximum value and the cement has not yet set. Initial
expansion is subtracted out from the total displacement of the
piston from the start of the test till the final temperature time is
reached, which is approximately four hours. The movement of
the floating piston is responsible for determining the shrinkage
or expansion of cement.
Rheology and Settling
Rheology values for 101 and 118 pcf cements tested were in
the expected ranges. Rheologies of pressurized HCS blend for
well A-1 showed some higher than planned values. The
surface density was planned to be 79 pcf with the planned
6 SPE 95816

down hole density to be 82 pcf. Note the inconsistency of Hussain Al-Shammary who performed many experiments in
density and rheology between the two field samples shown the laboratory in the support of this work.
below (table 2).
Table 2 REFRENCES
Well- Slurry 600 300 200 100 6 3 1. Mukhalalaty, T., Al Suwaidi, A., Shaeen, M., “Increasing
A-1 Density RPM RPM RPM RPM RPM RPM Well Life Cycle By Eliminating The Multistage Cementer
4200 PCF And Utilizing A Light Weight High Performance Slurry,”
psi SPE 53283, Middle East Oil Show held in Manama,
No. 1 82.0 210 127 92 56 17 14 Bahrain 20-23 February, 1999
No. 2 90.5 300+ 238 195 139 37 29
2. Rucker, R., Sauvabgeau, K. and Randolph, T. “A New
Approach to an Old Problem – Lightweight Liquid
Settling tests of HCS blend exhibited some density Concentrate,” SPE 67193, SPE Production and Operations
segregation (four pcf from top to bottom). Settling tests Symposium held in Oklahoma City, Oklahoma, 2001
specimens left in the curing chamber showed significant
density increases. Additional settling tests performed for well- 3. Baret, J. F., Garnier, A., Rashad, B., “High Performance
A-2 had densities as high as 94.3 pcf for a 71 pcf cement Water Reduced Cement Slurries Prepared With Low Cost
mixed at surface. Another HCS blend for well 10 had a high Optimized Blend,” IADC/SPE 35088, 1996
density of 93.2 pcf for 71 pcf cement mixed at surface. This
4. Sorgard, E., Villar, J. P., “Reducing the Environmental
increase in density clearly shows that the hollow ceramic Impact by Replacing Chemistry with Physics,” SPE 66551,
spheres in the HCS blend are failing or being consumed by the 2001
cement reaction with the silica sphere shells. This allows
water and cement crystals to fill the pore spaces that were 5. Revil, P., Jain, B., “A New Approach to Designing High-
once occupied by air. In field situations where no extra water performance Lightweight Cement Slurries for Improved
is allowed to enter the cement matrix, the void spaces from the Zonal Isolation in Challenging Situations,” IADC/SPE
broken spheres allow cement crystalline growth and 47830, 1998
shrinkage.
6. American Petroleum Institute: “API Recommended
Practice 10B,” 22nd Edition, December 1997
Conclusions
1. Compressive strength of HCS blend declined 81% in 7. Chandler Engineering: “Cement Expansion/Shrinkage
11.75 months when cured at 300 0F and 3,000 psi. Cell,” Instruction Manual, Rev. 1, June, 2003
2. Permeability of HCS blend has increased 7.7 fold in one
year. 8. American Petroleum Institute: “Shrinkage and Expansion
3. Young’s modulus of HCS blend has decreased 81% over in Oilwell Cements,” API Technical Report 10TR2, 1st
1 year. Edition, July 1997. PP 17.
4. One year testing of Poisson ratio of HCS blend reveals the
9. Backe, K. R., Lile, O.B., Lyomov, S. K., Elvebakk, H. and
cement has deteriorated to brittle failure.
Skalle, P., “Characterizing Curing-Cement Slurries by
5. Shrinkage of HCS blend after initial setting is Permeability, Tensile Strength and Shrinkage,” SPE
unacceptably high. Drilling & Completion 14 (3), September 1999
6. Normal density (118 pcf) cement was the most durable of
the three cements tested. Nomenclature:

Future Work API = American Petroleum Institute

Future work should include investigating long term sealing bbls = Barrels
performance of both mechanical and inflatable packer BHCT = Bottom hole circulating temperature
elements that are attached to DV tool. Another area for further bwob = by weight of blend
research is developing a durable lightweight cement system bwoc = by weight of cement
that has minimal shrinkage with acceptable set cement CEST = Cement Expansion & Shrinkage Tester
physical properties at high temperature for the long term. DV = Differential Valve
FLA = fluid loss additive
Acknowledgements gps = Gallons per sack
The authors would like to thank the management of Saudi HCS = hollow ceramic spheres
Aramco for permission to publish this paper. Special thanks HGS = hollow glass spheres
to Dave Larson and Jeff Moon of Chandler Engineering for HSR = High sulfate resistant
their fine work associated with the manufacture of the CEST. HP/HT = High Pressure/High Temperature
The authors would also like to thank all Saudi Aramco Deep IADC = International Association of Drilling Contractors
Gas Drilling Foremen and Engineers for their on-site support in. = inch
and valuable contributions. The authors further acknowledge ft. = feet
the fine work and contributions of the Saudi Aramco R & D mD = milli Darcy
Center’s, drilling fluids and cementing personnel A.S. Al- ml = milliliter (mL=cm3)
Yami, A.S. Al-Humaidi, A.I. Khafaji, M.H. Al-Ariani, and pcf = Pounds per cubic foot
SPE 95816 7

psi = Pounds per square inch

UCA = Ultrasonic Cement Analyzer
0
F = degrees Fahrenheit

SI Metric Conversion Factors

bbl x 1.589 873 E­01 = m3
ft x 3.048* E­01 = m
ft2 x 9.290 304* E­02 = m2
ft3 x 2.831 685 E­02 = m3
ºF (ºF ­ 32)/1.8 = ºC
gal x 3.785 412 E­03 = m3
in.x 2.54* E­00 = cm
in.2 x 6.451* E­00 = cm2
lbmx 4.535 924 E­01 = kg
mL x 1.0* E­00 = cm3
psi x 6.894 757 E­00 = kPa
* Conversion factor is exact