SPE-172020-MS

New Developed Acid Soluble Cement and Sodium Silicate Gel to Cure Lost
Circulation Zones
Abdullah S. Al-Yami and Abdullah Al-Ateeq, Wagle; Vikrant B, Ziad AlAbdullatif, and Mohammad Al-Qahtani,
Saudi ARAMCO

Copyright 2014, Society of Petroleum Engineers

This paper was prepared for presentation at the Abu Dhabi International Petroleum Exhibition and Conference held in Abu Dhabi, UAE, 10 –13 November 2014.

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
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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
Moderate to severe loss of circulation problem encountered while drilling in Aramco field is a major
economic burden that increases the total well construction cost dramatically in some cases. Complete or
even partial control of the moderate to massive loss circulation problem may save thousands of dollars/per
well and thus can make the drilling economics more economical.
Saudi ARAMCO has developed a LCM formulation that can be used to cure lost circulation in the
Middle East. The formulation consists of acid soluble cement and a sodium silicate gel that has a high
potential to control moderate to severe loss circulation problem.
Experimental data indicate that the control of loss of circulation using the silicate gel and soluble
cement can be achieved as follows: 1) injection of the gel first into the fracture to penetrate the near
fracture rock matrix, 2) pumping a small volume of spacer after the gel to delay the contact between the
sodium silicate gel and the soluble cement, and finally 3) injection of soluble cement into the fracture to
plug the fracture zone.
Silicates have been used with cement to cure lost circulation and for water shut off treatment over the
past 50 years. The major limitation of such technicue is rapid reaction and acid insoubility, Bauer et al.
(2005). The objective of this paper is to introduce the use of acid soluble cement and sodium silicate gel
as a possible solution to cure lost circulation zones in Saudi Arabia fields.

Introduction
Lost circulation occurs when formation fluid pressure is less than the fluid column pressure in the wellbore
causing drilling fluid lost into the formation, Bauer et al. (2005).
Operators set cement plugs for a variety of reasons: abandonment, sidetracking, lost-circulation control,
or remedial work. However, as important as plug cementing can be to the overall success of a well
program, the process often is performed without regard to wellbore conditions. Studies have highlighted
many of the problems encountered in plug cementing. To avoid such problems, a procedure was
developed which provides a reliable plug-setting procedure and a method to monitor success rates.
When lost circulatin of drilling fluid is expeirnced, cement plugs can be common initial solution.
Drilling will be stopped and cement plug will be placed to be cured then re-drilled. However, high cross
2 SPE-172020-MS

Figure 1—Schematical illustration of polymerization of silica, from ller (1979)

flow rates or large lost circulation zone will provide

environment for cement plugs to work. Cement can
be washed out or the amount of cement may not fill
the lost circulation zone, Bauer et al. (2005).
There is also available literature which discusses
the application of various cement types and process
designs as loss circulation materials. The paper de-
scribes criterion for selecting the best cement com-
positions, optimal strategies and solutions to prob- Figure 2—Silicate monomer
lematic field cases are provided, Byung-Sik et al.
(2008).
Additionally, there is literature which describes the use of reactive materials viz. cement and sodium
silicate to form plugs for blowout control, Al-Dhafeeri et al. (2008). The use of cement to react with
sodium silicate requires simple chemistries that are fairly retarded, highly dispersed, and only modified
with silica flour at high temperatures, Bauer et al. (2005).
Silicate hydrates have been used in a grouting system that was developed for high-temperature
grouting/plugging for lost circulation. The system involves means to introduce sodium silicate and an
activator through a single tubular by encapsulating the activator in a material that is temperature sensitive,
thus delaying the initiation of the reaction. The formation of silicate hydrate plugs was studied over the
range of 80°C to 300°C as well as the chemical stability of silicate hydrate for 10-12 weeks, Bauer et al.
(2005).
Silicate based gel systems have also been employed to solve water conformance problems on injector
and producer wells, for casing leak repairs and other applications including loss circulation, Stavland et
al. (2011). The SPI gel system developed was a low cost, multi-component silicate based gel, mixed at
surface and pumped as a single stage with controlled gel times ranging from a few hours to several days
to form a variety of resilient gels from hard, “ringing” to soft, weak gels. This gel system used low
SPE-172020-MS 3

Figure 3—Silica tetrahedral

Figure 4 —Silicate-cement gel development

chemical concentrations and no heavy metals for a low overall cost. The SPI pre-gelled system has a low
viscosity for deep penetration of leaks and tight formations and it can be designed for special applications.
A soluble silicate has also been used as loss circulation material wherein when the pH of the silicate
solution is lowered such that the solubility limit is surpassed; the silicate species cross-link to form a silica
gel, Herring et al. (1984). In addition to their gelling action, silicates react with polyvalent metal ions to
produce metal silicate precipitates that are less soluble across a broader pH range than the metal
hydroxides produced by non-silicate processes.
Silicates have been used with cement to cure lost circulation and for water shut off treatment over the
past 50 years. The major limitation of such technicue is rapid reaction and acid insoubility, Bauer et al.
(2005). The objective of this paper is to introduce the use of acid soluble cement and sodium silicate gel
as a possible solution to cure lost circulation zones in Saudi Arabia fields.
4 SPE-172020-MS

Figure 5—Sodium Silicate solution and Acid-soluble Magnesia Cement was soluble in 15% HCl acid

Loss Circulation Zones in Saudi Arabia

Rus Formation
Rus formation is a regular casing point. Rus casing is intended to prevent shallower formations collapsing
(Hofuf, Dam, Hadrukh, and Dammam). These shallow formations are mainly loose with loss of
circulation zones, such as the Khobar Member. Therefore, such a large sized hole collapsing is highly
possible. A secondary objective of the Rus casing is to protect the Umm Er Radhuma aquifer below Rus.
Umm Er Radhuma Formation
UER is a major aquifer in Saudi Arabia. It is mainly consists of limestone and/or dolomite. Thin beds of
shale and marl are present, especially toward the lower part of the formation.
Shu’aiba Formation
Shuaiba mainly consists of different types of carbonates depending on the well location. The vast extent
of Shuaiba is porous with fast ROP. In many areas Shuaiba is a loss of circulation zone.
Arab Formation
There is partical lost circulation zone within Arab-D formation.
Drilling Practices in Lost Circulation Formation
Lost circulation zones can be classified as follow:
Seeping loss (5 - 10 bbls/Hr)
Partial loss (10 - 30 bbls/Hr)
Total loss (30 - 70 bbls/Hr), mud level drops around 500 ft
Total severe loss (⬎ 70 bbls/Hr), mud level drops significantly below 500 ft
It is very difficult to cure lost circulation in UER. The drilling practice in this case is to drill with water
to the next casing point. Mud cap can be used if H2S gas is encountered. In workover operations, it is
difficult to cure losses in UER through a casing leak. CaCl2 fluid can be used followed by sodium silicate
to form a gel plug and then pumping cement behind it. All pumping must be performed with EZ-SV
cement retainer. The success of this method is limited and immature setting of cement is always a concern.
Squeezing cement was practiced to cure the severe losses. Setting depth of casing is the root cause of
this problem. Pumping LCM was not successful in many cases in Arab-D lost circulation in deep gas
SPE-172020-MS 5

Table 1—FAN-35 Model Viscometer Dial Reading

Temperatures F° Solution Type 600 rpm 300 rpm 200 rpm 100 rpm 6 rpm 3 rpm

75 100% Sodium Silicate 7 5 4 2 1 1

100 100% Sodium Silicate 7 3 2 2 1 1
195 100% Sodium Silicate 4 3 2 1 1 1
75 100% Soluble Cement 80 65 53 40 27 21
100 100% Soluble Cement 62 49 42 33 21 18
195 100% Soluble Cement 60 40 34 26 10 8
75 50% Sodium Silicate⫹50% 110 86 74 67 49 48
Soluble cement
100 50% Sodium Silicate⫹50% gelled gelled gelled gelled gelled gelled
Soluble cement
195 50% Sodium Silicate⫹50% gelled gelled gelled gelled gelled gelled
Soluble cement

rpm: revolution per minute

Remarks: gelled means solution was gelled and not moved at all.

wells. Other different plugs such as “gunk and/or cement plugs” have been tried. It is recommended to use
EZ-SV retainer to pump cement if the casing size allows using EZ-SV.
Using LCM pills to cure lost circulation in Shuaiba is not really effective in curing lost circulation.
More work is required to identify the type of existent fractures when preparing LCM pills. However
Arab-D lost circulation can be cured to some degree by using proper LCM pill formulation. Pumping
LCM pills at high rate is the key factor for successful job.
In severe lost circulation pumping LCM pills is not helping the situation, the best practice is not to use
any LCM pills, and to drill blindly and use mud cap as needed and try to reach the planned casing point
as fast as possible.
Monitoring ECD by Proper hydraulic program and running pressure While Drilling “PWD” may
minimize the risk of inducing fractures. Large nozzles size can be used while drilling and pumping can
be done at good rate without causing any washout of sand and reduce cuttings loading in the annulus.

The Developed Lost Circulaiton Material

Sodium silicate has been applied for deeper treatment mainly for water shut off treatment. Commercial
sodium silicate (SiO2) n: Na2O is a clear fluid with a pH in the range of 11-13, based on the SiO2:Na2O
molar ratio. Alkalinity increases by decreasing SiO2:Na2O molar ratio. At high pH the dimer silicate
structure dominates. At low pH the liquid silicate will gel trhough polymerization of the silicate species,
Stavland et al. (2011).
Acid soulbe cement can be used as a diverter plug for water shut off treatment. It can be used in open
hole reservoir because of its acid solubility. Sodium silicate is available in different forms with various
ratios of sodium oxide (Na2O) to silicate (SiO2). Typical sodium silicate solution will have a ratio of Na2O
to SiO2 as 3.2:1. The advantages of using this system are controllable gelation time, deep gel penetration
and low cost, Al-Dhafeeri et al. (2008).
Stavland et al. 2011 mentioned that divalent ions such as Mg (OH) 2 will be precipitated when mixed
with sodium silicate so the makeup water needs to be properly designed to be able to pump big quantities
of sodium silicate. Dimentionsional gel network can be obtained by adding salt such as calcium or
Magnisum at pH of 7-10 or by redcuing pH value lower than 7, Fig.1.
Soluble silicate has three components: water, alkali and silica. Silicates exist as polymeric forms in
solution. Tetrahedral silicon atom is the fundamental block in the silicate solution. We can have silicate
monomer (tetrahedral silicon at the center of an oxygen-cornered, four-sideded pyramid), Fig. 2. In
6 SPE-172020-MS

sodium silicate, the oxygen atom is connected to

sodium or hydrogen atom or linked to another silica
tetrahedral (Silicate Trimer, Fig. 3), Stavland et al.
(2011).
Silicates can react with polyvalent metal ions to
produce metal silicate precipitates. For example cal-
cium will react with sodium silicate to form calcium
silicate hydrate this can be obvious when we add
cement (calcium source) to sodium silicate.
In general, cement is composed of four main
components: tricalcium silicate (C3S) responsible
for the early strength development, dicalcium sili-
cate (C2S) responsible for the final strength, trical-
cium aluminate (C3A) contributing to the early
Figure 6 —Sodium Silicate solution and Acid-soluble Magnesia Cement
strength and tetracalcium aluminaferrite (C4AF). In
addition, gypsum is added to control the setting time
of cement, Nelson (1990).
When sodium silicate Na2SiO3 is mixed with cement where calcium hydroxide (Ca (OH) 2) is the
principal ingradient silicate cement gel is created. Formula 1, 2, and 3 and Fig.4 detailed the silicate-
cement gel development:
(1)

(2)

(3)

Sodium ion concentration in the absorption water of cement particles is affected by the exchange
activity between Sodium ion Na⫹ and calcium ion Ca 2⫹ of sodium silicate. Solubility of Calcium oxide
is increased by increase in concentration of sodium hydroxide (NaOH) in the curing water and calcium
hydroxide (Ca (OH) 2). When designing cement slurries with sodium silicate we need to pay attention to
the concentration used. If we have high thick silica gel the cement will be retarded due to delay in
hydration of cement. The reason behind this is the slow movment of cement particles into the semiper-
meable membeance, Herring et al. (1984).
Cement can be used as an activator for sodium silicate solution. However, major problems that can
occure are immature setting. Removing cement from casing is difficult, Herring et al. (1984).
Acid-soluble Magnesia Cement has been used before since 1975 to cure lost circulation. Magnesia
cement is a mixture of magnesium and calcium oxide, carbonates, and sulfates. When adding water to the
mixure magnesium-hydroxy-sulfate/chloride inorganic polyhydrte with high compressive strength. The
dry blend of Magnesia cement has a relateive density of 2.92 g/cm3. Magesium cement is mixed with oil
well cement at any desired ratio. Magnesia cement can be mixed with different retarders’ concentration
at various temperatures, Sweatman et al. (1990).
Retarders are cement additives whose function is to retard, or delay the setting of cement slurries. For
a well with temperature about 125 °F or less, no retarder is needed to be added to the cement slurry when
API class H or G is used, Brothers et al. (1991). However, as temperature increases, the hydration process
of C3S increases and, hence, the thickening time decreases, Bensted (1991). Typical examples of
compounds used as retraders include: calcium lignosulfonate, sodium lignosulfonate, sodium tetraborate
decahydrate (borax), starch derivatives, hydroxyethyl cellulose and weak organic acids, Eoff et al. (1995).
SPE-172020-MS 7

Table 2—Acid-soluble Magnesia Cement without sodium silicate solution

parameter Formulation 1 Formulation 2 Formulation 3 Formulation 4

water, gallons per sack 4.93 4.99 5.04 5.03

sodium silicate gel, gallons per sack 0 0 0 0
retarder, % BWOC 0 10 18 15
BHST, F 234 234 234 234
BHCT calculated, F 185 185 185 185
Bottom hole pressure, psi 2917 2917 2917 2917
setting time, minutes 32 152 ⬎280 ⬎280

Selection of retarder depends significantly on the type of cement and well conditions, Brothers et al.
(1991). Due to the readily availability, lignosulfonates are the most commonly used retarders. However,
this type of retarders is not applicable at high temperatures because of the carbohydrate content and
chemical structure. Instead, organic acids and water soluble borates are the retarders of choice at these
conditions, Eoff et al. (1995).
For the testing conducted in this paper, we have used HCl-soluble borate salt. Acid-Soluble Magnesia
cement is a solid bridge on the surface of the formation and will not penetrate inside the pores. To solve
this limitation of acid soluble magnesia cement, sodium silicate solution can be introduced into the
formation first for deeper penetration.
The control of loss of circulation using the silicate gel and acid soluble magnesia cement can be
achieved as follows: 1) injection of the gel first into the fracture to penetrate the near fracture rock matrix,
2) pumping a small volume of spacer after the gel to delay the contact between the sodium silicate gel and
the soluble cement, and finally 3) injection of soluble cement into the fracture to plug the fracture zone.
Once the Sodium Silicate solution is in contact with Acid-soluble Magnesia Cement then a rapid
gelling effect takes place., Fig.5. The soluble cement was prepared by adding water to the dry soluble
cement to make a homogonous fluid. FAN-35 Model Viscometer was used to measure the viscosity of the
fluid. The soluble cement and the sodium silicate solutions viscosities are measured each individually at
three temperatures 75, 100 and 190 °F. After that, a mixture composed from 50% by volume of soluble
cement fluid and 50% by volume of sodium silicate fluid is mixed. The mixture is then transferred to
FAN-35 Model Viscometer to measure its viscosity at 75, 100 and 190° F and at 600 rpm, 300 rpm, 200
rpm, 100 rpm, 6 rpm, and 3 rpm, Table 1.
Conventional Portland cement and an activated sodium silicate gel were used in the industry as a water
or gas shutoff material. However this is the first study to demonstrate the use of a combination of acid
soluble cement and sodium silicate gel as an effective option for a water or gas shutoff or curing lost
circulation both for non-reservoir and reservoir zones because the gel-cement LCM is soluble in 15% HCl
acid. The solubility of the solution was around 87%., Fig.5.
As mentioned earlier the control of loss of circulation using the silicate gel and acid soluble magnesia
cement can be achieved as follows: 1) injection of the gel first into the fracture to penetrate the near
fracture rock matrix, 2) pumping a small volume of spacer after the gel to delay the contact between the
sodium silicate gel and the soluble cement, and finally 3) injection of soluble cement into the fracture to
plug the fracture zone. The next section describes testing the lost circulation at the formation that is after
the third stage.
Testing at elevated tempature and pressure was also conducted on combination of Sodium Silicate
solution and Acid-soluble Magnesia Cement. The prepared slurry was poured into API standard HP/HT
consistometer slurry cup for thickening time to evaluate the pumpability of the cement slurry. The slurry
was conditioned in the atmospheric consistometer before obtaining the rheological readings. A Fann
viscometer (Model-35) was used to measure the slurry rheology.
8 SPE-172020-MS

Table 3—Acid-soluble Magnesia Cement sodium silicate solution

parameter Formulation 5 Formulation 6 Formulation 7 Formulation 8 Formulation 9

water, gallons per sack 5.19 5.09 5.22 5.12 5.1

sodium silicate gel, gallons per sack 0.3 0.15 0.3 0.15 0.15
retarder, % BWOC 10 10 15 15 11
BHST, F 234 234 234 234 234
BHCT calculated, F 185 185 185 185 185
Bottom hole pressure, psi 2917 2917 2917 2917 2917
setting time, minutes 129 152 294 ⬎280 201

Set cubes of combined Sodium Silicate solution Table 4 —FAN-35 Model Viscometer Dial Reading for formulation 9
and Acid-soluble Magnesia Cement were removed Parameter Information
from the molds (Fig.6), and placed in a hydraulic Viscosity @ 3 rpm 18.65
press where increasing force was exerted until fail- Viscosity @ 3 rpm 25.45
ure. The hydraulic press system used in this study Viscosity @ 3 rpm 43.35
applied known compressive loads to the samples. Viscosity @ 3 rpm 47
Viscosity @ 3 rpm 51
This system was designed to test the compressive
Viscosity @ 3 rpm 64.6
strength of sample cement cubes in compliance with Viscosity @ 3 rpm 72.6
API specifications for oil wells cement testing. The 10 seconds gel strength 24.3
compressive strength was measured to be 500 psi. 10 minutes gel strength 33.2
Nine formulation were tested at elevated temper-
ature for setting time. Table 2 shows retarder re-
sponse on Acid-soluble Magnesia Cement without sodium silicate solution. Setting time was controlled
by varying the concentration of retarders. Table 3 shows the effect of adding small concentration of
sodium silicate solution to the acid soluble magnesia cement. The setting time was reduced from 152
minutes to 129 in formulation 5. Formulation 4 showed excessive setting time without using soduium
silicate solution and with using 15 % BWOC retarder. The setting time was controlled to be 294 minutes
when using 0.3 gallons per sack of sodium silicate gel. However, the slurry was thick so to improve the
rheology of the slurry lower concentration of sodium silicate gel was used as shown in formulation 8 and
9. Table 4 shows the rheology results of the lost circulation slurrly.
Any conentation of soldium silicate gel from Table 5 can be used since the treatment will be in stages.
So the thick slurry with short setting time will be experience in the formation not in the pipe due to the
use of spacers and stage treatmetns.

Conclusions
1. Saudi ARAMCO has developed a LCM formulation that can be used to cure lost circulation. The
formulation consists of acid soluble cement and a sodium silicate gel that has a high potential to
control moderate to severe loss circulation problem.
2. Experimental data indicate that the control of loss of circulation using the silicate gel and soluble
cement can be achieved as follows: 1) injection of the gel first into the fracture to penetrate the near
fracture rock matrix, 2) pumping a small volume of spacer after the gel to delay the contact
between the sodium silicate gel and the soluble cement, and finally 3) injection of soluble cement
into the fracture to plug the fracture zone.
3. Silicate gel and acid soluble magnesia cement showed controlled setting time at different
concentration of sodium silicate gel and retarders. So for big lost circulation short setting time is
required. This can be achieved by using higher concentaion of sodium silicate or lower concen-
tration of retarders.
SPE-172020-MS 9

4. Rheology and compressive strength for the lost circulation material was acceptable (more than 500
psi).
5. Acid soulibility showed that Silicate gel and acid soluble magnesia cement is soulbe in 15% HCl
acid.

Acknowledgements
The authors would like to thank Saudi Aramco for permission to present and publish this paper.

Abbreviations
API : American Petroleum Institute
Bc : Bearden consistency
BHCT : Bottom Hole Circulating Temperature, °F
BHST : Bottom Hole Static Temperature, °F
BP : British Petroleum
BV : Bulk Volume, inch3
DP : Differential Pressure, psig
ECD : Equivalent Circulating Density, lb/gal
HT/HP : High Temprature/High Pressure
ID : Inside Diameter, inch
LDC : Low Density Cement
OD : Outside Diameter, inch
POOH : Pull-out of hole
PV : Plastic Viscosity, cp
TD : Total Depth, ft
TDS : Total Dissolved solids, mg/l
XRD : X-Ray Diffraction
YP : Yield Point, lb/100 ft2

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SI Metric Conversion Factors

in. ⫻ 2.54* E⫺02 ⫽ m
(°F-32) / 1.8* E⫹00 ⫽ °C
ft ⫻ 3.048* E⫺01 ⫽ m
gal ⫻ 3.785 412 E⫺03 ⫽ m3
lbm ⫻ 4.535 924 E⫺01 ⫽ kg
psi ⫻ 6.894 757 E-03 ⫽ Mpa
lbm/gal ⫻ 1.198 26 E-01 ⫽ S.G
bbl ⫻ 1.58987 E-01 ⫽ m3
*Conversion factor is exact