SCHOOL OF PETROLEUM TECHNOLOGY

M.Tech Thesis Presentation

“A NOVEL APPROACH OF USING COW DUNG AS FLUID

ADDITIVE IN DESIGNING OF CEMENT SLURRY AND STUDY
OF SPACER COMPATABILITY WITH CEMENT SLURRY AND
WATER BASED MUD”

Guided by:
DR. ANIRBID SIRCAR
Mr. MAUNISH SHAH

Presented by:
RAJNISH TRIPATHI
16MPE10

Gandhinagar ∙ 22. May 2018 ∙ www.pdpu.ac.in

 Outline

• Motivation
• Introduction
• Problem Description
• Literature Review
• Research Methodology
• Results and Discussions
• Conclusion
• Reference
 Motivation of Research
• It is generally clearly acknowledged that a lack of fluid loss control may be responsible for primary
cementing failures, due to excessive density increase or annulus bridging and that formation invasion by
cement filtrate may be deleterious to the production.

Fig 1: Cement dehydration Fig 2: Uneven cement setting

Thus, motivation of the research is to use environmental friendly fluid loss additive.
Introduction
Cement Slurry Design: Cement Slurry Parameters:
Factors influencing slurry design are as follows:  Slurry density
1) Well depth, diameter and casing size  Thickening time
2) Bottom hole circulating temperature(BHCT)  Rheology
3) Bottom hole static temperature(BHST)  Fluid loss control
4) Bottom hole pressure(BHP)  Free water content
5) Sample of cement ,cement additive mixing water  Compressive strength

 The ideal cement slurry has no measurable free water, provides adequate fluid-loss control, has
adequate retarder to ensure proper placement, and maintains stable density to ensure
hydrostatic control.
Introduction

Cement Additives:

• Accelerator • Lost circulation additives

• Retarder • Defoamers
• Extender • Expanding additives
• Heavyweight additives • Gas Migration control additives
Fig 3: Hematite
• Dispersant • Anti settling agents
• Fluidloss additive • Fluidloss additive

 The properties of cement slurries can be modified to meet the

demands of a particular well application. These modifications are
accomplished by the admixing of chemical compounds commonly
referred to as additives that effectively alter the hydration Fig 4:Micromax
chemistry.
Introduction

Spacers:
• Spacers are viscous fluid placed ahead of cement slurry
and after drilling fluid before primary cementation.

• The purpose is to prevent contamination of cement slurry

with drilling mud.

• They are made in a manner to be compatible with both

the cement slurry and the drilling mud in use.

• It is very important that the fluids be compatible as the

majority of drilling muds are flocculated by cement

• This can result in phase separation, settling of solids,

poor cleaning, and insufficient water-wetting.

FIG 5: Spacer System

Introduction

Spacer design parameters:

• They should be compatible with both the cement slurry and the drilling mud.
• Their densities, gel strengths and viscosity should be more than that of the drilling fluid and less than to
that of the cement slurry.
• Spacer should also be capable of maintaining a separation between cement slurry and drilling mud.
• The effective viscosity of the spacer should ideally lie between the effective viscosity of the WB / OBM
mud and cement, over the range of shear rates of interest, confirming an effective mud removal.

NOTE: The ideal shear rheogram would be half - way between the mud and cement rheogram (Theron., 2002).
Problem Description

• Oil and gas cement slurry is combination of cement , water and different properties.
• Inclusion of too many additives to impart different properties can result into complex rheology.
• It is difficult to use too many additives in offshore environment as it will directly affect the logistics and
expenditure of cementing operations.
• Improper selection of fluidloss additives results in cement hydration, early setting of cement slurry and
sometimes leads to gas migration.
• Synthetic polymers used as fluid loss additives are not environmental friendly.
• Many additives impart required property when brought to higher temperature and behave differently at
lower temperature.
 Literature Review
Author/ Journal or
Sr No. Title Inference
conference/year
Slurry fluidloss endangers
“Why Cement Fluidloss cementing operation in two ways:
1. J.F Baret et.al/SPE/1996
Additives Are Necessary” 1) During placement
2) During waiting on time

For non crosslinked polyvinyl

“Comparative study of working
J. Planck et al./SPE alcohol, main mechanism is
mechanism of chemically
2. International plugging of cement filter cake by
different cement fluid loss
symposium/2009 film formation. This is most
polymers “
commonly used FLA.

The study confirms that over

“High Temperature Cementing : A.Cadix et al./Abu Dhabi wide temperature range and
3. Fluid loss Control Polymer International Petroleum cement grades fluidloss is
Performance and Limitations” Conference/2016 directly correlated to polymer
adsorption on cement surface.
 Literature Review
Author/ Journal or
Sr No. Title Inference
conference/year
Low molecular weight HEC can
“Environmentally Acceptable increase to the level of synthetic
4. Bach Dao et.al/SPE/2002
Fluidloss Additive” fluid loss additive and is
environmentally acceptable.

Barite nanoparticle reduced

Amin et al./SPE fluidloss by 50% at low
“Barite nanoparticles Reduce
5. Oklahoma City concentrations improving the
the Cement Fluid Loss”
Symposium/2017 cement quality along the
wellbore.

Flexural and Compressive

“Effect on Compressive and
R. Reddy et al./Indian strengths are higher at 5% of cow
Flexural Properties of Cow
6. Journal of Advances in dung at constant glass fiber this
Dung/Glass Fiber Reinforced
Chemical Science /2014 supports to enhance the other
Polyester Hybrid Composites”
properties of materials
 Literature Review
Sr No. Title
“An Experimental Investigation
on Strength of Concrete made
7.
with Cow dung Ash and Glass
Fibre”
“Effect of thixotropic agent in
prevention gas migration
8.
through cement slurries”
Author/ Journal or
Inference
conference/year
The replacement of cement with
CDA with 8% leads to increase in
Anisha G et al./
compressive strength whereas the
IJERT/2017
percentage replacement leads to
decrease in compressive strength.
By addition of 0.5 gm of
Arian Velayati et al./ oil thixotropic agent to a slurry
and gas expo/ composed of anti gas migration
Dubai,UAE/2015 agent, cement slurry transition
time reduced by 250 minutes
.
Research Methodology

Objectives of Research

• Eliminating complexity in preparing conventional cement slurry by introducing novel organic

multifunctional additive and improving the cement slurry properties.
• To identify environmental friendly and cost efficient additive.
• To analyze the effect of Cow dung particles on different cement properties such as thickening time,
compressive strength, fluid loss, free water and density.
• Designing spacer and checking its compatibility with cement slurry and water soluble mud.
• Evaluating R-Index value of Spacer system.
Research Methodology

Cow dung as fluidloss additive:

Cow Manure
Moisture
0.4% 0.35% Organic
0.9% 0.7% Matter
Nitrogen
Cellulose(60%)
24.20% Phosphorus
H.Cellulose (27%)
75.3% Potassium
Lignin (13%)

FIG 7: Cow manure composition

Research Methodology

Working Mechanism:
• Long chain of glucose molecules
linked together
1. Choking • Resistant to moisture
2. Adsorption • Insoluble in water
Cellulose(60%)

• Amorphous structure
H.Cellulose (27%) • Susceptible to moisture
• Soluble in water
Lignin (13%)
• Cross linked polymer chain
• Resistant to temperature
• Strong covalent bond
 Research Methodology

Experimental Setup:

HPHT CONSTANT SPEED ATMOSPHERIC CURING CHAMBER

CONSISTOMETER MIXER CONSISTOMETER
Research Methodology

FLUID BALANCE

STRENGTH TESTING
HPHT FILTER PRESS VISCOMETER
MACHINE
Research Methodology
Experimental Methodology:

Materials used:
• Class “G” HSR (High Sulphate Resistant) cement was used in all the experiments conducted for
cement slurry formulation.
• 600 grams of class G cement was used along with the additives in below given proportion.
• According to API Specification, 10A, water requirement for cement slurry is 44% BWOC (By
weight of cement).
• CDPs in varied compositions as FLA were used.
• Some other dispersants and Defoamers were also used.
Research Methodology

S. No. Component % BWOC

1 Class ‘G’ Cement 100

2. Water 54

3. Silica flour 35

4. CDPs Variable

5. Dispersant 0.1

6. Defoamer 0.1

Table : Additives used in different proportions of BWOC

Research Methodology

CONDITIONING OF CEMENT SLURRY

FLUID LOSS TEST

FREE WATER TEST

COMPRESSIVE STRENGTH TEST

THICKENING TIME TEST

Fig 16: Sequence of slurry tests Fig 17: Selection of additives,

Research Methodology

Spacer Design Methodology:

1.Preparation of Fluids
Ratio mud or cement to
No. Mixing scheme
A. Cement slurry spacer (vol. %)

B. Spacer 1 95/5 760 ml mud or cement/40 ml spacer

2 75/25 100 ml spacer plus 375 ml of No.1
C. Mud
3 5/95 40 ml mud or cement/760 ml spacer
D. Fluid mixture 4 25/75 100 ml mud or cement plus 375 ml of No.3
5 50/50 Equal parts of No.1 and No. 3
TABLE: Ratio Mixtures

 Preparation and Conditioning of fluid train is done according to section 5.4 of API RP 10 B-2, 2013
Research Methodology

2. Determination of R Index Value

If R < 0 Fluids are compatible.

Fluids are compatible, but friction pressures should be verified to avoid

0 < R< 40
fracturing the formation.

41< R < 70 Fluids are slightly incompatible. Additional testing is required.

R >71 Definitely Incompatible. An alternative formulation must be found.

R = Highest 100-rpm reading from a mixture – 100-rpm reading from individual fluid
Results and Discussions
Sample slurry design:

Cement Silica Flour Water FLA Dispersant Retarder Defoamer

C/100 35 W/54 DO-60/0.6 DO-65/0.1 D-800/0.1 DO-47/0.1

600 210 324 3.6 0.6 0.6 0.6

Sample slurry parameters:

S. No. Parameters Value

1. Specific gravity 1.9

2. BHCT/BHST 100/105° C

3. Fluid loss 254 ml

4. Free water NIL

5. Thickening time 264 min

 Result and Discussions
Cement slurry design without any FLA:

Cement Silica Flour Water FLA Dispersant Retarder Defoamer

C/100 35 W/54 0 DO-65/0.1 D-800/0.1 DO-47/0.1

600 210 324 0 0.6 0.6 0.6

Rheogram of slurry without FLA Rheological parameters:

50
45
Plastic Viscosity (Cp.) 24
40
35
Yield Point (lbf/100ft2) 28.98
Dial readiing

30
25
20
Fluid loss = 2065 ml/30 min Critical Velocity (ft./sec) 1.379
15
10 n (Flow behaviour index) 0.462
5
0 k (Consistency index) 0.36
0 50 100 150 200 250 300 350
RPM
 Result and Discussions
Cement slurry design using CDPs:

Cement Silica Flour Water CDPs Dispersant Retarder Defoamer

C/100 35 W/54 0.6 DO-65/0.1 D-800/0.1 DO-47/0.1

600 210 324 3.6 0.6 0.6 0.6

Rheogram of slurry with CD-0.6% (<300 mm) Rheological parameters:

300
Plastic Viscosity (Cp.) 41.4
250

200
Dial readings

Yield Point (lbf/100ft2) 13.26

150

100 Fluid loss = 2086 ml/30 min Critical Velocity (ft./sec) 10

50 n (Flow behaviour index) 0.575

0
0 50 100 150 200 250 300 k (Consistency index) 0.154
RPM
 Result and Discussions
Cement slurry design using CDPs:

Cement Silica Flour Water CDPs Dispersant Retarder Defoamer

C/100 35 W/54 2 DO-65/0.1 D-800/0.1 DO-47/0.1

600 210 324 12 0.6 0.6 0.6

Rheogram of cement slurry with CD-2% (<300 mm) Rheological parameters:

300

250
Plastic Viscosity (Cp.) 62.1

200 Yield Point (lbf/100ft2) 10.98

Dial readings

150
Critical Velocity (ft./sec) 28.268
100
Fluid loss = 1864 ml/30 min
n (Flow behaviour index) 0.992
50

0 k (Consistency index) 0.436

0 50 100 150 200 250 300
RPM
 Result and Discussions
Cement slurry design using CDPs:
Cement Silica Flour Water CDPs Dispersant Retarder Defoamer

C/100 35 W/54 4 DO-65/0.1 D-800/0.1 DO-47/0.1

600 210 324 24 0.6 0.6 0.6

Rheogram of cement slurry with CD-4% (<300 mm) Rheological parameters:

300

250 Plastic Viscosity (Cp.) 146.9

200
Yield Point (lbf/100ft2) 8.82
Dial readings

150 Fluid loss = 1305 ml/30 min

Critical Velocity (ft./sec) 10
100

n (Flow behaviour index) 0.99

50

0 k (Consistency index) 0.148

0 50 100 150 200 250 300
RPM
 Result and Discussions
Cement slurry design using CDPs:

Cement Silica Flour Water CDPs Dispersant Retarder Defoamer

C/100 35 W/54 5 DO-65/0.6 D-800/0.1 DO-47/0.1

600 210 324 30 3.6 0.6 0.6

Rheogram of Cement slurry with CD-5% (<300 µm) Rheological parameters:

300

250 Plastic Viscosity (Cp.) 277

200
Yield Point (lbf/100ft2) 7.19
Dial readings

150
Critical Velocity (ft./sec) 19.13
100

50
Fluid loss = 241 ml/30 min n (Flow behaviour index) 0.9266

0 k (Consistency index) 0.44

0 50 100 150 200 250 300
RPM
 Result and Discussions
Cement slurry design using CDPs:

Cement Silica Flour Water CDPs Dispersant Retarder Defoamer

C/100 35 W/54 5 DO-65/0.1 D-800/0.1 DO-47/0.1

600 210 324 30 0.6 0.6 0.6

Rheogram of cement slurry with CD-5% (>300 µm) Rheological parameters:

300

250 Plastic Viscosity (Cp.) 134

200
Yield Point (lbf/100ft2) 7.76
Dial readings

150
Fluid loss = 180 ml/30 min
Critical Velocity (ft./sec) 10.43
100
n (Flow behaviour index) 0.864
50

0 k (Consistency index) 0.325

0 50 100 150 200 250 300
RPM
Result and Discussions

Fluid loss (ml/30 min) vs CD

2500

2065 2060

2000 1859

1500
Fluid loss(ml)

1305

1000

249
500

180
0
0 1 2 3 4 5 6
CD (%)
Result and Discussions

Plastic viscosity (cp) vs CD (%)

300
277

250

200
PV (cP)

146.9
150 134

100

62

50 41.4
24.1

0
0 1 2 3 4 5 6

CD (%)
 Result and Discussions

YP (lbf/ft2) vs CD (%)
35

3028.98

25
YP (lbf/100ft2)

20

15 13.26

10.96
7.76
10 8.82

5
7.19

0
0 1 2 3 4 5 6
CD (%)
Result and Discussions

Free water (ml) Vs

CD (%)
6

5 5
5

4 4
4

2 2
2

1
1 0.6 0.5
0 0 0
0
1 2 3 4 5 6

CD(%) Free water (ml)

Result and Discussions

Fluidloss Comparison

300
251
241
250

180
200

150

100

50

0
Sample < 300 µm >300 µm
Result and Discussions

24 HRS COMP.STRENGTH (PSI)

3330

3100

2800

Neat Sample CD (5%)

Comp.Strength (psi) 2800 3100 3330
Result and Discussions

Thickening Time (hour)

7.75

4.4

0.75
Neat Sample CD (5%)
TT (hour) 0.75 4.4 7.75
Result and Discussions
Cement and Spacer additives : Schlumberger

Fluid Sp. Gr. Composition

Cement - 100 + Water - 44+ Silica flour - 35+ DO47 - 0.1 + Bentonite - 0.1 + D255
Cement
1.97 - 0.42 + DO65 - 0.65 + D093 - 0.4+ DO28 – 1.3
Slurry :
All additives are % BWOC.

Weighted Water-100 + B250- 2.5 + DO47- 0.1+ Barytes

1.80
Spacer : All additives are % BWOW.

Water -100 + Biocide - 0.05 + Soda Ash - 0.1 + KCL- 5 + PAC L - 0.25 + PHPA - 0.3
Mud + XC Polymer - 0.35 + Polyol - 5 + Asphalt - 2 + Barytes
1.65
(KCl-PHPA): All additives are % BWOW.
Mud prepared in the laboratory were used.
Result and Discussions
Rheological Compatibility & R-Index Value at 88 0C, Schlumberger

Rheometer dial readings Yield Point

R-Index
Fluid Mixture PV (cps) (lbs/ Remarks
300 200 100 60 30 6 3 Value
100ft2)

100% Cement 175 106 71 52 24 5 2 168.5 6.05 -

100% Spacer 82 73 59 51 39 28 18 57.4 37.1 -

100% Mud 39 32 21 15 10 5 3 32.9 8.4 -
95% C : 5% S 172 105 68 43 24 6 2 159.4 9.1

75% C : 25% S 155 115 70 50 30 8 5 137.5 20.9

50% C : 50% S 106 86 60 41 32 13 9 83.1 26.7 -1 Compatible

25% C : 75% S 90 70 53 45 36 21 16 58.3 31.9

5% C : 95% S 92 78 58 49 41 28 20 56.7 37.4
95% S : 5% M 89 80 67 60 50 34 28 42.9 50.2
75% S : 25% M 77 68 55 47 28 24 18 38.4 40.9
50% S : 50% M 54 46 37 32 27 14 10 29.4 25.8 +8 Compatible
25% S :75% M 36 32 24 20 15 8 5 20.6 16.8
5% S : 95% M 28 23 16 13 10 5 3 20.1 8.8
Result and Discussions
Cement and Spacer additives : Halliburton

Fluid Sp. Gr. Composition

Cement - 100 + Water - 46 + Micromax - 53 + Silica flour - 35+

Cement Metakaoline - 10 + H413 - 0.6 + CFR3 - 1.0 +\HR25 - 0.5 + Gas Stop
1.97
slurry: HT - 0.4 + DAir 3500L - 0.1
All additives are % BWOC

W-100 + Tuned Spacer III – 6 + Bentonite - 2.0 + Defoamer - 0.1 +

Spacer : 1.80 Barytes
All additives are % BWOW)

Water - 100 + Biocide - 0.05 + Soda Ash - 0.1 + KCL - 5 + PAC L - 0.25
Mud + PHPA - 0.3 + XC Polymer - 0.35 + Polyol - 5 + Asphalt - 2.0 + Barytes
1.65
(KCL-PHPA) All additives are % BWOW.
Mud prepared in the laboratory were used.
Result and Discussions
Rheological Compatibility & R-Index Value at 88 0C, Halliburton
Rheometer dial readings Yield
Point R-Index
Fluid Mixture PV (cps) Remarks
300 200 100 60 30 6 3 (lbs/ Value
100ft2)
100% Cement 102 69 36 22 12 5 4 99.5 2.6 -
100% Spacer 52 41 33 28 22 16 14 29.4 21.4 -
100% Mud 39 32 21 15 10 5 3 31.1 8.4 -
95% C : 5% S 98 68 36 23 12 5 4 95.7 3.26
75% C : 25% S 49 35 22 16 15 8 7 39.3 9.34
50% C : 50% S 50 40 29 24 18 11 9 34.6 16.4 0 Compatible
25% C : 75% S 53 44 35 29 20 14 9 29 24.3
5% C : 95% S 55 43 34 27 21 16 14 36.8 19.2
95% S : 5% M 61 52 40 36 32 19 15 32.5 29.2
75% S : 25% M 59 50 39 35 30 18 15 34.8 27.9
50% S : 50% M 40 36 27 23 19 10 8 24.6 17.7 +7 Compatible
25% S :75% M 35 29 21 17 12 6 4 25.4 11.1
5% S : 95% M 33 27 20 16 11 6 4 21 12.4
 Result and Discussions

180 180
160 160
cmt spacer cmt spacer
140 140
SHEAR STRESS, Pa

SHEAR STRESS, Pa
Cement
120 120
100 100 Ceme
80 80
Spacer
60 Spacer 60
40 40
20 Mud
20
Mud
0 0
Shear 5.1 10.2 51 102 170 340 510 Shear 5.1 10.2 51 102 170 340 510
rate SHEAR RATE, sec-1 rate
SHEAR RATE,
sec-1
Figure 1: Rheological Hierarchy of Cement, Spacer & Mud Figure 2 :Rheological Hierarchy of Cement, Spacer and
at 88 0C of 110-140°C Package (Spacer & Cement Mud at 88 0C of 110-140°C Package (Spacer & Cement
additives: Schlumberger, WBM: KCl-PHPA) additives: Halliburton, WBM: KCl-PHPA)
Conclusion

• The cow dung particles(CDPs) having size more than 300 micronmeter has shown promising fluid
loss control capability at 5% concentration BWOC.

• It showed better and acceptable rheological properties than cow dung having size less than 300
micronmeter.

• No significance changes were seen in compressive strength of cement slurry when cow dung
particles were used as fluid loss additive.

• The thickening time obtained using CDPs as fluid loss additive exhibited signs of retarding
property in cement slurry.

• . Halliburton spacer package showed better stability because it achieved rheological compatibility
at 51 shear rate, which is less than 100 rpm shear rate.
References
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Cements." 2nd Edition, April 2013.
3. API, Recommended Practice (2005), 10B-2. “Recommended practice for testing well cement”, p 171.
4. API Specification, (2005), 10A “Specification for cements and materials for well cementing”, p 45.
5. Bannister, Charles E. “Aqueous Chemical Wash Compositions”, U S Patent 4681165.
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environmentally preferred multifunctional polymer”, SPE Europe/EAGE Annual Conference. Society of
Petroleum Engineers.
7. Brandl, A., Bray, W. S., & Narvaez, G. G. (2012b), “New slurry design concepts using multifunctional
additives to improve quality and sustainability of cementing systems for zonal isolation”, SPE Eastern
Regional Meeting. Society of Petroleum Engineers.
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prevent gas invasion during cementing operations”, annual technical conference and exhibition, San
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Common Types”, Oil Gas Res, 2, 112.
Thank you