DRILLING ENGINEERING LABORATORY

SKPP 3741

EXPERIMENT 5

DRILLIND MUD CONTAMINATIONS

SECTION 03, GROUP 3

GROUP MEMBERS : 1. DINESH RAMAMURTHY (LEADER)

2. PRASAD MANOGER

3. SARAVIN SELLEYITOREEA

4. KUMARESAN RAVICHANDRAN

SUPERVISOR : DR. MOHD FAUZI ABD. HAMID

ASST.ENGINEER : MS. HASANAH HUSSEIN

DATE OF EXPERIMENT : 8TH OCTOBER 2017

DATE OF SUBMISSION : 15TH OCTOBER 2017

ABSTRACT

Drilling mud are added into the wellbore during drilling to facilitate the drilling process by
suspending cuttings, controlling pressure, stabilizing exposed rock, providing buoyancy, and
cooling and lubrication. However, mud become contaminated when a foreign material such as salt
and cement enters the mud system and causes undesirable changes in mud rheological properties,
such as density, viscosity, gel strength and filtrate volume. Generally, water-based mud
systems are the most susceptible to contamination while drilling, completion and workover. At
elevated temperature and pressure, drilling fluid with stable rheological properties is required to
have a better mud efficiency.

There are few types of contaminants that usually cause severe mud contaminations such as
soluble salts and cement. Example of soluble salts are NaCl, KCl, CaSO4, CaCl2, MgSO4, and
MgCl2. These types of salts need to undergo suitable treatment to reduce the effect of contaminants
and hence to revert the mud properties to original state.

In this experiment, 6 mud samples were prepared for testing. First was the basic mud
sample with no contamination which was tested to find out the mud properties such as mud density
(ppg), plastic viscosity (cp), apparent viscosity (cp), yield point (lb/sq.ft), gel strength (10 sec and
10 min), pH, filtrate volume (cc) and mud cake thickness (/32in). Consecutively, NaCl, KCl,
CaCl2, CaSO4 and cement were added and mixed thoroughly in the basic mud for the remaining 5
samples. Then, these 5 samples were tested for their mud properties and compared with the basic
mud sample. The mud filtrate obtained was used to calculate the chloride and sulphate content and
the hardness of the filtrate. This procedure was to confirm the presence and the amount of the
contaminants in the mud.

As a result, sample with KCl and cement altered the mud properties drastically meanwhile
sample with NaCl showed a slight change in the properties.
TABLE OF CONTENTS

1.0 INTRODUCTION 1

2.0 THEORY 2

3.0 METHODOLOGY 3-5

4.0 RESULTS 6-8

5.0 DISCUSSIONS 9-12

6.0 CONCLUSIONS 13

7.0 SUGGESTION 13

8.0 REFERENCES 14

9.0 APPENDICES 15-16

1.0 INTRODUCTION

This experiment was aimed to investigate the effects of mud contamination on the mud
properties. Besides, three parameters were calculated which are chloride content, sulphate content
and hardness to know the amount of contaminants present in each mud sample.

Rheological properties of drilling mud can be affected by many factors during drilling
operation like temperature, pressure and contaminants. During drilling operation, the drilling mud
picks up contaminants such as salts, drill solids, and cement. At elevated temperatures the drilling
mud remedy is often necessary because the mud may be unable to tolerate the contaminants.

Salt contamination may be a result of salty makeup water, drilling salt stringers, or
saltwater flows. Saltwater-based drilling fluids are used when salt is drilled in large quantities or
where salty makeup water is used. In saltwater muds, salt is not a problem; however, in freshwater
muds salt becomes a contaminant. Salt contamination is usually easy to detect. It will be
accompanied by an increase in the chlorides content of the filtrate. Other possible indications are
an increase in rheology, specifically the yield point, an increase in fluid loss, and a possible
decrease in pH and alkalinities. If the salt source is a saltwater flow, there may also be a decrease
in mud density.

Meanwhile, cement contamination occurs in every well drilled. It is contamination from

calcium hydroxide which can result in increased pH, severe thickening and increased fluid loss of
bentonite based mud systems (flocculation of the bentonite clay). The main source of this
contamination is the drilling of green cement or adoption of poor placement procedures. The
severity of the problem will depend on the level of pre-treatment and thinner concentration in the
mud. When large quantities of cement are drilled it may not be economical to treat out the
contamination due to the large concentrations of bicarbonate required. In this case, the best course
of action may be to change out the contaminated mud for new mud or drill cement with sea water
if available.

The chemical CaSO4, which occurs naturally as the mineral anhydrite can cause
contamination when drilling even small stringers of these minerals. This will result in flocculation
of bentonite muds resulting in an increase in yield point, gel strengths and fluid loss.

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2.0 THEORY

Contamination is a steady process while drilling, as drilled solids are continually entering
the mud. While much of the drilled solids are inert, there are certain materials which can cause
severe chemical and physical problems. Any contamination must be treated immediately so it is
essential that careful and frequent checks are maintained on the mud properties at all times. Mostly,
salt contamination become frequent during drilling process.

Soluble salts causing contamination can be divided into monovalent and divalents.
Monovalent is an atom, ion, or chemical group with a valence of one, which thus can form one
covalent bond. The most commonly known monovalent and encountered while drilling are NaCl
and KCl. Meanwhile, a divalent is an element, ion, functional group, or molecule has a valence of
two. Most commonly encountered divalent are CaCl2, CaSO4, MgCl and MgSO. The divalent
cations Ca2+ and Mg2+ contribute to the properties of water that cause it to be hard, such as the
formation of limescale.

Chloride concentration in mud can be determined by titration with a silver nitrate solution.
The amount of chloride must be checked frequently. If there are any abnormal changes in the
chloride content, it can be an indication of drilling into a salt formation or taking water influx from
the reservoirs.

Cement contamination occurs one or more times when casing strings are cemented and the
plugs are drilled out. The extent of contamination and its effect on mud properties depends on
several factors like solids content, type and concentration of deflocculants, and the quantity of
cement incorporated. Cement concentration can be tested through test of hardness using different
types of hardness solution.

Calcium sulfate contamination is similar to cement contamination because both liberate

calcium ions, which in turn cause flocculation. Unlike cement, calcium sulfate does not cause a
pH increase since it supplies a sulfate ion in lieu of a hydroxyl ion. The sulfate ion contributes to
flocculation of clay solids, although its effect is small compared to calcium ions. Fann sulphate
indicator solution estimates the sulfate ion content according to the precipitate formed.

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3.0 Methodology
Apparatus:
1. Mud mixer
2. Mud balance
3. Rheometer
4. Thermometer
5. Filter press
6. Graduated cylinder
7. pH meter/pH paper
8. Resistivity meter
9. Vernier caliper
Materials:
1. Bentonite
2. Sodium Chloride (NaCl)
3. Potassium Chloride (KCl)
4. Calcium Chloride (CaCl2)
5. Calcium Sulphate (CaSO4)
6. Cement Class G
Experimental Procedure:
1. Using a basic mud prepared, basic mud was stirred thoroughly for 10-15 minutes for
complete mixing. The following mud properties was tested:
a. Mud Density (ppg)
b. Plastic Viscosity (cp)
c. Apparent Viscosity (cp)
d. Yield Point (lb/100sqft)
e. Gel Strength (10 sec and 10 min)
f. pH
g. Filtration (cc) for 30 min
h. Mud cake thickness (/32 in.)

3
 2. 10 g of NaCl was added into 680 ml of the basic mud, mixed evenly for 10 minutes and
the mud properties was measured as stated in Procedure (1).
3. 10 g of KCl was added into 680 ml of the basic mud, mixed evenly for 10 minutes and
the mud properties was measured as stated in Procedure (1).
4. 10 g of CaCl2 was added into 680 ml of the basic mud, mixed evenly for 10 minutes and
the mud properties was measured as stated in Procedure (1).
5. 10 g of CaSO4 was added into 680 ml of the basic mud, mixed evenly for 10 minutes and
the mud properties was measured as stated in Procedure (1).
6. 10 g of Cement Class G was added into 680 ml of the basic mud, mixed evenly for 10
minutes and the mud properties was measured as stated in Procedure (1).

For the chloride content, sulphate content and hardness, a test is conducted using the filtrate
collected at the end of filtration. The detailed procedures are as below:

Chloride test

a) 1ml of the filtrate water was added into the measuring cylinder.
b) 2 to 3 drops of phenolphthalein solution was added next.
c) If the filtrate water changes to pink color, sulphuric acid was added drop by drop while
the filtrate water was continuously stirred, until the pink color disappears.
d) Following that, 25ml of distilled water was added and the filtrate water was stirred.
e) 10 drops of potassium chromate solution were the added into the filtrate water and stirred
again.
f) Silver nitrate solution (0.01) was dropped little by little using a pipette till the color
changes from yellow to reddish orange.
g) The volume of silver nitrate used was recorded according to the following formula:
Chloride mg/L = 10,000 (0.01 x volume of silver nitrate)
Volume of filtrate water

** Volume of silver nitrate is the volume taken for the solution to change color from yellow to
reddish orange.

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Sulphate test

a) 2ml of the filtrate water was added into the measuring cylinder.
b) 3 drops of sulphate indicator solution was added next.
c) The measuring cylinder was shaken well and left for 2 minutes.
d) The solution in the measuring cylinder created a white precipitate.
e) The quantity of sulphate ion is determined based on:
Clear white precipitate: 0-10 epm of sulphate ion
Milky white precipitate: 10-20 epm of sulphate ion
Cloudy white precipitate: >20 epm of sulphate ion
Hardness test (Versenate method)

a) 50cc of distilled water was added into the titration bowl.

b) 3cc of Hardness Buffer Solution and 5 to 10 drops of Hardness Indicator Solution was
added next. If red color is formed it indicates the hardness in distilled water. Hence,
Hardness Titrating Solution was added drop by drop until the red color changed to blue.

** Do not add in the volume of Titrating Solution in calculation of hardness in Procedure (d)

c) Following that, 1cc of sample was added into the titration bowl. If there are presence of
Mg and Ca ions, the color changes from pink to wine color.
d) Hardness Titrating Solution was kept on added and the solution was continuously stirred
until the sample changes color to blue.
e) The amount of hardness was calculated using the following formula:
Volume of titrate solution x 20 = Ca epm + Mg when Hardness Solution
1ml = 20 epm used

Volume of titrate solution x 2 = Ca epm + Mg when Hardness Solution

1ml = 2 epm used

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 4.0 RESULT & DATA

Mud Properties 700ml of 680ml Basic 680ml Basic 680ml Basic 680ml Basic 680ml Basic
Basic Mud + 10g Mud + 10g Mud + 10g Mud + 10g Mud + 10g
Mud of NaCl of KCl of CaCl2 of CaSO4 Cement
class G

Mud Density (ppg) 8.6 8.7 8.6 8.6 8.7 8.7

Plastic Viscosity (cp) 3.5 3.0 4.0 1.0 2.0 2.0

Apparent Viscosity (cp) 4.50 6.00 15.50 4.25 4.50 8.00

Yield Point (Ib/100sq.ft) 2.0 6.0 11.5 6.5 5.0 12.0

Gel Strength 10 sec 2.5 9.0 10.0 3.0 3.0 6.5

(Pa) 10 min 3.0 5.0 9.0 3.5 3.0 7.5

pH 9.00 6.50 8.70 7.92 8.65 13.06

Average mud cake 0.0653 0.1655 0.3170 0.2513 0.2528 0.5308

thickness (/32 in)

Filtrate Time Volume Volume (cc) Volume (cc) Volume (cc) Volume (cc) Volume (cc)
volume (ml) (min) (cc)

1 4.5 7.5 15.0 14.5 12.0 18.0

2 7.0 11.0 21.0 20.0 18.0 24.0

3 8.5 13.0 26.0 24.5 22.0 31.0

5 11.0 17.0 33.5 32.0 29.0 41.0

7.5 13.5 21.0 41.0 39.0 35.5 51.5

10 16.0 24.5 47.5 45.0 41.0 60.0

15 19.5 30.5 58.0 55.0 50.0 73.5

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 20 23.0 35.0 67.0 64.5 58.0 87.5

25 26.0 39.5 76.0 71.5 64.5 100.5

30 28.5 43.5 83.0 78.5 70.0 109.5

Chloride Test - Brick red Brick red Brick red - -

precipitate precipitate precipitate
7.5ml 9.4ml AgNO3 8.1ml AgNO3
AgNO3
Sulphate Test - - - - Milky white -
precipitate
0.10 epm

Hardness - - - - - 80 epm C +
Mg
8 epm Ca +
Mg

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 Volume Filtrate vs Time

120

100

80
Volume Flitrate (cc)

Basic Mud
NaCl
60
KCl
CaCl2
40 CaSO4
Cement Class G

20

0
0 5 10 15 20 25 30 35
Time (Minute)

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5.0 DISCUSSION

This experiment is carried out to study the effects mud contaminations on the properties of
water based mud and the effectiveness of treating material. All substance have the chance to get
contaminated by mixing or influenced by foreign substance. Mud contaminations usually occur
during drilling or cementing processes. A mud is said to be contaminated when a foreign
material enters the mud system and causes undesirable changes in mud properties, such as
density, viscosity, and filtration. Mud contamination can result from overtreatment of the mud
system with additives or from material entering the mud during drilling. The contaminants that
are used in this experiment are NaCl, KCl, CaSO4, CaCl2 and Cement Class G. For this
experiment, basic muds will be prepared and its properties will be recorded as usual to compare
with all the other contaminated muds.

Basic Mud

At first, 700 ml of basic mud which was prepared by the technician was used to determine
the initial mud properties to be compared with the mud properties of mud with different type of
mud contaminants. The mud properties that must be recorded are mud density, plastic viscosity,
apparent viscosity, yield point, gel strength, filtration for 30 minutes and mud cake thickness. All
the initial mud properties are measured and recorded with respective techniques. The density of
this basic mud was 8.60ppg. The plastic viscosity was 3.50cp while the apparent viscosity was
4.50cp. The yield point was 2.00 lb/100sq.ft. Gel strength for 10 seconds and 10 minutes were
2.5 and 3.0 respectively. Focusing on the mud filtrate, the average mud cake thickness that we
obtained was 0.0653 inch while the volume of filtrate was 28.5 ml.

Mud Contaminants

1. 10 g NaCl

2. 10 g KCl

3. 10 g CaCl2

4. 10 g CaSO4

5. 10 g Cement class G

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 These are the different types of mud contaminants used for the experiment. Since the time is
limited, each group were given one type of contaminant to do the experiment. The mud density
for all sample are almost same. Firstly, the mud density for all the samples are either 8.6 ppg or
8.7 ppg which is almost the same and shows very slight difference. This is because the amount of
contaminant added into the basic mud is small compared to the big amount of mud used.
Theoretically, the change in density will affect the hydrostatic pressure as higher density may
lead to higher pressure which may cause formation damage or fracture. On the other hand, lower
density results in low pressure that may lead to a kick or blowout.

Besides, the mud samples with different contaminants shows different pH value. The pH
value of basic mud is 9.0, and when added with contaminant NaCl, it becomes acidic with pH
6.5. this is because the ions Na+ and Cl- are acidic in nature. Other mud samples with CaCl2 and
CaSO4 shows decrease in pH of 7.92 and 8.65. The other mud sample with cement
contamination shows big increase in pH of 13.06. this is merely because cement contains
calcium hydroxide, in which its OH- is a strong base meaning high pH.

Moreover, the basic mud apparent viscosity is 4.5 cp while the contaminated mud samples
with NaCl, KCl, CaCl2, CaSO4 and cement has apparent viscosity with the range from 4.25 to
15.50 cp. The changes in viscosity will affect the flowrate of each mud samples.

For the other properties, the yield point and the gel strength of almost all the contaminated
samples are higher compared to the yield point and gel strength of basic mud. For the gel
strength for 10 minutes, basic mud has the lowest gel strength of 3.0 Pa, followed by mud
samples contaminated by NaCl, CaCl2 and cement G with gel strength 5.0 Pa, 3.5 Pa and 7.5 Pa.
Mud contaminated with KCl has the highest gel strength of 9.0 Pa. There must be a minor error
while taking the gel strength of CaSO4 (3.0Pa same as basic mud), which should be higher
than basic mud theoretically. The yield point of all the contaminated mud samples is higher than
the yield point of basic mud. The increase in gel strength, yield point and viscosity are all due to
flocculation. This means that all the fine particles in the mud aggregate or clumped together and
formed into a floc and less watery.

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 Furthermore, there is increment in the filtrate volume and mud thickness of all the mud
contamination samples. Based on the results, basic mud has the lowest filtrate volume of 28.5cc.
The filtrate volume for each contaminated mud increases. Mud with NaCl recorded filtrate
volume of 43.5cc, followed by KCl with volume of 83.0cc, CaCl2 with 78.5cc, CaSo4 with
70.0cc and lastly the mud contaminated with cement with 109.5cc which is the highest among
the rest. This may be related to the high fluid loss and loss circulation when mud is
contaminated. Logically, the more the filtrate volume, the thicker the mud cake of the samples.
The mud sample with cement G contamination has the thickest mud cake with 0.5308/32in,
whereas the basic mud has the thinnest mud cake with 0.0653/32in.

Finally, we carried out Chloride Test for NaCl, KCl and CaCl2 contaminated mud. Silver
nitrate is added into these three solutions until the color changes and the volume of silver nitrate
added is recorded. All three solution changes to brick-red precipitate. The volume of silver
nitrate needed to change the colour of NaCl is 7.5ml, CaCl2 which is 8.1ml and the highest KCl
which is 9.4ml. This is because the ionic strength of KCl is higher than CaCl2 and NaCl. The
more the ionic strength of a solution, the solubility of precipitate will be more and the faster it is
titrated. Sulphate test was also carried out in which we tested the CaSO4 contaminated mud. The
required volume was 0-10 epm. Milky white precipitate was formed at the end of titration.
Finally, hardness test was conducted on mud contaminated with cement and the result was 4ml x
20 = 80epm C+Mg and 4ml x 2 = 8epm Ca+Mg.

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 Application

Calcium-ions contamination

The sources of calcium ions are:

Gypsum

Anhydrite

Cement

Lime

Seawater

Hard/brackish makeup water

The calcium ion is a major contaminant to freshwater-based sodium-clay treated mud

systems. The calcium ion tends to replace the sodium ions on the clay surface through a base
exchange, thus causing undesirable changes in mud properties such as rheology and filtration. It
also causes added thinners to the mud system to become ineffective. The treatment depends on
the source of the calcium ion. For example, sodium carbonate (soda ash) is used if the source is
gypsum or anhydrite. Sodium bicarbonate is the preferred treatment if the calcium ion is from
lime or cement. If treatment becomes economically unacceptable, break over to a mud system,
such as gypsum mud or lime mud, that can tolerate the contaminant.

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6.0 CONCLUSION

As our objective for the experiment is to study the effects mud contaminations on the properties
of water based mud and the effectiveness of treating material, we are now making conclusion. The
contaminants that are used in this experiment are NaCl, KCl, CaSO4, CaCl2 and Cement Class G.
Calcium ion contamination is the major contamination. In this experiment, calcium ion can be
found in calcium sulphate and cement. Due to this contaminations agents, the yield point, gel
strength, filtration volume and also the mud thickness also increases.

Besides, the other ions which are the sodium and chloride ions also contribute their part as
contamination agents. As I mentioned above, these ions also increases the yield point, gel strength,
filtration volume and also the mud thickness. At the same time, the pH also increases compared to
basic mud. Hence, we can conclude that mud contaminations effects the properties of water base
mud by resulting higher values than basic mud. The best way to threat this mud contamination
would be fresh water. Because fresh water will reduce the concentration of these ions in the mud.

7.0 SUGGESTION

There are few error that might happened during the experiments. Those errors actually can be
overcame if we do some precaution steps.

From the beginning of the experiment, the mud should be measured correctly and continued the
experiment. The mud should be stirred for a long time to make sure the mud precipitates dissolve
thoroughly. The rheometer should be calibrated before being used to avod zero error which effect
the result. Lastly, our eyes should be on the measuring cylinder and stopwatch while recording the
filtrate volume for 30 minutes. By taking consideration these things, we might avoid our errors
and can provide more accurate result.

8.0 REFERENCES

13
 1. Mud contamination. (2015, June 25). Retrieved November 8, 2015, from Petrowiki:
http://petrowiki.org/Mud_contamination
2. Chilingarian, G.V. and Vorabutr, P.1981. Drilling And Drilling Fluids, Elsevier
Scientific Publishing Company, The Netherlands.
3. Gray, G.R. and Darley, H.C.H. 1981. Composition And Properties Of Oil Well Drilling
Fluids , Gulf Publishing Company, USA.
4. Kirkley,C, 1984. Drilling Mud, Unit II, 3rd Edition, Pertoleum Engineering.
5. Rogers, W. F, 1963. Composition And Properties of Oil Well Drilling Fluids, Gulf
Publishing Company, Houston.

9.0 APPENDICES

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SAMPLE CALCULATION
The sample calculation for 1 ppb starch

600 = 18.5, 300 = 12.5

Plastic viscosity, p = 600 300

= 18.5 12.5

= 6.0 cp

Apparent viscosity, a = 600 / 2

= 18.5 / 2

= 9.25 cp

Yield Point, Yb = 300 -p

= 12.5 6.0

= 8.0 lb/ 100 ft

Average Mud cake thickness = 0.0905+0.0995

= 0.0950

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