Drilling Fluids Lab PETE 3265 Section 1.

Spring 2015.

Lab partners: Briana Dodson, Aziz Al-Umairy

Report by: Alan Alexeyev

Experiment #5:

Physical and Chemical tests of a mud contaminated with

calcium chlorite

Date performed: 3/11/2015

Date submitted: 3/25/2015

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Purpose:

The purpose of this experiment was to investigate the effects of calcium chlorite
contamination on a mud using physical and chemical tests. The sub-purpose was to
learn about the role of contamination in the drilling mud and its effects on drilling.

Abstract:

In this experiment we were introduced to the chemical properties of the mud. They
needed to be measured and analyzed on how they affect drilling operations. The
various tests were performed, such as chloride concentration, methyl orange filtrate
alkalinity, phenolphthalein alkalinity, and test for hardness. In addition to that, the
physical measurements and preparation of mud were done as usual. At the end of the
lab the evaluation of the influence of contamination of calcium chloride on the physical
properties was done, along with discussion of high-salinity muds theory. The results and
conclusions were followed.

Introduction:

The introduction of some new definitions related to the chemical analysis will be
described below.

There have been developed a standard set of chemical tests for determining the
concentrations of various ions present in the mud. (1) In this experiment, 4 of those
tests have been conducted. They are: phenolphthalein alkalinity of the mud and filtrate
(Pm and Pf), methyl orange filtrate alkalinity (Mf), chloride concentration (Cl), and test
for hardness. There are a lot of ways to determine the concentration, and sometimes
having so many options may confuse people. There is molarity, molality, normality,
ppm, milligrams per litre, weight percent. Whatever that is or however it is presented to

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an engineer, he always needs to remember that concentration would be a ratio of mass
per volume thats a good way to check if one is confused with the names.

Alkalinity is the ability of a solution to react with the mixture. Phenolphthalein alkalinity
is the amount of acid required to reduce the pH to 8.3. Methyl orange test is needed to
reduce the pH to 4.3. (1)

Salt can enter and contaminate the mud system when salt formations are drilled and
when saline formation water enter the wellbore. Chloride concentration is determined
by titrating with silver nitrate solutions. From that chemical reaction the chloride will get
removed as AgCl, the white precipitate. The end of the titration is detected by
potassium chromate indicator. (1)

Water is considered to be hard if the amount of Ca or Mg ions is too large. That

phenomenon is knows as water hardness. Those ions are usually present in the water
available for use as a drilling mud. Cement can also contain calcium and may
contaminate the mud. Water hardness can tell the engineers about the calcium
concentration in the mud. (1).

The teacher also instructed us to discuss the high salinity muds. Upon reading the
Applied Drilling Engineering book (1), some important points of that theory are about
to be discussed. Salt waters usually create problems for treatment and maintenance
because the contaminants in the make-up water. The problems arise along with high
temperatures, salts and hardness. Muds that have a NaCl concentration of more than 1%
of weight are considered as high-salinity muds. High salinity waters are usually formed
from another type of inhibitive mud capable of tolerating salt contamination. (1).
Saltwater muds may be needed to permit drilling a relatively in-gauge hole through
salt formations. Another benefit they may present is the reduction of the ability of
active clays to hydrate. But, that introduction of salt into the mud also increases the
chemical treatments required to maintain acceptable mud properties. (1)

Physical measurements such as pH, Mud Weight, Viscosity, cake thickness and others
were performed in the previous labs, and description of them was introduced there. (3).

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Equipment and Materials used:

Beakers, pH Meter, Blender, Marsh Funnel, Stopwatch, Mud balance by OHAUS,

Sand Screen, OFITE manufactured 8-speed Rotational Viscometer Model 800,
shearometer, OFITE filter press, OFITE-manufactured CHLORIDE, ALKALINITY &
HARDNESS DETERMINATION kit.
Distilled water, Bentonite, CaCl*2H2O
Towel, safety glasses, lab coat

The Kit contained the following: (2)

Titration Dish, Polyethylene 153-26
1 Stirring Rod, Polyethylene 153-28
2 1 ml Pipette 153-34
2 10 ml Pipette 153-40
1 Indicator soln., Ver Hardness, 2 oz 205-02
1 Buffer soln., Hardness, 2 oz 205-04
1 Titration soln., (EDTA), 40 mg/L, 2 EPM, 8 oz 205-06
1 Titration soln., (EDTA), 400 mg/L, 20 EPM, 4 oz 205-08
1 Distilled Water, 16 fl oz.. 206-02
1 Pot Chromate Ind Soln 2 fl oz. 215-00
1 Phenolphthalein Ind Soln. 2 fl oz. 220-00
1 N/50 Sulfuric Acid, 16 fl oz. 230-04
1 Brom Cresol Green-Methyl Red (Ind Soln, 2 fl oz.) 245-00
1 0.0282N Silver Nitrate, 8 fl oz. 265-00
1 0.28N Silver Nitrate, 4 fl oz 265-13
1 Calcium Carbonate, 35 grams

Procedure:

As with previous labs, the measurements of pH, MW, FV, PV, YP, 10-sec and others had
to be performed. Their description was mentioned in the previous labs. (3). In this lab,
the 4 lab bbl mud that had to be prepared needed to have the concentration of 20 ppb
of bentonite and 4 ppb of CaCl*2H2O. The distilled water was used this time instead of
the tap one. There was 1400 mL of water, 80g of bentonite and 16g CaCl*2H2O. The
physical measurement were performed only once.

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For chemical test, there were 4 ones, and they were all performed twice. OFITE chemical
test kit was used for these purposes and the procedures described in that kit were
followed. Below are highlights of those procedures (2):

1. Phenolphthalein alkalinity (Pm and Pf):

2-3 drops of Phenolphthalein. If theres no color change, Pf =0. If pink
color develops, keep adding the N/50 sulfuric acid.
2. methyl orange filtrate alkalinity (Mf),
2-3 drops of indicator were added to the filtrate. If pink color appeared, to
continue titrating with N/50 sulfuric acid until color changed to the
original one. If there was no color change, continue the experiment
3. chloride concentration (Cl)
Add 2 3 drops of phenolphthalein indicator to the filtrate. If a pink color
appeared, titrate with N/50 sulfuric acid until the color changes from pink
to the original one. If no pink color appears, the test can be continued.
4. test for hardness
50mL of distilled water were added to the titration dish. About 20-40
drops of harness buffer solution and 10-15 of hardness indicator solution
were added to see the color change. If wine red appeared, the water
contained hardness. Continue adding the total titration solution until blue
color appears.

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 Figure 1. OFITE - CHLORIDE, ALKALINITY & HARDNESS
DETERMINATION kit

Results:

Below are the measurements:

Table 1. Physical measurements of the mud:

The mud
MW,
Trial pH ppg FV, sec PV, cp YP, cp Sand Content
1 6.8 9.1 40.2 6-3 = 3 3*2-6=0 0.4

AV300 AV600 10 sec

1 3 6 1 cp

Cake
Thickness WL 1.0 WL 2.5 WL 5.0 WL 7.5
7.5min -
4/32" 27 mL 34 mL 47 mL 52.5 mL

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For mud, the calculated MW was:
16 CaCl 2H2O + 80 + 1400
= 1.04 = .
80 16 CaCl 2H2O 3
+ + 1400 3
2.6 /3 1.85/3

a) Phenolphthalein alkalinity
a. Mud Alkalinity - Trial 1: Pm=1 mL, Trail 2: Pm = 1.1 mL
b. Filtrate Alkalinity - Trial 2: Pm=0, Trial 2: Pm=0 Color didnt change
c. Filtrate: trial 1: Pf=0, trial 2: Pf = 0
b) Methyl Orange (Mf)
a. Mf = Trial 1: 0.3mL; Trial 2: 0.2mL
c) Chloride Concentration: 50 mL of water
a. Mud: trial 1: Sn: 0.6; trial 2: SN: 0.65
b. Filtrate: trial 1: Sn:0.5; trial 2: 0.46mL
d) Test of Hardness to use filtrate only.
a. mL of silvernitrate: 0.3 & 0.25 will be used to calculate chloride ion
determination.
b. Mg or Ca present it showed dark color.
c. Never turned blue after adding indicators

Table 2: Chemical Test Results preseed abovein tabulated form

Trial Pm (ml) Pf (ml) Mf (ml) Cl (mud) Cl Hardness

(ml) (filtrate)
(ml)
1 1 0 .3 .6 .5 0
2 1.1 0 .2 .65 .46 0

Mf*1220 = mg/L of HCO3

1st trial: Mf = 0.3* 1220 = 366

2nd trial: Mf = 0.2* 1220 = 244

Chlorite concentration:

Mud: 1st Trial: Cl= 0.6 x 10000 = 6000 ppm

o 2nd Trial: Cl= .65 x 10000 = 6500 ppm

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 Trial 2 (Filtrate):

o 1st Trial: 0.5 x 1000 = 5000 ppm

o 2nd Trial: 0.46 x 1000 = 4600 ppm

Discussions:
Comparing the results from calculated and measured MW, it can be seen that measured
MW is again larger than the theoretical one. The root of the error is probably the
misjudgments in reading the scale or inaccuracies in getting the raw materials into the
mixture. Muds MW calculated was 8.7 ppg, while the measured value was 9.1 ppg.

When performing a water loss experiment, the mud showed a large water loss. In fact,
our group had to supply several beakers to accommodate the incoming water flow.

The ionic strength of water is 0.7M, while in this lab the chlorite concentration is 0.65M.
Its pretty close. Sea water is knows to be a very salty one, so this result is expectable.

The methods of calculation of Mf and Pf were mostly effective in this lab, as it tells us
the level of contamination by the known concentration. Sometimes for the more
complex muds an additional testing may be required. Pf in this lab was 0; that could
mean that perhaps the mud was already contaminated.

The titrant, which was used in the chlorite concentration, was Silver Nitrate 0.28. For
certain salty formation the mud has to be specifically designed to withstand that
salinity, thats why that property such as chlorite concentration needs to be considered.

Water hardness test produced no color changed; that may indicate that the water was
not hard. Since Pf was also a zero, that does correlate with that result. During the drilling
itself, water is most likely to get harder because other minerals from the ground
formation will get mixed with the water (even if just a clean water used as a mud). With
those changes the mud engineers need to account for that and plan accordingly.

pH was relatively low, at 6.8. it indicates it was more acidic than usual. And that makes
sense since acids were added to the mixture.

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Safety Comments:

Regarding the safety, we were using the goggles and lab coats. The safety instructions
from OFITE were followed. That company treats safety very seriously, I got a proof of
that by visiting their company and they always emphasized on safety, even showed us
what to do in case of emergency. One needed to be careful when measuring, filling up
the water to avoid spilling or break the equipment. Another important thing was to
pour the fluids very carefully to a) avoid spillage, so that we will not lose any amount of
fluids for further measurements, b) spilling fluids in general may be dangerous as they
may contain chemical that negatively impact on the health and environment.

Conclusions:
Chemical tests were performed in this lab. Knowing the content and concentration is
important for mud engineers to ensure the drilling mud is operating normally. By
knowing those quantitative results, he can adjust them as needed.

By performing the chemical tests, our group learned how to measure the chemical
contamination quantitatively. We were able to see on practice that some filtrates do not
react with certain indicators, i.e they dont change colors.

Measuring the MW, pH, viscosity and other physical properties didnt create any
difficulties since those procedures were learnt in the previous labs and repeated in every
lab. The lab has served its purpose. The learning process of chemical contamination
went successfully and without any safety issues during the experiment.

References:
1. Pages 45-75. Adam T. Bourgoyne, Martin Chenevert, Keith Millheim, F.S. Young
Jr., Applied Drilling Engineering, Vol.2, SPE, Richardson, TX. 1986
2. OFITE Chloride, Alkalinity and Hardness determination, Part #144-80.
3. Drilling fluids lab 1, 2, 3, 4 by Alan Alexeyev. February March 2015.