DRLG 310B

DRILLING FLUIDS LAB MANUAL

Table of Contents
INTRODUCTION...............................................................................................................................................................2

SUGGESTIONS FOR GOOD LABORATORY TECHNIQUE...................................................................................................2

LABORATORY SAFETY PROCEDURES...............................................................................................................................3

1. 0 GENERAL/HOUSEKEEPING RULES IN THE LABORATORY.......................................................................3

1.1 PROTECTIVE CLOTHING AND EQUIPMENT.............................................................................................4
1.2 CHEMICALS...........................................................................................................................................5
1.3 SPILL RESPONSE....................................................................................................................................6
1.4 EQUIPMENT SAFETY..............................................................................................................................7
LABORATORY REPORTING...............................................................................................................................................9

CONTRIBUTION OF PRACTICAL TO FINAL MARK..........................................................................................................10

LABORATORY ORIENTATION..........................................................................................................................................10

EXPERIMENT 1 – DENSITY AND RHEOLOGICAL PROPERTIES........................................................................................11

EXPERIMENT 2 – RETORT ANALYSIS..............................................................................................................................16

EXPERIMENT 3 – SAND CONTENT OF WATER BASED DRILLING FLUIDS (WBDF)........................................................21

EXPERIMENT 4 – API FLUID LOSS..................................................................................................................................23

EXPERIMENT 5 – CHEMICAL ANALYSIS.........................................................................................................................27

EXPERIMENT 6– SALT ANALYSIS....................................................................................................................................38

(i) Determination of Sodium Chloride content.....................................................................................................38

(ii) Determination of Potassium Chloride content..............................................................................................41

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 INTRODUCTION

Suggestions for Good Laboratory Technique

1. Never begin any experiment unless you understand its overall purpose and
reason for each operation involved in the experiment.

2. Always be neat, careful in handling chemicals and the use of equipment.

3. Be observant during all stages of an experiment.

4. Record your observations and results in the results sheet provided and/or bound
notebook. Write in ink and number pages of your notebook.

5. Your notebook should show the date and title of each experiment. You should
show the quantities (weight) of materials used, the blending procedure and the
results of the test asked.

6. Your notebook should show each new experiment on a new page.

7. Save the final products (drilling fluid, filtrate, filter cake, etc) for examination.

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 LABORATORY SAFETY PROCEDURES

Safety in the Laboratory is often taken for granted. The hazards of the materials that
are used are often underestimated. However the potential for injury, explosions, and
chronic illnesses is real. Know what these hazards are.

1.0 GENERAL/HOUSEKEEPING RULES IN THE LABORATORY

1. Keep bench tops free from clutter.

2. Do not place materials near the edges of counters/Shelves.

3. Discard sharp objects, e.g. broken glass, in puncture-resistant containers.

4. Never handle broken glass with bare hands

5. Disposal of chemical containers must be done in accordance with recommended

procedures.

6. Check on emergency equipment; ensure access to these is clear.

7. Do not eat, drink, smoke, chew gum or apply facial creams in the Lab.

8. Never try to push glass tubing through a cork or rubber bung.

9. Never wander around the Lab, with sharp objects like scalpels, knives.

10. Always check apparatus for loose or bare wires before plugging in or unplugging.

11. Check eyewash and shower.

12. Never handle electrical apparatus with wet hands.

13. Always ensure that the switch is off before plugging in equipment.

14. Never taste any substance in the Lab.

15. Never inhale from any glass, plastic or metal containers while in the lab.

16. Keep bacteria and fungus cultures covered as they can easily get into the air.
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 17. Always work at arm’s length.

18. Keep broken fragments of glass out of sinks and regular trash containers.

19. Do not store reference samples in front of electrical panel.

1.1 PROTECTIVE CLOTHING AND EQUIPMENT

1. Laboratory coats and suitable protective clothing must be worn and kept
properly fastened.

2. Open-toed and high-heeled shoes should not be worn.

3. Use the appropriate glove to protect against chemical hazards.

4. Gloves should be inspected before use for discoloration, puncture or tears.

5. Gloves should be cleaned and then removed before touching environmental

surfaces e.g. telephones, door knobs etc. to prevent transfer of contamination.

6. Face and eye protection (glasses, goggles, face shields) should be worn for
protection from splashing chemicals, flying particles and other harmful
substances. During experimental work safety glasses must be worn.

7. Use gloves when handling hot items.

8. Wearers of contact lenses should be advised about the hazards associated with
the use of contact lenses. Hard contact lenses can become bonded to the eye in
the event of a splash of a caustic solution, and organic vapors can be absorbed
by soft lenses.

9. In some situations, it may be necessary to use respiratory protection. Full face

masks and filter cartridges are available for this purpose.

10. No armless top, navel breakers, short pants or shit must be worn in the
laboratory to avoid any hazards.

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1.2 CHEMICALS

1. All chemical containers must be properly labeled and stored. Make sure the
chemical in use is the correct chemical.

2. Know the potential hazards of each chemical being dealt with, e.g. they may be
flammable, corrosive, toxic. Read label carefully, read MSDS and consult other
reference material as required.

3. Chemicals that are likely to react must be stored separately.

4. Pour liquids carefully so that drips do not run down the bottle, preferably over a
sink or chemical resistant surface.

5. When pouring from a large bottle, use both hands. Do not rest the bottle on its
neck when pouring.

6. Use siphon or plastic dispensers for pouring large volumes of corrosive liquids.

7. Never carry a reagent bottle by its neck.

8. Always use standard operating procedures when handling chemicals.

9. If chemicals are spilled on your skin, wash off immediately.

10. Never store chemicals in food containers.

11. Chemicals that are easily oxidized may be explosive when exposed to ignition
sources. These must be carefully monitored by visual inspection for peroxide
formation and controlled through proper inventory management. Formation of
crystals on a bottleneck is a potential hazard.

12. Never use an unknown or unlabeled chemical.

13. All chemicals should be secured in a cool, dry place or in accordance with the
MSDS.

14. Avoid contamination of chemicals by ensuring clean containers are used at all
times, and never return chemicals into the original container.

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 15. Do not store food with chemicals.

16. Wash hand thoroughly after use of chemicals.

17. When mixing or heating chemicals always point the mouth of the container away
from other people and yourself.

18. Use proper lifting technique when lifting chemicals

1.3 SPILL RESPONSE

The spilling of hazardous substances is the most common laboratory accident. The
speed with which a chemical spill is controlled may prevent a minor spill from
becoming a major spill. If you are the person who discovered the hazardous chemical
spill, then ensure that you follow these steps:

1. Identify what you see.

2. Use signage.

3. Get help.

4. Ventilate area

5. Seal off the area and alert others

6. Identify the hazards

7. Get proper equipment and materials

8. Contain the spill

9. Clean up the spill

a) Identify:

 What is it?
 What was it?
 Did you see a label on the container?
 Was it foaming or fuming?

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  Was there a fire?
 What did it smell like?
 What colour was it?
 What was it doing?

b) Get help. Call someone from the laboratory to assist in the clean-up.

c) Clean up the spill

 - When neutralising a spill, identify the spilled chemical before

applying a neutraliser. The wrong neutraliser may be worse than
none at all.

 - Absorbents, whether in their original form or in the form of

pillows or pads, are effective on almost all types of chemical.

 - Most acid spills may be neutralised by adding Baking Soda.

 - The best absorbents are inert substances such as sand,

diatomaceous earth (bleaching earth).

1.4 EQUIPMENT SAFETY

(a) Glass Items:

1. Never use chipped or broken glass items.

2. Use standard glassware.

3. Wrap or enclose glassware in case in implosion (collapse) when using low

pressure.

4. Pause and observe glass equipment before actually touching, it may be

hot.

5. Use heat resistant gloves to handle hot glass ware

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(b) Compressed Gas Cylinders:

1. Do not store at elevated temperatures.

2. Always cap secure cylinders in storage and transportation.

3. Do not improvise with gauges, fittings, and regulators.

4. Do not leave freestanding cylinders unattended.

(c) Pipettes:
1. Never pipette by mouth, you can ingest hazardous substances.
(d) Fume Cupboard:
1. Use fume hoods for all hazardous chemicals. These hoods must be tested
periodically to ensure they are functional.
(e) Burners:
1. Everyone must be informed before an open flame is used.
(f) Guards:
1. Machines must be shielded when they emit splashes or spatters.
(g) Fire extinguishers:
Fire extinguishers are located at strategic points in the laboratory. Make sure
you know their location and how to use them. In case of Fire, your first concern
must be to remove yourself from danger. Then bring it to notice of the
instructor or lecturer or technician.
Note:
When a person clothing is on fire he/she usually needs help from his/her
neighbour and the demonstrator in smothering the flame with a fire blanket, a
coat or anything similar which can be seized instantly.
(h) Egress Route:
The instructor or lecturer will conduct a safety walkthrough indicating all exits and if
there are any planned drill for today.

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 LABORATORY REPORTING

Your laboratory report should show the date, title of each experiment, the preparatory
work required for each experiment, a complete record of all observations and data, the
details of all required calculations, and all other forms of rough written work relevant to
the experiment.

The laboratory report must include the following headings:

1. Student name and ID number

2. Experiment date

3. The title of the experiment

4. Executive Summary (5 marks)

5. Objective / Aim

6. Theory – Brief Summary of all experiments (10 marks)

7. Procedure: state…as per lab manual

8. Results - the observations and data to be tabulated and clearly

represented. (30 marks)

9. Calculations – sample calculations will suffice where these are repetitive,

10. Overall Discussion – comment on significant aspects of the experiment

and results (23 marks)

11. Answer further questions, if any. (15 marks)

12. Conclusion (15 marks)

13. References – Books, Journals, etc (2marks)

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The laboratory report should contain a general Executive Summary, Theory,
Conclusion and References. Separate Results, Questions and Discussions can be done
for each individual experiment.

Note the signed raw data obtained for the experiment must be attached to the lab
report.

CONTRIBUTION OF PRACTICAL TO FINAL MARK

The practical coursework (labs) contributes 15% of the final course mark for DRLL 310B.

LABORATORY ORIENTATION
Orientation for the students to the laboratory and equipment, including demonstrations
of equipment, rigging up/rigging down, calibration, care and maintenance instructions,
and operational safety.

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Experiment 1 – Density and Rheological Properties

Objective: To determine the density and the rheological properties of the original and
contaminated samples.

Equipment:

1. Mud Balance

2. Viscometer

Procedure:
Density

1. The calibration of the mud balance should be checked by measuring the density of
fresh water. Fill the cup with fresh water at around 70F (21C), and set the rider
on 8.3ppg (pounds per gallon) or 1.0 specific gravity. Add or remove lead shot
from the shotwell until the instrument is in balance

2. Place the mud balance base (preferably in carrying case) on a flat level surface.

3. Measure and record the temperature of the fluid.

4. Fill the clean, dry cup to the top with the mud sample to be weighed; put the cap
on the filled drilling-fluid holding cup and rotate the cap until it is firmly seated.
Ensure that some of the drilling fluid is expelled through the hole in the cap.

5. Cover the hole in the lid with a finger and wash all mud from the outside of the
cup and arm. Then thoroughly dry the entire balance.

6. Place the balance on the knife edge and move the rider along the outside of the
arm until the cup and arm are balanced as indicated by the bubble.

7. Read mud weight at the edge of the rider toward the mud cup.

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8. Clean and dry the mud balance after each use.

9. Report the mud weight to the nearest 0.1 ppg (pound per gallon).

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Rheological Properties

1. Place a sample in the container and immerse the rotor sleeve exactly to the
scribed line.

2. Insert thermometer in thermocup hole and adjust to required temperature.

3. With the sleeve rotating at 600 rpm, wait for the dial reading to reach a steady
value (the time required is dependent on the mud characteristics). Record the dial
reading for 600 revolutions per minute.

4. Shift to 300 rpm and wait for the dial reading to reach steady value. Record the
dial reading for 300 rpm. Do the same for the following readings: 200rpm,
100rpm, 6rpm and 3rpm. The 3rpm reading can be taken at the ‘Gel’ dial.

5. Stir the drilling fluid sample for 10 seconds at high speed.

6. Allow the drilling fluid sample to stand undisturbed for 10 seconds. Slowly and
steadily turn the hand-wheel to ‘Gel’. The maximum reading is the 10 seconds gel
strength in lb/100ft2.

7. Re-stir the drilling fluid sample at high speed for 10 seconds and then allow the
mud to stand undisturbed for 10 minutes.

8. Repeat the measurements as in steps 6, & 7 and report the maximum reading as
10-minute gel in pounds per 100 lb/100ft2.

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 8 – Speed Viscometer

Calculations:

PV (plastic viscosity, (lbs/100 ft2)/300 rpm) = θ600 - θ300

YP (yield point in lbs/100 ft2) = θ300 - PV

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Results Reporting:

Sample Original (4 marks)

Density, lb/bbl
Temperature
Viscometer
750F 1200F 750F 1200F
Speed/RPM
600
300
200
100
6
3
Pv
Yp
10 second gel
10 minute gel

Questions:
1. Compare the rheological properties of the original sample with the
contaminated sample and give reasons for the differences. (2marks)

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EXPERIMENT 2 – Retort Analysis

The retort provides a means for separating and measuring the volumes of water, oil, and
solids contained in a sample of drilling fluid. A known volume of sample is heated to
vaporize the liquid components which are then condensed and collected in a graduated
cylinder. Liquid volumes are determined from reading the oil and water phases on the
graduated cylinder. The total volume of solids, both suspended and dissolved, is
obtained by noting the difference of the total sample volume versus the final liquid
volume collected. Calculations are necessary to determine the volume of suspended
solids since any dissolved solids will be retained in the retort. Relative volumes of low-
gravity solids and weight materials may also be calculated.

Equipment:

1. 10 ml Retort Apparatus

2. Fine Steel Wool

3. Grease: Never-Seez®. Used for a thread seal and lubricant at high temperatures

4. T-handle Drill: To remove steel wool from retort chamber

5. Pipe Cleaner: Used for cleaning the retort chamber and condenser passage

6. Spatula: Shaped to fit the inside dimensions of the sample cup

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Procedure:

1. The inside of the sample cup and lid must be thoroughly cleaned prior to each
test.

2. The condenser passage should be cleaned and dried before each test using pipe
cleaner as build-up of material in the condenser can decrease condensation
efficiency and cause erroneous liquid readings in a test.

3. Collect a representative sample of water-based mud and allow it to cool to

approximately 80°F (26°C).

4. If the mud sample contains gas or air, add 2 drops to 3 drops of defoaming agent
to about 300 cubic centimeters of mud, and stir slowly for 2 minutes to 3
minutes to release gases.

5. Lubricate the threads on the sample cup and condenser tube with a light coating
of silicone grease.

6. Lightly pack balls of steel wool into the chamber above the sample cup. Use only
enough steel wool too prevent vent a boiling over of solids into the liquid
receiver.

7. Using a clean syringe, fill the retort cup slowly with the non-aerated sample in
order to avoid air entrapment. Lightly tap the side of the cup to expel any air and
place the lid onto the cup.

8. Carefully place the lid on the sample cup and allow an overflow of the sample
through the hole in the lid to insure that the correct volume of the sample is in
the cup. That is, rotate the lid to obtain a proper fit and be sure a small excess of
fluid flows out the hole in the lid.

9. With the lid held tightly in place, wipe the overflow from the sample cup and lid.
Be sure that the sample cup threads are still covered with silicone grease after
wiping and that the hole in the lids not plugged.

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10. Carefully hand tighten the retort cup onto the retort chamber and connect the
assembly to the condenser. Thread the chamber arm into the condenser. Be
careful not to over-tighten and strip out the threads in the condenser. Place the
chamber into the heating jacket and close the insulating lid.

11. Place a clean, dry liquid receiver under the condenser discharge tube.

12. Connect the retort to an electrical outlet to turn it on. Allow it to run a minimum
of 45 minutes.

13. Remove the liquid receiver and allow it to cool. Read the volumes of water and
oil in the liquid receiver after it has cooled to ambient temperature. Record the
volumes (or volume percentage) of the following: a. total liquid volume; b. oil
volume; c. water volume.

14. If an emulsion interface is present between the oil and water phases, heating the
interface may break the emulsion. One way to do this is to remove the retort
assembly from the heating jacket by grasping the condenser. Carefully heat the
receiver along the emulsion band by gently touching the receiver for short
intervals with the hot retort chamber. Avoid boiling the liquid. After the
emulsion interface is broken, allow the receiver to cool and read the water
volume at the lowest point of the meniscus.

15. Turn off the retort and allow it to cool prior to cleaning. Do not use cold water to
try to rapidly cool down the chamber

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Calculations:
The measured volumes (mL) of oil and water are converted into volume percent based
on the volume of whole mud in the retort cup.

Results Reporting:

Sample Original (2 marks)

Percent Volume Oil - Vo
Percent Volume Water - Vw
Percent Volume Solids - Vs

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Question:

1. Estimate the approximate percent solids present in original sample from the
results obtained from the Bentonite & lubricant contaminated sample. (2 marks)

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EXPERIMENT 3 – Sand Content of Water Based Drilling Fluids
(WBDF)

Objective: To determine the sand content of water based drilling samples.

Equipment:
1. Sand Content Funnel
2. Sand Content tube
3. Sand Content Sieve, 75μm
4. Wash Bottle
5. 15% HCl

Procedure:

1. Fill the sand content or glass measuring tube with mud to the “mud” mark and
add water to the next mark. Close the mouth of the tube with your thumb and
shake it vigorously.

2. Pour the mixture onto the clean, wet screen and discard the liquid passing through
the screen. Add more tap water to the tube, shake, and again pour it onto the
screen. Repeat this process until the tube is clean. Wash the sand retained on the
screen to free it of any remaining mud.

3. Put the funnel upside down over the top of the sieve. Slowly invert he assembly
and insert the tip of the funnel the mouth of the glass tube. Wash the sand into
the tube by playing a fine spray of water through the screen. Allow the sand to
settle. From the graduations on the tube, read the volume percent of the sand.

4. Note to determine if the solids is purely sand and not carbonates, wash the
contents with tap water with water into the tube. Add 15% HCl solution to the
contents of the tube until no effervescence is observed. Shake vigorously to

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 ensure complete dissolution of calcium carbonate and allow the sample to settle.
If effervescence was observed, the calcium carbonate test will confirm.

5. From the graduations on the tube, read the volume percent of the sand.

Results Reporting:

Sample Original (2 marks)

% Solids b/f acidization
% Solids after acidization
% Sand

Questions:

1. From the results infer which sample is contaminated with sand, and which
sample is contaminated with calcium carbonate. (2 marks)

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EXPERIMENT 4 – API FLUID LOSS

Measurements of the filtration behavior and wall cake-building characteristics of a

drilling fluid are fundamental to control and treatment of drilling fluids, as are various
characteristics of the filtrate such as oil, water or emulsion content. These factors are
affected by the types and quantities of the solids in the fluid and their physical and
chemical interactions, which in turn are affected by changing temperatures and
pressures.

Objective:
To determine the filtration behavior and wall-cake-building characteristics of the drilling
fluid (s) at low temperature and pressure.

Equipment:

1. Quart or mud cup

2. API LPLT Filter press

3. CO2 or Nitrogen cartridges

4. Stop watch or clock

Procedure:

1. Be sure each part of the cell is clean and dry, particularly the screen, and that the
gaskets are not distorted or worn. The screen should be free of sharp edges, burrs
or tears.

2. Assemble the cell as follows: Base Cap, rubber gasket, screen, filter paper, rubber
gasket and cell body.

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3. Pour the freshly stirred sample of fluid into the cell to within 0.5 inch (13
millimeters) to the top in order to minimize CO 2 contamination of the filtrate.
Check the top cap to insure the rubber gasket is in place and seated all the way
around and complete the assembly. Place the cell assy. into the frame and secure
with the T-screw.

4. Place a clean dry graduated cylinder under the filtrate exit tube.

5. Turn the regulator “T-screw” counter-clockwise until the screw is free-turning and
the diaphragm pressure is relieved.

6. Close the relief valve and adjust the regulator by turning the “T-screw” clockwise
so that a pressure of 100 ± 5 pounds per square inch (690 ± 35 kilopascals) is
applied in 30 seconds or less. The test period begins at the time of initial
pressurization.

7. Record the filtrate loss every according to the table below.

8. At the end of 30 minutes, measure the volume of filtrate collected. Shut off the air
flow through the pressure regulator by turning the “T-screw” in a counter-clock
wise direction and open the relief valve carefully.

9. Report the volume of filtrate collected in cubic centimeters to the nearest 1/10th
cm3 as the API filtrate. Report the time interval and the mud temperature in °F (°C)
at the start of the test. Save the filtrate for running chemical analysis, if desired.

10. Check to see that all pressure has been removed from the cell, and then remove
the cell from the frame. Disassemble the cell, discard any remaining mud and
using extreme care save the filter paper and deposited cake with a minimum of
disturbance to the cake. Wash the filter cake on the paper with a gentle stream of
water or with diesel oil if oil mud is being tested.

11. Measure and report the thickness of the filter cake to the nearest 1/32 inch (0.8
millimeter). A cake-thickness less than 2/32 inch is usually considered acceptable.
Observations as to the quality of the cake should be noted. Notations such as

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 hardness, softness, toughness, slickness, rubberiness, firmness, flexibility and
sponginess are appropriate descriptions.

12. After each use, the filter press cell should be disassembled and after each use, the
filter press cell should be disassembled and cleaned of all drilling fluid by washing
and thoroughly rinsing. Wipe off the rest of the filter press, and dry all parts
completely. Replace the filter paper on the screen, and assembly the end cap onto
the cell. Loosely reassemble the cell onto the frame for storage.

Schematic diagram of an API LPLT Filter Press

Results Reporting:

Page 25 of
 Sample Original (4 marks)
Time, min API LTLP FL, mL API LTLP FL, mL
1
2
3
4
5
7.5
10
12.5
15
17.5
20
22.5
25
27.5
30
API Filter Cake thickness, 32”
Filter cake properties,
(soft, pliable, brittle etc)

Questions:

1. Why is the fluid loss different for the two drilling fluids? (1 mark)

2. What can be used to improve the fluid loss properties of the drilling fluids? (1 mark)

3. What factors are responsible for the difference in filter cake obtained? (1 mark)

4. Plot fluid loss versus the square root of time and calculate the spurt loss (2 marks)

5. Comment on the 30 minute fluid loss as compared with twice times the 7.5
minute fluid loss value. What conclusion can be drawn? (1 mark)

Page 26 of
Page 27 of
EXPERIMENT 5 – Chemical Analysis

Objective:
To determine the chemical properties of the water based drilling samples.

Filtrate pH

Equipment:
1. pH paper
2. Small beaker or measuring cylinder

Procedure:

1. Lay one pH strip on the surface of the filtrate with the colored indicator squares
face down and in direct contact with the fluid.

2. Allow sufficient time for the indicator squares to soak up liquid from the mud.
This usually takes from a few seconds to a couple of minutes.

3. Remove the pH strip from the mud and gently wash off any remaining mud form
the strip.

4. While the color squares are still wet, match the pattern of the squares against
the chart on the side of the dispenser.

5. Report the pH to the nearest 0.5 pH unit.

Page 28 of
Whole Mud Alkalinity, Pm

Equipment:
1. Titration dish
2. Measuring Cylinder
3. Pipette and Pipette Filler
4. Syringe
5. Phenolphthalein Indicator solution
6. N/50 Sulfuric acid

Procedure:

1. Measure 1 mL of drilling mud into the titration dish and dilute with 25 to 50 ml of
distilled water.

2. Add four or five drops of Phenolphthalein Indicator solution and while stirring,
titrate with N/50 Sulfuric acid solution until the pink color just disappears. If the
end point color change cannot be seen, it can be taken when the pH drops to pH
8.3 as measured on a pH meter.

3. Report the Phenolphthalein alkalinity of the whole mud, P m, as the number of

milliliters of N/50 Sulfuric acid required per mL of mud.

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Pf, Mf

Equipment:
1. Titration Dish
2. Pipette and Pipette filler
3. Phenolphthalein Indicator solution
4. N/50 Sulfuric Acid
5. Methyl
6. Orange Indicator

Procedure:

1. Measure one or more milliliters of filtrate into the titration dish.

2. Add two or more drops of Phenolphthalein Indicator solution. If the solution

turns pink, add N/50 Sulfuric Acid, drop by drop from the pipette, while stirring,
until the pink color just disappears. If the filtrate is so colored that the end point
cannot be seen, use a pH meter and titrate until the pH of the solution drops to
pH 8.3, and this will be the end point.

3. Report the Phenolphthalein Alkalinity of the filtrate, P f, as the number of

milliliters of N/50 Sulfuric Acid required per milliliters of filtrate.

4. To the same sample which was titrated to the P f endpoint, add two or three
drops of Methyl Orange Indicator solution. Add the N/50 Sulfuric Acid drop by
drop from the pipette while stirring until the color of the indicator changes from
yellow to pink. The end point may also be taken when the pH of the sample
drops to pH 4.3 as measured with a pH meter (more accurate).

5. Report the Methyl Orange Alkalinity of the filtrate, Mf, as the total milliliters of
N/50 Sulfuric Acid per milliliters of filtrate required to reach the Methyl-Orange
end-point. This also includes the amount of acid used to reach the
Phenolphthalein, Pf, end-point.

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MBT and Bentonite equivalent

Equipment:
1. Syringe
2. Erlenmeyer Flask
3. 3% Hydrogen Peroxide
4. 5N Sulfuric Acid
5. Methylene Blue solution
6. Hot Plate
7. Distilled water
8. Measuring Cylinder
9. Stirring rod
10. Filter paper

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Procedure:

1. With the syringe add 2.0 mL of drilling fluid to the Erlenmeyer Flask. Air or gas
entrained in the drilling fluid must be removed prior to injection. Vigorously stir
the drilling fluid to break the gel and quickly draw the mud into the syringe. Then
slowly discharge the syringe back into the drilling fluid keeping the tip
submerged. Again draw the fluid into the syringe and deliver exactly 2.0 mL of
fluid to the flask.

2. Add 10 mL of distilled water to the Erlenmeyer Flask.

3. Add 15 mL of 3% Hydrogen Peroxide to the Flask.

4. Add 0.5 mL of 5N Sulfuric Acid to the mixture.

5. Using the Hot Plate, boil gently for 10 minutes, but do not allow to boil to
dryness.

6. Dilute the mixture to about 50 mL using Distilled Water.

7. Add Methylene Blue solution to the flask in increments of 0.5 mL. If the
approximate amount of Methylene Blue dye is known from previous testing,
then larger increments may be used at the beginning of the procedure. After
each addition of Methylene Blue solution swirl the contents of the flask for
about 30 seconds.

8. While the solids are still suspended, remove one drop of liquid with the stirring
rod and place the drop on the filter paper. The initial end point of the titration is
reached when the dye appears as a blue turquoise ring surrounding the dyed
solids.

9. When the blue tint halo spreading from the spot is detected, shake the flask an
additional 2 minutes and place another drop on the filter paper. If the blue ring
is again evident, the final endpoint has been reached. If the blue ring does not

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 appear, then continue as before until a drop taken after 2 minutes shows the
blue tint halo.

Example of determining the MBT end point

Calculations:
Methylene Blue Capacity (MBT) = Methylene Blue, ml / Drilling Fluid, mL
Bentonite equivalent, lb/bbl = 5 (Methylene Blue, mL) / Drilling Fluid, mL
Bentonite equivalent, kg/m3g = 2.85 (Bentonite equivalent, lb/bbl)

Page 33 of
Calcium Carbonate Determination

Equipment:

1. Deionized or Distilled Water

2. Magnetic stir plate & stir bar

3. Calver II Indicator

4. 400mL beaker

5. Syringe(large)

6. 15% HCl

7. 200ml Volumetric Flask

8. Titrating Dish

9. 1.0N NaOH

10. 20 Epm Versanate Hardness Titrating Solution

Procedure:

1. Add 100mL distilled water with stirring bar into a 400ml beaker and place on a stir
plate.

2. Using a syringe, measure 10mL of whole mud and dispense into beaker while
stirring.

3. While stirring test sample, Carefully add 25cc’s of 15% HCl to beaker. Be sure to
add the HCl very slowly at first to prevent the effervescence from becoming
uncontrollable. Stir the solution for 5 minutes.

4. Pour the solution into a 200mL volumetric flask. Rinse the beaker with deionized
(or distilled) water and add this liquid to the flask. Continue until all the material
has been rinsed into the flask, and then add deionized (or distilled) water to bring

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 the total volume in the flask to the 200ml mark. Cap flask and shake solution to
be sure it is homogeneous.

5. Transfer exactly 2mL of solution from the flask into a titrating dish. Add a stir bar.
Add 2mL of 1.0N Versenate Hardness Buffer Solution and a pinch of Calver II
Indicator. Add 50mL of deionized (or distilled) water.

6. While stirring sample, titrate from wine colour (purple) to blue/grey (black) colour
with Versenate Hardness Titrating Solution (1ml = 20 epm Ca) and record your end
point.

Calculations:

(volume (mL) titrating solution) * (3.5) = lb/bbl calcium carbonate

Example: 25.7 mL * 3.5 = 90 lb/bbl calcium carbonate

Note if used 250mL volumetric flask the calculations are as follows:

(volume (mL) titrating solution) * (4.375) = lb/bbl calcium carbonate

Page 35 of
Calcium Test

Equipment:
1. 150ml Beaker
2. 50ml measuring cylinder
3. Versenate Hardness Buffer Solution
4. Versenate Hardness Indicator Solution
5. Versenate Hardness Titrant 0.02N (EDTA)
6. 10ml Pipette
7. Pipette filler
8. Magnetic Stirrer and stirring bar

Procedure:
1. Measure 1cm3 of sample into a 150ml beaker.
2. Rinse the inside of the beaker with deionized water and dilute the sample to 50ml
with deionized water. Add approximately 2ml buffer solution and swirl to mix.
3. Add sufficient hardness indicator (2 to 6 drops) and mix. A wine red colour will
develop if calcium and/ or magnesium is present.
4. While stirring titrate with the EDTA solution until the colour changes from red to
blue. The endpoint is best described as the point at which additional EDTA
produces no further change.

Calculation:
Total Hardness as Calcium, mg/l = 400 x (VEDTA / Vs)\
Where VEDTA = volume of EDTA solution, mg/l
Vs = volume of sample, ml

Page 36 of
Chloride Ion content

Equipment:
1. Titrating vessel
2. 0.02N (N/50) Sulphuric Acid
3. Potassium Chromate Indicator Solution
4. 0.0282N Silver Nitrate Solution (S-N)
5. 10ml Pipette
6. Pipette Filler
7. 50ml Measuring cylinder

Procedure:
1. Measure 1cm3 of filtrate into the filtration vessel and add 2 to 3 drops
phenolphthalein solution.
2. If the filtrate turns pink, add acid drop by drop from the pipette while stirring until
he colour has disappeared.
3. If the filtrate was originally deeply coloured, add an additional 2 ml of 0.02N
(N/50) Sulphuric acid or Nitric acid and stir. Then add 1g calcium carbonate and
stir.
4. Add 25 to 50ml distilled water and 5 to 10 drops of potassium chromate solution.
5. Stir continuously while adding standard silver nitrate solution drop by drop from
the pipette until the colour changes from yellow to orange-red and persists for 30
seconds.
6. Record the volume of silver nitrate required to reach the endpoint.

Calculation:
c[Cl-] = 1000 x (Vsn / Vf )
Where Vsn = the volume of silver nitrate solution, ml
Vf = the volume of filtrate sample, ml

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Questions:

1. What is a typical use of sized calcium carbonated in drilling fluids? (1 mark)

2. Assuming a linear relationship determine the concentration of calcium

carbonate required to lower the fluid loss of the sample to less than 2mL.
(1mark)

Results Reporting:

Chemical Analysis (8marks)

Sample Original
Filtrate pH
Pm
Pf
Chlorides, mg/l
Calcium, mg/l
MBT
Bentonite Eq., lb/bbl
CaCO3, lb/bbl

Page 38 of
Experiment 6– Salt analysis
(i) Determination of Sodium Chloride content

Objective: To determine the presence of sodium chloride

Equipment:
1. Magnetic Stirrer and bar 5. 0.282N Silver Nitrate Solution
2. Phenolphthalein Indicator Solution 6. Pipette and Pipette filler
3. 0.02N Sulphuric Acid solution 7. 50ml Measuring cylinder
4. Potassium Chromate Indicator Solution

Procedure:
7. Measure 1cm3 of filtrate into the filtration vessel and add 2 to 3 drops
phenolphthalein solution.
8. If the filtrate turns pink, add acid drop by drop from the pipette while stirring until
he colour has disappeared.
9. if the filtrate was originally deeply coloured, add an additional 2 ml of 0.02N
(N/50) Sulphuric acid or Nitric acid and stir. Then add 1g calcium carbonate and
stir.
10. Add 25 to 50ml distilled water and 5 to 10 drops of potassium chromate solution.
11. Stir continuously while adding standard silver nitrate solution drop by drop from
the pipette until the colour changes from yellow to orange-red and persists for 30
seconds.
12. Record the volume of silver nitrate required to reach the endpoint.

Calculation:
c[Cl-] = 10000 x (Vsn / Vf )
Where Vsn = the volume of silver nitrate solution, ml
Vf = the volume of filtrate sample, ml

Page 39 of
Salt (NaCl) mg/l = 1.65 x Chloride content, mg/l

Table Showing Conversion of Mg/l to Weight Percent and PPM at 680F (200F)

Page 40 of
 Graph of NaCl weight % against NaCl mg/l

18

16

14

12

10
NaCl

0
0 20000 40000 60000 80000 100000 120000 140000 160000 180000
NaCl mg/L

Page 41 of
(ii) Determination of Potassium Chloride content

Objective: To determine the presence of potassium chloride

Equipment:
1. Hand Crank Centrifuge
2. Kolmer tubes
3. Standard Sodium Perchlorate

Procedure:
1. Measure 7ml of filtrate in the centrifuge tube.
2. Add 3ml of standard sodium perchlorate solution but do not agitate. If
potassium is present, precipitation occurs at once.
3. Centrifuge at constant speed (approximately 1800 rpm) for 1 minute. Read the
precipitate volume and immediately record.
4. Determine the potassium ion concentration by comparing the precipitate
volume measure with the standard calibration curve given.
5. Report the potassium ion concentration in pounds per barrel (ppb).

Calculation
c[KCl], ppb = (7/ Vf ) x (x-axis value from standard curve, ppb)

c[K+]+ = 1500 x (c[KCl], pounds per barrel)

Page 42 of
 Standard calibration Curve for Potassium Chloride Determination

1.5

1.4

1.3

1.2

1.1

1
Precipitate,

0.9

0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25

KCl, lb/bbl

Results reporting:

Salts (4 marks)
Sample O A B C D E
% KCl
% NaCl

Page 43 of
Questions:
1. Which sample contained KCl and which sample had NaCl? (1 mark)
2. Give reasons for your answer. (1 mark)

Page 44 of
 SUMMARY RESULTS SHEET

Sample Original A B C D E
Density, lb/bbl
Rheological Properties
Viscometer Speed/RPM 0
75 F 120 F 0
75 F 1200F
0
750F 1200F 750F 1200F 750F 1200F 750F 1200F
600
300
200
100
6
3
Pv
Yp
10 second gel
10 minute gel

5 min
7.5 min
10 min
15 min
20 min
30 min
FC Properties
Chemical Analysis
Filtrate pH
Pm
Pf
Chlorides, mg/l
Calcium, mg/l
MBT
Bentonite Eq., lb/bbl
CaCO3, lb/bbl
Sand Content
% Solids b/f acidization
% Solids after acidization
% Sand
Retort Analysis
% Oil
% Water
% Solids
Salts
% KCl
% NaCl

Page 45 of